CN115109908A - 一种致密型金键合丝的制备方法 - Google Patents
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- 229910052737 gold Inorganic materials 0.000 title claims abstract description 31
- 239000010931 gold Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 15
- 239000000839 emulsion Substances 0.000 claims abstract description 13
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 150000001299 aldehydes Chemical class 0.000 claims description 11
- 239000000956 alloy Substances 0.000 claims description 11
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 10
- 229920002125 Sokalan® Polymers 0.000 claims description 7
- 239000004584 polyacrylic acid Substances 0.000 claims description 7
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
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- 239000003353 gold alloy Substances 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 abstract description 11
- 239000004332 silver Substances 0.000 abstract description 9
- 238000005266 casting Methods 0.000 abstract description 8
- -1 silver ions Chemical class 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract description 3
- 230000008021 deposition Effects 0.000 abstract description 3
- 239000007888 film coating Substances 0.000 abstract description 2
- 238000009501 film coating Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002243 precursor Substances 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000010622 cold drawing Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
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- 239000005022 packaging material Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
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- 238000004513 sizing Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/06—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
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- B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
- B21C1/003—Drawing materials of special alloys so far as the composition of the alloy requires or permits special drawing methods or sequences
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- B21C43/00—Devices for cleaning metal products combined with or specially adapted for use with machines or apparatus provided for in this subclass
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- C22C5/00—Alloys based on noble metals
