CA1303472C

CA1303472C - Pressure-sensitive adhesive closure for disposable diaper

Info

Publication number: CA1303472C
Application number: CA 581717
Authority: CA
Inventors: Alan J. Sipinen; Theresa L. Carpenter; Stephen W. Bany
Original assignee: Minnesota Mining and Manufacturing Co
Current assignee: 3M Co
Priority date: 1987-11-06
Filing date: 1988-10-31
Publication date: 1992-06-16
Anticipated expiration: 2009-06-16
Also published as: ES2045057T3; IL87983A0; EP0316601A2; EP0316601B1; DE3883162D1; BR8805738A; IE63072B1; JPH01162804A; ZA887698B; DE3883162T2; AU2379988A; KR0125278B1; IL87983A; JP2831007B2; EP0316601A3; AU613096B2; US5342339A; US4861635A; KR890008282A; IE883071L

Abstract

Pressure-Sensitive Adhesive Closure for Disposable Diaper Abstract A pressure-sensitive adhesive closure for a disposable diaper can exhibit high peel resistance both at low and high speeds while its peelability at high speeds is not excessively shocky when it employs a pressure-sensitive adhesive of a certain rheology and it has, covering the fastening area, a polyolefin layer having microtopographical features as in Figs. 1-6 of the drawing. As seen in Figs. 1-6, suitable microtopographical features are provided by a large number of closely spaced asperities at least two micrometers in height that have a jagged appearance at 500x. A pressure-sensitive adhesive of suitable rheology can be provided by a blend of an AB block copolymer, such as a copolymer of styrene and either isoprene or butadiene, and tackifying resin, preferably a mixture of liquid and solid tackifying resins.

Description

~3I~39L~2 Descriptio_ PRESSURE--SENSITIVE ADHESIVE: CLOSURE
FOR DISPOS~LE DIAPER

Te~hnical Field -The invention concerns disposable garments such as diapers for infants and for incontinent adults, more specifically a pressure-sensitive adhesive closure that can be peeled open and reclosed. The invention particularly concerns improvements in the closure.

Background Art Many disposable diapers have a reinforced fastening area (sometimes called a "target area") to which a pressure-sensitive adhesive fastening tape (sometimes called a "closure tab") is pressed and adhered to fasten the diaper around an infant or other person wearing the diaper. Whether or not the fastening area is reinforced, the fasten,ing tape should remain securely in place while the diaper is being worn and should be cleanly peelable from the fastening area and capable of being securely reattached. Although forces which may cause the fastening tape to become loose during use of the diaper generally occur at low speeds, e.g., up t:o about 30 cm/min., a person who readjusts or removes a diaper may judge the closure to be of poor quality if the fastening tape peels off too easily or in an excessively shocky manner when removed quickly, e.g., at about 500 to 1250 cm/min. we are not aware of any report in the prior art of a pressure sensitive adhesive closure for a diaper that would provide high peel resistance both at low and high speeds without being excessively shocky at high speeds, nor do we believe that any such diaper closure has been s~ld or offered for sale.
U.S. Patent No. 4,376,147 (Byrne et al.) concerns an embossed thermoplastic polyoleEin film which has a matte ~3~,34~

finish that "is extremely low in gloss even on both sides and tape adhesion values are achieved which render the film particularly useful for fabrication into ... disposable diapers where such adhesion values are needed" (col. 2, lines 54-59). The adhesive which provides "such adhesion values" is not disclosed, and the only adhesion values given are at col. 5, line 38 without indicating their significance.
U.S. Patent No. 4,546,029 (Cancio et al.), like the Byrne patent, concerns an embossed thermoplastic polyolefin film simulating a matte or dull finish, but its embossing is asymmetric as opposed to the symmetry of the ~yrne embossing, thus providing "a totally different visual appearance" (col. 3, lines 9-10). Unlike the 8yrne patent, the Cancio patent explains the reported tape adhesion values. Its Table (col. 7) gives such values for the asymmetrically embossed film, showing improvement versus the Byrne film, but as in the Byrne patent, there is no disclosure of the adhesive tape used in making those 20 measurements.
U.S; Patent No. 4,436,520 (Lipko et al.) says that the exposed surface of a film used as a diaper back sheet typically is embossed to reduce gloss, but that "the embossing materially reduces the adhesion of the embossed surface for the closure tabs so that the diaper is no longer secure in its use on the infant" (col. 1, lines 19 22). The Lipko patent concerns the discovery "in embossed films of polyethylene having a (45) gloss of no greater than 8, the adhesion of the embossed surface is markedly enhanced when said surface has a mean value of maximum profile height of less than 150 and maximum peak to valley height of less than 230" (col. 1, lines 35-40). The profile measurements are made with a "Surtronic" 3 apparatus sold by Taylor-Hobson. The adhesive tape used for making the reported tape adhesion values is not disclosed~

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U.S. Patent No. 4,237,889 (Gobran) concerns an improved closure tab or fastening tape for a disposable diaper. The improvement is in the tape backing which is a substantially untensilized crystalline polypropylene or linear polyethylene foil having one smooth face and one textured face.
European Patent Application 82110676.4 (Raphael et al.), published Allgust 6, 1983, concerns a diaper having an impermeable outer sheet which has been calendered to provide a matte appearance. This is reinforced at the fastening area with an impermeable sheet which may be polypropylene that is perfectly smooth as opposed to the matte surface of the underlying sheet. The smoothness is said to improve adhesion by the fastening tape.
German Patent Application P 33 38 201.8 (Widlund), laid open April 26, 1984, indicates that a disposable diaper typically has an outer polyethylene layer to which a pressure-sensitive adhesive fastening tape will not adhere well because the ~urface of the polyethylene layer is not sufficiently smooth. This problem is avoided by applying to the fastening area of the diaper one or several plastic strips which are selected to provide good adhesion by the fastening tape and preferably are smooth and flat.

