CN107326364B - 一种Cu-Sn-Ti的金刚石钎焊涂层及其制备方法 - Google Patents

一种Cu-Sn-Ti的金刚石钎焊涂层及其制备方法 Download PDF

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CN107326364B
CN107326364B CN201710412312.7A CN201710412312A CN107326364B CN 107326364 B CN107326364 B CN 107326364B CN 201710412312 A CN201710412312 A CN 201710412312A CN 107326364 B CN107326364 B CN 107326364B
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杨宏
李斌
黄梓杰
傅圣利
李婕
袁兵云
张文忠
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Quanzhou Zhongzhi Diamond Tools Co ltd
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Abstract

本发明公开了一种Cu‑Sn‑Ti的金刚石钎焊涂层，包括钛粉层、锡镀层和附着在金刚石上的铜镀层，锡镀层位于铜镀层和钛粉层之间。其中，各组分按照质量百分比如下：铜60～80％，锡10～25％，钛5～15％。本发明还公开了一种使用电镀的制备方法，先在金刚石表面镀上铜层和锡层，再把镀好的金刚石与钛粉混合烧结，就得到了Cu‑Sn‑Ti的金刚石钎焊料涂层。本发明与金刚石界面结合强度高，包覆钎焊料涂层的金刚石与其他粘接料烧结具有更好的结合力。

