CN116984775A - 一种高CuNi含量低熔点高熵合金钎料及其钎焊金刚石 - Google Patents
一种高CuNi含量低熔点高熵合金钎料及其钎焊金刚石 Download PDFInfo
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- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
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- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/302—Cu as the principal constituent
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- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3033—Ni as the principal constituent
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Abstract
一种高CuNi含量低熔点高熵合金钎料及其钎焊金刚石,高熵合金钎料的化学成分原子百分比为:Cu:33%~35%、Ni:33%~35%、Fe:8%~10%、Cr:8%~10%、Sn:8%~10%,通过真空电弧熔炼制备合金钎料。高熵合金冷却后形成富FeCrNi的FCC相、富Cu相和富Sn相,硬度为330HV,熔点为935℃,这使得钎料可在1000℃以下较低温度对金刚石钎焊。与传统镍基钎料需在1050℃以上较高温度钎焊金刚石相比,本发明高熵合金钎料能够显著降低金刚石钎焊温度及焊后热损伤,金刚石焊后表面形貌完整,磨粒具有较高的出露度,未出现明显的裂纹、腐蚀坑和石墨化现象。同时,高熵效应和迟滞扩散效应减少了钎缝脆性相的形成,保证了接头的力学性能,对金刚石的把持力和润湿性更高,钎焊后具备更优的耐磨性。
Description
技术领域
本发明属于钎焊技术领域,具体涉及一种高CuNi含量低熔点高熵合金钎料及其钎焊金刚石的方法。
背景技术
钎焊金刚石工具因其高强度、高硬度、高耐磨性常被用来加工硬脆材料。目前,用于钎焊金刚石工具的钎料主要有Ag基、Ni基和Cu基,Ag基钎料能很好地润湿金刚石,但其成本过高;Ni基钎料具有较高的耐磨性能,结合强度高,但熔点较高,高温钎焊后金刚石表面容易形成脆性化合物,并产生石墨化等热损伤;Cu基钎料的熔点低,对金刚石的浸润性较好,并且Cu元素的成本较低,是工业应用较为广泛的金刚石钎焊用钎料,主要的铜基钎料有Cu-Sn、Cu-Mn和Cu-Fe系等。但是Cu基钎料的硬度和强度较低,一般低于200HV,造成钎焊层的耐磨性不高,且与金刚石结合强度较低,高速磨削过程中易出现金刚石磨粒的过早脱落缺陷。
高熵合金作为近年来快速发展的新型合金,因其优异的力学性能如高强度、高韧性、良好的化学稳定性和耐腐蚀性能而备受关注。特别是其“高熵效应”和“迟滞扩散效应”可显著降低钎料与母材之间的过度扩散和脆性化合物的大量形成。此外,利用成分“鸡尾酒效应”,可以加入反应活性元素提高填充金属在母材表面的润湿性,已在钎焊高熔点的异种金属或硬质陶瓷领域展现明显的优势。但大多数高熵合金熔点较高,难以避免金刚石工具过高温度钎焊易产生的热损伤难题。本发明提供了一种高CuNi含量低熔点高熵合金钎料,Cu/Ni含量高使其兼具Cu基、Ni基钎料的优势,Sn元素的添加使其熔点降低至935℃,可实现1000℃以下钎焊金刚石。超饱和固溶强化作用使得钎料硬度和耐磨性明显优于Cu基钎料,钎缝接头处复杂脆性相和金刚石表面石墨化等热损伤问题明显优于Ni基钎料。
发明内容