Disclosure of Invention The invention provides for the first time a pressure-sensitive adhesive closure for a disposable article such as a diaper that affords high peel resistance at both low and high speeds while being smoothly peelable at high speeds. By "high peel resistance" is meant that the closure has a "Mean Peel Force" as described below of at least 175 Njm. ~y "low speed" is meant 12 inches (30 cm) per minute, and bv "high speed" is meant at least 500 inches (1250 cm) per minute. Extensive testing indicates that the peelability of a pressure-sensitive adhesive closure is not excessively shocky at high speeds whenever 3 3~, 3L~ Z

its Mean Peel Force at 1250 cm/min. is at least 80~ of its Mean Peel Force at 30 cm/min. At less than 80%, excessively "shocky" peel has been encountered.
Preferably, the instantaneous peel force at 1250 cm/min.
stays substantially within 20~ of the Mean Peel Force. The pressure-sensitive adhesive should afford good resistance to shear, i.e., a Shear Adhesion Value (as described below) of at least 150 minutes. Furthermore, in order to permit the pressure-sensitive adhesive fastening tape to be shipped in commerce, the adhesive should not ooze from long rolls ~e.g., lengths of about 500 m or more), and it should be possible to unwind the rolls without offsetting of adhesive after long and possibly adverse storage conditions.
This desirable combination of properties is preerably achieved by both a) using a certain class of pressure-sensitive adhesives in the fastening tape and b) employing at the fastening area a polyolefin layer having certain microtopographical features. More specifically, the pressure-sensitive adhesive of the fastening tape comprises a blend of 13 an ~B block copolymer wherein A comprises vinylarene, B comprises a polymer of at least one monomer selected from conjugated dienes and alkenes, and A comprises from 8 to 50 weight percent of th~ block copolymer, and 2~
tackifying resin (preferably a blend of liquid and solid tackifying resins), the AB copolymer comprising from 20 to 60 weight percent of total AB copolymer plus tackifier and the B phase of the blend having a composite Tg of from 250 to 275K, and the surface of the polyolefin layer at the fastening area has a large number of closely spaced asperities that have a jagged appearance when viewed at a magnification of about 500X and are at least two micrometers in height.

~3~39L~2 By "jagged'l is meant a sharply uneven surface. As much as half of the total area of the surface of the polyolefin at the faskening area can have a smooth or rounded appearance at SOOX.
According to a further aspect of the present invention there is provided pressure-sensitive adhesive closura for a disposable garment comprising a pressure-sensitive adhesive fastening tape, the adhesive of which comprises a blend of 1) an ABA block copolymer wherein A
comprises vinylarene, B is selected from homopolymers of lsoprene and butadiene and copolymers of ethylene and butylene, and A
comprises from 10 tc 40 weigh~ percent of the block copolymer, and 2) tackifying resin, the AB copolymer comprising from 25 to 50 weight percent of total AB copolymer plus tackifier and the B
phase of the blend having a composite Tg of from 250 and 275K, and a polyolefin layer which forms the fasteniny area of the garment, the fastening surface of which has a large number of closely spaced asperities at least two micrometers in height that have a jagged appearance when viewed at 500X and are present over at least one-half the ~astening surfac~, said closure ~ffording a Mean Peel Force of at least 175 Nim both at 30 and 1250 cm/min.
while its Mean Peal Force at 1250 cm/min. is at least 80% of it~
Mean Peel Force at 30 cm/min.
According to another aspect of the present lnvention there ls provided pressure-sensitive adhesive closure for a dlsposable diaper comprising a pressure-sens.itive adhesive ~astening tape and a polyolefin polymer covering the fastening area, whereln the improvement comprises ~3~ 7Z
5a 60557-3s07 the pressure-sensitive adhesive of the fastening ~ape comprises a blend of 13 an ABA block copolymer wherein A comprises styrene, B comprlses a~ least one monomer selected from isoprene and butadiene, and A comprises from 8 to 35 weight percent of the block copolymer, and 2) tackifler, the ABA copolymer coinprising from 20 to 60 weight percent of total ABA copolymer plus tackifier and the B or midblock phase of the blend haviny a composite Tg of from 258 to 267K, and the surface of the polyolefin polymer at the fastening area has Ra of from 0.5 to 6~m Sm of from 50 to 200~m Lo of from 1.01 to 1.15 S of from 60 to 400~cm as measured by a "Perthometer" pro~ilometer.

