1、Designation: F3166 16Standard Specification forHigh-Purity Titanium Sputtering Target Used for Through-Silicon Vias (TSV) Metallization1This standard is issued under the fixed designation F3166; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification details the generic criteria require-ments of high pure titanium sputtering
3、 targets used as thin filmmaterial for through-silicon vias (TSV) metallization in ad-vance packaging.1.2 Sputtering target purity, grain size, inner quality,bonding, dimension, and appearance specifications are in-cluded in this specification along with references for qualifi-cation test methods. R
4、eliability, certification, traceability, andpackaging requirements are also included.1.2.1 Purity Requirements:1.2.1.1 Metallic element impurities, and1.2.1.2 Non-metallic element impurities.1.2.2 Grain Size RequirementsGrain size.1.2.3 Inner Quality RequirementsInternal defect.1.2.4 Bonding Require
5、ments:1.2.4.1 Backing plate, and1.2.4.2 Bonding ratio.1.2.5 Configuration Requirements:1.2.5.1 Dimension,1.2.5.2 Tolerance, and1.2.5.3 Surface roughness.1.2.6 Appearance RequirementsSurface cleanness.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are i
6、ncluded in thisstandard.1.4 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 health practices and determine the applica-bility of regulatory limitations prio
7、r to use.2. Referenced Documents2.1 ASTM Standards:2B209 Specification for Aluminum and Aluminum-AlloySheet and PlateB248 Specification for General Requirements for WroughtCopper and Copper-Alloy Plate, Sheet, Strip, and RolledBarE112 Test Methods for Determining Average Grain SizeE1001 Practice for
8、 Detection and Evaluation of Discontinui-ties by the Immersed Pulse-Echo Ultrasonic MethodUsing Longitudinal WavesF1512 Practice for Ultrasonic C-Scan Bond Evaluation ofSputtering Target-Backing Plate AssembliesF1709 Specification for High Purity Titanium SputteringTargets for Electronic Thin Film A
9、pplicationsF1710 Test Method for Trace Metallic Impurities in Elec-tronic Grade Titanium by High Mass-Resolution GlowDischarge Mass Spectrometer2.2 ASME Standard:Y14.5M Dimensioning and Tolerancing33. Terminology3.1 Definitions:3.1.1 backing plate, nplate used to support the sputteringmaterial used
10、in deposition processes.3.1.1.1 DiscussionAssembling with the sputtering mate-rial by various bonding methods.3.1.2 sputtering target, nsource material during sputterdeposition processes; typically, a piece of material inside thevacuum chamber that is exposed to bombarding ions, knockingsource atoms
11、 loose and onto samples.3.1.2.1 DiscussionThe sputtering target product can beclassified as monolithic or assembly type according to theconfigurations as shown in Fig. 1.1This specification is under the jurisdiction of ASTM Committee F01 onElectronics and is the direct responsibility of Subcommittee
12、 F01.17 on SputterMetallization.Current edition approved May 1, 2016. Published July 2016. DOI: 10.1520/16.2For 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 stand
13、ards Document Summary page onthe ASTM website.3Available from American Society of Mechanical Engineers (ASME), ASMEInternational Headquarters, Two Park Ave., New York, NY 10016-5990, http:/www.asme.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959
14、. United States13.2 Definitions of Terms Specific to This Standard:3.2.1 finished product, nfor the purposes of this standard,a manufactured sputtering target ready for use.3.2.2 material lot, nfor the purposes of this standard,material melted into one ingot and processed as one continuousbatch in s
15、ubsequent thermal-mechanical treatments.4. Ordering Information4.1 Advance packaging manufacturers may use this speci-fication to specify required target performance to the supplierwhen purchasing sputtering target. Target suppliers may alsouse this specification to specify material requirements to
16、rawmaterial suppliers.4.2 Orders for pure titanium sputtering targets shall includethe following:4.2.1 Grade and special requirements concerning impurities,if required (Section 5),4.2.2 Grain size, if required (Section 6),4.2.3 Inner quality, if required (Section 7),4.2.4 Bonding ratio, if required
17、(Section 8),4.2.5 Dimensions, Tolerance and Surface Roughness (Sec-tion 9),4.2.6 Certification required (Section 14), and4.2.7 Whether or not a sample representative of the finishedproduct is required to be provided by the supplier to thepurchaser.5. Purity Requirement5.1 Metallic Element Impurities
18、:5.1.1 Grades of titanium sputtering targets for through-silicon vias (TSV) metallization are defined in Table 1 based ontypical metallic impurity content of the elements listed in thetable. Impurity contents are reported in parts per million byweight (wt ppm). Additional elements may be analyzed an
