WO2010119156A1 - Device for holding a sample inside an x-ray diffraction or dispersion chamber - Google Patents

Device for holding a sample inside an x-ray diffraction or dispersion chamber Download PDF

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Publication number
WO2010119156A1
WO2010119156A1 PCT/ES2010/070224 ES2010070224W WO2010119156A1 WO 2010119156 A1 WO2010119156 A1 WO 2010119156A1 ES 2010070224 W ES2010070224 W ES 2010070224W WO 2010119156 A1 WO2010119156 A1 WO 2010119156A1
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WO
WIPO (PCT)
Prior art keywords
bushing
sample
chamber
sealing
housing
Prior art date
Application number
PCT/ES2010/070224
Other languages
Spanish (es)
French (fr)
Inventor
Ramón PONS PONS
Original Assignee
Consejo Superior De Investigaciones Científicas (Csic)
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Consejo Superior De Investigaciones Científicas (Csic) filed Critical Consejo Superior De Investigaciones Científicas (Csic)
Publication of WO2010119156A1 publication Critical patent/WO2010119156A1/en

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/20025—Sample holders or supports therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material

Definitions

  • the present invention can be included within the technical field of the characterization of substances by means of X-ray diffraction or dispersion, in particular by SAXS (low angle X-ray diffraction, of the English “Small Angle X-Ray Scattering") , WAXS (X-ray diffraction at a large angle, from English "Wide Angle X-Ray Scattering”), GISAXS
  • the cameras used today have a cavity inside to locate the sample that you want to characterize. Said cavity keeps the optical path and the sample holder in a vacuum, and the chamber can accommodate means to position the sample.
  • sample carriers consisting of glass capillaries of approximately 1 or 2 mm. of internal diameter and a wall thickness of around 20 ⁇ m. Which greatly hinders the task of depositing from the outside a sample inside that is not of the liquid type.
  • the technical problem that arises is to be able to use diffraction or X-ray scattering machines for characterization of substantially non-zero moisture samples, providing the possibility that the samples are in a controlled atmosphere, thus as additionally procure a means of orienting said samples in these conditions.
  • the present invention resolves the aforementioned limitation by means of the use of a device that allows a sample to be isolated from vacuum to be characterized by dispersion or diffraction of X-rays, said device comprising the following essential characteristics:
  • - a hollow body, elongated and open at one or both ends, vacuum resistant, adapted to accommodate inside the sample to be analyzed;
  • - radiation passage means practiced on the surface of the body and through which X-rays pass before and after interacting with said sample
  • the invention comprises a hollow body whose material and dimensions are suitable to guarantee
  • suitable materials for the body are, by way of non-limiting explanatory example, steel, aluminum or copper, as well as plastic, glass, or metal alloys.
  • a particularly preferred material for the body is stainless steel.
  • the dimension maximum exterior of the body is limited by the space available in a cavity subjected to vacuum located in the X-ray chamber itself to accommodate the sample, while the minimum dimension of the interior hollow of said body is in relation to the size of the sample holder that you want to use, which must fit inside the body.
  • the body is preferably open at its two ends, although it is also possible that it is only open at one.
  • the cavity of the X-ray chamber has a cover in the upper part of the chamber and at least one opening in one side as well as another in the lower part of the chamber, communicated with the outside.
  • the body is introduced into the chamber through one of said openings.
  • the invention provides first means of sealing, which allow to maintain the vacuum inside the chamber by sealing the space between the walls of said chamber and the open end or ends of the body.
  • said first hermetic sealing means can comprise hermetic plugs or elastic seals, preferably of rubber, so that, once the first hermetic sealing means are used and the lid of the upper part of the cavity is closed, it is possible to proceed to make the void in said cavity.
  • Said seals tightly adjust the exterior of the body to the lateral opening of the chamber, avoiding on one side that the void of the cavity is lost, isolating on the other hand the interior of the body from the void of the cavity, and allowing also the possibility of a communication between the inside of the body and the outside of the chamber.
  • This last possibility means that, depending on the design of the first hermetic closing means, they allow or not that the interior of the body is kept open to the laboratory conditions, or under a controlled atmosphere, by means of adequate means of atmosphere control .
  • the main advantage of said arrangement is that of providing, in the path of X-rays, a controllable atmosphere space, with the advantages that this implies, without substantially increasing the background noise, such as He has explained previously, since this space represents a comparatively small dimension compared to the rest of the X-ray path, performed in a vacuum.
  • the body comprises radiation passage means.
  • Said radiation passage means are sealed by sealing means, which may comprise a sheet of a sealing material transparent to X-rays and of suitable mechanical properties to resist vacuum.
  • suitable materials are, depending on the anode used in the production of X-rays, polymers or plastics, for example Mylar®, Kapton®, glass or mica, as well as beryllium, silicon nitride, plastic, a natural mineral , an artificial mineral, quartz, or metal.
  • the X-rays pass through the radiation passage means of the body, and affect the sample lodged inside the mentioned body.
  • the radiation passage means can be materialized in various ways, and in particular in the form of openings in the lateral surface of the body to free the path of the X-rays. According to the size of the opening in the direction perpendicular to the longitudinal axis of the body , it can be two opposite openings, or a single opening or slit large enough to allow both the entry and exit of the X-rays.
  • the invention enables the characterization of, for example, non-zero moisture samples that generally require an atmosphere other than vacuum in diffraction or X-ray scattering chambers, and especially, but not limited to, those that use the SAXS, GISAXS or GIWAXS technologies, more particularly in SAXS, GISAXS or GIWAXS Kratky type cameras.
  • Some types of controlled atmosphere for which the invention is suitable are: atmospheric pressure, atmosphere with a pre-established percentage of controlled humidity, inert atmosphere, oxidizing atmosphere or reducing atmosphere, atmosphere at a set temperature or pressure, among others.
  • the larger size of the body of the device of the invention with respect to the sample holders or devices known in the state of the art, which have a capillary shape, allows better access to the sample as well as convenient handling thereof regardless of its liquid state or not, while presenting adequate mechanical resistance properties.
  • the device allows the location and orientation of a sample within a diffraction or X-ray dispersion chamber of Kratky type, with adequate precision, so that it is positioned in the plane that is desired relatively to the X-ray beam.
  • said invention in addition to that described in the first preferred embodiment, incorporates and houses within it a positioning assembly of a sample within the body.
  • the positioning set consists of the following elements:
  • a hollow cylindrical housing comprising a first window on the lateral surface of said carcass, - a hollow cylindrical bushing, housed inside the carcass, comprising at least a second window on the lateral surface of said bushing,
  • a device for housing a sample inside an X-ray dispersion or diffraction chamber, which compactly combines the characteristics of the preferred embodiment 2, regardless of the housing.
  • a part of the lateral surface of the body is removable in the form of a first cover, which when removed causes the body to have a third window.
  • the main function of this third window is to facilitate access to the interior of the body and the insertion of the bushing.
  • Said cover is adapted to be hermetically fixed to the outer surface of the rest of the body, adjusting to the third window. Said cover has the additional function of holding the bushing.
  • This third preferred embodiment of the invention comprises pressure means, one of whose ends acts on the inner part of the lid, while the other end acts on the bushing.
  • the alignment means of the bushing are in accordance with the second preferred embodiment.
  • the invention further incorporates, with respect to what is indicated in the first preferred embodiment:
  • a second hollow housing comprising at least a fourth window that allows the passage of X-rays on its lateral surface
  • the body consists of a fifth window in its lower part and is embodied as a cover located in the upper part of the block between the second sealing means and the second housing, covering the latter.
  • This cover can be of a removable or fixed nature, and in the first case especially, it can be accompanied by a third means of sealing between the cover and the block.
  • the radiation passage means may consist of a slit or, preferably, two facing openings.
  • the first sealing means consist of second covers, preferably cylindrical, which are introduced through each of the lateral openings of the chamber and which in turn comprise some:
  • - fourth sealed means (preferably an o-ring or flat seal) that seal the contact area between the cover and said second covers
  • second covers can be of different designs, of which several non-limiting examples are given below, depending on whether they are one piece or more pieces.
  • they can have two basic models: one only to close the interior space of the body, in which case the lid would be completely closed in at least one of its ends, without allowing the communication of the interior of the body with the exterior of the chamber, and another model to close the interior space of the body allowing the communication between it and the exterior of the chamber, in particular to allow the passage of atmosphere control means as well as of the transmission means of the movement of an engine (which is not part of the invention) that rotates the sample holder.
  • the second covers of more than one piece they can consist of a piece that is introduced mostly by the lateral opening of the chamber except for one of its ends, in the form of a plate, which fits the wall of said chamber by its external side, and another piece that is fixed on the previous one (by means of screws or a thread for example) on the outside of the chamber.
  • Figure 1. Shows a perspective view of the first embodiment of the invention.
  • Figure 2. Shows a view corresponding to section AB of Figure 1.
  • Figure 3. Shows a perspective view of the second embodiment mounted on an x-ray diffraction or dispersion machine.
  • Figure 4.- Shows a perspective view of the positioning assembly of the second embodiment of the invention.
  • Figure 5. Shows another perspective view of the positioning assembly of the second embodiment of the invention, from a different point of view.
  • Figure 6.- Shows a view in longitudinal section of the second embodiment of the invention.
  • Figure 7.- Shows a perspective view of the third embodiment of the invention.
  • Figure 8.- Shows a view corresponding to the CD section of Figure 7.
  • Figure 9.- Shows a view in longitudinal section of the third embodiment of the invention.
  • Figure 10. Shows a perspective view of the sample holder.
  • Figure 11. Shows a perspective view of the fourth embodiment of the invention.
  • Figure 12 Shows a perspective view of a part of the alignment means (without the buttons and without the fixing of said alignment means, which are shown in previous figures).
  • the first practical embodiment of the invention describes a device for housing a sample inside an X-ray scattering or diffraction chamber (4).
  • the first embodiment allows incorporating a non-empty section within the path of the X-rays.
  • the device of the first embodiment comprises a hollow, elongated and open body (1) at both ends, vacuum resistant, adapted to accommodate inside the sample to be analyzed, as well as comprising two radiation passage means ( 2) facing each other, which pass through said body (1), through which X-rays pass before and after interacting with said sample.
  • the device also incorporates first means of sealing (5) of the ends of the body (1), which allow to maintain the vacuum inside the chamber (4) by sealing the space between the walls of said chamber (4) and the ends of the body (1), as well as incorporating sealing means of the radiation passage means (2), transparent to X-rays and resistant to vacuum, which allow to keep the atmosphere of the body (1) isolated with respect to the vacuum of The camera (4).
  • the sample housed inside can be reached by X-rays protected from vacuum.
  • a suitable atmosphere can be provided to the sample being analyzed or to the appropriate measurement conditions, for which the invention additionally comprises means for controlling the interior atmosphere of the body (1) , which in turn comprise at least one tube (7) connected to means providing selected atmospheric conditions.
  • the atmospheric conditions that can be selected are very varied, among which are preferred: atmospheric pressure, atmosphere with a pre-established percentage of controlled humidity, inert atmosphere, oxidizing atmosphere or reducing atmosphere, as well as atmosphere at a certain temperature or pressure, among others .
  • the preferred materials for building the body (1) are steel, aluminum, copper, plastic, glass, and metal alloys, with stainless steel being the most preferred material.
  • the body (1) has a cylindrical shape, although other shapes are equally possible.
  • the first sealing means (5) may be or preferably comprise seals and / or plugs, although any other equivalent means of closure is equally valid.
  • the sheet (6) is preferably made of one of the following materials: glass, metal, preferably beryllium, a polymeric material, preferably Mylar®, Kapton®, silicon nitride, plastic, a natural mineral, an artificial mineral, mica or quartz .
  • the second practical embodiment of the invention has a device like that of the first practical embodiment, with a body (1), radiation passage means, sealing means and hermetic closing means, which is additionally provided, housed inside, of a positioning set to position and orient the sample, which in turn comprises:
  • a hollow cylindrical housing (8) comprising a first window (9) on the lateral surface of said housing (8),
  • sample holder housed inside the bush (13), said sample holder (15) being adapted for coupling to turning means (32) (outside the invention) which, from the outside of the chamber ( 4), allow to govern the rotation of the sample holder (15) along the axis longitudinal of said sample holder (15).
  • the alignment means comprise
  • first displacer within which the support shaft (22) is housed, in the form of a hollow rod partially threaded externally and housed inside the first displacement hole (18), the threaded section being the one that passes inside the wedge, and producing the rotation of the first displacer (23) the longitudinal displacement of the first wedge (16) exclusively, - a second displacer (24), within which the tree is housed
  • the wedges (16, 17) are hollow cylinders with a conical inner surface.
  • the movement of the displacer (23, 24) orients the bushing (13), while the inner conical surface to the wedges (16, 17) prevents lateral balancing of said bushing (13).
  • the wedges (16, 17) can also be flat, in which case the invention additionally comprises retaining means (not shown) to avoid balancing the bushing (13).
  • the displacement assembly comprises two buttons (25 and 26) integral with the displacers (23 and 24 respectively) and whose rotation produces the rotation of said displacers (23 and 24 respectively).
  • the invention additionally incorporates contact elements (12) located externally to the bushing (13) and integral with it, which serve as contact between said bushing (13) and the wedges (16, 17).
  • Said contact elements (12) are preferably contact rings.
  • the rings are for example rubber, and that the wedges are for example Teflon or other equivalent, non-stick material.
  • the third practical embodiment of the invention consists of a device for accommodating a sample inside an X-ray dispersion or diffraction chamber (4), which comprises, in accordance with Ia third preferred embodiment:
  • a cover (35) adapted to be hermetically fixed to the outer surface of the body (1), covering the third window (11), incorporating said cover:
  • the alignment means of the bushing comprise at least one fastener (3) whose function is to prevent the longitudinal sliding of the elements of the displacement assembly with respect to the body (1).
  • Said fastener (3) is at least one of the ends of the displacement assembly, and can take the form of, for example, a hood of the buttons (25, 26) or of a clamp at the opposite end of the shaft of support (22).
  • the rods are attached at least by one of their ends, to the corresponding end of the housing or body.
  • the fourth practical embodiment of the invention consists of a device according to the preferred embodiment, characterized in that it incorporates, in addition to that indicated for the first preferred embodiment:
  • a second hollow housing (8) comprising at least a fourth window (34) on its lateral surface that allows the rays to pass through
  • the body (1) is a cover (28) located in the upper part of the block (27) between the second sealing means and the housing (8), covering said housing (8), and provided with radiation passage means (2) consisting of at least one opening (36) that allows the passage of x-rays.
  • the first sealing means (5) consist of second covers, preferably cylindrical, hollow, and introducible by the lateral openings of the chamber (4), comprising: sealing means (30) that seal the contact area between the cover (28) and the second covers, and fifth fifth means of sealing (31) that seal the contact area between the second covers and the chamber wall (4).
  • said second covers are of various models, some of which incorporate at least one opening at each end or a channel that allows selected actions from a list comprising: the introduction of the sample, the passage or connection of the atmosphere control means, or the passage of the transmission means of the movement of an engine that rotates the sample holder (15).
  • the fourth seal means (30) and the fifth seal means (31) are o-rings or flat.
  • the second sealing means and the third sealing means coincide in a single combined sealing element.
  • said combined sealing element comprises:
  • the block (27) incorporates means for regulating the position of the sample.
  • the third sealing means consist of a joint connection of the body (1) with the block (27).
  • (27) is selected from the list: welding, adhesive, mechanization, magnetic.