d ~5 ~M~o~ aL~I~n~9~5_Th~ y~ n For a full evaluation of the nature of the asperities, the fastening ar~a should also be examined at lesser and greater magnifications, e.g~, at lOOX and 1500X. Examination at lOOX
should ind1cate ~hether the area at SOOX is truly representative, and examination at 1500~ can better reveal the true nature of ind~vidual asperities.
In an intensive effort to ascertaln whether microtopographical measurements could be made of polyolefin surfaces to show which of those surfaces would be useful in ~he ?`

~3~ i72 5b 60557-3507 presen~ invention and whlch woulcl not, various instruments have been usad. One sucl- instrumen~ ls the "Surtronic" 3 pro~ilometer mentioned above in the discussion of the Lipko patent. Another is the "Perthometer'` profilometer made by Perthen GmbH of Go~tingen, West Germany~ which is a more sophisticated instrument than the "Surtronic" 3 and, accordingly, provides measurements which have been ~ound to be more meaningful than those obtained with the "Surtronic" 3~ Optical microtopographical measurements have also been made, as well as gloss readings. ~owever, no combination of microtopographical measurements has heen found which can provide a reliable prediction as to whether a new polyolefin surface would or would not provide the objectives oi the invention. In contrast, photomicrographs o~ the polyolefin surfaces permlt one skilled in the art to predict with reasonable confidence which surfaces will afford to ~he pressure-sensitive adhesive closure high peel resistance both at low and high speeds while not encountering excessively shocky peel at high speeds. The photomicrographs also permit reasonably ,~ .. ..

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reliable prediction of when a polyolefin surface might be so rough that the peel resistance might be 50 high that it might be overly difficult for some users to peel back the adhesive closure.
of microtopographical measurements that have been made, those obtained using the "Perthometer"
profilometer, when equipped with a stylus 5 ~m in radius, have proven to be the most meaningful. Measurements with this instrument indicate that the surface of the polyolefin layer at the fastening area should have Ra of from 0.5 to 6 ~m Sm of from 50 to 200 ~m Lo of rom 1.01 to 1.15 S of from 60 to 400/cm wherein Ra ~ arithmetical mean deviation of the profile Sm ~ mean spacing of the profile irregularities Lo - relative length of the profile S - no. of peaks per cm that exceed 0.1 ~m in height.
Polyolefin surfaces which satisfy each of these microtopographical measurements do not necessarily afford smooth peelability at high speeds when the above described class of pressure-sensitive adhesive tapes is used for the fastening tape.
~he AB block copolymer of the pressure-sensitive adhesive closure of the invention can have any of a variety of configurations including linear triblock, star, radial, branched, and tapered geometries. The A block is ri~id at the service temperature and preferably is styrene or alpha-methylstyrene. The B block is flexible at the service temperature and preferably is either a homopolymer of isoprene or butadiene or a copolymer of ethylene and butylene. The rigid A block usually is present in the range of 8~ to 30~ by weight of the total block copolymer when the B block is isoprene-based and 20~ to 50% by weight when the ~ block is butadiene-based.

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Preferred AB block copolymers include A~A linear triblock copolymers of styrene and isoprene ranging from 10~ to about 21~ styrene by weight such as those commercially available from Shell Chemical Company as "~raton" 1107 and 1111 or fro~ Nippon-Zeon as "Quintac"
3420r 3430~ and 3530~ AlSo preferred are ABA block copolymers of styrene and butadiene ranging from 25% to 40% styrene by weight such as those commercially available from Firestone Synthetic Latex and Rubber Company as 10 "Stereon" 840A and 845Ao The Tg of the B phase of the blend of AB block copolymer and tackifying resin is calculated from the Fox Equation usin~ the Tg of each component, namely, the Tg of the B block of the block copolymer and the Tg of each tackifying resin in the blend. The Fox equation is 1/composite Tg = ~ Wi/Tgi wherein Wi is the weight fraction of each component i and Tgi is the glass transition temperature of each component io To enhance the attainment of a composite Tg within the aPorementloned range, it is desirable to employ both a liquid and a solid tackifier, even though this can be accomplished with a single semisolid tackifier.
As has been pointed out, the B phase of the blend of AB copolymer and tackifying resin should have a composite Tg between 250 and 275K, preferably from 258 to 267K. When the AB block copolymer is a styrene-isoprene-styrene triblock copolymer, the preferred range o~ composite ~g is indicated by Fig. 19 of the drawing as discussed below.
In preferred pressure-sensitive adhesive closures of the invention, the proportion by weight of the AB block copolymer is from 25 to 50%, more preferably from 30 to 40%; of solid tackifying resin is from 20 to 60%, more preferably from 30 to 50%; and of liquid tackifying resin is from 5 to 45%~ more preferably from 10 to 30~.

