CN102779558A - Soft X-ray shading film and preparation method thereof - Google Patents
Soft X-ray shading film and preparation method thereof Download PDFInfo
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- CN102779558A CN102779558A CN2012102895017A CN201210289501A CN102779558A CN 102779558 A CN102779558 A CN 102779558A CN 2012102895017 A CN2012102895017 A CN 2012102895017A CN 201210289501 A CN201210289501 A CN 201210289501A CN 102779558 A CN102779558 A CN 102779558A
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Abstract
The invention provides a soft X-ray shading film which comprises a high polymer material film, a support net and an aluminum layer, wherein the support net is arranged on the high polymer material film and the aluminum layer is coated on the surfaces of the high polymer material film and the support net. The aluminum film is coated on the soft X-ray shading film, thus only soft X-rays can transmit the soft X-ray shading film and other light rays are blocked; and the soft X-ray shading film has better mechanical property. The invention also provides a preparation method for the soft X-ray shading film.
Description
Technical field
The present invention relates to a kind of grenz ray photomask, particularly a kind of space exploration is with grenz ray photomask and preparation method thereof.
Background technology
Because domestic space exploration starts late, the researcher is less to the research of photomask, and at present domestic still do not have available space exploration and use the grenz ray photomask.And become during along with hard X-ray Modulation Telescope and X ray and the carrying out and propelling of project such as polarization explorer satellite (XTP) beforehand research, domestic demand to the grenz ray photomask is also more and more stronger.
It is the important component part of space X ray astrosurveillance that space grenz ray (0.1-10keV) is surveyed, and is the important means of research black hole, pulse magnitude celestial body character and differentiation.Yet most of high-resolution soft x-ray detector also can produce strong response to infrared, visible light and ultraviolet signal, thereby influence the energy resolution of detector when surveying grenz ray., ultraviolet infrared in order to eliminate and visible light be to the influence of grenz ray detectable signal, needs one can stop that infrared, ultraviolet and visible light can see through the photomask of grenz ray again.According to the electromagnetic theory of Zener, a lot of membraneous materials all have a band logical with respect to grenz ray, and this band is logical can to see through grenz ray, stops visible light and ultraviolet ray.The aluminium film is processed easily; Have transmitance preferably at the grenz ray wave band, simultaneously visible light and ultraviolet ray are had good interception, thereby become the first-selected functional material of preparation photomask; But the mechanical property of simple aluminium film is very poor, can not satisfy the space exploration demand.
Therefore, how to provide a kind of grenz ray photomask of aluminium coating film to become the technical matters that those skilled in the art are badly in need of solving.
Summary of the invention
To the problem that exists in the prior art, one object of the present invention is to provide a kind of grenz ray photomask, and this grenz ray photomask is coated with the aluminium film, can only stop other light through grenz ray, and have good mechanical property.
For realizing above-mentioned purpose; The present invention provides a kind of grenz ray photomask, comprises macromolecule material film, supporting network and aluminium lamination, wherein; Said supporting network is arranged on the said macromolecule material film, and said aluminium lamination is coated on said macromolecule material film and the supporting network surface.
According to design of the present invention, said macromolecule material film is a Kapton, and said supporting network is a nickel screen.
According to design of the present invention, said Kapton thickness is 500 nanometers, and said nickel screen thickness is below 500 microns, and said aluminum layer thickness is the 100-500 nanometer.
The beneficial effect of grenz ray photomask provided by the invention is that this grenz ray photomask is coated with the aluminium film; Have the aluminium film can only stop other light through grenz ray characteristic, reach the nickel screen support owing to the use polyimide is thin simultaneously and therefore also have the good mechanical performance.
Another object of the present invention is to provide a kind of method for preparing above-mentioned grenz ray photomask; This method directly will support the form of nickel screen through micro electronmechanical processing and be incorporated into polyimide surface; Avoided in the gummed mode residual glue to the influence of grenz ray transmitance, and the adhesion of nickel screen and polyimide is strong.The present invention has very strong practical value aspect the grenz ray space exploration.