Abstract

The device comprises a body (1) that is open at both ends, for holding the sample to be analysed, and radiation passage means (2) that pass through the body (1), through which means the X rays pass before and after interacting with said sample. The device has first means (5) for hermetically sealing the ends of the body (1), which keep the chamber (4) under vacuum by sealing off the space between the walls of said chamber (4) and the ends of the body (1), and means for sealing the radiation passage means (2), which isolate the atmosphere inside the body (1) from the vacuum in the chamber (4). According to a second embodiment, the device comprises a positioning system for positioning and orienting the sample, with a sample-holder (15) and means for aligning the sample-holder (15). In a fourth embodiment it includes a block (27) and the body (1) is a cover (28).

Description

DISPOSITIVO PARA ALOJAR UNA MUESTRA EN EL INTERIOR DE UNA CÁMARA DE DISPERSIÓN O DIFRACCIÓN DE RAYOS X DEVICE FOR STAYING A SAMPLE INSIDE A DISPERSION CHAMBER OR X-RAY DIFFACTION
D E S C R I P C I Ó ND E S C R I P C I Ó N
OBJETO DE LA INVENCIÓNOBJECT OF THE INVENTION
La presente invención se puede incluir dentro del campo técnico de Ia caracterización de sustancias por medio de Ia difracción o dispersión de rayos X, en particular mediante SAXS (difracción de rayos X a ángulo bajo, del inglés "Small Angle X-Ray Scattering"), WAXS (difracción de rayos X a ángulo grande, del inglés "Wide Angle X-Ray Scattering"), GISAXSThe present invention can be included within the technical field of the characterization of substances by means of X-ray diffraction or dispersion, in particular by SAXS (low angle X-ray diffraction, of the English "Small Angle X-Ray Scattering") , WAXS (X-ray diffraction at a large angle, from English "Wide Angle X-Ray Scattering"), GISAXS
(difracción de rayos X a ángulo bajo con incidencia rasante, del inglés "Grazing Incidence Small Angle X-Ray Scattering"), y GIWAXS (difracción de rayos X a ángulo grande con incidencia rasante, del inglés "Grazing(low angle X-ray diffraction with flush incidence, from "Grazing Incidence Small Angle X-Ray Scattering"), and GIWAXS (large angle X-ray diffraction with flush incidence, from English "Grazing
Incidence Wide Angle X-Ray Scattering").Incidence Wide Angle X-Ray Scattering ").
El objeto de Ia invención se centra en un dispositivo que permite Ia caracterización de muestras por medio de cámaras de rayos X, sin necesidad de que las muestras se encuentren en condiciones de vacío.The object of the invention focuses on a device that allows the characterization of samples by means of X-ray cameras, without the need for the samples to be in vacuum conditions.
ANTECEDENTES DE LA INVENCIÓNBACKGROUND OF THE INVENTION
Las cámaras empleadas en Ia actualidad para Ia caracterización de muestras por medio de difracción o de dispersión de rayos X precisan de Ia generación de vacío en el camino óptico de los rayos X, puesto que Ia existencia de un medio material en dicho camino óptico produciría un ruido de fondo, así como absorción y distorsión, que dificultarían Ia interpretación de las medidas. En el caso particular de las cámaras de rayos X dentro de las cuales se coloca bajo vacío Ia muestra a analizar y que emplean las tecnologías SAXS, WAXS, GISAXS y o GIWAXS, no es posible el empleo de muestras que presentan humedad sensiblemente distinta de cero salvo que se hallen confinadas en algún portamuestras que las aisle del vacío. Los portamuestras disponibles actualmente suelen ser del tipo capilar y son muy limitantes en las tecnologías mencionadas puesto que, o bien encierran herméticamente Ia muestra impidiendo Ia regulación de su atmósfera, o bien no ofrecen Ia superficie plana necesaria para las tecnologías de incidencia rasante. Así, por ejemplo, en el Estado de Ia Técnica, no se conoce para las cámaras de tipo Kratky ninguna solución que ofrezca por un lado Ia posibilidad de regular Ia atmósfera de Ia muestra y por otro lado una superficie plana orientable para los experimentos de incidencia rasante.The cameras used at present for the characterization of samples by means of diffraction or dispersion of X-rays require the generation of vacuum in the optical path of the X-rays, since the existence of a material medium in said optical path would produce a background noise, as well as absorption and distortion, which would make the interpretation of the measurements difficult. In the particular case of the X-ray cameras within which the sample to be analyzed is placed under vacuum and which use the SAXS, WAXS, GISAXS and GIWAXS technologies, it is not possible to use samples that present humidity significantly different from zero unless they are confined in a sample holder that isolates them from the vacuum. The currently available sample holders are usually of the capillary type and are very limiting in the aforementioned technologies since, either they tightly enclose the sample preventing the regulation of their atmosphere, or they do not offer the flat surface necessary for flush incidence technologies. Thus, for example, in the State of the Art, no solution is known for Kratky-type cameras that offers, on the one hand, the possibility of regulating the atmosphere of the sample and, on the other hand, a flat orientable surface for incidence experiments. flush
Las cámaras empleadas hoy en día presentan una cavidad en su interior destinada a situar Ia muestra que se desea caracterizar. Dicha cavidad mantiene el camino óptico y el portamuestras en el vacío, y Ia cámara puede acomodar medios para posicionar Ia muestra.The cameras used today have a cavity inside to locate the sample that you want to characterize. Said cavity keeps the optical path and the sample holder in a vacuum, and the chamber can accommodate means to position the sample.
Asimismo, algunas de las cámaras de difracción de rayos X conocidas presentan portadores de muestra consistentes en capilares de vidrio de aproximadamente 1 ó 2 mm. de diámetro interior y un espesor de pared de en torno a 20 μm. Io cual dificulta grandemente Ia tarea de depositar desde el exterior una muestra en el interior que no sea de tipo líquido.Also, some of the known X-ray diffraction chambers have sample carriers consisting of glass capillaries of approximately 1 or 2 mm. of internal diameter and a wall thickness of around 20 μm. Which greatly hinders the task of depositing from the outside a sample inside that is not of the liquid type.
Otras cámaras, pertenecientes a Ia casa HECUS, disponen en su parte inferior de una cavidad por Ia que se introduce un bloque debidamente sellado que contiene medios para alojar un portamuestras.Other cameras, belonging to the HECUS house, have in their lower part a cavity through which a duly sealed block is inserted that contains means to accommodate a sample holder.
El problema técnico que se plantea trata de poder emplear las máquinas de difracción o de dispersión de rayos X para caracterización de muestras de humedad sustancialmente no nula, proporcionando Ia posibilidad de que las muestras se encuentren en atmósfera controlada, así como adicionalmente procurar un medio de orientar dichas muestras en estas condiciones.The technical problem that arises is to be able to use diffraction or X-ray scattering machines for characterization of substantially non-zero moisture samples, providing the possibility that the samples are in a controlled atmosphere, thus as additionally procure a means of orienting said samples in these conditions.
DESCRIPCIÓN DE LA INVENCIÓNDESCRIPTION OF THE INVENTION
La presente invención resuelve Ia limitación mencionada anteriormente por medio del empleo de un dispositivo que permite aislar del vacío una muestra que se desea caracterizar mediante dispersión o difracción de rayos X, comprendiendo dicho dispositivo las siguientes características esenciales:The present invention resolves the aforementioned limitation by means of the use of a device that allows a sample to be isolated from vacuum to be characterized by dispersion or diffraction of X-rays, said device comprising the following essential characteristics:
- un cuerpo hueco, alargado y abierto en uno o en ambos extremos, resistente al vacío, adaptado para alojar en su interior Ia muestra que se desea analizar;- a hollow body, elongated and open at one or both ends, vacuum resistant, adapted to accommodate inside the sample to be analyzed;
- unos medios de paso de radiación practicados en Ia superficie del cuerpo y a través de los cuales pasan los rayos X antes y después de interaccionar con dicha muestra;- radiation passage means practiced on the surface of the body and through which X-rays pass before and after interacting with said sample;
- unos primeros medios de cierre hermético de los extremos del cuerpo, que permiten mantener el vacío dentro de Ia cámara al sellar el espacio entre las paredes de dicha cámara y los extremos del cuerpo; y - unos medios de sellado de los medios de paso de radiación, transparentes a los rayos X y resistentes al vacío, que permiten mantener Ia atmósfera interior del cuerpo aislada con respecto al vacío de Ia cámara.- First means of sealing the ends of the body, which allow to maintain the vacuum inside the chamber by sealing the space between the walls of said chamber and the ends of the body; and - sealing means of the radiation passage means, transparent to X-rays and vacuum resistant, which allow to keep the interior atmosphere of the insulated body with respect to the vacuum of the chamber.
Según una primera realización preferida, Ia invención comprende un cuerpo hueco cuyos material y dimensiones son adecuados para garantizarAccording to a first preferred embodiment, the invention comprises a hollow body whose material and dimensions are suitable to guarantee
Ia rigidez y Ia estabilidad de dicho cuerpo cuando su superficie lateral exterior está sometida al vacío y Ia superficie interior está sometida a condiciones de atmósfera controlada distintas del vacío. Algunos materiales adecuados para el cuerpo son, a título de de ejemplo explicativo no limitativo, acero, aluminio o cobre, así como plástico, vidrio, o aleaciones metálicas. Un material especialmente preferido para el cuerpo es el acero inoxidable. La dimensión máxima exterior del cuerpo está limitada por el espacio disponible en una cavidad sometida a vacío situada en Ia propia cámara de rayos X para alojar Ia muestra, mientras que Ia dimensión mínima del hueco interior de dicho cuerpo está en relación con el tamaño de los portamuestras que se desee utilizar, que han de caber dentro del cuerpo. El cuerpo está abierto preferentemente por sus dos extremos, aunque también es posible que solo esté abierto por uno.The stiffness and stability of said body when its outer lateral surface is subjected to vacuum and the inner surface is subjected to controlled atmosphere conditions other than vacuum. Some suitable materials for the body are, by way of non-limiting explanatory example, steel, aluminum or copper, as well as plastic, glass, or metal alloys. A particularly preferred material for the body is stainless steel. The dimension maximum exterior of the body is limited by the space available in a cavity subjected to vacuum located in the X-ray chamber itself to accommodate the sample, while the minimum dimension of the interior hollow of said body is in relation to the size of the sample holder that you want to use, which must fit inside the body. The body is preferably open at its two ends, although it is also possible that it is only open at one.