3~! 3 -a-Useful solid tackifying resins belong to severalof the commercially important resin classes including rosin esters; hydrogenated rosin esters; polyterpene resins; polymerized hydrocarbon resins based on piperylene, isoprene, and other conjugated dienes containing 4 to 6 carbon atoms as well as hydrogenated versions of these materials; resins from polymeriæed and hydrogenated C9 hydrocarbon streams; resins from polymerized and hydrogenated cyclic dienes such as cyclopentadiene; resins from polymerized and hydrogenated pure monomer species such as styrene, vinyl toluene, alphamethyl styrene. Preferred solid tackifying resins include a hydrocarbon resin consisting essentially of polymerized structures derived primarily from a stream of aliphatic petroleum derivatives, both dienes and mono-olefins, containing 4 to 6 carbon atoms. Piperylene and isoprene are the most common species. Such resins are commercially available from Exxon Chemical Company as "Escorez" 1310 and from the Goodyear Chemical Company as "Wingtack Plus" and "Wingtack" 95. Other preferred solid tackifying resins include predominantly cyclopentadiene species that have been polymerized and hydrogenated. Such solid tacki~ying resins are available from Exxon Chemical Company as "Escorez" 5380, "Escorez" 5300, and "Escorez"
5320. A preferred solid tackiying resin is produced from the polymerization and hydrogenation of a pure monomer feedstock comprising styrene, vinyl toluene, and alpha-methylstyrene, such as "Regalrez" 1094, '~Regalrez" 1126 and "Regalrez" 6108 resins a~ailable from Hercules Chemical Company. An additional preferrsd hydrogenated hydrocarbon solid resin is Arkon P-90 available from Arakawa Chemical, USA. Another preferred solid tackifying resin is a partially hydrogenated rosin ester, such as "Permalyn" 1105 available from Hercules Chemical Company.
~n additional pre~erred rosin ester is "Permalyn" 305N. A
preferred solid tackifying resin for styrene/butadiene block copolymers is a polymerized alpha-pinene resin ~3~
g having a softening point of about 100~ C available from Arizona Chemical Company as "Zonarez" A-100. A second preEerred solid tackifying resin for styrene/butadiene block copolymers is a styrenated terpene type resin available as "wingtack" ~6.
Useful liquid tackifying resins include liquid hydrocarbo~ resins and hydrogenated hydrocarbon resins, liquid polystyrenes, liquid rosin esters, liquid polyterpenes, liquid resins from polymerized and hydrogenated C9 hydrocarbon streams; liquid resins from polymerization and hydrogenation of a cyclic diene such as dicyclopentadiene; liquid resins from polymerized and hydrogenated pure monomer species such as styrene, vinyl toluene, alphamethyl styrene; oils such as naphthenic oils and parafinic oils. Preferred liquid tackifying resins include a liquid hydrocarbon resin consisting essentially of polymerized structures derived primarily from a stream of aliphatic petroleum derivatives, both dienes and mono-olefins, containing 4 to 6 carbon atoms. One such resin is "Wingtack" 10. Another class of liquid tackifying resins can be produced from mixtures of aliphatic and aromatic monomers as exemplified by "Escoreæ" 2520. Such resins may be further hydrogenated.
Another preferred liquid tackifying resin comprises predominantly cyclic dienes that have been polymerized and hydrogenated, e.g., ECR-327 from Exxon Chemical Co.
Another preferred liquid tackifying resin is produced from the polymerization and hydrogenation of a pure monomer feedstock comprising styrene, vinyl toluene, and alphamethyl styrene, such as "Regalrez" 1018. Another preferred liquid tackifying resin is a polymerized alpha-pinene resin having a softening point around 25C
available as "Zonarez" A-25. "Zonarez" A-25 is especially preferred for formulations containing styrene/butadiene block copolymers.
Semisolid tackifying resins suitable for use in this invention include a resin produced from the ~L3~
- 1 o -polymerization and hydrogenation of a pure monomer feedstock comprising styrene, vinyl toluene, and alpha-methylstyrene, e.g., "Regalrez" 1065. Another preferred semisolid tackifying resin is a rosin ester available form Hercules as "Foral" 65.
Conventional additives and fillers may be used in the pressure-sensitive adhesive formulations, including antioxidants such as 2,5-di(tertiary amyl)hydroquinone and t-butylcresol, heat stabilizers such as zinc alkyl , dithiocarbamates, ultraviolet stabilizers, pigments, and coloring agents such as zinc oxide, titanium dioxide, carbon black, clay, and calcium carbonate.
Twenty-six pressure sensitive adhesive tapes which have been tested for use in the invention are described below. Two of these, Tapes E and Y, did not exhibit acceptable Shear Adhesion Values although they did exhibit usefully high peel resistance at both low and high speeds. Three others, Tapes F, M, and Z, did not exhibit an acceptably smooth peel at high speeds, although they did exhibit acceptable Shear Adhesion Values. A11 of the other tapes satisfy the re~uirements for use in pressure-sensitive adhesive closures of this invention.

Press~r~ nsitive Adhesive Tape C
A 4-mil (0.1 mm) polypropylene film with a matte surface on both sides was knife-coated with a solution of a pressure-sensitive adhesive. The adhesive solution comprised 35 parts of a styrene-isoprene-styrene (AsA) block copolymer ("Kraton" 1107 from Shell Chemical Co.), 49 parts of a solid hydrocarbon tackifying resin ("Wingtack Plus"), 15 parts of a liquid hydrocarbon tackifying resin ("Wingtack" 10), and 1 parS of an antioxidant t"Irganox" 1076 from Ciba Geigy Co.). The solution was 50~ solids in 4:1 toluene:heptane. The coating was dried at 70C for 5 minutes to result in an adhesive coating weight of 35 g/m2.

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Pressure-sensitive Adhesive Tapes A; s, D-U and Z
Each of Pressure-sensitive Adhesive Tapes A, B, D-U and Z was prepared in the same manner as was Pressure-sensitive Adhesive Tape A except as indicated in Table I.