For realizing above-mentioned purpose, the present invention provides a kind of method for preparing the grenz ray photomask, may further comprise the steps:
A. prepare Kapton;
B. utilize little electrocasting method on said Kapton, to prepare nickel screen;
B. having vapor deposition aluminium lamination on the Kapton of said nickel screen.
According to design of the present invention, the preparation Kapton may further comprise the steps:
A. utilize dianhydride and diamines in aprotic polar solvent, to prepare polyamic acid solution;
B., one substrate is provided, and the said polyamic acid solution of spin coating forms the polyamic acid film on said substrate;
C. be Kapton with the cyclisation of said polyamic acid film high temperature;
Wherein, said diamines comprises 4,4 '-diaminodiphenyl ether, p-phenylenediamine (PPD), 4, and 4 '-DADPS, and their analog, they can use separately or mix by arbitrary proportion and use; Dianhydride comprises pyromellitic acid dianhydride, 3, and 3 ', 4,4 '-biphenyl tetracarboxylic dianhydride, 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydride and their analog, they can use separately or mix use by arbitrary proportion; Said aprotic polar solvent comprises N, dinethylformamide, DMAC N,N, N-N-methyl-2-2-pyrrolidone N-etc.Said substrate comprises silicon chip, piezoid or glass sheet; The temperature of said high temperature cyclisation is 350-400 ℃, and the time is 4 hours.Before imidization, earlier sample was dried by the fire 20 minutes under 80 ℃ of conditions, to dry most of solvent.
According to design of the present invention, utilize little electrocasting method on said Kapton, to prepare nickel screen and may further comprise the steps:
D. coating thickness first photoresist layer on said Kapton, said first photoresist layer and said nickel screen pattern are complementary;
E. vapor deposition conductive seed layer on the said Kapton and the first photoresist layer surface;
F. remove said first photoresist layer and cover the lip-deep conductive seed layer of said first photoresist layer, said conductive seed layer is consistent with said nickel screen pattern;
G. on said Kapton and said conductive seed layer, apply second photoresist layer;
H. remove second photoresist layer on the conductive seed layer;
I. on exposed conductive seed layer, carry out little nickel screen electroforming, said nickel screen thickness is no more than second photoresist layer;
J. remove second residual on the said Kapton photoresist layer;
K. remove said substrate.
According to design of the present invention, said first photoresist layer comprises AZ4620, and thickness is the 3-10 micron; Said second photoresist layer comprises SU8-2000 series photoresist, the PMMA with the X source correspondence, KMPR and AZ50XT series photoresist; Thickness is below 500 microns, and said conductive seed layer comprises Cr/Cu, Cr/Au; Ti/Cu or Ti/Au, thickness are 50/50 nanometer.
According to design of the present invention, the technology of vapor deposition conductive seed layer comprises vacuum thermal evaporation, electron beam evaporation plating and magnetron sputtering etc. on the said Kapton and the first photoresist layer surface.
According to design of the present invention, when removing said first photoresist layer and covering the lip-deep conductive seed layer of said first photoresist layer employed glue-dispenser should with said first photoresist layer coupling, for example can be acetone etc.
According to design of the present invention, during second photoresist layer on removing conductive seed layer, utilizes the mask exposure imaging consistent with said nickel screen after, obtain conductive seed layer and come out, and the pattern that polyimide is protected by said second photoresist;
According to design of the present invention, be used Omnicoat when removing second residual on the said Kapton photoresist layer.
According to design of the present invention, be to put into the WS that is mixed with alcohol to boil and boil about 4 hours when removing said substrate.
According to design of the present invention, in the said i step, electroplate liquid is that nickel sulfamic acid is electroplated system; Wherein, and nickel sulfamic acid (500～600g/L), nickel chloride (5～15g/L); Boric acid (30～40g/L), pH value (3.5～4.5), cathode-current density (8～90A/dm
2).