19、dreported as agreed upon between the purchaser and thesupplier.5.1.2 Acceptable analysis methods and detection limits arespecified in Specification F1709. Use Test Method F1709 toanalyze the purity of titanium by high-mass resolution glowdischarge mass spectrometer (GDMS).FIG. 1 Sputtering Target Co
20、nfigurationTABLE 1 Suggested Titanium Sputtering Target Grades and Impurity Content RequirementsNOTE 1Ti purity is 100 % subtract the sum of impurities contents listed in this table.Element Units Test MethodTi Purity, %99.995 %(4N5)99.999 %(5N)Ag ppmw GDMS #0.2 #0.2Al ppmw GDMS #5.0 #2.0B ppmw GDMS
21、#0.1 #0.1Ca ppmw GDMS #1.0Co ppmw GDMS #1.0 #0.1Cr ppmw GDMS #5.0 #1.0Cu ppmw GDMS #2.0 #1.0Fe ppmw GDMS #15.0 #7.0K ppmw GDMS #0.1 #0.1Li ppmw GDMS #0.1 #0.1Mg ppmw GDMS #1.0 #0.1Mn ppmw GDMS #1.0 #0.3Mo ppmw GDMS #4.0 #0.5Na ppmw GDMS #0.2 #0.1Ni ppmw GDMS #5.0 #0.5Pb ppmw GDMS #2.0 #0.1Si ppmw GD
22、MS #5.0 #2.0Sn ppmw GDMS #2.0 #1.0Th ppmw GDMS #0.001 #0.001U ppmw GDMS #0.001 #0.001V ppmw GDMS #1.0 #1.0W ppmw GDMS #1.0 #0.5Zn ppmw GDMS #1.0 #0.5Zr ppmw GDMS #5.0 #1.0Total amount ppmw #50 #10F3166 1625.1.3 For most metallic species, the detection limit byGDMS is on the order of 0.01 wt ppm. Wit
23、h specialprecautions, detection limits to sub-ppb levels are possible.Elements not detected will be counted and reported as presentat the minimum detection limit (mdl).5.1.4 Other analytical techniques may be used providedthey can be proved equivalent to the methods specified andhave mdl less than o
24、r equal to the specified methods.5.1.5 Acceptable limits and analytical techniques for par-ticular elements in critical applications may be agreed uponbetween the purchaser and the supplier.5.2 Nonmetallic Element Impurities:5.2.1 Nonmetallic element impurities that shall be analyzedand reported are
25、 carbon, hydrogen, nitrogen, oxygen, andsulfur. Maximum limits for nonmetallic impurities shall be asagreed upon between the purchaser and the supplier. Typically,nonmetallic impurities should be as low as shown in Table 2.5.2.2 Acceptable analysis methods and detection limits arespecified in Specif
26、ication F1709. Elements not detected will becounted and reported as present at the mdl.5.2.3 Other analytical techniques may be used providedthey can be proved equivalent to the methods specified andhave mdl less than or equal to the specified methods.6. Grain Size Requirement6.1 The average and the
27、 maximum grain size shall be asagreed upon between the purchaser and the supplier. Theaverage and the maximum grain size are generally controlledwithin 50 and 100 m.6.2 Average grain size shall be measured and reported inaccordance with Test Methods E112 or another equivalentmethod.6.3 Maximum grain
28、 size shall be established by making anoptical or scanning electron micrograph of a polished andetched specimen typical of the finished product. The magnifi-cation shall be calibrated to 610 % of nominal using anappropriate gage. At least 50 grains shall be resolved in themicrograph. The maximum gra
29、in size is the diagonal measureof the largest titanium crystal visible in the field of viewdivided by the magnification.6.4 Average grain size and maximum grain size can alter-natively be established using computer-assisted image analysismethods. If image analysis methods are used, then the averageg
30、rain size is defined as the mean value obtained from the graindiameter distribution data. The maximum grain size is definedas the largest grain diameter recorded in the grain sizedistribution set. At least 50 grains shall be included in theimage analysis data set.7. Inner Quality Requirement7.1 Inte
31、rnal defect such as inclusions and pores which affectsputtering film quality shall not exist inside the target. Thesupplier should promise the target inner quality by rawmaterials control and target fabricating methods.7.2 Internal defects which are defined as discontinuities inthe bulk material sha
32、ll be measured and reported in accordancewith Guide E1001 or another equivalent method.8. Bonding Requirement8.1 Backing PlateFor the assembly sputtering target, alu-minum alloy and copper alloy can be used as a backing platefor bonding. The backing plate materials should meet therequirements of Spe
33、cifications B209 or B248. Other backingplate material and requirements shall be agreed upon betweenthe purchaser and the supplier.8.2 Diffusion bonding is very commonly used in sputteringtarget-backing plate assembly. The bonding quality shall meetthe requirements of Table 3.8.3 The bonding ratio sh
34、all be measured and reported inaccordance with Practice F1512 or another equivalent method.9. Dimensions, Tolerance, and Surface RoughnessRequirement9.1 Each product shall conform to an appropriate engineer-ing drawing agreed upon between the purchaser and thesupplier.9.2 Nominal dimensions, toleran