Pressure-sensitive Adhesive Tape V-Y
Each of Pressure-sensitive Adhesive Tapes V-Y
were prepared by hot melt coating the adhesive onto a 4-~il (0.1 mm) polypropylene film with a matte sur~ace on both sides. This coating was achieved using typical co-rotating twin screw extrusion equipment, speeifically, a Werner Pfleiderer model number ZSK-30, as available from Werner P1eiderer Company, Ramsey, New Jersey. The block copolymer was fed at the back of the barrel, and the premelted tackifying resins were introduced into the barrel via injection ports along the length of the barrel.
~he temperature of the molten adhesive was about 310F
(155C) as it exited the coating die.

Test_ ~
To evaluate the performance of pressure-sensitive adhesive closures, the following tests were made:

Mean Peel Force -"Mean Peel Force" was tested using a MTS Model 810 high speed tensile tester in accordance with ~STM
D1876 - 76 except as follows. EAch pressure-sensitive adhesive tape sample was one inch (2.54 cm) by 8 inches (20.32 cm), and was laminated by its adhesive layer to the face of a test sample of polyolefin film [2.S inches (6.35 cm) by 8 inches ~20.32 cm)] using two passes of a 4.5-pound (2.04 kg) mechanical roller (at 30 cm/min.) conformin~ to Federal Standard 147. The whole was then inserted into the jaws of the tensile tester along with a steel panel 12 inches (5.08 cm) by~5 inches ~12.7 cm) and ~3i~

0.0~25 inch (0.159 cm) in thickness], against which the polyolefin film cested in order to keep it aligned with the direction of movement of the jaws.

Shear ~dhesion Value "Shear Adhesion Value" was tested by PSTC-7 except as follows. A polyolefin film was reinforced by laminating to the non test surface of the film the adhesive layer of a pressure-sensitive adhesive tape having a 0.089 mm thick polypropylene backing (Y-8450 from Minnesota Mining and Manufacturing Company~. A fastening tape then was laminated by its adhesive layer to the test surface of the polyolefin film [1 inch by 1 inch (2.54 by 2.54 cm) test area]. After being allowed to dwell for 15 minutes in an air-circulating oven at 100F (38C), the bond to the polyolefin film was tested with a 1000-gram weight attached immediately. The time to fail was recorded, and the test was discontinued if no failure occurred within 1500 minutes.

Table I
Formulations of each of Tapes A-Z are given in Table I togethec with their dried coating weights and the composite Tg of the B or midblock phase of the blend of the ABA copolymec and tackiEying resin as calculated in the Fox equation. Table I also reports testing for Mean Peel Force (average of 2 tests) and Shear Adhesion Values (average of 5 tests) using Polyolefin Film 1 (described below) as the polyolefin film.

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Brief De~cription of Drawin~s The invention may be better understood in connection with the drawing in which:
Figs. 1-12 are photomicrographs at 500X of surfaces of the below-described Polyolefin Films 1-12, respectively, of which Polyolefin Films 1-6 can be used to cover the fastening areas of a diaper in a pressure-sensitive adhesive closure of the invention ~hereas preferred peel characteristics have not been achieved when using polyolefin Films 7-12;
Figs. 13, 14 and 15 are photomicrographs at 1500X of Polyolefin Films 2, 1 and 7, respectively;
Fig. 16 is a photomicrograph at lOOX of Polyolefin Fi lm 9;
Fig. 17 is a perspective view of a diaper incorporating a pressure-sensitive adhesive closure of the invention;
Fig. 1~ shows the diaper of Fig. 17 laid flat;
and Fig. 19 is a diagram indicating key features of pressure-sensitive adhesives which have been used in diaper closures, some of which have achieved preferred peel characteristics and some of which have not.
~eferring first to Figs. 17 and 18, a diaper 10 has a pressure-sensitive adhesive closure consistlng of a pressure-sensitive adhesive tape 12 and a rectangle 14 of polyolefin film covering the fastening area of the diaper.
The end of the tape has been folded over to provide a narrow nonadhesive tab 16 while leaving a pressure-sensitive adhesive area 18. The diaper can be opened andeither discarded, or the closure can be refastened by pressing the adhesive-bearing area 18 of the tape against the rectangle 14.
Fig. 19 of the drawing shows key characteristics of each of the adhesive blends of each of Pressure-sensitive Adhesive Tapes A-Z. Those blends having characteristics bstween lines 20 and 22 of Fig. 19, . . .. .

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when tested with Polyolefin Film 1 (as reported in Table I, above), afforded prefecred peel characteristics while the other blends did not. As indicated in Table I, Tapes E and Y (below line 22) were deficient in Shear Adhesion Values; and Tapes, F, M and Z (above line 20) exhibited excessively shocky peel at high speeds. Tapes close to either of lines 20 or 22 generally provided marginal performance, while optimum results generally were attained midway between the lines, e.g., by Tapes A, B, C, P, and W.
When the pressure-sensitive adhesive is a styrene-butadiene-styrene (~A) triblock copolymer, each of the lines 20 and 22 would be lowered about 5-10K in order to encompass formulations that would afford the objectives of the invention. Substitution of other polyolefin films for Polyolefin Film 1 may also result in a shift in the lines 20 and 22. Differences in adhesive coating thickness can also affect performance as is well known in the art.
A large number of polyolefin films have been tested for use in the invention. Illustrative of polyolefin films which have been tested include Polyolefin Films 1-6, each of which has provided the objectives of the invention, and Polyolefin E'ilms 7-12, which have not.
In describing these polyolefin films, all parts are given by weight.