According to design of the present invention, having two-sided vapor deposition aluminium lamination on the Kapton of said nickel screen, said aluminum layer thickness is the 100-500 nanometer.The mode of wherein, aluminizing can be used modes such as vacuum thermal evaporation, electron beam evaporation plating or magnetron sputtering.
The beneficial effect of preparation grenz ray photomask method provided by the invention: combine ultrathin membrane preparation technology, little galvanoplastics and technique for vacuum coating, accomplish the development of domestic space exploration first with the grenz ray photomask.Take directly in the technological breakthrough of polyimide surface electroformed nickel the limitation of traditional gummed mode in the concrete technology, ensured the homogeneity of grenz ray transmitance.Take in the isolation technics of polyimide film with the alcoholic WS mode of boiling of boiling, avoided since the reagent of back side corrosion usefulness to the destruction of polyimide film.
Description of drawings
Fig. 1 prepares the schematic flow sheet of grenz ray photomask method for the present invention;
Fig. 2 a to Fig. 2 i prepares the process schematic representation of grenz ray photomask method for the present invention;
Fig. 3 is the first sample product synoptic diagram of grenz ray photomask of the present invention;
Fig. 4 is the transmitance synoptic diagram of grenz ray photomask of the present invention at the grenz ray wave band;
Fig. 5 is the transmitance synoptic diagram of grenz ray photomask of the present invention to visible light and ultraviolet light.
The critical piece symbol description
201 substrates; 202 Kaptons;
203 first photoresist layers; 204 conductive seed layers;
205 second photoresist layers; 206 nickel screens;
207 aluminium films.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described further.Thought of the present invention be by spin coating proceeding, micromachined and the preparation of various film-forming process be applied to space flight can block visible light and ultraviolet ray and see through the photomask of grenz ray.But the present invention is not limited to following embodiment.
Embodiment:
At first take by weighing 0.27035g p-phenylenediamine (PPD) (PPD, brand: ACROS) join in the three-necked bottle, add 20ml N then; N-dimethyl acetamide (DMAc, brand: ACROS), be stirred to dissolving fully; Add 0.73898g 3,3 ' again, 4; 4 '-(BPDA, brand: TCI), the mol ratio that makes BPDA and PPD is 1.005: 1 to bibenzene tetracarboxylic dianhydride.React and obtained the DMAc solution that solid content is 5.11% polyamic acid (PAA) in 6 hours; Utilize DMAc with the lean solution of solution dilution to apparent viscosity for 428CP; (production firm: Luoyang MCL Electronic Materials, Ltd.) surface was with the rotating speed low speed spin coating of 500rpm 10 seconds at 4 inches silicon chips 201 to utilize MSC-400B-6N type high precision spin coating appearance that LAURELL company produces; Rotating speed spin coating with 1000rpm obtained polyamide acid film after 20 seconds again, and most of solvent was removed in baking in 20 minutes under 80 ℃ of conditions, and the high temperature cyclisation is 4 hours under 350 ℃, the condition of nitrogen protection; Obtaining thickness is the polyimide film 202 of 500nm, shown in Fig. 2 a.Wherein, diamines also can comprise 4,4 '-diaminodiphenyl ether, 4, and 4 '-DADPS, and their analog, they can use separately or mix by arbitrary proportion and use; Dianhydride also can comprise pyromellitic acid dianhydride, 3, and 3 ', 4,4 '-benzophenone tetracarboxylic dianhydride and their analog, they can use separately or mix use by arbitrary proportion; Aprotic polar solvent also can comprise N, dinethylformamide, N-N-methyl-2-2-pyrrolidone N-etc.Substrate also can comprise piezoid or glass sheet, the invention is not restricted to this.
