CN112941514A - 一种铜/镍反应性纳米多层膜的制备方法 - Google Patents

一种铜/镍反应性纳米多层膜的制备方法 Download PDF

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CN112941514A
CN112941514A CN202110159522.6A CN202110159522A CN112941514A CN 112941514 A CN112941514 A CN 112941514A CN 202110159522 A CN202110159522 A CN 202110159522A CN 112941514 A CN112941514 A CN 112941514A
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nickel
copper
titanium alloy
multilayer film
alloy sheet
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殷祚炷
周东鹏
薛名山
袁锋
李坚
罗一丹
谢宇
洪珍
谢婵
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Nanchang Hangkong University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C18/16—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 by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1646—Characteristics of the product obtained
    • C23C18/165—Multilayered product
    • C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C18/16—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 by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
    • C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
    • C23C18/1837—Multistep pretreatment
    • C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C18/16—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 by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces

Abstract

本发明一种铜/镍反应性纳米多层膜的制备方法通过前处理去除油脂、氧化膜，再采用化学镀、电化学沉积的方法制备出A‑B‑A‑B 形式排列的Cu/Ni多层膜结构，再利用压力机将其与钛合金垛叠在一起反复轧制，直到多层薄膜达到纳米级厚度，最外层的镍层能很好地防止铜层被氧化，具有优异的焊接稳定性。本发明一种铜/镍反应性纳米多层膜制备简单便捷，能够通过控制制备参数改变其性能，镀层厚度、反应温度可控性强，可有效降低钎焊温度，大幅提高钎焊接头的强度，而且成本较低，对环境影响较小，适合工业化生产，作为钛合金的钎料，在航空航天、军工及3D集成电路中均有广泛应用前景。