La cavidad de Ia cámara de rayos X presenta una tapa en Ia parte superior de Ia cámara y al menos una abertura en un lateral así como otra en Ia parte inferior de Ia cámara, comunicadas con el exterior. El cuerpo se introduce en Ia cámara a través de alguna de dichas aberturas. La invención proporciona unos primeros medios de cierre hermético, que permiten mantener el vacío dentro de Ia cámara al sellar el espacio entre las paredes de dicha cámara y el extremo o extremos abiertos del cuerpo. De manera preferente, dichos primeros medios de cierre hermético pueden comprender tapones herméticos o juntas elásticas, preferentemente de goma, de modo que, una vez empleados los primeros medios de cierre hermético y cerrada Ia tapa de Ia parte superior de Ia cavidad, se puede proceder a hacer el vacío en dicha cavidad. Dichas juntas (o elementos equivalentes) ajustan herméticamente el exterior del cuerpo a Ia abertura lateral de Ia cámara, evitando por un lado que se pierda el vacío de Ia cavidad, aislando por otro lado el interior del cuerpo del vacío de Ia cavidad, y permitiendo además Ia posibilidad de una comunicación entre el interior del cuerpo y el exterior de Ia cámara. Esta última posibilidad significa que, en función del diseño de los primeros medios de cierre hermético, éstos permitan o no que el interior del cuerpo se mantenga abierto a las condiciones del laboratorio, o bien bajo una atmósfera controlada, mediante medios adecuados de control de atmósfera. La ventaja principal de dicha disposición es Ia de proporcionar, en el camino de los rayos X, un espacio de atmósfera controlable, con las ventajas que esto implica, sin aumentar sustancialmente el ruido de fondo, tal como se ha explicado anteriormente, ya que dicho espacio representa una dimensión comparativamente reducida frente al resto del camino de los rayos X, efectuado en vacío.The cavity of the X-ray chamber has a cover in the upper part of the chamber and at least one opening in one side as well as another in the lower part of the chamber, communicated with the outside. The body is introduced into the chamber through one of said openings. The invention provides first means of sealing, which allow to maintain the vacuum inside the chamber by sealing the space between the walls of said chamber and the open end or ends of the body. Preferably, said first hermetic sealing means can comprise hermetic plugs or elastic seals, preferably of rubber, so that, once the first hermetic sealing means are used and the lid of the upper part of the cavity is closed, it is possible to proceed to make the void in said cavity. Said seals (or equivalent elements) tightly adjust the exterior of the body to the lateral opening of the chamber, avoiding on one side that the void of the cavity is lost, isolating on the other hand the interior of the body from the void of the cavity, and allowing also the possibility of a communication between the inside of the body and the outside of the chamber. This last possibility means that, depending on the design of the first hermetic closing means, they allow or not that the interior of the body is kept open to the laboratory conditions, or under a controlled atmosphere, by means of adequate means of atmosphere control . The main advantage of said arrangement is that of providing, in the path of X-rays, a controllable atmosphere space, with the advantages that this implies, without substantially increasing the background noise, such as He has explained previously, since this space represents a comparatively small dimension compared to the rest of the X-ray path, performed in a vacuum.
Asimismo, el cuerpo comprende unos medios de paso de radiación.Also, the body comprises radiation passage means.
Dichos medios de paso de radiación están sellados por unos medios de sellado, que pueden comprender una lámina de un material de sellado transparente a los rayos X y de propiedades mecánicas apropiadas para resistir el vacío. Algunos ejemplos no limitativos de materiales adecuados son, en función del ánodo empleado en Ia producción de rayos X, polímeros o plásticos, por ejemplo Mylar®, Kapton®, vidrio o mica, así como berilio, nitruro de silicio, plástico, un mineral natural, un mineral artificial, cuarzo, o metal. Los rayos X atraviesan los medios de paso de radiación del cuerpo, e inciden sobre Ia muestra alojada en el interior del mencionado cuerpo. Los medios de paso de radiación pueden estar materializados de diversas formas, y en particular en forma de aberturas en Ia superficie lateral del cuerpo para dejar libre el camino de los rayos X. Según el tamaño de abertura en Ia dirección perpendicular al eje longitudinal del cuerpo, puede tratarse de dos aberturas enfrentadas, o bien de una única abertura o hendidura suficientemente grande para permitir tanto Ia entrada como Ia salida de los rayos X.Said radiation passage means are sealed by sealing means, which may comprise a sheet of a sealing material transparent to X-rays and of suitable mechanical properties to resist vacuum. Some non-limiting examples of suitable materials are, depending on the anode used in the production of X-rays, polymers or plastics, for example Mylar®, Kapton®, glass or mica, as well as beryllium, silicon nitride, plastic, a natural mineral , an artificial mineral, quartz, or metal. The X-rays pass through the radiation passage means of the body, and affect the sample lodged inside the mentioned body. The radiation passage means can be materialized in various ways, and in particular in the form of openings in the lateral surface of the body to free the path of the X-rays. According to the size of the opening in the direction perpendicular to the longitudinal axis of the body , it can be two opposite openings, or a single opening or slit large enough to allow both the entry and exit of the X-rays.
De este modo, Ia invención posibilita Ia caracterización de, por ejemplo, muestras de humedad no nula que requieran en general una atmósfera distinta del vacío en cámaras de difracción o de dispersión de rayos X, y especialmente, pero no limitativamente, las que utilizan las tecnologías SAXS, GISAXS o GIWAXS, más particularmente en cámaras SAXS, GISAXS o GIWAXS de tipo Kratky. Algunos tipos de atmósfera controlada para los que Ia invención es adecuada son: presión atmosférica, atmósfera con un porcentaje de humedad preestablecido controlado, atmósfera inerte, atmósfera oxidante o atmósfera reductora, atmósfera a una temperatura o presión determinadas, entre otras.Thus, the invention enables the characterization of, for example, non-zero moisture samples that generally require an atmosphere other than vacuum in diffraction or X-ray scattering chambers, and especially, but not limited to, those that use the SAXS, GISAXS or GIWAXS technologies, more particularly in SAXS, GISAXS or GIWAXS Kratky type cameras. Some types of controlled atmosphere for which the invention is suitable are: atmospheric pressure, atmosphere with a pre-established percentage of controlled humidity, inert atmosphere, oxidizing atmosphere or reducing atmosphere, atmosphere at a set temperature or pressure, among others.
El mayor tamaño del cuerpo del dispositivo de Ia invención con respecto a los portamuestras o dispositivos conocidos en el estado de Ia técnica, que tienen forma de capilar, permite un mejor acceso a Ia muestra así como un cómodo manejo de Ia misma con independencia de su estado líquido o no, presentando a Ia vez propiedades adecuadas de resistencia mecánica.The larger size of the body of the device of the invention with respect to the sample holders or devices known in the state of the art, which have a capillary shape, allows better access to the sample as well as convenient handling thereof regardless of its liquid state or not, while presenting adequate mechanical resistance properties.
La invención destaca porque, según se describe en las siguientes realizaciones preferidas, además del aislamiento del vacío, el dispositivo permite Ia ubicación y Ia orientación de una muestra dentro de una cámara de difracción o de dispersión de rayos X de vacío de tipo Kratky, con una precisión adecuada, de forma que quede posicionada en el plano que se desee relativamente al haz de rayos X.The invention stands out because, as described in the following preferred embodiments, in addition to vacuum isolation, the device allows the location and orientation of a sample within a diffraction or X-ray dispersion chamber of Kratky type, with adequate precision, so that it is positioned in the plane that is desired relatively to the X-ray beam.
Así, según una segunda realización preferida, dicha invención, adicionalmente a Io descrito en Ia primera realización preferida, incorpora y aloja en su interior un conjunto de posicionamiento de una muestra dentro del cuerpo.Thus, according to a second preferred embodiment, said invention, in addition to that described in the first preferred embodiment, incorporates and houses within it a positioning assembly of a sample within the body.
El conjunto de posicionamiento está formado por los siguientes elementos:The positioning set consists of the following elements:
- una carcasa cilindrica hueca, que comprende una primera ventana en Ia superficie lateral de dicha carcasa, - un casquillo cilindrico hueco, alojado en el interior de Ia carcasa, que comprende al menos una segunda ventana en Ia superficie lateral de dicho casquillo,- a hollow cylindrical housing, comprising a first window on the lateral surface of said carcass, - a hollow cylindrical bushing, housed inside the carcass, comprising at least a second window on the lateral surface of said bushing,
- unos medios de presión solidarios con Ia superficie lateral interior de Ia carcasa, que presionan el casquillo contra unos medios de alineación, - unos medios de alineación del casquillo que permiten regular Ia altura e inclinación del mismo con respecto al eje de Ia carcasa, estando dichos medios adaptados para su control desde el exterior, y- pressure means integral with the inner lateral surface of the housing, which press the bushing against alignment means, - alignment means of the bushing that allow regulating the height and inclination thereof with respect to the axis of the housing, being said means adapted for external control, and
- un portamuestras, alojado en el interior del casquillo, estando dicho portamuestras adaptado para su acoplamiento a unos medios de giro (que no forman parte de Ia invención) que, desde el exterior de Ia cámara, permiten gobernar el giro del portamuestras según el eje longitudinal de dicho portamuestras. Dicho portamuestras puede ser igual a, o diferente de los que existen en el Estado de Ia Técnica.- a sample holder, housed inside the bush, said sample holder being adapted for coupling to means of rotation (which are not part of the invention) which, from outside the chamber, allow the rotation of the sample holder according to the axis. longitudinal of said sample holder. Said sample holder can be equal to, or different from those that exist in the State of the Art.
Los medios de alineación comprenden una primera cuña y una segunda cuña móviles, alojadas en el interior de Ia carcasa. Las cuñas presionan el casquillo, con Io cual Ia posición del casquillo depende del movimiento de dichas cuñas, que se transmite al casquillo a través de los puntos de contacto entre Ia superficie lateral del mismo y las cuñas.The alignment means comprise a first wedge and a second mobile wedge, housed inside the housing. The wedges press the bushing, with which the position of the bushing depends on the movement of said wedges, which is transmitted to the bushing through the contact points between the lateral surface thereof and the wedges.