Utilize above-mentioned spin coating appearance that the AZ4620 type photoresist that U.S. An Zhi company produces is spun on polyimide film 202 surfaces; Utilize hot platform under 95 ℃ of conditions, to toast 5min; Obtain the photoresist film that thickness is approximately 10 microns; Remove the solvent in the photoresist; Utilize the MJB4 type photo-etching machine exposal 40 seconds that German Hughes Electronics produces, utilize the dilution (volume ratio of AZ400K and water: 1:3) at room temperature soak to develop after 3 minutes and obtain first photoresist layer 203 with the complementation of nickel screen 206 patterns, shown in Fig. 2 b of the AZ400K type developer solution that An Zhi company provides.
Shown in Fig. 2 c, on first photoresist layer 203 and polyimide film 202 surfaces of coming out, the ACS-4000-C4 type magnetic control sputtering device that utilizes Japanese ULVAC company to produce; Adopt the working method of radio frequency, the working vacuum degree is 5.0E-4, and temperature is a room temperature; The airshed of argon gas is 25ccm, utilizes 1140 second time earlier, and output power is 150W; Sputter one layer thickness is approximately the Cr layer of 50nm, utilizes 833 seconds time then, and output power is 50W; Sputter one layer thickness is approximately the Au layer of 50nm, and then makes the Cr/Au layer.Conductive seed layer also can be Cr/Cu, Ti/Cu or Ti/Au, and the method for plating conductive seed layer also can comprise vacuum thermal evaporation or electron beam evaporation plating etc., the invention is not restricted to this.
Shown in Fig. 2 d, whole sample is put into the glue-dispenser pure acetone soak, be aided with ultrasonic about 5 minutes, the Cr/Au layer on first photoresist layer 203 and surface thereof is removed, obtain the consistent Cr/Au conductive seed layer 204 of pattern and nickel screen 206.
Shown in Fig. 2 e; Utilize above-mentioned spin coating appearance that the SU8-2150 type photoresist that U.S. Microchem company produces is spun on polyimide film 202 surfaces, utilize hot platform under 95 ℃ of conditions, to toast 2 hours, remove the solvent in the SU8-2150 type photoresist; Obtain second photoresist layer 205 that thickness is approximately 500 microns; The MJB4 type litho machine engage sleeves lithography that utilizes German Hughes Electronics to produce makes reticle pattern accurately align with conductive seed layer 204 patterns, makes public then 30 seconds; Sample is placed on the hot platform baking 2 hours; After the Developer type developer solution that utilizes Microchem company to provide at room temperature soaks and develops after 10 minutes second photoresist layer 205 of conductive seed layer top is removed, conductive seed layer 204 is come out, for next step little electroforming is got ready.Second photoresist layer also can be PMMA, KMPR and AZ50XT series photoresist, the invention is not restricted to this.
Shown in Fig. 2 f; The SMD-30 bidirectional pulse electroplating power supply that utilizes the big Shun in Handan to produce carries out little electroforming to sample; Wherein the prescription of nickel plating solution and condition are: nickel sulfamic acid (500～600g/L), and nickel chloride (5～15g/L), boric acid (30～40g/L); PH value (3.5～4.5), cathode-current density (8～90A/dm2).The dutycycle of the forward current of electroplating process is 30%, and the dutycycle of inverse current is 10%, and forward and reverse peak current density all is 35A/dm2.Electroforming obtains the nickel screen 206 that thickness is approximately 400 microns after 60 hours; In order to guarantee the live width of nickel screen 206; Its thickness should not surpass the thickness of second photoresist layer 205; If surpass the thickness of second photoresist layer 205, cross growth will take place in nickel screen electroforming 206, and the live width that causes nickel screen 206 is greater than the actual design live width.