35、ces, and other attributesshall be measured and reported in accordance with ASMEY14.5M or another equivalent method.9.3 Normally, the sputtering surface roughness prepared bymachining or polishing shall be less than 1.6 m.10. Appearance Requirement10.1 The target surface appearance shall be agreed up
36、onbetween the purchaser and the supplier.10.2 Surfaces shall be free of any contaminates such as dirtor oils that could adversely affect the performance of thematerial as agreed upon between the purchaser and thesupplier.TABLE 2 Suggested Nonmetallic Impurity RequirementElement Units Test MethodTi P
37、urity, %99.995 %(4N5)99.999 %(5N)C ppmw fusion and gas extraction/infrared spectroscopy#50 #40H ppmw fusion and gas extraction #10 #10N ppmw fusion and gas extraction #50 #50O ppmw fusion and gas extraction/infrared spectroscopy#300 #250S ppmw fusion and gas extraction/infrared spectroscopy#10 #10F3
38、166 16311. Sampling Requirement11.1 Analysis for target properties (including impurity, grainsize, inner quality, bonding ratio, dimension and tolerances,and surface roughness and appearance) shall be performed onsamples that are representative of the finished sputtering target.11.1.1 Unless otherwi
39、se agreed upon between the purchaserand the supplier, impurity analyses for metallic and nonmetal-lic impurities shall be made by the supplier for one or moresample specimens that are representative of the production lot.These data shall be averaged to establish conformance with thegrade designation
40、 (5.1), other metallic impurity limits (5.1),and the agreed upon limits for nonmetallic content (5.2).11.1.2 Unless otherwise agreed upon between the purchaserand the supplier, grain size analyses shall be made by thesupplier for one or more sample specimens after thermal-mechanical treatments for t
41、he lot of titanium material. Thesedata shall be averaged to establish conformance with the grainsize designation (6.1).11.2 Suggested Sampling InformationSee Table 4.12. Traceability Requirements12.1 It will be the responsibility of the target supplier toestablish and maintain an incoming raw materi
42、al certification,inspection, and traceability process, which will ensure thatmanufactured target components meet the requirements of thisspecification.12.2 Every deliverable item shall have some scheme ofidentification on the exterior bag or box so that traceability isprovided from the raw material
43、supplier to the final finished,packaged product.13. Reliability Requirements13.1 Upon request, the manufacturer should provide sput-tering reliability data accompanied by the sputtering qualifica-tion test. This typically involves lifetime testing of the sputter-ing target with desired film properti
44、es (usually kwh is used asmeasurement unit). The spent target can be analyzed byprofilometer to learn the left minimum thickness, h1, of thesputtering material as shown in Fig. 2. Normally, for safety, theh1 should be more than 2 mm.14. Certification14.1 The target supplier is responsible for defini
45、ng,establishing, and executing a testing program for sputteringtarget based on the requirements outlined within this specifi-cation.14.2 When required by the purchaser a certificate ofanalysis/compliance that documents the finished target shall beprovided by the supplier.14.3 The certificate of anal
46、ysis/compliance shall state themanufacturers or suppliers name, the suppliers lot number,the grade level, impurity levels, method of analysis (Section 5),and any other information as agreed upon between the pur-chaser and the supplier.15. Packaging15.1 Every target shall be packed as one single unit
47、. Eachpiece shall be sealed by vacuuming inert gas to avoid contami-nation and oxidation and shall be packaged well with cushionmaterial and enhanced structure to avoid damage.15.2 The packaging shall have a label affixed that clearlyidentifies the product name (with purity grade and material), lotn
48、umber, and any other necessary traceability characteristics(Section 12).15.3 The packaging shall be capable of withstanding astorage period of target shelf-life, without the purity of thematerial being affected.16. Keywords16.1 high-purity titanium; sputtering target; TSVmetallizationTABLE 3 Suggest
49、ed Bonding RequirementABonding Method Bonding Ratio Single-Defect Area/the Whole Bonding AreaDiffusion bonding $98 % #1.5 %AOther bonding method and bonding ratio request shall be agreed upon between the purchaser and the supplier.TABLE 4 Suggested Sampling RequirementMeasurement Item Sampling Time Sample Numbers NotesImpurities After ingot cutting 1 or 2 pieces/lot 5.1Grain size After thermal-mechanicaltreatments1 or 2 pieces/lot 6.1Inner quality After thermal-mechanicaltreatmentsEach 7.1Bonding ratio After bonding Each 8.2Dimension and tolerances Finished produ