Description

一种Cu-Sn-Ti的金刚石钎焊涂层及其制备方法
技术领域
本发明涉及钎焊料的技术领域，特指一种Cu-Sn-Ti的金刚石钎焊涂层及其制备方法。
背景技术
金刚石的高硬度和优良物理机械性能使得金刚石工具成为加工各种坚硬材料不可缺少的有效工具。胎体金属基对金刚石的粘结性(胎体的包镶能力)是影响金刚石工具使用寿命和性能的主要因素之一。
由于金刚石与一般金属和合金之间具有很高的界面能，致使金刚石颗粒不能为一般低熔点合金所浸润，粘结性极差。在传统的金属基烧结金刚石工具制造技术中，金刚石颗粒仅靠胎体冷缩后产生的机械夹持力镶嵌于胎体金属基中，而没有形成牢固的化学键结或冶金结合，胎体与金刚石界面结合不牢，导致金刚石颗粒在工作中易与胎体金属基分离，存在金刚石大量脱落问题，大大降低了金刚石工具的寿命及性能水平。大部分孕镶式工具中金刚石的利用率较低，大量昂贵的金刚石在工作中脱落流失于废屑之中。
在金刚石表面增加金属涂层，可有效改善金刚石的脱落，目前应用最普遍的金属涂层是在金刚石表面微蒸发镀钛。由于钛镀层太薄，不能抵挡烧结过程中胎体石墨化元素对金刚石的侵蚀，钛镀层与胎体金属结合强度不高，金刚石脱落的现象仍然较严重。
目前，用钎焊法制作金刚石(或立方氮化硼)工具已开始成为热点技术，钎焊料是指由铜锡钛等金属烧结而成的合金，它是粉状或片状；使用的时候把钎焊料放到胎体金属上，再把金刚石放到钎焊料上，再进行加热烧结，金刚石就结到胎体金属上了。例如，中国专利CN201610763289中公开了一种活性钎料合金，该活性钎料合金含有以下质量百分比的组分：铜45.0％～70.0％、锌3.0％～47.0％、锡0.5％～40.0％、钛0.1％～15.0％。
钎焊料对金刚石表面润湿性很好，与金刚石界面结合强度高，把钎焊料做成涂层，应该能很好地解决金刚石脱落的问题，但是如何把钎焊料做成涂层，目前还没有很好的办法。因此，本发明人对此做进一步研究，研发出一种Cu-Sn-Ti的金刚石钎焊涂层及其制备方法，本案由此产生。
发明内容
本发明所要解决的技术问题在于提供一种Cu-Sn-Ti的金刚石钎焊涂层及其制备方法，与金刚石界面结合强度高，包覆钎焊料涂层的金刚石与其他粘接料烧结具有更好的结合力。
为解决上述技术问题，本发明的技术解决方案是：
一种Cu-Sn-Ti的金刚石钎焊涂层，包括钛粉层、锡镀层和附着在金刚石上的铜镀层，锡镀层位于铜镀层和钛粉层之间。
进一步，所述的钎焊涂层，各组分按照质量百分比如下：铜60～80％，锡10～25％，钛5～15％。
进一步，所述的钎焊涂层，各组分按照质量百分比如下：铜60％，锡25％，钛15％。
进一步，所述的钎焊涂层，各组分按照质量百分比如下：铜80％，锡15％，钛5％。
进一步，所述的钎焊涂层，各组分按照质量百分比如下：铜75％，锡17.5％，钛7.5％。
一种Cu-Sn-Ti的金刚石钎焊涂层的制备方法，包括以下步骤：
步骤一、金刚石表面化学镀铜：把金刚石放入化学镀铜溶液中，60℃-70℃镀施5min-45min，得到铜镀层，铜镀层增重用时间控制，用量为45-50目金刚石5g/150-750ml镀铜溶液；
步骤二、金刚石表面再滚镀锡：把镀好铜的金刚石洗净，放入电镀锡或化学镀锡溶液中，60℃-70℃滚镀50min-180min，得到锡镀层，锡镀层增重用时间和电流控制；
步骤三、钛粉烧结：把镀好的金刚石洗净，烘干，再和300目钛粉混匀，用量比为：3g金刚石/10g钛粉，放入真空炉中，抽真空1-30Pa，720-860℃保温60-300min，在锡镀层熔化时，钛粉也熔入或粘接形成钛粉层。由于钛粉包围，金刚石之间不会粘连，冷却后，筛分金刚石与钛粉，就得到了包覆Cu-Sn-Ti钎焊料涂层的金刚石。
进一步，步骤一还包括预处理金刚石：把金刚石浸入10％NaOH溶液中煮沸5min，用水洗净；再放入浓HNO3中煮沸30min，用水洗至中性，再将金刚石浸泡在20g/L SnCl2与30ml/L 36％HCl混合溶液中，超声震荡30min，用水洗净，再在2g/L 70℃AgNO3溶液中浸泡，搅拌30min，洗净，再放入40g/L NaH2PO2·H2O浸泡15min，水洗3次。
进一步，在步骤一中化学镀铜溶液配方如下：CuSO4·5H2O 10-30g/L，酒石酸钾钠NaKC4H4O6·4H2O 10-30g/L，Na2EDTA 10-30g/L，NaOH 10-30g/L，甲醛CH2O 8-20ml/L。
进一步，在步骤二中，电镀锡溶液配方如下：K2SnO3·3H2O 160-230g/L，CH3COOK0-15g/L，KOH 10-30g/L，溶液温度：60～90℃，电镀锡溶液的电流密度为3-15A/dm2，电压为4-6V。
进一步，在步骤二中，化学镀锡配方如下：氯化亚锡90～120g/L，酒石酸钾钠150～200g/L，氢氧化钠100～150g/L，次亚磷酸钠90～200g/L，温度为75～90℃，时间为30～120min。