Shown in Fig. 2 g, second photoresist layer 205 (also being SU8-2150 type photoresist) is removed.For the convenience of removing photoresist; Often cooperate the Omnicoat that produces by U.S. Microchem company to use; Its method of application is before being coated with SU8-2150 type photoresist, is coated with one deck Omnicoat earlier, utilizes oxygen plasma to remove Omnicoat behind the SU8-2150 type photoresist developing; Wherein the power of oxygen plasma is 200W; Bombardment time is 120 seconds, and the mixed solution (ethyl acetate and acetone respectively account for 50%) with ethyl acetate and acetone when removing photoresist can dissolve Omnicoat, and SU8-2150 type photoresist is able to remove.
Shown in Fig. 2 h, in mass ratio is 20% alcohol water blend, boil and boil about 4 hours, silicon chip 201 is removed, obtain polyimide film 202 with nickel screen 206.
Shown in Fig. 2 i, the ACS-4000-C4 type magnetic control sputtering device that utilizes Japanese ULVAC company to produce adopts the working method of radio frequency; The working vacuum degree is 5.0E-4; Temperature is a room temperature, and the airshed of argon gas is 25ccm, utilizes 1800 second time earlier; Output power is 150W, and sputter one layer thickness is approximately the aluminium film 207 of 100nm.The method of aluminizing also can comprise vacuum thermal evaporation or electron beam evaporation plating etc., the invention is not restricted to this.
Grenz ray photomask according to method for preparing is as shown in Figure 3.Fig. 4 and Fig. 5 are respectively the transmitance synoptic diagram of grenz ray photomask sample to grenz ray and visible light.By finding out among Fig. 4 and Fig. 5, at the grenz ray wave band, most grenz ray has seen through the grenz ray photomask of preparation, and at visible light wave range, its transmitance is almost nil.Thereby verified that X ray photomask provided by the invention and preparation method thereof reaches the effect that only sees through grenz ray and stop other light.
Above-described; Be merely preferred embodiment of the present invention; Be not in order to limiting scope of the present invention, promptly every simple, equivalence of doing according to the claims and the description of application of the present invention changes and modifies, and all falls into the claim protection domain of patent of the present invention.
Claims (17)
1. a grenz ray photomask is characterized in that, comprises macromolecule material film, supporting network and aluminium lamination, and wherein, said supporting network is arranged on the said macromolecule material film, and said aluminium lamination is coated on said macromolecule material film and the supporting network surface.
2. grenz ray photomask as claimed in claim 1 is characterized in that, said macromolecule material film is a Kapton, and said supporting network is a nickel screen.
3. grenz ray photomask as claimed in claim 2 is characterized in that, said Kapton thickness is 500 nanometers, and said nickel screen thickness is below 500 microns, and said aluminum layer thickness is the 100-500 nanometer.
4. a method for preparing like the described grenz ray photomask of claim 1 to 3 is characterized in that, may further comprise the steps:
A. prepare Kapton;
B. utilize little electrocasting method on said Kapton, to prepare nickel screen;
C. having vapor deposition aluminium lamination on the Kapton of said nickel screen.
5. method as claimed in claim 4 is characterized in that, the preparation Kapton may further comprise the steps:
A. utilize dianhydride and diamines in aprotic polar solvent, to prepare polyamic acid solution;
B., one substrate is provided, and the said polyamic acid solution of spin coating forms the polyamic acid film on said substrate;
C. be Kapton with the cyclisation of said polyamic acid film high temperature;
Wherein, said diamines comprises 4,4 '-diaminodiphenyl ether, p-phenylenediamine (PPD), 4, a kind of in 4 '-DADPS and composition thereof; Dianhydride comprises pyromellitic acid dianhydride, 3, and 3 ', 4,4 '-biphenyl tetracarboxylic dianhydride, 3,3 ', 4, a kind of in 4 '-benzophenone tetracarboxylic dianhydride and the potpourri; Said aprotic polar solvent comprises N, dinethylformamide, DMAC N,N or N-N-methyl-2-2-pyrrolidone N-; Said substrate comprises silicon chip, piezoid or glass sheet; The temperature of said high temperature cyclisation is 350-400 ℃, and the time is 4 hours.
