CN109553417A - 一种金刚石预制件及其制备方法 - Google Patents

一种金刚石预制件及其制备方法 Download PDF

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CN109553417A
CN109553417A CN201811601792.2A CN201811601792A CN109553417A CN 109553417 A CN109553417 A CN 109553417A CN 201811601792 A CN201811601792 A CN 201811601792A CN 109553417 A CN109553417 A CN 109553417A
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张习敏
郭宏
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GRIMN Engineering Technology Research Institute Co Ltd
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Abstract

本发明属于金属基复合材料技术领域的一种金刚石预制件及其制备方法。金刚石预制件的组分包括金刚石颗粒和低温陶瓷结合剂,低温陶瓷结合剂在金刚石颗粒之间形成结合剂桥;所述低温陶瓷结合剂通式为R2O‑RO‑B2O3‑Al2O3‑SiO2;R2O为碱金属氧化物,RO为碱土金属氧化物。本发明提供的金刚石预制件强度高,有利于实现形状复杂复合材料器件的近净成形制备,缩短了生产周期。

Description

一种金刚石预制件及其制备方法
技术领域
本发明属于金属基复合材料技术领域,特别涉及一种金刚石预制件及其制备方法。
背景技术
随着电子封装领域热管理材料的发展,金刚石增强的铜基、铝基、银基等复合材料日益受到关注,主要用于解决第三代宽禁带半导体芯片散热问题。此类复合材料的制备工艺采用预制件-压力/无压浸渗工艺,因此金刚石预制件的制备尤为重要。然而,现有技术中金刚石预制件存在强度差、搬运过程中易碎、熔渗过程中易出现浮粉等致使制备的复合材料不完整的问题。
发明内容
本发明的目的在于提供一种金刚石预制件及其制备方法,具体技术方案如下:
一种金刚石预制件组分包括金刚石颗粒和低温陶瓷结合剂,低温陶瓷结合剂在金刚石颗粒之间形成结合剂桥;所述低温陶瓷结合剂通式为R2O-RO-B2O3-Al2O3-SiO2;所述R2O为碱金属氧化物,RO为碱土金属氧化物。
优选地,所述R2O为Na2O、K2O、Li2O中的一种或多种;所述RO为CaO、MgO、SrO、BaO中的一种或多种。
所述低温陶瓷结合剂以硼玻璃、硼酸、含有Al2O3和SiO2的矿物、各种金属氧化物、碳酸盐等为原料混合、烧结、研磨得到;可以理解的是,本领域技术人员通过现有技术即可得到通式为R2O-RO-B2O3-Al2O3-SiO2的低温陶瓷结合剂。
所述金刚石预制件的制备方法具体为:以低温陶瓷结合剂、湿润剂、金刚石粉体为原料,采用冷压压制、烘干、真空烧结得到金刚石预制件。
所述低温陶瓷结合剂、湿润剂均匀混合成混合物,再加入金刚石粉体混合均匀、过筛。
所述低温陶瓷结合剂、湿润剂以质量比为1:1-1:2均匀混合成混合物。
所述低温陶瓷结合剂粉料粒度为2-50μm,金刚石粉体粒度为10-200μm。
所述湿润剂为糊精、纸浆废液或聚乙烯醇。
所述金刚石粉体质量与低温陶瓷结合剂和湿润剂混合物的质量之比为10:1~10:2。
所述冷压压制的压力为50-80MPa,保压时间为2-5min。
所述冷压压制后脱模再进行烘干,烘干的温度为80-120℃,烘干时间为6-10h。
所述真空烧结温度为680℃-880℃,烧结时间为20-30min。
本发明的有益效果为:
(1)本发明首次将低温陶瓷结合剂用于制备金刚石预制件,由于金刚石不能烧结到一起,通过低温陶瓷结合剂连接,形成多孔的预制体;本发明加入的结合剂不占用体积,填充在金刚石颗粒堆积形成的孔隙中,通过烧结留下起连接作用的结合剂形成结合桥;
(2)本发明低温陶瓷结合剂与金刚石的润湿性好,烧结后金刚石颗粒之间形成烧结颈(结合剂桥),预制件强度高,可对预制件直接加工,有利于实现形状复杂复合材料器件的近净成形制备,缩短了生产周期;本发明制备的金刚石预制件开口气孔可控,能够满足后期熔渗需要,可广泛应用于压力浸渗/无压浸渗/气压浸渗等工艺制备金刚石增强金属基复合材料,有利于提高金属基复合材料的生产效率。
附图说明
附图1为本发明金刚石预制件制备方法流程图;
附图2为本发明金刚石预制件微观结构示意图;
标号说明:1-金刚石颗粒;2-结合剂桥。
具体实施方式
本发明提供了一种金刚石预制件及其制备方法,下面结合实施例对本发明做进一步的说明。
实施例1
按照图1所示的流程制备多孔金刚石预制件:
(1)将硼玻璃和另一种含有Al2O3和SiO2的矿物按比例均匀混合(如矿物中不含R2O、RO,则加入金属氧化物或碳酸盐),使得SiO2:Al2O3:B2O3:CaO:MgO:K2O:Na2O:Li2O重量份数比为47:17:9:2:3:1:2:1,得到颗粒粒度为50μm的低温陶瓷结合剂粉体,以糊精作湿润剂,将低温陶瓷结合剂粉体和糊精按重量比3:4混合均匀,得到混合物M;然后按照金刚石与混合物M质量比10:1加入粒度为200μm的金刚石颗粒,混合均匀;
(2)将步骤(1)所得混合粉体,在60MPa冷压压力下保压2min,脱模后,在120℃下烘干6h,得到金刚石预制件坯体;
(3)将步骤(2)所得金刚石预制件坯体置于真空烧结炉中,于690℃烧结20min,冷却后制得多孔金刚石预制件。
所制备的多孔金刚石预制件微观结构具体如图2所示,低温陶瓷结合剂在金刚石颗粒1之间形成结合剂桥2;所制备的多孔金刚石预制件的抗弯强度达到20MPa,可满足搬运及二次加工要求。
实施例2
按照图1所示的流程制备多孔金刚石预制件:
(1)将硼玻璃和另一种含有Al2O3和SiO2的矿物按比例均匀混合(如矿物中不含R2O、RO,则加入金属氧化物或碳酸盐),使得SiO2:Al2O3:B2O3:CaO:MgO:K2O:Na2O:Li2O重量份数比为50:20:12:5:5:4:3:1,得到颗粒粒度为10μm的低温陶瓷结合剂粉体,以糊精作湿润剂,将低温陶瓷结合剂粉体和糊精按重量比1:2混合均匀,得到混合物M;然后按照金刚石与混合物M质量比8:1加入粒度为100μm的金刚石颗粒,混合均匀;
(2)将步骤(1)所得混合粉体,在50MPa冷压压力下保压3min,脱模后,在100℃下烘干10h,得到金刚石预制件坯体;
(3)将步骤(2)所得金刚石预制件坯体置于真空烧结炉中,于680℃烧结25min,冷却后制得多孔金刚石预制件。
所制备的多孔金刚石预制件的抗弯强度达到33MPa,可满足搬运及二次加工要求。
实施例3
按照图1所示的流程制备多孔金刚石预制件:
(1)将氧化硅、氧化铝、氧化钙、硼酸、碳酸钙和碳酸钾按比例均匀混合,使得SiO2:Al2O3:B2O3:CaO:K2O重量份数比为52:22:14:6:3,得到颗粒粒度为10μm的低温陶瓷结合剂粉体,以纸浆废液作湿润剂,将低温陶瓷结合剂粉体和纸浆废液按重量比2:5混合均匀,得到混合物M;然后按照金刚石与混合物M质量比7:1加入粒度为50μm的金刚石颗粒,混合均匀;
(2)将步骤(1)所得混合粉体,在70MPa冷压压力下保压5min,脱模后,在120℃下烘干8h,得到金刚石预制件坯体;
(3)将步骤(2)所得金刚石预制件坯体置于真空烧结炉中,于780℃烧结30min,冷却后制得多孔金刚石预制件。
所制备的多孔金刚石预制件的抗弯强度达到45MPa,可满足搬运及二次加工要求。
实施例4
按照图1所示的流程制备多孔金刚石预制件:
(1)将氧化硅、氧化铝、氧化钙、硼酸、碳酸钙、碳酸钾和碳酸钠按比例均匀混合,使得SiO2:Al2O3:B2O3:CaO:K2O:Na2O重量份数比为53:18:10:12:4:3,得到颗粒粒度为2μm的低温陶瓷结合剂粉体,以聚乙烯醇作湿润剂,将低温陶瓷结合剂粉体和聚乙烯醇按重量比1:1混合均匀,得到混合物M;然后按照金刚石与混合物M质量比5:1加入粒度为10μm的金刚石颗粒,混合均匀;
(2)将步骤(1)所得混合粉体,在80MPa冷压压力下保压5min,脱模后,在100℃下烘干10h,得到金刚石预制件坯体;
(3)将步骤(2)所得金刚石预制件坯体置于真空烧结炉中,于800℃烧结20min,冷却后制得多孔金刚石预制件。
所制备的多孔金刚石预制件的抗弯强度达到74MPa,可满足搬运及二次加工要求。