Según una tercera realización preferida, se presenta un dispositivo para alojar una muestra en el interior de una cámara de dispersión o difracción de rayos X, que reúne de forma compacta las características de Ia realización preferida 2, prescindiendo de Ia carcasa. En Ia tercera realización preferida, una parte de Ia superficie lateral del cuerpo es amovible en forma de una primera tapa, que al ser retirada hace que el cuerpo presente una tercera ventana. La función principal de esta tercera ventana es facilitar el acceso al interior del cuerpo y Ia inserción del casquillo. La mencionada tapa está adaptada para ser fijada herméticamente a Ia superficie exterior del resto del cuerpo, ajustándose a Ia tercera ventana. Dicha tapa tiene Ia función adicional de sujetar el casquillo.According to a third preferred embodiment, a device is presented for housing a sample inside an X-ray dispersion or diffraction chamber, which compactly combines the characteristics of the preferred embodiment 2, regardless of the housing. In the third preferred embodiment, a part of the lateral surface of the body is removable in the form of a first cover, which when removed causes the body to have a third window. The main function of this third window is to facilitate access to the interior of the body and the insertion of the bushing. Said cover is adapted to be hermetically fixed to the outer surface of the rest of the body, adjusting to the third window. Said cover has the additional function of holding the bushing.
Esta tercera realización preferida de Ia invención comprende unos medios de presión, uno de cuyos extremos actúa sobre Ia parte interior de Ia tapa, mientras que el otro extremo actúa sobre el casquillo. Los medios de alineación del casquillo son acordes a Ia segunda realización preferida. Según una cuarta realización preferida, Ia invención incorpora adicionalmente, respecto a Io indicado en Ia primera realización preferida:This third preferred embodiment of the invention comprises pressure means, one of whose ends acts on the inner part of the lid, while the other end acts on the bushing. The alignment means of the bushing are in accordance with the second preferred embodiment. According to a fourth preferred embodiment, the invention further incorporates, with respect to what is indicated in the first preferred embodiment:
- un bloque adaptado para ser insertado en Ia cámara de rayos X y provisto de unos segundos medios de cierre hermético con respecto a las paredes de dicha cámara de rayos X, y- a block adapted to be inserted in the X-ray chamber and provided with a second means of sealing with respect to the walls of said X-ray chamber, and
- una segunda carcasa hueca, que comprende al menos una cuarta ventana que permite el paso de los rayos X en su superficie lateral, donde el cuerpo consta de una quinta ventana en su parte inferior y se materializa como una cubierta situada en Ia parte superior del bloque entre los segundos medios de cierre hermético y Ia segunda carcasa, cubriendo esta última. Esta cubierta puede ser de naturaleza amovible o fija, y en el primer caso especialmente, puede ir acompañada de unos terceros medios de cierre hermético entre Ia cubierta y el bloque. Los medios de paso de radiación pueden consistir en una hendidura o bien, preferentemente, en dos aberturas enfrentadas.- a second hollow housing, comprising at least a fourth window that allows the passage of X-rays on its lateral surface, where the body consists of a fifth window in its lower part and is embodied as a cover located in the upper part of the block between the second sealing means and the second housing, covering the latter. This cover can be of a removable or fixed nature, and in the first case especially, it can be accompanied by a third means of sealing between the cover and the block. The radiation passage means may consist of a slit or, preferably, two facing openings.
Asimismo, en esta realización preferida, los primeros medios de cierre hermético consisten en unas segundas tapas, preferentemente cilindricas, que se introducen por cada una de las aberturas laterales de Ia cámara y que comprenden a su vez unos:Likewise, in this preferred embodiment, the first sealing means consist of second covers, preferably cylindrical, which are introduced through each of the lateral openings of the chamber and which in turn comprise some:
- cuartos medios de cierre hermético (preferentemente una junta tórica o plana) que sellan el área de contacto entre Ia cubierta y dichas segundas tapas, y- fourth sealed means (preferably an o-ring or flat seal) that seal the contact area between the cover and said second covers, and
- quintos medios de cierre hermético (preferentemente una junta tórica o plana) que sellan el área de contacto entre las segundas tapas y Ia pared de Ia cámara.- Fifth sealing means (preferably an o-ring or flat) that seal the contact area between the second covers and the wall of the chamber.
Dichas segundas tapas pueden ser de diferentes diseños, de los que a continuación se ofrecen varios ejemplos no limitativos, según sean de una sola pieza o más piezas. En el caso de ser las segundas tapas de una sola pieza, pueden tener dos modelos básicos: uno tan solo para cerrar el espacio interior del cuerpo, en cuyo caso Ia tapa vendría completamente cerrada en al menos uno de sus extremos, sin permitir Ia comunicación del interior del cuerpo con el exterior de Ia cámara, y otro modelo para cerrar el espacio interior del cuerpo permitiendo Ia comunicación entre éste y el exterior de Ia cámara, en particular para permitir el paso de medios de control de atmósfera así como de los medios de transmisión del movimiento de un motor (que no forma parte de Ia invención) que haga girar el portamuestras. Por otro lado, en el caso de ser las segundas tapas de más de una pieza, pueden consistir en una pieza que se introduce en su mayor parte por Ia abertura lateral de Ia cámara a excepción de uno de sus extremos, en forma de placa, que se ajusta a Ia pared de dicha cámara por su lado externo, y otra pieza que se fija sobre Ia anterior (mediante tornillos o una rosca por ejemplo) en el exterior de Ia cámara. Esta última pieza puede ser también en forma de placa e incorporar una junta en su superficie de contacto con Ia pieza anterior, y puede existir en al menos dos variantes: una en forma de placa que sirve tan solo para cerrar el espacio interior del cuerpo, en cuyo caso Ia segunda tapa no permite Ia comunicación del interior del cuerpo con el exterior de Ia cámara, y otra para cerrar el espacio interior del cuerpo permitiendo el paso de medios de control de atmósfera y/o de medios de transmisión del movimiento de un motor (que no forma parte de Ia invención) que haga girar el portamuestras.These second covers can be of different designs, of which several non-limiting examples are given below, depending on whether they are one piece or more pieces. In the case of being the second one-piece covers, they can have two basic models: one only to close the interior space of the body, in which case the lid would be completely closed in at least one of its ends, without allowing the communication of the interior of the body with the exterior of the chamber, and another model to close the interior space of the body allowing the communication between it and the exterior of the chamber, in particular to allow the passage of atmosphere control means as well as of the transmission means of the movement of an engine (which is not part of the invention) that rotates the sample holder. On the other hand, in the case of being the second covers of more than one piece, they can consist of a piece that is introduced mostly by the lateral opening of the chamber except for one of its ends, in the form of a plate, which fits the wall of said chamber by its external side, and another piece that is fixed on the previous one (by means of screws or a thread for example) on the outside of the chamber. This last piece can also be in the form of a plate and incorporate a joint in its contact surface with the previous piece, and it can exist in at least two variants: one in the form of a plate that serves only to close the interior space of the body, in which case the second cover does not allow the communication of the interior of the body with the exterior of the chamber, and another to close the interior space of the body allowing the passage of atmosphere control means and / or means of transmission of the movement of a engine (which is not part of the invention) that rotates the sample holder.
DESCRIPCIÓN DE LOS DIBUJOSDESCRIPTION OF THE DRAWINGS
Para complementar Ia descripción que se está realizando y con objeto de ayudar a una mejor comprensión de las características de Ia invención, de acuerdo con un ejemplo preferente de realización práctica de Ia misma, se acompaña como parte integrante de dicha descripción, un juego de dibujos en donde con carácter ilustrativo y no limitativo, se ha representado Io siguiente:To complement the description that is being made and in order to help a better understanding of the characteristics of the invention, according to a preferred example of practical implementation thereof, a set of drawings is attached as an integral part of said description. where, for the purposes of illustration and not limitation, the following has been represented:
Figura 1.- Muestra una vista en perspectiva de Ia primera realización de la invención.Figure 1.- Shows a perspective view of the first embodiment of the invention.
Figura 2.- Muestra una vista correspondiente a Ia sección AB de Ia figura 1.Figure 2.- Shows a view corresponding to section AB of Figure 1.
Figura 3.- Muestra una vista en perspectiva de Ia segunda realización montada en una máquina de difracción o dispersión de rayos x.Figure 3.- Shows a perspective view of the second embodiment mounted on an x-ray diffraction or dispersion machine.
Figura 4.- Muestra una vista en perspectiva del conjunto de posicionamiento de Ia segunda realización de Ia invención.Figure 4.- Shows a perspective view of the positioning assembly of the second embodiment of the invention.
Figura 5.- Muestra otra vista en perspectiva del conjunto de posicionamiento de Ia segunda realización de Ia invención, desde diferente punto de vista.Figure 5.- Shows another perspective view of the positioning assembly of the second embodiment of the invention, from a different point of view.
Figura 6.- Muestra una vista en sección longitudinal de Ia segunda realización de Ia invención.Figure 6.- Shows a view in longitudinal section of the second embodiment of the invention.
Figura 7.- Muestra una vista en perspectiva de Ia tercera realización de Ia invención.Figure 7.- Shows a perspective view of the third embodiment of the invention.
Figura 8.- Muestra una vista correspondiente a Ia sección CD de Ia figura 7.Figure 8.- Shows a view corresponding to the CD section of Figure 7.
Figura 9.- Muestra una vista en sección longitudinal de Ia tercera realización de Ia invención.Figure 9.- Shows a view in longitudinal section of the third embodiment of the invention.
Figura 10.- Muestra una vista en perspectiva del portamuestras. Figura 11.- Muestra una vista en perspectiva de Ia cuarta realización de Ia invención. Figura 12: Muestra una vista en perspectiva de una parte de los medios de alineación (sin los botones y sin el fijador de dichos medios de alineación, que se representan en figuras anteriores).Figure 10.- Shows a perspective view of the sample holder. Figure 11.- Shows a perspective view of the fourth embodiment of the invention. Figure 12: Shows a perspective view of a part of the alignment means (without the buttons and without the fixing of said alignment means, which are shown in previous figures).
EJEMPLOS DE REALIZACIÓN DE LA INVENCIÓNEXAMPLES OF EMBODIMENT OF THE INVENTION
PRIMER EJEMPLO DE REALIZACIÓN, CORRESPONDIENTE A LA PRIMERA REALIZACIÓN PREFERIDA.FIRST EXAMPLE OF REALIZATION, CORRESPONDING TO THE FIRST PREFERRED EMBODIMENT.
La primera realización práctica de Ia invención describe un dispositivo para alojar una muestra en el interior de una cámara (4) de dispersión o de difracción de rayos X. La primera realización permite incorporar un tramo de no vacío dentro del camino de los rayos X.The first practical embodiment of the invention describes a device for housing a sample inside an X-ray scattering or diffraction chamber (4). The first embodiment allows incorporating a non-empty section within the path of the X-rays.