本发明提供了一种高CuNi含量低熔点高熵合金钎料、制备方法及其钎焊金刚石。本发明所述高熵合金钎料具有较低的熔点,改善了传统Ni基钎料因钎焊温度过高易形成复杂脆性相,及金刚石表面石墨化等热损伤问题。而且,硬度和耐磨性等力学性能明显优于现有铜基钎料,可明显提高钎焊金刚石工具的加工性能和使用寿命。
为了实现以上目的,本发明公开了一种高CuNi含量低熔点高熵合金钎料,按原子百分比包括以下成分:Cu:33%~35%、Ni:33%~35%、Fe:8%~10%、Cr:8%~10%、Sn:8%~10%。钎料合金由富FeCrNi的FCC相、富Cu相和富Sn固溶体相组成,硬度达到330HV。
本发明公开了一种高CuNi含量低熔点高熵合金钎料,熔点为935℃,可在1000℃以下实现金刚石的钎焊,所述的钎料与金刚石高温钎焊具有良好的润湿性。
本发明还公开了上述高熵合金钎料的制备方法,包括以下步骤:
(1)按质量百分比称量称取相应的金属单质原料,放入酒精和丙酮溶液中用超声波清洗10min,然后烘干;
(2)将步骤(1)中的原料按照熔点由低到高的顺序放入真空电弧熔炼炉中,在真空度为5×10-3MPa,氩气作为保护气的条件下,反复熔炼5次,待合金随炉冷却后从炉中取出,得到高熵合金铸锭。
优选的,所述步骤(1)中低熔点高熵合金中单质Fe、Cr、Ni、Cu、Sn的纯度均大于99.9%以上;步骤(2)中熔炼时脉冲电弧加热电流范围为50~100A。
本发明还公开了上述高熵合金钎料钎焊金刚石工具的方法,包括以下步骤:
(1)通过线切割将高熵合金铸锭切割成薄片状,放入丙酮酒精溶液中用超声波清洗10min,烘干;
(2)用400#和600#砂纸打磨45号钢块的表面,将45号钢块和金刚石磨料先后放在丙酮和酒精溶液中进行超声清洗,然后烘干;
(3)将片状钎料铺在45号钢块表面,金刚石磨粒铺在钎料层表面,然后放入真空热压炉中进行钎焊,真空度为5.0×10-3MPa,在970℃~1000℃温度下保温8min,待冷至室温后取出样品。
优选的,所述步骤(1)中钎料厚度为0.15mm,尺寸为15mm×6mm;步骤(2)中基体尺寸为为15mm×10mm×6mm;步骤(3)中升温速率10℃/min。
与现有技术相比,本发明具有以下有益效果:
(1)本发明所述高CuNi含量低熔点高熵合金凝固后形成富FeCrNi-FCC相、富Cu相和富Sn固溶体相。低熔点富Sn相在836℃首先熔化,合金最终在935℃时完全熔化成液相,这使得合金钎料可以在1000℃以下较低钎焊温度实现金刚石与钎料合金的高强度结合。与传统镍基钎料需在1050℃以上较高温度钎焊相比,显著降低了金刚石钎焊后的高温热损伤。
(2)本发明所述高CuNi含量低熔点高熵合金中,富FeCrNi-FCC增强相中高硬度Fe、Cr、Ni元素以及富Cu、富Sn相的固溶强化作用,使得高熵合金钎料硬度达到330HV,高于传统Cu基钎料200HV以下的显微硬度。
(3)本发明所述高CuNi含量低熔点高熵合金中,研究发现Ni、Cu元素等摩尔添加提高了钎料合金的系统熵值,且由于Cu和Ni无限固溶,削弱了触媒元素Ni对金刚石石墨化的催化作用,钎焊后金刚石表面未出现石墨化等热损伤。Sn的熔点较低,能够显著降低合金的熔点并提高对金刚石的润湿性。Fe和强碳化物形成元素Cr的加入进一步提高合金的混合熵,同时具有提高钎料和金刚石高强度结合力的作用。
(4)本发明所述高CuNi含量低熔点高熵合金,由于热力学上的高熵效应和迟滞扩散效应,钎缝处无复杂脆性金属间化合物的生成,显著提高了钎焊金刚石工具的力学性能和使用寿命。
附图说明
图1为本发明实施例低熔点高熵合金钎料的X-射线物相分析;
图2为本发明实施例低熔点高熵合金钎料的SEM凝固组织;
图3为本发明实施例低熔点高熵合金钎料的DSC曲线;
图4为本发明实施例高熵合金钎料钎焊后的金刚石表面形貌;
图5为本发明实施例高熵合金钎焊后的金刚石表面拉曼光谱;
图6为本发明实施例高熵合金钎料钎焊时与金刚石的润湿角;
图7为本发明实施例不同温度钎焊金刚石后的摩擦磨损结果。