- C22C5/02—Alloys based on gold
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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- C23C18/1601—Process or apparatus
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- C23C18/1632—Features specific for the apparatus, e.g. layout of cells and of its equipment, multiple cells
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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Abstract
本发明公开了一种致密型金键合丝的制备方法：将直径为0.1‑0.2mm的金键合丝半成品丝退火后导入添加有硝酸银水性乳液的一级超细拉容器中拉至0.07‑0.15mm，得一级超细拉丝，将其导入添加有醛的稀溶液的二级超细拉容器中拉细至0.03‑0.1mm，水洗后得二级超细拉丝，氮气保护下加热到200‑350℃后退火，酸洗后水洗干燥，即得。本发明方法在键合丝最后拉铸成型时进行银离子沉积反应，反应时间长且反应条件温和，并且将银离子渗入到键合丝微裂痕中之后再进行反应可将微裂痕充分填充，制备出致密性更好的键合丝，避免了覆膜法制备的键合丝镀层下仍存在微裂痕的问题。
Description
技术领域
本发明涉及键合丝技术领域，尤其涉及一种致密型金键合丝的制备方法。
背景技术
键合丝作为一种重要的封装材料，对其各项指标的精度要求很高。键合丝的最后成型多为拉铸成型，现有键合丝多为单一合金的均相结构，在拉伸时内外受力不均键合丝的表面会产生微裂痕。
解决键合丝成型过程中产生微裂痕主要有两种方案，一种是减少冷拉的次数，从概率上减低出现微裂痕的几率；一种是在成型之后进行补救，如进行镀层或者回火处理。中国专利CN 114086021 A公开了一种键合丝快速定向铸造方法，该方法即采用减少多级冷拉成型次数的工艺，实现快速成型的目的。但是该方法无法使用传统的键合丝成型设备，前提投入成本较高，还需重新探索新的工艺。中国专利CN 110164776 A公开了一种键合丝保护镀层的制作方法，该方法将原丝从450-550μm拉制成10-50μm之后采用激光诱导沉积覆膜，实现原丝冷拉后的致密化。但是镀层是在原丝成型之后激光诱导沉积上的，仅仅是沉积在原丝的表层，无法对原丝微裂痕进行填充，制备出的键合丝成品表面虽然致密，但镀层下仍然有微裂痕的存在。
发明内容
针对上述问题，本发明提供一种致密型金键合丝的制备方法，包括以下步骤：
1)将金键合丝合金熔融后制备成固定尺寸的金合金锭，将金合金锭经过粗拉、中拉和细拉，制备成直径为0.1-0.2mm的半成品丝；
2)将步骤1)所得半成品丝退火后导入一级超细拉容器中进行一次超细拉，将直径拉至0.07-0.15mm，得一级超细拉丝，一级超细拉容器中添加有硝酸银的水性乳液，一级超细拉丝从一级超细拉容器中导出后50-70℃下烘干；
3)将步骤2)烘干后的一级超细拉丝导入二级超细拉容器中，进行再次超细拉，进一步拉细至0.03-0.1mm，二级超细拉容器中添加有醛的稀溶液，导出二级超细拉容器后水洗，得二级超细拉丝；
4)将步骤3)所得二级超细拉丝，氮气保护下加热到200-350℃后退火，酸洗后水洗，干燥，制得致密型金键合丝。
本发明的方法是针对金键合丝的半成品丝在超细拉步骤中进行的防微裂痕的处理，因此只要是以金为主合金的键合丝都适用本方法，金含量不低于85wt％的金键合丝均可。
本发明制备致密型金键合丝的原理是，将常规超细拉细分成一级超细拉和二级超细拉两个步骤，一级超细拉的容器中硝酸银的水性乳液的组成为去离子水65-87wt％、硝酸银8-20wt％和聚丙烯酸5-15wt％，半成品丝在被拉至 0.07-0.15mm过程中产生的微裂痕中会渗入银离子，烘干后会被聚丙烯酸封住；二级超细拉容器中添醛的稀溶液为乙醛和葡萄糖的碱溶液，浓度为 3wt％-10wt％，pH为8-10，在二级超细拉的过程中，聚丙烯酸会再次溶解，银离子在还原性醛的碱性溶液中，温度适当的情况下会被还原成单质银而沉积，从而填补微裂痕。
本发明通过对一级超细拉和二级超细拉的条件控制实现银离子在微裂痕中被还原成单质银而沉积：一级超细拉容器中停留时间为10-20min，二级超细拉容器中的停留时间为15-60min；硝酸银的水性乳液的温度恒定在 30-50℃，醛的稀溶液的温度恒定在50-80℃。
本发明方法在键合丝最后拉铸成型时进行银离子沉积反应，反应时间长且反应条件温和，并且将银离子渗入到键合丝微裂痕中之后再进行反应可将微裂痕充分填充，制备出致密性更好的键合丝，避免了覆膜法制备的键合丝镀层下仍存在微裂痕的问题。此外，本发明方法可以在现有键合丝生产线的基础上进行局部改进，在最后的拉铸设备上增加银离子上浆池，再连接沉积反应池以及辅助性的洗涤干燥设备，即可完成设备改造。
附图说明
图1为本发明采用的一级超细拉容器和二级超细拉容器一种可选的结构示意图。
图中标号：1、一级超细拉容器，2、二级超细拉容器，3、导辊。
具体实施方式