El dispositivo del primer ejemplo de realización comprende un cuerpo (1 ) hueco, alargado y abierto en ambos extremos, resistente al vacío, adaptado para alojar en su interior Ia muestra que se desea analizar, así como comprende igualmente dos medios de paso de radiación (2) enfrentados, que atraviesan dicho cuerpo (1 ), a través de los cuales pasan los rayos X antes y después de interaccionar con dicha muestra.The device of the first embodiment comprises a hollow, elongated and open body (1) at both ends, vacuum resistant, adapted to accommodate inside the sample to be analyzed, as well as comprising two radiation passage means ( 2) facing each other, which pass through said body (1), through which X-rays pass before and after interacting with said sample.
El dispositivo incorpora además unos primeros medios de cierre hermético (5) de los extremos del cuerpo (1 ), que permiten mantener el vacío dentro de Ia cámara (4) sellando el espacio entre las paredes de dicha cámara (4) y los extremos del cuerpo (1 ), así como incorpora también unos medios de sellado de los medios de paso de radiación (2), transparentes a los rayos X y resistentes al vacío, que permiten mantener Ia atmósfera del cuerpo (1 ) aislada con respecto al vacío de Ia cámara (4).The device also incorporates first means of sealing (5) of the ends of the body (1), which allow to maintain the vacuum inside the chamber (4) by sealing the space between the walls of said chamber (4) and the ends of the body (1), as well as incorporating sealing means of the radiation passage means (2), transparent to X-rays and resistant to vacuum, which allow to keep the atmosphere of the body (1) isolated with respect to the vacuum of The camera (4).
Una vez instalados los primeros medios de cierre hermético en los extremos del cuerpo (1 ), Ia muestra alojada en el interior puede ser alcanzada por los rayos X protegida del vacío. Además, en el interior del cuerpo (1 ) se puede proporcionar una atmósfera adecuada a Ia muestra que se está analizando o a las condiciones de medida adecuadas, para Io cual Ia invención comprende adicionalmente unos medios de control de Ia atmósfera interior del cuerpo (1 ), que comprenden a su vez al menos un tubo (7) conectado a unos medios proveedores de condiciones atmosféricas seleccionadas. Las condiciones atmosféricas que se pueden seleccionar son muy variadas, entre las que se prefieren: presión atmosférica, atmósfera con un porcentaje de humedad preestablecido controlado, atmósfera inerte, atmósfera oxidante o atmósfera reductora, así como atmósfera a una temperatura o presión determinadas, entre otras.Once the first means of sealing are installed in the body ends (1), the sample housed inside can be reached by X-rays protected from vacuum. In addition, inside the body (1) a suitable atmosphere can be provided to the sample being analyzed or to the appropriate measurement conditions, for which the invention additionally comprises means for controlling the interior atmosphere of the body (1) , which in turn comprise at least one tube (7) connected to means providing selected atmospheric conditions. The atmospheric conditions that can be selected are very varied, among which are preferred: atmospheric pressure, atmosphere with a pre-established percentage of controlled humidity, inert atmosphere, oxidizing atmosphere or reducing atmosphere, as well as atmosphere at a certain temperature or pressure, among others .
Los materiales preferidos para construir el cuerpo (1 ) son acero, aluminio, cobre, plástico, vidrio, y aleaciones metálicas, siendo el acero inoxidable el material más preferido.The preferred materials for building the body (1) are steel, aluminum, copper, plastic, glass, and metal alloys, with stainless steel being the most preferred material.
En este primer ejemplo de realización de Ia invención, el cuerpo (1 ) tiene forma cilindrica, aunque son igualmente posibles otras formas.In this first embodiment of the invention, the body (1) has a cylindrical shape, although other shapes are equally possible.
Los primeros medios de cierre hermético (5) pueden ser o comprender juntas y/o tapones de manera preferente, si bien cualquier otro medio equivalente de cierre es igualmente válido.The first sealing means (5) may be or preferably comprise seals and / or plugs, although any other equivalent means of closure is equally valid.
Preferentemente los medios de sellado comprenden al menos una lámina (6) y elementos de fijación de Ia lámina (6) al cuerpo (1 ). De manera alternativa, los medios de sellado pueden comprender una tapadera perforada roscada al exterior del cuerpo (1 ) y una junta, como se representa en Ia Figura 8. Entre los medios de fijación pueden incluirse mordazas, uniones roscadas, soldadura, adhesivos, etc. La propia lámina (6) puede contener los elementos de fijación, en el caso, por ejemplo, de que Ia fijación se produzca por aplicación de un tratamiento térmico que funda los bordes de Ia lámina, sirviendo dichos bordes de medios de fijación. La lámina (6) está fabricada preferiblemente de uno de los materiales siguientes: vidrio, metal, preferentemente berilio, un material polimérico, preferentemente Mylar®, Kapton®, nitruro de silicio, plástico, un mineral natural, un mineral artificial, mica o cuarzo.Preferably the sealing means comprise at least one sheet (6) and fixing elements of the sheet (6) to the body (1). Alternatively, the sealing means can comprise a threaded perforated cover to the outside of the body (1) and a gasket, as shown in Figure 8. Among the fixing means can be included jaws, threaded joints, welding, adhesives, etc. . The sheet itself (6) can contain the fixing elements, in the case, for example, of which the fixing is produced by application of a heat treatment that melts the edges of the sheet, said edges serving fixing means. The sheet (6) is preferably made of one of the following materials: glass, metal, preferably beryllium, a polymeric material, preferably Mylar®, Kapton®, silicon nitride, plastic, a natural mineral, an artificial mineral, mica or quartz .
SEGUNDO EJEMPLO DE REALIZACIÓN, CORRESPONDIENTE A LA SEGUNDA REALIZACIÓN PREFERIDASECOND EXAMPLE OF REALIZATION, CORRESPONDING TO THE SECOND PREFERRED EMBODIMENT
La segunda realización práctica de Ia invención presenta un dispositivo como el de Ia primera realización práctica, con un cuerpo (1 ), medios de paso de radiación, medios de sellado y medios de cierre hermético, que está provisto adicionalmente, alojado en su interior, de un conjunto de posicionamiento para posicionar y orientar Ia muestra, que comprende a su vez:The second practical embodiment of the invention has a device like that of the first practical embodiment, with a body (1), radiation passage means, sealing means and hermetic closing means, which is additionally provided, housed inside, of a positioning set to position and orient the sample, which in turn comprises:
- una carcasa (8) cilindrica hueca, que comprende una primera ventana (9) en Ia superficie lateral de dicha carcasa (8),- a hollow cylindrical housing (8), comprising a first window (9) on the lateral surface of said housing (8),
- un casquillo (13) cilindrico hueco, alojado en el interior de Ia carcasa (8), que comprende al menos una segunda ventana (10) en Ia superficie lateral de dicho casquillo (13),- a hollow cylindrical bushing (13), housed inside the housing (8), comprising at least a second window (10) on the lateral surface of said bushing (13),
- unos medios de presión (14) solidarios a Ia superficie lateral interior de Ia carcasa (8), que presionan el casquillo (13) contra los medios de alineación, - unos medios de alineación del casquillo (13) que permiten regular Ia altura e inclinación del mismo con respecto al eje de Ia carcasa (8), estando dichos medios adaptados para su control desde el exterior, y- pressure means (14) integral with the inner lateral surface of the housing (8), which press the bushing (13) against the alignment means, - alignment means of the bushing (13) that allow regulating the height e inclination thereof with respect to the axis of the housing (8), said means being adapted for control from the outside, and
- un portamuestras (15), alojado en el interior del casquillo (13), estando dicho portamuestras (15) adaptado para su acoplamiento a unos medios de giro (32) (ajenos a Ia invención) que, desde el exterior de Ia cámara (4), permiten gobernar el giro del portamuestras (15) según el eje longitudinal de dicho portamuestras (15).- a sample holder (15), housed inside the bush (13), said sample holder (15) being adapted for coupling to turning means (32) (outside the invention) which, from the outside of the chamber ( 4), allow to govern the rotation of the sample holder (15) along the axis longitudinal of said sample holder (15).
De manera preferente, los medios de alineación comprendenPreferably, the alignment means comprise
- una primera cuña (16) y una segunda cuña (17) en el interior de Ia carcasa (8), sobre las que reposa el casquillo (13), que incorporan respectivamente un primer agujero de desplazamiento (18) y un segundo agujero de desplazamiento (19) roscados, así como agujeros de guía (20),- a first wedge (16) and a second wedge (17) inside the housing (8), on which the bushing (13) rests, which respectively incorporate a first sliding hole (18) and a second hole of threaded displacement (19), as well as guide holes (20),
- dos guías (21 ), en forma de varilla, insertadas en los agujeros de guía (20) según direcciones paralelas, que permiten el libre desplazamiento longitudinal de las cuñas (16, 17), y- two guides (21), in the form of a rod, inserted in the guide holes (20) according to parallel directions, which allow the free longitudinal displacement of the wedges (16, 17), and
- un conjunto de desplazamiento de las cuñas (16, 17), que comprende:- a set of shifting of the wedges (16, 17), comprising:
- un árbol (22) de soporte, paralelamente a las guías (21 ),- a support shaft (22), parallel to the guides (21),
- un primer desplazador (23), dentro del cual se aloja el árbol (22) de soporte, en forma de varilla hueca parcialmente roscada exteriormente y alojada en el interior del primer agujero de desplazamiento (18), siendo el tramo roscado el que pasa por dentro de Ia cuña, y produciendo el giro del primer desplazador (23) el desplazamiento longitudinal de Ia primera cuña (16) exclusivamente, - un segundo desplazador (24), dentro del cual se aloja el árbol- a first displacer (23), within which the support shaft (22) is housed, in the form of a hollow rod partially threaded externally and housed inside the first displacement hole (18), the threaded section being the one that passes inside the wedge, and producing the rotation of the first displacer (23) the longitudinal displacement of the first wedge (16) exclusively, - a second displacer (24), within which the tree is housed
(22) de soporte con el cual es solidario, en forma de varilla hueca parcialmente roscada exteriormente y alojada en el segundo agujero de desplazamiento (19), y produciendo el giro del segundo desplazador (24) el desplazamiento de Ia segunda cuña (17) exclusivamente, y - un separador (33) que separa el primer desplazador (23) y el segundo desplazador (24), produciendo el desplazamiento de las cuñas (16, 17) variaciones en Ia posición y orientación del casquillo (13) con respecto a Ia carcasa (8).(22) of support with which it is integral, in the form of a hollow rod partially threaded externally and housed in the second displacement hole (19), and producing the rotation of the second displacer (24) the displacement of the second wedge (17) exclusively, and - a separator (33) that separates the first displacer (23) and the second displacer (24), causing the shifting of the wedges (16, 17) variations in the position and orientation of the bushing (13) with respect to The housing (8).
