1、Designation: D 6463/D 6463M 06Standard Test Method forTime to Failure of Pressure Sensitive Articles UnderSustained Shear Loading1This standard is issued under the fixed designation D 6463/D 6463M; the number immediately following the designation indicates theyear of original adoption or, in the cas
2、e of revision, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the ability of a pressure sensi-tive article (for example, tape, l
3、abel, sticker, etc.) to remainadhered to a stainless steel panel under a constant load appliedparallel to the bonding surface of the pressure sensitive article.1.2 Values stated in either SI or inch-pound units are to beregarded separately as standard. The values stated in eachsystem may not be exac
4、t equivalents, therefore, each systemmust be used independently without combining values in anyway.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and healt
5、h practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2A 666 Specification for Annealed or Cold-Worked Austen-itic Stainless Steel Sheet, Strip, Plate, and Flat BarD 907 Terminology of AdhesivesD 3654/D 3654M Test Methods for Sh
6、ear Adhesion ofPressure-Sensitive TapesD 5750/D 5750M Guide for Width and Length of Pressure-Sensitive TapeE 171 Specification for Atmospheres for Conditioning andTesting Flexible Barrier MaterialsE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 691 Practice for Conducting
7、 an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Many of the terms found in this test method are definedin Terminology D 907.4. Summary of Test Method4.1 This test method consists of bonding a standard area ofa pressure sensitive article to a stainless steel pane
8、l. Thebonded construction is allowed to dwell in a constant tempera-ture and humidity environment for 30 min. The construction isthen mounted vertically. A standard mass of 500 g 1.1 lb isattached to the pressure sensitive article and allowed to actuntil the construction separates or until 3000 min
9、elapse. Ifthere is no separation after 3000 min, the test is repeated on afresh specimen with a mass of 1000 g 2.2 lb and allowed toact until separation occurs or until 3000 min elapse. If noseparation occurs, perform Procedure C of Test MethodD 3654/D 3654M for shear holding power to stainless stee
10、l at49C 120F. The test result is the time in minutes toseparation.5. Significance and Use5.1 This test method measures the cohesive strength of theadhesive on a pressure sensitive article. The time to failure canpredict end use properties of pressure sensitive articles such as1This test method is un
11、der the jurisdiction of ASTM Committee D14 onAdhesives and is the direct responsibility of Subcommittee D14.50 on Hot Melts,Pressure Sensitives, and Archival Adhesives.Current edition approved March 1, 2006. Published April 2006. Originallyapproved in 1999. Last previous edition approved in 1999 as
12、D 6463 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Driv
13、e, PO Box C700, West Conshohocken, PA 19428-2959, United States.edge ooze from cold flow; trimming, slitting and die cuttingquality; telescoping in tapes; ability to seal packages; andvertical holding power.5.2 This test method is suitable for quality control, devel-opment and applications testing.5
14、.3 If the adhesive is not already coated, the adhesive can becoated on smooth, clear polyester (PET) film backing 0.05 mm0.002 in. thick. The recommended dry adhesive thickness is0.025 mm 0.001 in.5.4 Humidity has a strong effect on time to failure for manypressure sensitive articles. Therefore, hum
15、idity should becontrolled in accordance with 8.1.2.6. Apparatus6.1 Specimen Cutter3,4 The specimen cutter shall holdtwo single-edge razor blades in parallel planes, a precisedistance apart, to form a cutter of exact specimen width. Acutter of 12 mm 0.5 in. cutting width, shall be available orappropr
16、iate alternates, that will not cause edge damage.6.1.1 The 12 mm 0.5 in. cutter shall consist of a 12 mm0.5 in. thick by 200 mm 8 in. length of aluminum bar stock12 mm 0.5 in. wide. The edges for about 125 mm 5 in. fromone end shall be rounded slightly to form a handle. The widthof the bar for 75 mm
17、 3 in. shall be narrowed to exactly 12 mm0.5 in minus the thickness of a single-edge razor (one of twoused as cutting edges). The razor shall be held in position usingside plates. The end of the cutter shall be cut away at a 45angle to expose the cutting edges at one end of the blades. Theedges shal
18、l be separated by 12 6 0.10 mm 0.5 6 0.005 in.6.2 Dispensing System, for solvents, such as a wash bottle.6.3 Test Panel4No. 302 or 304 stainless steel sheet, notless than 1.1 mm 0.43 in. thick, having a bright annealedfinish, in accordance with Specification A 666. The panelshould be 25 by 25 mm 1.0