以下结合实例对本发明进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
实施例1
一种致密型金键合丝的制备方法，金键合丝的合金组成为：Au 87％、 Cu 10％、Ag2％和Pt 1％，采用现有拉铸工艺将合金锭经粗拉、中拉和细拉，制备成直径为0.2mm的半成品丝，退火后导入一级超细拉容器(1)中，一级超细拉容器(1)高80cm宽60cm长200cm，设有多个导辊(3)，其内盛有硝酸银的水性乳液，构成为：去离子水80wt％、硝酸银10wt％和聚丙烯酸10wt％，乳液温度为45℃；半成品丝在各个辊中穿过，控制各辊之间的速度差，将半成品丝拉至0.1mm，总停留时间为20min，出一级超细拉容器 (1)后用60℃的氮气吹干，导入二级超细拉容器(2)，二级超细拉容器(2) 高80cm宽60cm长200cm，设有多个导辊(3)，其内盛有醛的稀溶液，为质量比为1:3的乙醛和葡萄糖的5wt％的水溶液，加入氢氧化钠调节pH为9，温度为70℃，控制各辊之间的速度差，进一步拉至0.05mm，总停留时间为 40min，出二级超细拉容器(2)后水洗，氮气保护下加热到300℃后退火，用3％稀盐酸酸洗后水洗，干燥后制得致密型金键合丝。
实施例2
一种致密型金键合丝的制备方法，金键合丝的合金组成为：Au 90％、 Cu 5％、Ag4％和Pt 1％，采用现有拉铸工艺将合金锭经粗拉、中拉和细拉，制备成直径为0.15mm的半成品丝，采用实施例1的设备，一级超细拉容器 (1)中硝酸银的水性乳液构成为：去离子水70wt％、硝酸银20wt％和聚丙烯酸10wt％，乳液温度为50℃，在一级超细拉容器(1)中拉至0.1mm，总停留时间为10min；二级超细拉容器(2)中的醛的稀溶液为质量比为1:1的乙醛和葡萄糖的15wt％的水溶液，加入氢氧化钠调节pH为10，温度为50℃，拉细至0.06mm，停留时间为60min。
实施例3
一种致密型金键合丝的制备方法，金键合丝的合金组成为：Au 90％、 Ag 3％、Cu1.5％、Pt 1％、Al 1.5％、Pd 1％、Ti 1％、Si 0.5％和B 0.5％，采用现有拉铸工艺将合金锭经粗拉、中拉和细拉，制备成直径为0.1mm的半成品丝，采用实施例1的设备，一级超细拉容器(1)中硝酸银的水性乳液构成为：去离子水65wt％、硝酸银20wt％和聚丙烯酸15wt％，乳液温度为 30℃，在一级超细拉容器(1)中拉至0.07mm，总停留时间为15min；二级超细拉容器(2)中的醛的稀溶液为质量比为1:2的乙醛和葡萄糖的8wt％的水溶液，加入氢氧化钠调节pH为8，温度为80℃，拉细至0.04mm，停留时间为15min。
对比例1-3分别为实施例1-3的半成品丝直接超细拉至对应直径的金键合丝。
实施例1-3和对比例1-3所得金键合丝的检测结果如表1所示。从表1 中数据可以看出，相比于传统方法，采用本发明方法制备的金键合丝纤度有一定的提升，说明本发明的方法可以将银离子通过反应沉积在金键合丝表面，并且本发明方法所得金键合丝的机械性能也有一定的提升，说明沉积的银单质填充在了微裂痕中，增强了金键合丝的拉伸强度和延伸性能。
表1.实施例1-3和对比例1-3金键合丝的检测结果
| 拉断力B.L(gf) | 延伸率EL(％) | 纤度(D) | |
| 实施例1 | 40.33 | 14.84 | 2.8554 |
| 对比例1 | 37.62 | 14.15 | 2.6207 |
| 实施例2 | 52.07 | 17.55 | 4.7157 |
| 对比例2 | 47.68 | 16.42 | 4.5534 |
| 实施例3 | 32.84 | 12.33 | 2.1495 |
| 对比例3 | 27.95 | 11.86 | 2.0311 |
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (6)
1.一种致密型金键合丝的制备方法，其特征在于，包括以下步骤：
1)将金键合丝合金熔融后制备成固定尺寸的金合金锭，将金合金锭经过粗拉、中拉和细拉，制备成直径为0.1-0.2mm的半成品丝；
2)将步骤1)所得半成品丝退火后导入一级超细拉容器中进行一次超细拉，将直径拉至0.07-0.15mm，得一级超细拉丝，一级超细拉容器中添加有硝酸银的水性乳液，一级超细拉丝从一级超细拉容器中导出后50-70℃下烘干；
3)将步骤2)烘干后的一级超细拉丝导入二级超细拉容器中，进行再次超细拉，进一步拉细至0.03-0.1mm，二级超细拉容器中添加有醛的稀溶液，导出二级超细拉容器后水洗，得二级超细拉丝；
4)将步骤3)所得二级超细拉丝，氮气保护下加热到200-350℃后退火，酸洗后水洗，干燥，制得致密型金键合丝。
2.根据权利要求1所述的方法，其特征在于，所述金键合丝中金含量不低于85wt％。
3.根据权利要求1或2所述的方法，其特征在于，所述硝酸银的水性乳液的组成包括以下重量比的组分：去离子水65-87％、硝酸银8-20％、聚丙烯酸5-15％。
4.根据权利要求1或2所述的方法，其特征在于，所述醛的稀溶液为乙醛和葡萄糖的碱溶液，浓度为3wt％-10wt％，pH为8-10。
5.根据权利要求1或2所述的方法，其特征在于，一级超细拉容器中停留时间为10-20min；二级超细拉容器中的停留时间为15-60min。
6.根据权利要求1或2所述的方法，其特征在于，硝酸银的水性乳液的温度恒定在30-50℃，醛的稀溶液的温度恒定在50-80℃。
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