Description

一种铜/镍反应性纳米多层膜的制备方法
技术领域
本发明涉及一种铜/镍反应性纳米多层膜的制备方法，具体属于材料微纳连接技术领域。
背景技术
钛合金比强度高，耐热性、耐腐蚀性好，作为结构材料在航空航天领域广泛应用。但高达1725 0C的熔点使其对生产条件的要求比较严格，且存在焊接处强度不足的缺点，生产中常采用钎焊的方式，因此寻求一种合适的钎料迫在眉睫。
反应性纳米多层膜是一种新型含能材料，较低温度下能诱发自蔓延反应，反应瞬间可以获得超过1000 0C的高温，反应波传播速度高达100m/s，在真空或大气环境下可以实现微电子芯片、金属与非金属（陶瓷、碳泡沫等）以及金属与非晶合金等的钎焊和扩散焊连接，是材料微-纳连接领域研究的热点。本发明先采用化学镀、电化学沉积的方法制备出A-B-A-B 形式排列的Cu/Ni多层膜结构，再利用压力机将其与钛合金垛叠在一起反复轧制，直到多层薄膜达到纳米级厚度，该铜镍反应性纳米多层膜不仅可作为钛合金的钎料，在航空航天、军工及3D集成电路中均有广泛应用前景。
发明内容
针对现有技术的不足，本发明提出了一种铜/镍反应性纳米多层膜的制备方法。
为了实现上述目的，本发明一种铜/镍反应性纳米多层膜的制备方法按以下步骤依次进行：
步骤1：前处理
将2 mm×50 mm×2 mm的钛合金片浸入丙酮，超声清洗后取出，用无水乙醇冲洗，热风吹干；其后将其放入浓度为20 g/L的氢氧化钠溶液中碱洗10~30 s后取出，用无水乙醇冲洗，热风吹干；再将其放入酸性溶液中进行酸洗8~15 s后取出，再用无水乙醇冲洗，热风吹干，得到表面处理的钛合金片；
所述的酸性溶液的质量百分比组成为：浓度为1.3~1.4 mol/L的硝酸50%、浓度为0.4~0.5 mol/L的氢氟酸48%和去离子水2%；
步骤2：化学镀镍
将表面处理的钛合金片悬挂浸入pH值为5～6的化学镀溶液中，在60～80℃温度和搅拌条件下，化学镀持续50～80 min，得到镀镍的钛合金片；
所述的化学镀溶液的组成为：硫酸镍30 g/L、磷酸二氢钠30 g/L、柠檬酸钠8 g/L、丁二酸10 g/L、醋酸钠15 g/L；
步骤3：电化学沉积镀铜
将碳片和镀镍的钛合金片分别接在正、负铂片电极上，并固定在装有电解液的电解槽中，碳片和镀镍的钛合金片平行相对，且三分之二浸入电解液，其后在2～4 A/dm2的电流密度下，室温进行电化学沉积镀铜15～30 min；
所述的电解液的组成为：硫酸铜70～90 g/L、硫酸50～200 g/L、氯化钠50～80mg；
步骤4：交替镀镍、镀铜
交替重复步骤2和步骤3共计10次，得到载有多层铜/镍镀膜的钛合金片；
步骤5：轧制
将载有多层铜/镍镀膜的钛合金片放入热压机的模具中，多层铜/镍镀膜与钛合金片在热压机中反复轧制，获得铜/镍反应性纳米多层膜；热压机压制温度设为300~500 ℃、压制时间为0.5~1.5 h，加载压力设为270~290 MPa。
本发明有益效果：
1、本发明先采用化学镀、电化学沉积的方法制备出A-B-A-B 形式排列的Cu/Ni多层膜结构，再利用压力机将其与钛合金垛叠在一起反复轧制，直到多层薄膜达到纳米级厚度，最外层的镍层能很好地防止铜层被氧化，具有优异的焊接稳定性，作为钛合金的钎料，在航空航天、军工及3D集成电路中均有广泛应用前景。
2、本发明制备方法简单便捷，成本较低，对环境影响较小，适合工业化生产。
附图说明
图1为本发明铜/镍反应性纳米多层膜在热压机中示意图。
具体实施方式
实施例1
将2 mm×50 mm×2 mm的钛合金片浸入丙酮，超声清洗10 min，而后使用无水乙醇冲洗，热风吹干；然后将其放入20 g/L的氢氧化钠溶液中碱洗15 s，而后使用无水乙醇冲洗，热风吹干；再将其放入酸性溶液中进行酸洗若干秒，而后使用无水乙醇冲洗，热风吹干。再将其放入酸性溶液中进行酸洗10 s后取出，再用无水乙醇冲洗，热风吹干，得到表面处理的钛合金片；酸性溶液的质量百分比组成为：浓度为1.3mol/L的硝酸50%、浓度为0.4mol/L的氢氟酸48%和去离子水2%。
将表面处理的钛合金片悬挂浸入pH值为6的化学镀液中，在60 ℃温度和搅拌条件下，化学镀持续60 min，得到镀镍的钛合金片；化学镀溶液的组成为：硫酸镍30 g/L、磷酸二氢钠30 g/L、柠檬酸钠8 g/L、丁二酸10 g/L、醋酸钠15 g/L。
将碳片和镀镍的钛合金片分别接在正、负铂片电极上，并固定在装有电解液的电解槽中，碳片和镀镍的钛合金片平行相对，且三分之二浸入电解液，其后在3A/dm2的电流密度下，室温进行电化学沉积镀铜20 min；电解液的组成为：硫酸铜80 g/L、硫酸150g/L、氯化钠70 mg/L.
交替重复步骤2和步骤3共计10次，得到载有多层铜/镍镀膜的钛合金片；
将载有多层铜/镍镀膜的钛合金片放入热压机的模具中，多层铜/镍镀膜与钛合金片在热压机中反复轧制，获得铜/镍反应性纳米多层膜；热压机压制温度设为400 ℃、压制时间为1.0 h，加载压力设为280 MPa。
实施例2
按照实施例1的形式，与之不同之处在于：镀镍采取电沉积的方式。其电流密度为3.5A/dm2，室温进行电化学沉积镀镍40 min；电解液的组成为：硫酸镍70 g/L、柠檬酸钠10g/L、氯化钠120 mg/L。
对比试验采用TC4钛合金作为上下基板，TA18钛合金作为蜂窝芯材料，并使用Ti-Zr-Cu-Ni非晶箔带钎料进行真空钎焊，该钎料的熔点为1000℃。当焊接温度为1060℃，TA18钛合金蜂窝芯发生相变，晶粒长大粗化。钎焊接头的抗拉强度为钛合金母材的80%，其延伸率为5%。
而采用本实施例的铜/镍反应性纳米多层膜的熔点为800℃，在960℃下进行真空钎焊，钎焊接头界面处脆性金属间化合物明显减少，其抗拉强度为钛合金母材的93%，其延伸率为10%。通过使用铜/镍反应性纳米多层膜作为钎料，获得的钎焊接头的性能明显优于使用Ti-Zr-Cu-Ni非晶箔带钎料作为钎料获得的钎焊接头的性能。
实施例3
按照实施例2的形式，与之不同之处在于：镀镍采取电沉积的方式。其电流密度为4.0 A/dm2，室温进行电化学沉积镀镍60 min；电解液的组成为：硫酸镍70 g/L、柠檬酸钠10g/L、氯化钠120 mg/L，即可获得铜/镍反应性纳米多层膜钎料。采用本实施例制备的纳米多层薄膜的熔点为800℃，在960℃下进行真空钎焊，钎焊接头界面处脆性金属间化合物明显减少，其抗拉强度为钛合金母材的93%，其延伸率为10%。通过使用铜/镍反应性纳米多层膜作为钎料，获得的钎焊接头的性能明显优于使用Ti-Zr-Cu-Ni非晶箔带钎料作为钎料获得的钎焊接头的性能。