De preferencia, las cuñas (16, 17) son cilindros huecos con una superficie interior cónica. De este modo se consigue una doble función: por un lado, el movimiento de los desplazadores (23, 24) orienta el casquillo (13), mientras que Ia superficie cónica interior a las cuñas (16, 17) evita el balanceo lateral de dicho casquillo (13). Las cuñas (16, 17) también pueden ser planas, en cuyo caso Ia invención comprende adicionalmente unos medios de retención (no representados) para evitar el balanceo del casquillo (13).Preferably, the wedges (16, 17) are hollow cylinders with a conical inner surface. In this way a double function is achieved: on the one hand, the movement of the displacer (23, 24) orients the bushing (13), while the inner conical surface to the wedges (16, 17) prevents lateral balancing of said bushing (13). The wedges (16, 17) can also be flat, in which case the invention additionally comprises retaining means (not shown) to avoid balancing the bushing (13).
De manera preferente, el conjunto de desplazamiento comprende sendos botones (25 y 26) solidarios con los desplazadores (23 y 24 respectivamente) y cuyo giro produce el giro de dichos desplazadores (23 y 24 respectivamente).Preferably, the displacement assembly comprises two buttons (25 and 26) integral with the displacers (23 and 24 respectively) and whose rotation produces the rotation of said displacers (23 and 24 respectively).
Es preferible que Ia invención incorpore adicionalmente unos elementos de contacto (12) ubicados exteriormente al casquillo (13) y solidarios con él, que sirven de contacto entre dicho casquillo (13) y las cuñas (16, 17). Dichos elementos de contacto (12) son preferentemente aros de contacto. Una buena opción es que los aros sean por ejemplo de goma, y que las cuñas sean por ejemplo de teflón u otro material equivalente, antiadherente.It is preferable that the invention additionally incorporates contact elements (12) located externally to the bushing (13) and integral with it, which serve as contact between said bushing (13) and the wedges (16, 17). Said contact elements (12) are preferably contact rings. A good option is that the rings are for example rubber, and that the wedges are for example Teflon or other equivalent, non-stick material.
Preferentemente, en esta realización práctica, los medios de presiónPreferably, in this practical embodiment, the pressure means
(14) comprenden una lengüeta solidaria con Ia superficie interior de Ia carcasa (8) y que presiona contra Ia superficie exterior del casquillo (13). Optativamente, cuando los elementos de contacto (12) consisten en aros, Ia antedicha lengüeta se insiere y queda aprisionada entre uno de los aros y el casquillo.(14) comprise a tongue integral with the inner surface of the housing (8) and pressing against the outer surface of the bushing (13). Optionally, when the contact elements (12) consist of rings, the said tongue is inserted and is imprisoned between one of the rings and the bushing.
TERCER EJEMPLO DE REALIZACIÓN, CORRESPONDIENTE A LA TERCERA REALIZACIÓN PREFERIDATHIRD EXAMPLE OF REALIZATION, CORRESPONDING TO THE THIRD PREFERRED EMBODIMENT
La tercera realización práctica de Ia invención consiste en un dispositivo para alojar una muestra en el interior de una cámara (4) de dispersión o difracción de rayos X, que comprende, de acuerdo con Ia tercera realización preferida:The third practical embodiment of the invention consists of a device for accommodating a sample inside an X-ray dispersion or diffraction chamber (4), which comprises, in accordance with Ia third preferred embodiment:
- un cuerpo (1 ) hueco, resistente al vacío, provisto de al menos una tercera ventana (11 ) en su superficie lateral,- a hollow, vacuum-resistant body (1), provided with at least a third window (11) on its lateral surface,
- una tapa (35) adaptada para ser fijada herméticamente a Ia superficie exterior del cuerpo (1 ), cubriendo Ia tercera ventana (11 ), incorporando dicha tapa:- a cover (35) adapted to be hermetically fixed to the outer surface of the body (1), covering the third window (11), incorporating said cover:
- unos medios de presión (14) solidarios por un extremo con Ia parte interior de Ia tapa, y- pressure means (14) integral with one end with the inside of the lid, and
- un casquillo (13) en contacto con, o unido al extremo libre de los medios de presión, y- a bushing (13) in contact with, or attached to the free end of the pressure means, and
- unos medios de alineación del casquillo (13) con respecto al cuerpo (1 ), que producen un desplazamiento y un cambio de Ia orientación del casquillo (13) con respecto del cuerpo (1 ), estando dichos medios de alineación adaptados para su control desde el exterior.- means for aligning the bushing (13) with respect to the body (1), which produce a displacement and a change in the orientation of the bushing (13) with respect to the body (1), said alignment means being adapted for control from the outside.
Opcionalmente, los medios de presión comprenden una lengüeta solidaria a Ia superficie interior de Ia tapa (35) y unida a, o que presiona contra, Ia superficie exterior del casquillo (13).Optionally, the pressure means comprise a tongue integral to the inner surface of the cover (35) and attached to, or pressing against, the outer surface of the bushing (13).
En este tercer ejemplo de realización y también en el anterior, los medios de alineación del casquillo comprenden al menos un fijador (3) cuya función es impedir el corrimiento longitudinal de los elementos del conjunto de desplazamiento con respecto al cuerpo (1 ). Dicho fijador (3) se encuentra en al menos uno de los extremos del conjunto de desplazamiento, y puede tomar Ia forma de, por ejemplo, una capucha de los botones (25, 26) o de una abrazadera en el extremo opuesto del árbol de soporte (22).In this third embodiment and also in the previous one, the alignment means of the bushing comprise at least one fastener (3) whose function is to prevent the longitudinal sliding of the elements of the displacement assembly with respect to the body (1). Said fastener (3) is at least one of the ends of the displacement assembly, and can take the form of, for example, a hood of the buttons (25, 26) or of a clamp at the opposite end of the shaft of support (22).
Asimismo, en este tercer ejemplo de realización y también en el anterior, las varillas están sujetas al menos por uno de sus extremos, al correspondiente extremo de Ia carcasa o del cuerpo. CUARTO EJEMPLO DE REALIZACIÓN, CORRESPONDIENTE A LA CUARTA REALIZACIÓN PREFERIDALikewise, in this third embodiment and also in the previous one, the rods are attached at least by one of their ends, to the corresponding end of the housing or body. FOURTH EXAMPLE OF REALIZATION, CORRESPONDING TO THE FOURTH PREFERRED REALIZATION
La cuarta realización práctica de Ia invención consiste en un dispositivo de acuerdo con Ia realización preferida, caracterizado porque incorpora, adicionalmente a Io indicado para Ia primera realización preferida:The fourth practical embodiment of the invention consists of a device according to the preferred embodiment, characterized in that it incorporates, in addition to that indicated for the first preferred embodiment:
- un bloque (27) adaptado para ser insertado en Ia cámara (4) de rayos X y provisto de unos segundos medios de cierre hermético respecto a las paredes de dicha cámara (4) de rayos X, y- a block (27) adapted to be inserted in the X-ray chamber (4) and provided with a second means of sealing with respect to the walls of said X-ray chamber (4), and
- una segunda carcasa (8) hueca, que comprende al menos una cuarta ventana (34) en su superficie lateral que permite el paso de los rayos- a second hollow housing (8), comprising at least a fourth window (34) on its lateral surface that allows the rays to pass through
X, donde el cuerpo (1 ) es una cubierta (28) situada en Ia parte superior del bloque (27) entre los segundos medios de cierre hermético y Ia carcasa (8), cubriendo a dicha carcasa (8), y provista de unos medios de paso de radiación (2) que consisten en al menos una abertura (36) que permite el paso de los rayos x.X, where the body (1) is a cover (28) located in the upper part of the block (27) between the second sealing means and the housing (8), covering said housing (8), and provided with radiation passage means (2) consisting of at least one opening (36) that allows the passage of x-rays.
De manera preferente, en esta realización práctica de Ia invención, los primeros medios de cierre hermético (5) consisten en unas segundas tapas, preferentemente cilindricas, huecas, e introducibles por las aberturas laterales de Ia cámara (4), que comprenden: unos cuartos medios de cierre hermético (30) que sellan el área de contacto entre Ia cubierta (28) y las segundas tapas, y unos quintos medios de cierre hermético (31 ) que sellan el área de contacto entre las segundas tapas y Ia pared de Ia cámara (4). Más preferentemente, dichas segundas tapas son de diversos modelos, algunos de los cuales incorporanal menos una abertura en cada extremo o bien un canal que permita acciones seleccionadas de una lista que comprende: Ia introducción de Ia muestra, el paso o conexión de los medios de control de atmósfera, o el paso de los medios de transmisión del movimiento de un motor que haga girar el portamuestras (15).Preferably, in this practical embodiment of the invention, the first sealing means (5) consist of second covers, preferably cylindrical, hollow, and introducible by the lateral openings of the chamber (4), comprising: sealing means (30) that seal the contact area between the cover (28) and the second covers, and fifth fifth means of sealing (31) that seal the contact area between the second covers and the chamber wall (4). More preferably, said second covers are of various models, some of which incorporate at least one opening at each end or a channel that allows selected actions from a list comprising: the introduction of the sample, the passage or connection of the atmosphere control means, or the passage of the transmission means of the movement of an engine that rotates the sample holder (15).
De manera preferente, los cuartos medios de cierre hermético (30) y los quintos medios de cierre hermético (31 ) son juntas tóricas o planas.Preferably, the fourth seal means (30) and the fifth seal means (31) are o-rings or flat.
Asimismo, preferentemente, los segundos medios de cierre hermético y los terceros medios de cierre hermético coinciden en un único elemento combinado de cierre hermético.Likewise, preferably, the second sealing means and the third sealing means coincide in a single combined sealing element.
Más preferentemente, dicho elemento combinado de cierre hermético comprende:More preferably, said combined sealing element comprises:
-una ranura perimetral en Ia superficie superior del bloque (27); y-a perimeter groove in the upper surface of the block (27); Y
-una junta tórica que se aloja dentro de Ia ranura dejando el espacio justo, junto a Ia pared más interior de Ia ranura, para que en él pueda encajar Ia cubierta (28).-a O-ring that is housed inside the groove leaving the right space, next to the innermost wall of the groove, so that the cover (28) can fit into it.
Todavía más preferentemente, el bloque (27) incorpora medios de regulación de Ia posición de Ia muestra.Even more preferably, the block (27) incorporates means for regulating the position of the sample.
De manera opcional, los terceros medios de cierre hermético consisten en una unión solidaria del cuerpo (1 ) con el bloque (27).Optionally, the third sealing means consist of a joint connection of the body (1) with the block (27).
Preferentemente, el tipo de unión solidaria del cuerpo (1 ) con el bloquePreferably, the type of joint connection of the body (1) with the block
(27) se selecciona de Ia lista: soldadura, adhesivo, mecanización, magnética. (27) is selected from the list: welding, adhesive, mechanization, magnetic.