19、 by 1.0 in. or larger, as best suitedto the test stand (Fig. 1). The surface roughness height shall be50 6 25 nm 2.0 6 1.0 in. arithmetical average deviationfrom a mean line. One or both of the panel ends shall be groundto form a 90 angle with the panel surface. Panels showingstains, discolorations,
20、 or numerous scratches are not accept-able. New panels should be cleaned before use as described in10.1, except with ten washes of the final solvent. Between uses,the panels test surface shall be protected from scratches andcontamination, and the panels stored at conditions described inSection 8.6.4
21、 Roller, mechanically or hand-operated.46.4.1 Asteel roller 85 6 2.5 mm 3.25 6 0.1 in. in diameterand 45 6 1.5 mm 1.75 by 0.05 in. in width, covered withrubber approximately 6 mm 0.25 in. in thickness, having aShore scale A durometer hardness of 80 6 5. The surface shallbe a true cylinder void of an
22、y convex or concave deviations.The mass of the roller shall be 2040 6 45 g 4.5 6 0.1 lb.6.4.2 No part of the apparatus shall increase the mass of theroller during use. The roller shall move either mechanically orby hand at the rate of 10 6 0.2 mm/s 24 6 0.5 in./min.6.5 Test Stands and Ancillary Appa
23、ratus:6.5.1 Test Stand4A test stand that will hold the test panelwith the specimen applied at an angle of 2.0 6 0.5 fromvertical, so that when the mass is acting on the test specimen,no peel forces will be exerted on the specimen.6.5.2 Clamp/Clip/Cardboard Chipthat will allow attach-ment of the mass
24、 to the specimen, distributing the load equallyacross the specimen width.3These widths correspond to the primary metric (SI) units described in GuideD 5750/D 5750M. These so-called “ modular metric” units generally are usedthroughout the world. If it is desirable to test slightly different widths, t
25、his should benoted per 12.1.8 and calculations per 11.1 must account for the difference.4The sole source of supply of the apparatus known to the committee at this timeis Chemsultants International, 9349 Hamilton Drive, Mentor, OH 440611118. Ifyou are aware of alternative suppliers, please provide th
26、is information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1may attend.FIG. 1 Test Panel with Specimen and Mass (Side View)D 6463/D 6463M 0626.5.3 Massa 500 6 5 g 1.1 6 0.01 lb anda10006 5g 2.2 6 0.01 lb with
27、a hook on top.6.5.4 Timing Systemto measure the interval in minutes,between the application of the load to the specimen and itsseparation form the panel.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals should beused in all tests. Other grades may be used, provided it is firstas
28、certained that the reagent is of sufficiently high purity topermit its use without lessening accuracy of the determination.7.2 Solvents:7.2.1 Any of the following solvents may be used forcleaning:7.2.1.1 Diactone alcohol non-residual, technical grade orbetter,7.2.1.2 Methanol (95 %),7.2.1.3 Methyl e
29、thyl ketone (MEK),7.2.1.4 n-Heptane, or7.2.1.5 Acetone.7.2.2 Before selecting or using these solvents for cleaningtest panels, be sure to read and follow all precautions on thechemical Material Safety Data Sheets (MSDS) and consultwith Environmental, Health, and Safety (EHS) professionals.7.3 Cleani
30、ng MaterialAbsorbent, surgical gauze, cottonwool or tissue may be used. To be suitable, materials must belint-free during use, absorbent, contain no additives that aresoluble in the solvents listed in 7.2 and made exclusively formvirgin materials.8. Conditioning8.1 Testing RoomCondition and test sam
31、ples in a con-trolled temperature and humidity room is described below:8.1.1 Control the temperature to 23.0 6 2.0C 73.4 63.6F as specified in Specification E 171.8.1.2 Control the relative humidity to 50 % RH6 2 % RH.The humidity range specified in Specification E 171,50%65 % RH, is too large for t
32、his test.8.1.2.1 Two independent studies were conducted on theeffect of relative humidity on time to failure of pressuresensitive articles under sustained shear loading. For fouracrylate adhesive tapes, the time to failure decreased by 5.8,5.5, 8.4 and 6.1 % for each 1 % increase in relative humidit
33、y.For each sample, the rate of humidity decrease was determinedat 50 % RH. This high sensitivity to small humidity changesrequires that humidity be controlled during the test.8.2 Condition samples in a controlled temperature andhumidity room, as described in 8.1, for at least 24 h beforecutting the
34、samples into test specimens (Sample Preparation,See Section 9).9. Sample Preparation9.1 Cut sample into 12 mm 0.5 in. wide strips with thelong dimension in the machine direction of the pressuresensitive article. The dimensions of the shear stand will dictatethe specimen length. The mass drop distanc