具体实施方式
为了更好的理解本发明所提供的技术方案,以下结合附图和实例进一步说明本发明内容。
将高熵合金钎料的原子百分比Cu:33%~35%、Ni:33%~35%、Fe:8%~10%、Cr:8%~10%、Sn:8%~10%换算成质量百分比,称量单质铁、铬、铜、铁、镍、锡。将称取好的原料放入酒精和丙酮溶液中超声波清洗10min,然后烘干。将配好的原料按熔点由低到高的顺序依次放入真空电弧熔炼炉中,反复熔炼5次,得到合金铸锭。熔炼过程中,其真空度保持在5.0×10-3MPa,脉冲电弧加热电流范围为50~100A,高纯氩气作为保护气体。将熔炼好的高熵合金铸锭用线切割切成厚度为0.15mm,尺寸为15mm×6mm的薄片状,放入酒精丙酮溶液中清洗10min,然后烘干。本实施案例中基体选用为尺寸为15mm×10mm×6mm的45号钢,使用400#和600#砂纸对45号钢基体表面进行打磨以去除基体表面氧化物,将金刚石磨粒与45号钢放入丙酮和酒精溶液中用超声波清洗10min,然后烘干。将片状钎料平铺在45号钢基体表面,金刚石磨粒整齐铺在钎料层的表面,放入真空热压炉中,在970℃~1060℃的真空环境中钎焊保温8min,待冷却至室温后取出样品。
图1为本实施案例中低熔点高熵合金的XRD图,可以看出合金主要由富FeCrNi-FCC相、富Cu相和富Sn固溶体相组成,无复杂脆性相。图2为本实施例低熔点高熵合金钎料凝固组织照片,表1所示为图中三处典型区域的EDS能谱分析,其中A区为富FeCrNi的FCC相,B区为富Cu相,C区为富Sn相。
表1图2中三处典型组织区域的EDS能谱分析(at.%)
图3为本实施例中低熔点高熵合金的DSC曲线,从图中可以看出富Sn相在836℃首先熔化,合金完全熔化的熔点为935℃。图4为本实施例中高熵合金钎焊金刚石的表面形貌图,可以看出金刚石与基体牢固结合,金刚石表面形貌完整,有较高的出露度,表面未出现裂纹和蚀坑等缺陷。图5为本实施案例中低熔点高熵合金钎焊后金刚石表面的拉曼光谱图,图中仅存在1332cm-1处的金刚石峰,未发现明显的石墨峰,表明金刚石钎焊后表面无明显石墨化等热损伤。图6为本实施例高熵合金钎料钎焊时与金刚石的润湿角,仅为11°,具有良好的润湿性。图7为本实施例中低熔点高熵合金不同温度钎焊金刚石后的摩擦磨损结果,可以看出当钎焊温度为1000℃时,对磨材料瓷砖的去除量最高,达到68mg。而本发明对比采用传统Ni-Cr-B-Si-Fe钎料钎焊金刚石,在相同的摩擦磨损实验条件下,瓷砖去除量仅为36mg。表明本发明公开的高熵合金钎料不仅在1000℃具有最优的钎焊性能,且耐磨性能明显高于目前工业上广泛采用的Ni基钎料。
Claims (4)
1.一种高CuNi含量低熔点高熵合金钎料及其钎焊金刚石,其特征在于所述高熵合金的化学成分按原子百分比组成为:Cu:33%~35%、Ni:33%~35%、Fe:8%~10%、Cr:8%~10%、Sn:8%~10%。
2.根据权利要求1所述的一种高CuNi含量低熔点高熵合金钎料,其特征在于所述高熵合金由富FeCrNi的FCC相、富Cu相和富Sn固溶体相组成,无复杂脆性相,钎料与金刚石具有优异的润湿性和高的固溶强化效果。
3.根据权利要求1所述的一种高CuNi含量低熔点高熵合金钎料,其特征在于高熵合金钎料熔点为935℃,可在970~1000℃钎焊金刚石,钎焊真空度为5.0×10-3MPa,保温时间为8min,升温速率为10℃/min,焊后金刚石表面无石墨化损伤,并与钎料具有良好的结合强度。
4.根据权利要求1所述的一种高CuNi含量低熔点高熵合金钎料,其特征在于所述高熵合金钎焊后硬度和耐磨性高于Cu基和Ni基钎料,钎焊接头处复杂脆性相和金刚石热损伤问题明显好于Ni基钎料,可应用于砂轮、钻头、锯片等磨切削工具领域。
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