Claims (1)

1.一种铜/镍反应性纳米多层膜的制备方法，其特征在于：所述的制备方法按以下步骤依次进行：
步骤1：前处理
将2 mm×50 mm×2 mm的钛合金片浸入丙酮，超声清洗后取出，用无水乙醇冲洗，热风吹干；其后将其放入浓度为20 g/L的氢氧化钠溶液中碱洗10~30 s后取出，用无水乙醇冲洗，热风吹干；再将其放入酸性溶液中进行酸洗8~15 s后取出，再用无水乙醇冲洗，热风吹干，得到表面处理的钛合金片；
所述的酸性溶液的质量百分比组成为：浓度为1.3～1.4 mol/L的硝酸50%、浓度为0.4～0.5 mol/L的氢氟酸48%和去离子水2%；
步骤2：化学镀镍
将表面处理的钛合金片悬挂浸入pH值为5～6的化学镀溶液中，在60～80℃温度和搅拌条件下，化学镀持续50～80 min，得到镀镍的钛合金片；
所述的化学镀溶液的组成为：硫酸镍30 g/L、磷酸二氢钠30 g/L、柠檬酸钠8 g/L、丁二酸10 g/L、醋酸钠15 g/L；
步骤3：电化学沉积镀铜
将碳片和镀镍的钛合金片分别接在正、负铂片电极上，并固定在装有电解液的电解槽中，碳片和镀镍的钛合金片平行相对，且三分之二浸入电解液，其后在2～4 A/dm2的电流密度下，室温进行电化学沉积镀铜15～30 min；
所述的电解液的组成为：硫酸铜70～90 g/L、硫酸50～200 g/L、氯化钠50～80 mg；
步骤4：交替镀镍、镀铜
交替重复步骤2和步骤3共计10次，得到载有多层铜/镍镀膜的钛合金片；
步骤5：轧制
将载有多层铜/镍镀膜的钛合金片放入热压机的模具中，多层铜/镍镀膜与钛合金片在热压机中反复轧制，获得铜/镍反应性纳米多层膜；热压机压制温度设为300～500 ℃、压制时间为0.5～1.5 h，加载压力设为270～290 MPa。
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Application publication date: 20210611