6. method as claimed in claim 5 is characterized in that, before the cyclisation of said polyamic acid film high temperature is Kapton, under 80 ℃ of conditions, dries by the fire 20 minutes earlier, to dry most of solvent.
7. method as claimed in claim 6 is characterized in that, utilizes little electrocasting method on said Kapton, to prepare nickel screen and may further comprise the steps:
D. coating thickness first photoresist layer on said Kapton, said first photoresist layer and said nickel screen pattern are complementary;
E. on the said Kapton and the first photoresist layer surface, plate conductive seed layer;
F. remove said first photoresist layer and cover the lip-deep conductive seed layer of said first photoresist layer, said conductive seed layer is consistent with said nickel screen pattern;
G. on said Kapton and said conductive seed layer, apply second photoresist layer;
H. remove second photoresist layer on the conductive seed layer;
I. on exposed conductive seed layer, carry out little nickel screen electroforming, said nickel screen thickness is no more than second photoresist layer;
J. remove second residual on the said Kapton photoresist layer;
K. remove said substrate.
8. method as claimed in claim 7 is characterized in that, said first photoresist layer comprises AZ4620; Thickness is the 3-10 micron; Said second photoresist layer comprises SU8-2000 series photoresist, the PMMA with the X source correspondence, KMPR and AZ50XT series photoresist, and thickness is below 500 microns, and said conductive seed layer comprises Cr/Cu; Cr/Au, Ti/Cu or Ti/Au.
9. method as claimed in claim 7 is characterized in that the technology of said e step comprises vacuum thermal evaporation, electron beam evaporation plating and magnetically controlled sputter method.
10. method as claimed in claim 7 is characterized in that, in said f step, uses glue-dispenser, and said glue-dispenser and said first photoresist layer are complementary.
11. method as claimed in claim 10 is characterized in that, said glue-dispenser is an acetone.
12. method as claimed in claim 7 is characterized in that, in said h step, utilize the mask exposure imaging consistent with said nickel screen after, make said conductive seed layer come out.
13. method as claimed in claim 7 is characterized in that, in said j step, cooperates Omnicoat to use.
14. method as claimed in claim 7 is characterized in that, said k step is to put into the WS that is mixed with alcohol to boil and boil about 4 hours.
15. method as claimed in claim 7 is characterized in that, in the said i step; Electroplate liquid is that nickel sulfamic acid is electroplated system, wherein, and nickel sulfamic acid (500～600g/L); Nickel chloride (5～15g/L); Boric acid (30～40g/L), pH value (3.5～4.5), cathode-current density (8～90A/dm
2).
16. method as claimed in claim 7 is characterized in that, is having two-sided aluminium coated on the Kapton of said nickel screen, said aluminum layer thickness is the 100-500 nanometer.
17. method as claimed in claim 16 is characterized in that, said mode of aluminizing comprises vacuum thermal evaporation, electron beam evaporation plating or magnetically controlled sputter method.
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| CN105259733A (en) * | 2015-10-30 | 2016-01-20 | 上海交通大学 | Preparation method for flexible mask plate used for patterning curved surface |
| CN107024489A (en) * | 2017-04-20 | 2017-08-08 | 中国科学院高能物理研究所 | Grenz ray filter coating |
| CN111933327A (en) * | 2020-07-26 | 2020-11-13 | 同济大学 | Metal film filter disc with supporting structure and preparation thereof |
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| CN111933327A (en) * | 2020-07-26 | 2020-11-13 | 同济大学 | Metal film filter disc with supporting structure and preparation thereof |
| CN111933327B (en) * | 2020-07-26 | 2022-10-25 | 同济大学 | Metal film filter disc with supporting structure and preparation thereof |
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| Publication number | Publication date |
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| CN102779558B (en) | 2015-09-30 |
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