Polyolef in Fi 1:~ 1 A polypropylene resin (PP-3085 from Exxon Chemical Corp.) with a melt index of 35 g/10 minutes was extruded at a temperature of 260C through a slot extrusion die using a typical single-screw extruder. The melt exiting the die was passed into a nip between a metal roll covered with "Te1On" (polytetrafluoroethylene) and a water-cooled metal chill roll (water temperature, 18C) to result in a film with a basis weight of 44 g/m2 and a caliper of 56 ~m. soth the chill roll and the "Teflon"-covered roll had microtopographical features, the negative images of which were replicated in the polypropylene polymer film. The face of the film which contacted the metal chill roll is here called "Polyolefin Film 1" and is shown in Fig. 1 of the drawing.
The Fig. 1 face of Polyolefin Film 1 has a large number of closely spaced asperities at least two micrometers in height that have a jagged appearance at 500X. ~etween these asperities are a few isolated, relatively smooth areas. The asperities appear to be in the form of steep hills or peaks having an average height of about B-10 ~m, with the average distance between adjacent peaks being about 10 ~m. At the crowns of most of the peaks are what appear to be craters having sharp edges. The average distance between adjacent peaks is approximately the same in every direction.
By viewing Polyolefin Film 1 at 1500X as in Fig.
14, the nature of the individual steep hills can be better appreciated.

Polyolefin Film 2 A polypropylene resin as described in making Polyolefin Film l was extruded in the same manner except using a different metal chill roll and a metal roll covered with a silicone rubber coating instead of "Teflon." The resulting film had the same basis weight and caliper as did Polyolefin Film l. The ace of the film which contacted the silicone-covered roll is here called "Polyolefin Film 2" and is shown in Fig. 2 of the drawing.
The Fig. 2 face of the Polyolefin Film 2 has at ~ 500X a large number of closely spaced asperities that have a jagged appearance covering virtually 100% of its area.
~ The asperities appear to be in the form of craggy peaks having an average height of about 2 ~m, with the average distance between adjacent peaks being about 2 ~m. The average distance between adjacent peaks is approximately ~3~

the same in every direction. The true nature of these peaks can be better appreciated at lSOOX as seen in Fig.
13 of the drawing.
This Polyolefin Film 2 provides such high peel values that some users would be likely to complain that pressure-sensitive adhesive closures of the invention are too difficult to open if this film were to be used.
~ccordingly, it is suggested that surfaces rougher than the Fig. 2 face o Polyolefin Film 2 should be avoided in diaper closures of the invention.
PGlyolefin Film 3 Polyolefin Film 3 was prepared in the same manner as Polyolefin Film l except using a different chill roll. The description given above for Polyolefin Film l generally applies to Polyolefin Film 3, as seen in Fig. 3, except that the average distance between adjacent peaks appears to be about 12-15 ~m.

Polyolefin Film 4 Fig. 4 shows the matte ace of a polypropylene film 3.0 mils ~75 ~m) in thickness obtained as "Extrel" 30 from Exxon Chemical Film Division, Pottsville, PA. The Fig. 4 face of the Polyolefin E'ilm 4 is rather similar to the faces of Polyolefin Films 1 and 3 except that its individual asperities, while likewise being generally nondescript, are somewhat larger and no oraters a~e evident. The face of Polyolefin Film 4 appears to have a few smooth areas exceeding 100 ~m2, so that the asperities which have a jagged appearance cover only about 90% of the area.

Polyolefin Film 5 Fig. 5 shows the embossed face of a polypropylene film 2.5 mils (63 ~m) in thickness which had been embo~sed in a diamond pattern, as can be seen in Fig.

5. Although Polyolefin Film 5 has a smooth area at each ~3~

ridge of the diamond pattern and each smooth area substantially exceeds 100 ~m2 in area, the surface asperities covering about 85% of the total area of Polyolefin Film 5 have a jagged appearance that indicates S utility in the present invention. Like the ~urface asperities of Polyolefin Films 1, 3 and 4, those of Polyolefin Film 5 are of generally nondescript appearance.
They appear to average about 8-10 ~m in height, and the average distance between the peaks of the asperities appears to be about 10-20 ~m.

Polyolefin Film 6 Fig. 6 shows the embossed face of a polypropylene film 2.0 mils (S0 ~m) in thickness, obtained as "Microflex" Embossed Code XII from Clopay Corporation.
It had been embossed in a pattern similar to that of Polyolefin Film S except the embossed ridges extend to a greater height. The surface asperities of Polyolefin Film 6 appear to be somewhat smaller than those of Polyolefin Film 5, rising to what appears to be an average h~ight o~ about 4-6 ~m. Nevertheless, the asperities of Polyolefin Film 6 provide a jagged appearance at 500X
covering about 70% of the total area, thus indicating that the Fig. 6 face of Polyolefin Eilm 6 should be useful for covering the fastening area of a diaper of the present invention. The average distance between adjacent peaks of the individual asperities appears to ~e about 5-10 ~m, and the average distance between adjacent peaks is approximately the same in every direction.
Polvolefin Film 7 Fig. 7 shows the embossed face of a polypropylene film 2.G mil (50 ~m) in thickness obtained as "4301A" from Edison Plastics Company. It had been embossed in the same manner as were Poiyolefin Films 5 and 6. The smooth areas at the tops of the ridges of the embossed pattern appear to cover approximately 25% of the .