35、e (the distancebetween the bottom of the mass and the timer stop plate) mustbe a minimum of 12 mm 0.5 in. and should be such that theshear stand does not transmit shock forces to the specimensthat remain hanging when the mass drops. Cut at least threespecimens for each pressure sensitive article to
36、be tested (Fig.2).NOTE 1If the sample to be tested incorporates PVC (or any other typeof facestock with a tendency to elongate under load) as a facestock, thesample may be reinforced by overlaminating it with a non-elastic film,such as PET, prior to sample cutting. This minimizes the influence of th
37、efacestock on the time to failure.10. Procedure10.1 Dispense one of the solvents listed in 7.2.1 onto thepanel, wiping to dryness with fresh absorbent cleaning material(see 7.3). Repeat for a total of three washes. The final cleaningshall be with an alternate solvent, either MEK or acetone. Donot to
38、uch cleaned panel surfaces with fingers. The cleanedpanel should be allowed to dry at standard conditions for atleast 10 min. If cleaned panel is not used within 10 h, it shouldbe recleaned.NOTE 2All operations with solvents should be conducted in awell-ventilated hood.NOTE 3Discard panels showing s
39、tains, discoloration, or manyFIG. 2 Typical Sample of a Pressure Sensitive Article (Schematic for Sample Preparation)D 6463/D 6463M 063scratches. During storage, panels should be protected from damage orcontamination.10.2 Attach the adhesive surface of one end of the specimento a clip or piece of ca
40、rdboard to distribute the force of themass evenly across the width of the specimen. Reinforce thatend of the specimen with a piece of tape, a staple or both sothat it will hold the mass securely.10.3 Center the specimen on the bottom end of the clean testpanel. Remove any release liner and apply the
41、 specimen to thepanel without added pressure. The specimen covers 12 by 12mm 0.5 by 0.5 in. on the test panel.10.4 Adhere the specimen to the panel by rolling the rubbercovered roller over the covered area four times, twice back andforth, at a velocity of 600 mm 24 in./min. Either a hand or amechani
42、cal roller may be used.10.5 Insert the panel and specimen into the test stand holderand wait 30 min before applying the standard mass.10.6 Gently apply the 500 g 1.1 lb mass to the specimen sothat no impact force or oscillations are applied. The dropdistance should be as described in 9.1.10.7 Record
43、 the time elapsed in minutes when the specimenseparates from the test panel.10.7.1 If no separation occurs within 3000 min with the 500g 1.1 lb mass, repeat the test with a fresh specimen and attachthe 1000 g 2.2 lb mass in 10.6.10.7.2 If no separation occurs within 3000 min with the1000 g 2.2 lb ma
44、ss, terminate the test and use the conditionsspecified in Procedure C of Test Method D 3654/D 3654M.10.8 Repeat the procedure at least two additional times foreach sample to be tested for a total of three replicates.11. Calculation11.1 Calculate the average time to failure (of at least threespecimen
45、s) in minutes and the standard deviation for eachsample.12. Report12.1 Report the following information:12.1.1 Adhesive identification and type, if known,12.1.2 Cleaning solvent(s) used for cleaning test panel,12.1.3 Adhesive coat weight or thickness, if known,12.1.4 Facestock material and release l
46、iner used, if known,12.1.5 Temperature and relative humidity of testing room,12.1.6 Average time to failure (of at least three specimens)and standard deviation,12.1.7 Failure mode - adhesion, cohesion or transfer. Cohe-sion is the preferred failure mode for this test, and12.1.8 Any deviation from th
47、e procedure as written.13. Precision and Bias13.1 An interlaboratory study of this test method using theoriginalASTM roll-down procedure, two passes of the roller at300 mm 12 in./min., was conducted in accordance withPractice E 691. Seven laboratories reported three test results oneach of two adhesi
48、ve tapes. Results of the repeatability studyare summarized in Table 1. Repeatability and reproducibility ofthis test method with the new harmonized standard roll-downwill be conducted and available on or before December 12,2009. All other information herein refers to the original study.13.2 The prec
49、ision information given below was calculatedfor the comparison of the average of three individual testdeterminations as specified in the test method.13.3 The terms repeatability limit and reproducibility limitare used as specified in Practice E 177.13.4 RepeatabilityThe repeatability of this test methodwas an increasing function of the value of the test result. SeeTable 1.13.5 ReproducibilityThe reproducibility of this testmethod was an increasing function of the value of the testresult. S