采用上述方案后，由于本发明使用电镀的方法，先在金刚石表面镀上铜层和锡层，再把镀好的金刚石与钛粉混合烧结，就得到了Cu-Sn-Ti的金刚石钎焊料涂层。抗弯强度测试表明：用钎焊料涂层金刚石烧结的标准块比用镀钛金刚石烧结的标准块强度大。
附图说明
图1是本发明的结构示意图；
图2是本发明和粘接料混合烧结后的结构示意图。
标号说明
金刚石 1 铜镀层 2 锡镀层 3
钛粉层 4 铜锡钛钎焊料合金涂层 5
具体实施方式
下面结合附图和具体实施例对本发明作进一步详述。本发明所揭示的是一种Cu-Sn-Ti的金刚石钎焊涂层及其制备方法，如图1所示，为本发明的较佳实施例，包括钛粉层4、锡镀层3和附着在金刚石1的铜镀层2，锡镀层3位于铜镀层2和钛粉层4之间，其中各组分按照质量百分比如下：铜60～80％，锡10～25％，钛5～15％。
实施例1
一种Cu-Sn-Ti的金刚石钎焊涂层，其中各组分按照质量百分比如下：铜60％，锡25％，钛15％。其制备方法如下：
预处理金刚石：把金刚石浸入10％NaOH溶液中煮沸5min，用水洗净；再放入浓HNO3中煮沸30min，用水洗至中性，再将金刚石浸泡在20g/L SnCl2与30ml/L 36％HCl混合溶液中，超声震荡30min，用水洗净，再在2g/L 70℃AgNO3溶液中浸泡，搅拌30min，洗净，再放入40g/L NaH2PO2·H2O浸泡15min，水洗3次。
金刚石表面化学镀铜：把预处理后金刚石放入化学镀铜溶液中，60℃-70℃镀施5min-45min，得到铜镀层，铜镀层增重用时间控制，用量为45-50目金刚石5g/150-750ml镀铜溶液。化学镀铜溶液配方如下：CuSO4·5H2O 30g/L，酒石酸钾钠NaKC4H4O6·4H2O 10g/L，Na2EDTA 30g/L，NaOH 10g/L，甲醛CH2O 8ml/L。
金刚石表面再滚镀锡：把镀好铜的金刚石洗净，放入电镀锡溶液中，60℃-70℃滚镀50min-180min，得到锡镀层，锡镀层增重用时间和电流控制；电镀锡溶液配方如下：K2SnO3·3H2O 160g/L，CH3COOK 15g/L，KOH 10g/L，电镀锡溶液的电流密度为3-15A/dm2，电压为4-6V。
钛粉烧结：把镀好的金刚石洗净，烘干，再和300目钛粉混匀，用量比为：3g金刚石/10g钛粉。放入真空炉中，抽真空1-30Pa，720-860℃保温60-300min，镀层熔化时钛粉也熔入镀层。由于钛粉包围，金刚石之间不会粘连，冷却后，筛分金刚石与钛粉，就得到了包覆Cu-Sn-Ti钎焊料涂层的金刚石。
如图2所示，使用时，将包覆Cu-Sn-Ti钎焊料涂层的金刚石和粘接料混合烧结，烧结后钎焊料涂层就完全形成合金层，即铜锡钛钎焊料合金涂层5。
抗弯强度测试表明：用钎焊料涂层金刚石烧结的标准块抗弯强度为1254.2Mpa，比用镀钛金刚石烧结的标准块强度1173.0Mpa大。
实施例2
实施例2与实施例1采用一样的制备方法，与实施例1不同在于，金刚石钎焊涂层，其中各组分按照质量百分比如下：铜80％，锡15％，钛5％。
化学电镀铜溶液的配方如下：CuSO4·5H2O 10g/L，酒石酸钾钠NaKC4H4O6·4H2O30g/L，Na2EDTA 10g/L，NaOH 30g/L，甲醛CH2O 20ml/L。
化学电镀锡溶液配方如下：K2SnO3·3H2O 230g/L，KOH 30g/L，电镀锡溶液的电流密度为3-15A/dm2，电压为4-6V。
用该钎焊料涂层金刚石烧结的标准块抗弯强度为1211.6Mpa。
实施例3
实施例3与实施例1采用一样的制备方法，与实施例1不同在于，金刚石钎焊涂层，其中各组分按照质量百分比如下：铜75％，锡10％，钛15％。
化学电镀铜溶液的配方如下：CuSO4·5H2O 15g/L，酒石酸钾钠NaKC4H4O6·4H2O30g/L，Na2EDTA 15g/L，NaOH 25g/L，甲醛CH2O 20ml/L。
化学镀锡配方如下：氯化亚锡120g/L，酒石酸钾钠150g/L，氢氧化钠150g/L，次亚磷酸钠90g/L，温度为90℃，时间为30～120min。
用该钎焊料涂层金刚石烧结的标准块抗弯强度为1234.0Mpa。
实施例4
实施例4与实施例3采用一样的制备方法，与实施例3不同在于，金刚石钎焊涂层，其中各组分按照质量百分比如下：铜75％，锡17.5％，钛7.5％。
化学镀锡配方如下：氯化亚锡90g/L，酒石酸钾钠200g/L，氢氧化钠150g/L，次亚磷酸钠200g/L，温度为75℃，时间为30～120min。
用该钎焊料涂层金刚石烧结的标准块抗弯强度为1266.4Mpa。
综上所述，本发明直接在金刚石表面做Cu-Sn-Ti钎焊料涂层，在金刚石表面做一层钎焊料，在使用的时候，如图2所示，把有钎焊料涂层的金刚石和粘接料混合，热压烧结成块，做成锯片上用的刀头。本发明的金刚石界面结合强度高，包覆钎焊料涂层的金刚石与其他粘接料烧结具有更好的结合力，能很好地解决金刚石脱落的问题。
以上所述，仅是本发明的较佳实施例而已，并非对本发明的技术范围作任何限制，故但凡依本发明的权利要求和说明书所做的变化或修饰，皆应属于本发明专利涵盖的范围之内。