~3U 3~ 7X

total area. The surface asperities in the other areas have a jagged appearance at 500X, but when viewed in Fig.
15 at 1500X, it becomes more evident that individual asperities have an average height of only about 1 ~m and appear to be more flat than jagged. The Fig. 7 face of Polyolefin Film 7 has not afforded the preferred peel characteristics desired in pressure-sensitive adhesive closures of the invention.

lQ Polyolefin Film 8 Fig. 8 shows the embossed face of a polypropylene film 2O0 mil (50 ~m~ in thickness obtained as "EM-65R" from Consolidated Thermoplastics Company. It had been embossed with a pattern similar to those of lS Polyolefin Films 5, 6 and 7. At 500X, the surface asperities of Polyolefin Film 8 have a generally rounded appearance except at the edges of the embossing pattern.
The Fig. 8 face of Polyolefin Film 8 has not afforded the preferred peel characteristics desired in pressure-sensitive adhesive closures of the invention.
Polyolefin Film 9 Fig. 9 shows the obverse surface of PolyolefinFilm 6, which obverse surface appears to have a large number of surface asperities ~ridges) that have a jagged appearance at 500X and are more than 2 micrometers in height. Although these surface asperities appear to cover somewhat more than half of the total area of Fig. 9, it can be seen from Fig. 16 at lOOX that large areas of the surface are rather smooth and that the 500X magnification of Fig. 9 shows only a relatively rough portion of the total surface. From viewing both Figs. 9 and 16, it can be seen that more than half of the total surface would have a smooth or rounded appearance at 500X. The Fig. 9 face of Polyolefin Film 9 has not afforded the preferred peel characteristics desired in pressure-sensitive adhesive closures of the invention, but it is believed ~3~3~

that it might have afforded the desired properties if its Fig. 9 were representative of its overall appearance at 500X.

Polyolefin Film 10 Fig 10 shows the matte face of a polypropylene film 2.5 mils (63 ~m) in thickness obtained as "Extrel" 31 from Exxon Chemical ~mericas Film Division. Its surface asperities appear to be rounded depressions, a few of which appear to be greater than 10 ~m in depth~ The Fig.
10 face o~ Polyolefin Film 10 has not afforded the preferred peel characteristics desired in the present invention.

Polyolefin Film 11 Fig. 11 shows the obverse face of the film called "Polyolefin @ilm 4". "Polyolefin Film 11" has a generally smooth surface with some rounded ridges and valleys. The average height (and depth) of these ridges (and valleys) appears to be less than 1 ~m. The Fig. 11 face of Polyolefin Film 11 has not afforded the preferred peel characteristics desired in the present invention.

Polyolefin Film 12 Fig. 12 shows the obverse face of Polyolefin Film 5. At SOOX its surface asperities appear to be rounded. The Fig. 12 face of Polyolefin Film 12 has not afforded the preferred peel characteristics desired in pressure-sensitive adhesive closures of the present 3~ invention Reported in Table II are microtopographical measurements of Polyolefin Films 1-12 obtained using the above-cited "Perthometer" profilometer.

~L3~3~

TABLE II
Polyolefin Ra Sm Lo S
Film (~m (~m) _ (cm 1 1.78 106 1.056 246 2 0.51 69 1.015 390 3 1.72 100 1.038 195 ~ 1.42 74 l.Og2 244 5.70 177 1.059 71 6 5.38 101 l.lOg 103 7 10.62 210 1.095 58 8 4.89 188 1.047 60 9 1.21 100 1.025 206 6.42 231 1.08~ 81 11 1.26 69 1.041 271 12 0.88 215 1.009 198 Exa~ples o~ Simulated Diaper Closures Diaper closures were simulated in testing each of Polyolefin Films 1-12 in combination with Pressure- `
sensitive Adhesive A, and results are reported in Table III.

: 25 ~3~3~

Table III

Poly- Mean Peel Force ~N/m) Peel Shear olefin atat Quality* at Adhesion 5Film30 cm/min.1250 cm/min. 1250 cm/min. Value (min.) 1 435 830 Smooth 1500+
2 500 940 Smooth 1500~
3 550 1020 Smooth 1500+
4 340 745 Smooth 1500 10 5 195 560 Smooth 1500-~
6 220 630 Smooth 177 7 190 245 ~arginal lS0 8 380 235 Shocky 588 g 350 210 Shocky 1500+
1510 270 350 Marginal 91 11 320 160 Shocky 1500 12 290 130 Shocky lOS

* Smooth = Instantaneous peel force substantially within 20% of Mean Peel Force Shocky ~ Instantaneous peel force generally not within 20% of Mean Peel Force Marginal = Somewhat smooth and somewhat shocky