Claims

R E I V I N D I C A C I O N E S
1. Dispositivo para alojar una muestra en el interior de una cámara (4) de dispersión o difracción de rayos X, caracterizado porque comprende: - un cuerpo (1 ) hueco, alargado y abierto en uno o en ambos extremos, resistente al vacío, adaptado para alojar en su interior Ia muestra que se desea analizar;1. Device for accommodating a sample inside an X-ray dispersion or diffraction chamber (4), characterized in that it comprises: - a hollow, elongated and open body (1) at one or both ends, vacuum-resistant, adapted to accommodate inside the sample to be analyzed;
- unos medios de paso de radiación (2) practicados en Ia superficie del cuerpo (1 ) y a través de los cuales pasan los rayos X antes y después de interaccionar con dicha muestra;- radiation passage means (2) practiced on the surface of the body (1) and through which X-rays pass before and after interacting with said sample;
- unos primeros medios de cierre hermético (5) de los extremos del cuerpo (1 ), que permiten mantener el vacío dentro de Ia cámara (4) al sellar el espacio entre las paredes de dicha cámara (4) y los extremos del cuerpo- First sealing means (5) of the ends of the body (1), which allow to maintain the vacuum inside the chamber (4) by sealing the space between the walls of said chamber (4) and the ends of the body
0); y - unos medios de sellado de los medios de paso de radiación (2), transparentes a los rayos X y resistentes al vacío, que permiten mantener Ia atmósfera del cuerpo (1 ) aislada respecto del vacío de Ia cámara (4).0); and - sealing means of the radiation passage means (2), transparent to X-rays and resistant to vacuum, which allow to keep the body's atmosphere (1) isolated with respect to the vacuum of the chamber (4).
2.- Dispositivo de acuerdo con Ia reivindicación 1 , caracterizado porque los medios de paso de radiación son dos aberturas (2) enfrentadas que atraviesan el cuerpo (1 ) o bien una hendidura en el mismo.2. Device according to claim 1, characterized in that the radiation passage means are two openings (2) facing through the body (1) or a slot in it.
3.- Dispositivo de acuerdo con Ia reivindicación 1 , caracterizado porque los medios de paso de radiación es una tercera ventana (11 ).3. Device according to claim 1, characterized in that the radiation passage means is a third window (11).
4. Dispositivo de acuerdo con Ia reivindicación 1 , caracterizado porque comprende adicionalmente unos medios de control de Ia atmósfera interior del cuerpo (1 ), que comprenden al menos un tubo (7) conectado a unos medios proveedores de condiciones atmosféricas seleccionadas.4. Device according to claim 1, characterized in that it additionally comprises means for controlling the interior atmosphere of the body (1), comprising at least one tube (7) connected to means providing selected atmospheric conditions.
5. Dispositivo de acuerdo con Ia reivindicación 1 , caracterizado porque el cuerpo (1 ) está fabricado de un material seleccionado entre:5. Device according to claim 1, characterized in that the body (1) is made of a material selected from:
- acero,- steel,
- aluminio,- aluminum,
- cobre, - plástico,- copper, - plastic,
- vidrio, y- glass, and
- aleaciones metálicas.- metal alloys.
6. Dispositivo de acuerdo con Ia reivindicación 1 , caracterizado porque el cuerpo (1 ) tiene forma cilindrica.6. Device according to claim 1, characterized in that the body (1) has a cylindrical shape.
7. Dispositivo de acuerdo con Ia reivindicación 1 , caracterizado porque los medios de cierre hermético son juntas y/o tapones, o segundas tapas.7. Device according to claim 1, characterized in that the sealing means are seals and / or plugs, or second covers.
8. Dispositivo de acuerdo con Ia reivindicación 1 , caracterizado porque los medios de sellado comprenden al menos una lámina (6) y elementos de fijación de Ia lámina (6) al cuerpo (1 ).8. Device according to claim 1, characterized in that the sealing means comprise at least one sheet (6) and fixing elements of the sheet (6) to the body (1).
9. Dispositivo de acuerdo con Ia reivindicación 1 , caracterizado porque los medios de sellado comprenden una tapa perforada roscada al exterior del cuerpo (1 ) y una junta.9. Device according to claim 1, characterized in that the sealing means comprise a threaded perforated cover outside the body (1) and a gasket.
10. Dispositivo de acuerdo con Ia reivindicación 8, caracterizado porque los elementos de fijación comprenden una soldadura o un adhesivo.10. Device according to claim 8, characterized in that the fixing elements comprise a weld or an adhesive.
11. Dispositivo de acuerdo con Ia reivindicación 8, caracterizado porque los elementos de fijación forman parte de Ia lámina (6).11. Device according to claim 8, characterized in that the fixing elements are part of the sheet (6).
12. Dispositivo de acuerdo con Ia reivindicación 8, caracterizado porque Ia lámina (6) está fabricada de un material que se selecciona entre:12. Device according to claim 8, characterized in that the sheet (6) is made of a material that is selected from:
- vidrio, - un polímero,- glass, - a polymer,
- berilio,beryllium
- nitruro de silicio,- silicon nitride,
- plástico, - un mineral natural,- plastic, - a natural mineral,
- un mineral artificial,- an artificial mineral,
- mica,- mica,
- cuarzo, y- quartz, and
- un metal.- a metal.
13. Dispositivo de acuerdo con Ia reivindicación 8, caracterizado porque Ia lámina (6) está fabricada en poliéster Mylar® o en Kapton®.13. Device according to claim 8, characterized in that the sheet (6) is made of Mylar® polyester or Kapton®.
14. Dispositivo de acuerdo con Ia reivindicación 1 , caracterizado porque comprende adicionalmente, alojado en el interior del cuerpo (1 ), un conjunto de posicionamiento para posicionar y orientar una muestra, que comprende a su vez:14. Device according to claim 1, characterized in that it further comprises, housed inside the body (1), a positioning assembly for positioning and orienting a sample, which in turn comprises:
- una carcasa (8) cilindrica hueca, que comprende una primera ventana (9) en Ia superficie lateral de dicha carcasa (8), - un casquillo (13) cilindrico hueco, alojado en el interior de Ia carcasa- a hollow cylindrical housing (8), comprising a first window (9) on the lateral surface of said casing (8), - a hollow cylindrical bushing (13), housed inside the housing
(8), que comprende al menos una segunda ventana (10) en Ia superficie lateral de dicho casquillo (13),(8), which comprises at least a second window (10) on the lateral surface of said bushing (13),
- unos medios de presión (14) solidarios a Ia superficie lateral interior de Ia carcasa (8), que presionan el casquillo (13) contra unos medios de alineación,- pressure means (14) integral with the inner side surface of the housing (8), which press the bushing (13) against alignment means,
- unos medios de alineación del casquillo (13) que permiten regular Ia altura e inclinación del mismo con respecto al eje de Ia carcasa (8), estando dichos medios adaptados para su control desde el exterior, y- means for aligning the bushing (13) that allow regulating the height and inclination thereof with respect to the axis of the housing (8), said means being adapted for control from the outside, and
- un portamuestras (15), alojado en el interior del casquillo (13), estando dicho portamuestras (15) adaptado para su acoplamiento a unos medios de giro que, desde el exterior de Ia cámara (4), permiten gobernar el giro del portamuestras (15) según el eje longitudinal de dicho portamuestras (15).- a sample holder (15), housed inside the bush (13), said sample holder (15) being adapted for coupling to turning means which, from the outside of the chamber (4), allow to govern the rotation of the sample holder (15) along the longitudinal axis of said sample holder (15).
15. Dispositivo según Ia reivindicación 14 caracterizado porque los medios de alineación comprenden15. Device according to claim 14 characterized in that the alignment means comprise
- una primera cuña (16) y una segunda cuña (17) en el interior de Ia carcasa (8), sobre las que reposa el casquillo (13), que incorporan respectivamente un primer agujero de desplazamiento (18) y un segundo agujero de desplazamiento (19) roscados, así como agujeros de guía (20), - dos guías (21 ) en forma de varilla, insertadas en los agujeros de guía- a first wedge (16) and a second wedge (17) inside the housing (8), on which the bushing (13) rests, which respectively incorporate a first sliding hole (18) and a second hole of threaded displacement (19), as well as guide holes (20), - two rod-shaped guides (21), inserted into the guide holes
(20) según direcciones paralelas, que permiten el desplazamiento longitudinal de las cuñas (16, 17), y(20) according to parallel directions, which allow the longitudinal displacement of the wedges (16, 17), and
- un conjunto de desplazamiento de las cuñas (16, 17), que comprende: - un árbol (22) de soporte alojado en los agujeros de desplazamiento (18, 19), paralelamente a las guías (21 ),- a wedge displacement assembly (16, 17), comprising: - a support shaft (22) housed in the displacement holes (18, 19), parallel to the guides (21),
- un primer desplazador (23), dentro del cual se aloja el árbol (22) de soporte con el cual es solidario, en forma de varilla hueca roscada exteriormente alojada en el interior del primer agujero de desplazamiento (18), produciendo el giro del primer desplazador (23) el desplazamiento longitudinal de Ia primera cuña (16) exclusivamente,- a first displacer (23), within which the support shaft (22) with which it is integral is housed, in the form of an external threaded hollow rod housed inside the first displacement hole (18), producing the rotation of the first displacer (23) the longitudinal displacement of the first wedge (16) exclusively,
- un segundo desplazador (24), dentro del cual se aloja el árbol (22) de soporte, en forma de varilla hueca roscada exteriormente alojada en el segundo agujero de desplazamiento (19), y produciendo el giro del segundo desplazador (24) el desplazamiento de Ia segunda cuña (17) exclusivamente, y- a second displacer (24), within which the support shaft (22) is housed, in the form of a hollow rod threaded externally housed in the second displacement hole (19), and producing the rotation of the second displacer (24) the displacement of the second wedge (17) exclusively, and
- un separador (33) que separa el primer desplazador (23) y el segundo desplazador (24), produciendo el desplazamiento de las cuñas (16, 17) variaciones en Ia posición y orientación del casquillo (13) con respecto a Ia carcasa (8). - a separator (33) that separates the first displacer (23) and the second displacer (24), producing the shifting of the wedges (16, 17) variations in the position and orientation of the bushing (13) with respect to the housing ( 8).
16. Dispositivo según Ia reivindicación 15 caracterizado porque comprende unos medios de retención para evitar el balanceo del casquillo (13).16. Device according to claim 15 characterized in that it comprises retention means to prevent the balance of the bushing (13).
17. Dispositivo según Ia reivindicación 15, caracterizado porque las cuñas (16, 17) son cilindros huecos con una superficie interior cónica.17. Device according to claim 15, characterized in that the wedges (16, 17) are hollow cylinders with a conical inner surface.
18. Dispositivo según Ia reivindicación 15, caracterizado porque el conjunto de desplazamiento comprenden sendos botones (25) solidarios con los desplazadores (23, 24) y cuyo giro produce el giro de dichos desplazadores (23, 24).18. Device according to claim 15, characterized in that the displacement assembly comprises two buttons (25) integral with the displacers (23, 24) and whose rotation produces the rotation of said displacers (23, 24).
19. Dispositivo de acuerdo con Ia reivindicación 14, caracterizado porque los medios de presión (14) comprenden una lengüeta solidaria a Ia superficie interior de Ia carcasa (8) y que presiona contra Ia superficie exterior del casquillo (13).19. Device according to claim 14, characterized in that the pressure means (14) comprise a tongue integral with the inner surface of the housing (8) and pressing against the outer surface of the bushing (13).
20. Dispositivo según Ia reivindicación 14, caracterizado porque incorpora adicionalmente unos elementos de contacto ubicados exteriormente al casquillo (13) y que sirven de contacto entre dicho casquillo (13) y las cuñas20. Device according to claim 14, characterized in that it additionally incorporates contact elements located externally to the bushing (13) and which serve as contact between said bushing (13) and the wedges
(16, 17).(16, 17).
21. Dispositivo según Ia reivindicación 20, caracterizado porque los elementos de contacto son aros (26) de contacto.21. Device according to claim 20, characterized in that the contact elements are contact rings (26).
22. Dispositivo según Ia reivindicación 14, caracterizado porque comprende adicionalmente:22. Device according to claim 14, characterized in that it further comprises:
- una tapa (35) adaptada para ser fijada herméticamente a Ia superficie exterior del cuerpo (1 ), cubriendo Ia tercera ventana (11 ), incorporando dicha tapa unos medios de presión (14) unidos por un extremo a Ia parte interior de Ia tapa. - a cover (35) adapted to be hermetically fixed to the outer surface of the body (1), covering the third window (11), said cover incorporating pressure means (14) joined at one end to the inner part of the lid .
23. Dispositivo según Ia reivindicación 22 caracterizado porque comprende unos medios de retención para evitar el balanceo del casquillo (13).23. Device according to claim 22, characterized in that it comprises retention means to prevent the balance of the bushing (13).
24. Dispositivo de acuerdo con Ia reivindicación 19, caracterizado porque los medios de presión (14) comprenden una lengüeta solidaria a Ia superficie interior de Ia tapa (35) y unida a, o que presiona contra, Ia superficie exterior del casquillo (13).24. Device according to claim 19, characterized in that the pressure means (14) comprise a tongue integral with the inner surface of the cover (35) and attached to, or pressing against, the outer surface of the bushing (13) .
25. Dispositivo según Ia reivindicación 20, caracterizado porque incorpora adicionalmente unos elementos de contacto ubicados exteriormente al casquillo (13) y que sirven de contacto entre dicho casquillo (13) y las cuñas (16, 17).25. Device according to claim 20, characterized in that it additionally incorporates contact elements located externally to the bushing (13) and which serve as contact between said bushing (13) and the wedges (16, 17).
26. Dispositivo según Ia reivindicación 25, caracterizado porque los elementos de contacto son aros (26) de contacto.26. Device according to claim 25, characterized in that the contact elements are contact rings (26).
27. Dispositivo de acuerdo con Ia reivindicación 1 caracterizado porque: -el cuerpo (1 ) incorpora adicionalmente una cuarta ventana (36) en su parte inferior, que está conectada a un bloque (27) de soporte de Ia muestra que está adaptado para ser insertado en Ia cámara (4) de rayos27. Device according to claim 1 characterized in that: the body (1) additionally incorporates a fourth window (36) in its lower part, which is connected to a support block (27) of the sample that is adapted to be inserted in the ray chamber (4)
X; yX; Y
- está provisto de unos segundos medios de cierre hermético entre el cuerpo (1 ) y el bloque (27); y- it is provided with a second means of sealing between the body (1) and the block (27); Y
- el bloque (27) incorpora unos terceros medios de cierre hermético con respecto a las paredes de Ia cámara (4) de rayos X.- the block (27) incorporates a third means of sealing with respect to the walls of the X-ray chamber (4).
28. Dispositivo de acuerdo con Ia reivindicación 27 y caracterizado porque el bloque (27) incorpora medios de regulación de Ia posición de Ia muestra. 28. Device according to claim 27 and characterized in that the block (27) incorporates means for regulating the position of the sample.
29. Dispositivo de acuerdo con Ia reivindicación 27 y caracterizado porque los segundos medios de cierre hermético y los terceros medios de cierre hermético coinciden en un único elemento combinado de cierre hermético.29. Device according to claim 27 and characterized in that the second sealing means and the third sealing means coincide in a single combined sealing element.
30. Dispositivo de acuerdo con Ia reivindicación 29 y caracterizado porque el elemento combinado de cierre hermético comprende:30. Device according to claim 29 and characterized in that the combined sealing element comprises:
-una ranura perimetral en Ia superficie superior del bloque (27); y -una junta tórica que se aloja dentro de Ia ranura; y porque el cuerpo (1 ) encaja dentro de Ia ranura.-a perimeter groove in the upper surface of the block (27); and - an O-ring that is housed inside the groove; and because the body (1) fits inside the groove.
31. Dispositivo de acuerdo con Ia reivindicación 27 y caracterizado porque los segundos medios de cierre hermético consisten en una unión solidaria del cuerpo (1 ) con el bloque (27).31. Device according to claim 27 and characterized in that the second sealing means consist of a joint connection of the body (1) with the block (27).
32. Dispositivo de acuerdo con Ia reivindicación 31 y caracterizado porque el tipo de unión solidaria del cuerpo (1 ) con el bloque (27) se selecciona de Ia lista: soldadura, adhesivo, mecanización, magnética.32. Device according to claim 31 and characterized in that the type of joint connection of the body (1) with the block (27) is selected from the list: welding, adhesive, machining, magnetic.
33. Dispositivo de acuerdo con Ia reivindicación 27 y caracterizado porque los primeros medios de cierre hermético consisten en una tapa (35) que comprende: -un cilindro hueco; y -una junta tórica o plana en cada extremo del cilindro; de forma que dicha tapa (35) encaja en las aberturas cilindricas laterales de Ia cámara (4), sellando las juntas el espacio entre el cuerpo (1 ) y Ia tapa (35) por un lado, así como el espacio entre Ia pared de Ia cámara (4) y Ia tapa por el otro lado.33. Device according to claim 27 and characterized in that the first sealing means consist of a cover (35) comprising: a hollow cylinder; and - an o-ring or flat at each end of the cylinder; such that said cover (35) fits into the lateral cylindrical openings of the chamber (4), the joints sealing the space between the body (1) and the cover (35) on one side, as well as the space between the wall of The chamber (4) and the cover on the other side.
34. Dispositivo de acuerdo con Ia reivindicación 33 caracterizado porque Ia tapa (35) tiene aberturas en cada extremo que permiten acciones seleccionadas de una lista que comprende: Ia introducción de Ia muestra, el paso de los medios de control de atmósfera, o el paso de los medios de transmisión del movimiento de un motor que haga girar el portamuestras. 34. Device according to claim 33 characterized in that the lid (35) has openings at each end that allow actions selected from a list comprising: the introduction of the sample, the passage of the atmosphere control means, or the passage of the transmission means of the movement of an engine that rotates the sample holder.
PCT/ES2010/070224 2009-04-13 2010-04-12 Device for holding a sample inside an x-ray diffraction or dispersion chamber WO2010119156A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ES200930061A ES2378045B1 (en) 2009-04-13 2009-04-13 DEVICE FOR HOUSING A SAMPLE INSIDE A DISPERSION CHAMBER OR X-RAY DIFFACTION.
ESP200930061 2009-04-13