Claims (5)

1.一种Cu-Sn-Ti的金刚石钎焊涂层的制备方法，其特征在于：包括以下步骤：
步骤一、金刚石表面化学镀铜：把金刚石放入化学镀铜溶液中，60℃-70℃镀施5 min -20 min，得到铜镀层，铜镀层增重用时间控制，用量为45-50目金刚石5g /150ml-750ml镀铜溶液；
步骤二、金刚石表面再滚镀锡：把镀好铜的金刚石洗净，放入电镀锡或化学镀锡溶液中，60℃-70℃滚镀50 min -180 min，得到锡镀层，锡镀层增重用时间和电流控制；
步骤三、钛粉烧结：把镀好的金刚石洗净，烘干，再和300目钛粉混匀，用量比为：3g金刚石/10g钛粉，放入真空炉中，抽真空1-30Pa，720-860℃保温60-300min，在锡镀层熔化时，钛粉也熔入或粘接形成钛粉层，由于钛粉包围，金刚石之间不会粘连，冷却后，筛分金刚石与钛粉，就得到了包覆Cu-Sn-Ti钎焊料涂层的金刚石。
2.根据权利要求1所述的一种Cu-Sn-Ti的金刚石钎焊涂层的制备方法，其特征在于：步骤一还包括预处理金刚石：把金刚石浸入10%NaOH溶液中煮沸5min，用水洗净；再放入浓HNO3中煮沸30min，用水洗至中性，再将金刚石浸泡在20g/L SnCl2与30ml/L 36%HCl混合溶液中，超声震荡30min，用水洗净，再在2g/L 70℃ AgNO3溶液中浸泡，搅拌30min，洗净，再放入40g/L NaH2PO2·H2O浸泡15min，水洗3次。
3.根据权利要求1所述的一种Cu-Sn-Ti的金刚石钎焊涂层的制备方法，其特征在于：在步骤一中化学镀铜溶液配方如下：CuSO4·5H2O 10-30g/L，酒石酸钾钠NaKC4H4O6·4H2O 10-30g/L，Na2EDTA 10-30g/L，NaOH 10-30g/L，甲醛CH2O 8-20ml/L。
4.根据权利要求1所述的一种Cu-Sn-Ti的金刚石钎焊涂层的制备方法，其特征在于：在步骤二中，电镀锡溶液配方如下：K2SnO3·3H2O 160-230g/L，CH3COOK 0-15g/L，KOH 10-30g/L，溶液温度：60~90℃，电镀锡溶液的电流密度为3-15A/dm2，电压为4-6V。
5.根据权利要求1所述的一种Cu-Sn-Ti的金刚石钎焊涂层的制备方法，其特征在于：在步骤二中，化学镀锡配方如下：氯化亚锡 90~120g/L，酒石酸钾钠 150~200g/L，氢氧化钠100~150g/L，次亚磷酸钠 90~200g/L，温度为75~90℃，时间为30~120min。
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