Claims (10)

1.一种金刚石预制件,其特征在于,组分包括金刚石颗粒和低温陶瓷结合剂,低温陶瓷结合剂在金刚石颗粒之间形成结合剂桥;所述低温陶瓷结合剂通式为R2O-RO-B2O3-Al2O3-SiO2;所述R2O为碱金属氧化物,RO为碱土金属氧化物。
2.根据权利要求1所述的金刚石预制件,其特征在于,所述R2O为Na2O、K2O、Li2O中的一种或多种;所述RO为CaO、MgO、SrO、BaO中的一种或多种。
3.一种权利要求1或2所述金刚石预制件的制备方法,其特征在于,以低温陶瓷结合剂、湿润剂、金刚石粉体为原料,采用冷压压制、烘干、真空烧结得到金刚石预制件。
4.根据权利要求3所述的制备方法,其特征在于,所述低温陶瓷结合剂、湿润剂以质量比为1:1-1:2均匀混合成混合物,再加入金刚石粉体混合均匀。
5.根据权利要求3或4所述的制备方法,其特征在于,所述低温陶瓷结合剂粉料粒度为2-50μm,金刚石粉体粒度为10-200μm。
6.根据权利要求3或4所述的制备方法,其特征在于,所述湿润剂为糊精、纸浆废液或聚乙烯醇。
7.根据权利要求3或4所述的制备方法,其特征在于,所述金刚石粉体质量与低温陶瓷结合剂和湿润剂混合物的质量之比为10:1~10:2。
8.根据权利要求3所述的制备方法,其特征在于,所述冷压压制的压力为50-80MPa,保压时间为2-5min。
9.根据权利要求3所述的制备方法,其特征在于,所述烘干的温度为80-120℃,烘干时间为6-10h。
10.根据权利要求3所述的制备方法,其特征在于,所述真空烧结温度为680℃-880℃,烧结时间为20-30min。
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