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WO2010119156A1 true WO2010119156A1 (en) 2010-10-21

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Citations (11)

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US5181233A (en) * 1991-11-08 1993-01-19 Florida State University Specimen holder
JPH09166529A (en) * 1995-12-15 1997-06-24 Rigaku Corp Sample container of x-ray device
WO2000023795A1 (en) * 1998-10-21 2000-04-27 Glaxo Group Limited Environmentally controllable sample holder for x-ray diffractometer (xrd)
JP2000230912A (en) * 1999-02-08 2000-08-22 Rigaku Industrial Co X-ray analysis sample holder and x-ray analyzer
EP1484602A2 (en) * 2003-05-16 2004-12-08 Forschungszentrum Karlsruhe GmbH Sample chamber with coupling and adjusting means for reproducibly coupling the sample chamber to a X-ray diffractometer
US20080175352A1 (en) * 2007-01-19 2008-07-24 Panalytical B.V. X-Ray Diffraction Equipment for X-Ray Scattering

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3378684A (en) * 1965-06-16 1968-04-16 Gen Electric Fluid sample cell with means to keep constant pressure on the sample fluid
US3973120A (en) * 1974-03-07 1976-08-03 U.S. Philips Corporation Specimen holder for an X-ray diffraction apparatus
US4583242A (en) * 1983-12-29 1986-04-15 Shell Oil Company Apparatus for positioning a sample in a computerized axial tomographic scanner
US4643033A (en) * 1985-09-20 1987-02-17 Chemplex Industries, Inc. Sample cup for use in X-ray spectroscopy
US4827761A (en) * 1987-06-25 1989-05-09 Shell Oil Company Sample holder
US5181233A (en) * 1991-11-08 1993-01-19 Florida State University Specimen holder
JPH09166529A (en) * 1995-12-15 1997-06-24 Rigaku Corp Sample container of x-ray device
WO2000023795A1 (en) * 1998-10-21 2000-04-27 Glaxo Group Limited Environmentally controllable sample holder for x-ray diffractometer (xrd)
JP2000230912A (en) * 1999-02-08 2000-08-22 Rigaku Industrial Co X-ray analysis sample holder and x-ray analyzer
EP1484602A2 (en) * 2003-05-16 2004-12-08 Forschungszentrum Karlsruhe GmbH Sample chamber with coupling and adjusting means for reproducibly coupling the sample chamber to a X-ray diffractometer
US20080175352A1 (en) * 2007-01-19 2008-07-24 Panalytical B.V. X-Ray Diffraction Equipment for X-Ray Scattering

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ES2378045B1 (en) 2013-02-15

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