Claims

1. Pressure-sensitive adhesive closure for a disposable garment comprising a pressure-sensitive adhesive fastening tape, the adhesive of which comprises a blend of 1) an AB block copolymer wherein A
comprises vinylarene, B comprises a polymer of at least one monomer selected from conjugated dienes and lower alkenes, and A
comprises from 8 to 50 weight percent of the block copolymer, and

2) tackifying resin, the AB copolymer comprising from 20 to 60 weight percent of total AB copolymer plus tackifier and the B
phase of the blend having a composite Tg of from 250° to 275°K, and a polyolefin layer which forms the fastening area of the garment, the fastening surface of which has a large number of closely spaced asperities that have a jagged appearance at about 500X and are at least two micrometers in height, said closure affording a Mean Peel Force of at least 175 N/m both at 30 and 1250 cm/min.
2. Pressure-sensitive adhesive closure as defined in claim 1 wherein the jagged-appearing asperities are present over at least one-half the fastening surface.

3. Pressure-sensitive adhesive closure as defined in claim 1 wherein the surface asperities of the polyolefin polymer at the fastening area comprise peaks, and the average distance between adjacent peaks is less than five times their average height.

4. Pressure-sensitive adhesive closure as defined in claim 3 wherein the average distance between adjacent peaks is approximately the same in every direction.

5. Pressure-sensitive adhesive closure as defined in claim 1 wherein the surface of the polyolefin polymer at the fastening area has Ra of from 0.5 to 6µm Sm of from 50 to 200µm Lo of from 1.01 to 1.15 S of from 60 to 400/cm as measured by a "Perthometer" profilometer.

6. Pressure-sensitive adhesive as defined in claim 1 wherein the AB block copolymer is a styrene-isoprene-styrene triblock copolymer, and characteristics of the pressure sensitive adhesive blend lie between lines 20 and 22 of Fig. 19 of the drawing.

7. Pressure-sensitive adhesive closure as defined in claim 1 wherein the tackifying resin includes both liquid and solid tackifying resins.

8. Pressure-sensitive adhesive closure as defined in claim 1 wherein the tackifying resin is a single semisolid tackifying resin.

9. Pressure sensitive adhesive closure as defined in claim 1 wherein said polyolefin layer comprises polypropylene.

10. Pressure-sensitive adhesive closure as defined in claim 9 wherein said polyolefin layer comprises a copolymer of polypropylene and a copolymerizable monomer.

11. Pressure-sensitive adhesive closure as defined in claim 10 wherein said copolymerizable monomer is ethylene.

12. Pressure-sensitive adhesive closure as defined in claim 1 or 7 wherein the instantaneous peel force of the pressure-sensitive adhesive fastening tape stays substantially within 20%
of the Mean Peel Force as herein defined.

13. Pressure-sensitive adhesive closure as defined in claim 1 or 7 the pressure-sensitive adhesive fastening tape of which has a Shear Adhesion Value as herein defined of at least 150 minutes.

14. Pressure-sensitive adhesive closure for a disposable garment comprising a pressure-sensitive adhesive fastening taper the adhesive of which comprises a blend of 1) an ABA block copolymer wherein A
comprises vinylarene, B is selected from homopolymers of isoprene and butadiene and copolymers of ethylene and butylene, and A
comprises from 10 to 40 weight percent of the block copolymer, and 2) tackifying resin, the AB copolymer comprising from 25 to 50 weight percent of total AB copolymer plus tackifier and the B

phase of the blend having a composite Tg of from 250° to 275°K, and a polyolefin layer which forms the fastening area of the garment, the fastening surface of which has a large number of closely spaced asperities at least two micrometers in height that have a jagged appearance when viewed at 500X and are present over at least one-half the fastening surface, said closure affording a Mean Peel Force of at least 175 N/m both at 30 and 1250 cm/min.
while its Mean Peel Force at 1250 cm/min. is at least 80% of its Mean Peel Force at 30 cm/min.

15. Pressure-sensitive adhesive closure as defined in claim 14 wherein the surface asperities of the polyolefin polymer at the fastening area comprise peaks, and the average distance between adjacent peaks is less than five times their average height.

16. Pressure-sensitive adhesive closure as defined in claim 15 wherein the average distance between adjacent peaks is approximately the same in every direction.

17. Pressure-sensitive adhesive closure for a disposable diaper comprising a pressure-sensitive adhesive fastening tape and a polyolefin polymer covering the fastening area, wherein the improvement comprises the pressure-sensitive adhesive of the fastening tape comprises a blend of 1) an ABA block copolymer wherein A comprises styrene, B comprises at least one monomer selected from isoprene and butadiene, and A comprises from 8 to 35 weight percent of the block copolymer, and 2) tackifier, the ABA copolymer comprising from 20 to 60 weight percent of total ABA copolymer plus tackifier and the B or midblock phase of the blend having a composite Tg of from 258° to 267°K, and the surface of the polyolefin polymer at the fastening area has Ra of from 0.5 to 6µm Sm of from 50 to 200µm Lo of from 1.01 to 1.15 S of from 60 to 400/cm as measured by a "Perthometer" profilometer.

18. A diaper carrying a pressure-sensitive adhesive closure according to any one of claims 1 to 11 and 15 to 17.