CN105884375A - 一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法 - Google Patents

一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法 Download PDF

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CN105884375A
CN105884375A CN201610178439.2A CN201610178439A CN105884375A CN 105884375 A CN105884375 A CN 105884375A CN 201610178439 A CN201610178439 A CN 201610178439A CN 105884375 A CN105884375 A CN 105884375A
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江涌
吴澜尔
黄新华
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Abstract

一种Si3N4‑TiZrN2‑TiN复合导电陶瓷，合成该复合导电陶瓷的原料包括：Si3N4、ZrN、TiN、Y2O3、La2O3、AlN；该复合导电陶瓷的最终产物里包括Si3N4相、TiN相和金属氮化物的固溶体TiZrN2相。其中，AlN的加入避免了常规方式中加入Al2O3所引起的挥发，并且加入AlN会使最终产品的表面比加入Al2O3光滑；本发明名还给出一种Si3N4‑TiZrN2‑TiN复合导电陶瓷的液相烧结法。本发明有益效果如下：1.电阻率低；本发明的复合导电陶瓷用SX1944四探针测试仪测试样品电阻为10‑2Ω·cm量级，远远低于同类产品。2.机械强度高；本发明的复合导电陶瓷用载荷为10kg，加压时间为5s的条件测量样品的维氏硬度为14.7GPa；利用硬度压痕四角处扩展的裂纹长度计算样品的断裂韧性为7.8MPa.m0.5保持了氮化硅陶瓷原有的强度和硬度。

Description

一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法
技术领域：
本发明涉及导电陶瓷技术领域，具体地说，涉及一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法。
背景技术：
氮化硅(Si3N4)是一种性能很好的结构陶瓷材料，具有质量轻、高强度、高硬度、高耐腐蚀性等，可应用于各行各业。制备氮化硅陶瓷材料的方法很多，有热压、常压、反应等烧结方法，其中常压烧结方法简单易行，耗能少。由于氮化硅是共价键化合物，自扩散系数低，本身很难直接烧结成瓷，因此往往加入一些氧化物等作为烧结助剂进行烧结。常用的有Al2O3、Y2O3、MgO2等。这些添加物在烧结过程中形成液相促使氮化硅陶瓷烧结致密，以达到材料高强度、高硬度的要求。
由于Si3N4陶瓷本身高强度和高硬度的性能使得后期加工困难，常以金刚石刀具进行切割，但传统的金刚石加工的方法加工效率低且成本昂贵。成本低、效率高的放电(电火花)加工技术已成功用于金属制品加工，若能用于加工Si3N4陶瓷则会大大提高加工效率和降低加工成本，但能用放电加工的材料必须具有一定的导电性，其电阻率要求低达100Ω·cm量级及以下，但Si3N4陶瓷属于绝缘体，其电阻率约为1015Ω·cm量级，是不可能用放电方法进行加工的。所以人们想到了用另外一种导电性很好的材料加入Si3N4中制备成Si3N4基复合导电性材料，使其电阻率下降到能用于电火花加工的程度。在CN1272283C的专利里使用了金属Ti和Ta，从而使最终烧结的复合氮化硅电阻率降到100Ω·cm量级，刚刚达到放电加工的要求，并且其硬度和断裂韧性较未加导电助剂的氮化硅陶瓷差。
发明内容：
本发明旨在解决上述问题，提供一种电阻率低、硬度和断裂韧性优良的一种Si3N4-TiZrN2-TiN复合导电陶瓷；同时还提供一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法。
一种Si3N4-TiZrN2-TiN复合导电陶瓷，合成该复合导电陶瓷的原料包括：Si3N4、ZrN、TiN、Y2O3、La2O3、AlN；该复合导电陶瓷的的最终产物里包括Si3N4相、TiN相和金属氮化物的固溶体TiZrN2相。其中，AlN的加入可避免常规方式中加入Al2O3所引起的低温挥发，并且加入AlN会使最终产品的表面比加入Al2O3光滑。
由于是采用烧结工艺来制作的复合导电陶瓷材料，各材料烧结过程中的热膨胀系数是至关重要的的，如果热膨胀系数相差大，则不利于烧结，会影响最终成品的密度、硬度和断裂韧性，故所选择的导电助剂的除了要电阻率低，还要热膨胀系数要与氮化硅相差不大。另外，如果还兼有其它好的机械性能则更为理想。氮化钛和氮化锆都有高电导率，两者的电阻率都在10-4Ω·cm量级，ZrN比TiN更低(TiN：2.07×10-4Ω·cm；ZrN：1.4×10-4Ω·cm)；热膨胀系数和氮化硅在一个数量级，均为约10-6K-1，且ZrN更接近氮化硅(Si3N4：3.64×10-6K-1；ZrN：7.3×10-6K-1；TiN：9.35×10-6K-1)；另外TiN、ZrN本身都的硬度都比氮化硅高很多，其中，ZrN的硬度比TiN碳化钛更高，ZrN作为添加剂有增强韧性的作用。
优选的，Si3N4∶TiN∶Y2O3∶La2O3∶AlN＝(9～11)∶(5.4～6.6)∶(0.8～1.2)∶(0.8～1.2)∶(1.3～1.66)，ZrN的加入量为8～15w.t％。
一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法，包括以下步骤：
(1)配料混合：将Si3N4、TiN、Y2O3、La2O3、AlN以(9～11)∶(5.4～6.6)∶(0.8～1.2)∶(0.8～1.2)∶(1.3～1.66)的比例混合，ZrN的加入量为8～15w.t％，之后在研钵中加入酒精研磨1～3h后干燥；其中，Si3N4的α相含量高于70％，纯度高于97％，粒度为0.6～0.8μm，TiN粒度为18～22nm，ZrN粒度为16～21nm；
(2)成型及烧结：将干燥后的混合料用模具干压成型再经冷等静压后放入烧结炉中在N2保护气氛中进行烧结，烧结温度为1760±25℃，保温时间根据样品的大小可设为1～3h。
本发明有益效果如下：
1.电阻率低；本发明的复合导电陶瓷用SX1944四探针测试仪测试样品电阻为10-2Ω·cm量级，远低于同类产品。
2.机械强度高；本发明的复合导电陶瓷用载荷为10kg，加压时间为5s的条件测量样品的维氏硬度为14.7GPa；利用硬度压痕四角处扩展的裂纹长度计算样品的断裂韧性为7.8MPa.m0.5，达到了氮化硅陶瓷原有的高硬度和高断裂韧性。
具体实施方式：
一种Si3N4-TiZrN2-TiN复合导电陶瓷，合成该复合导电陶瓷的原料包括：Si3N4、ZrN、TiN、Y2O3、La2O3、AlN；该复合导电陶瓷的的最终产物里包括Si3N4相、TiN相和金属氮化物的固溶体TiZrN2相。
在本实施方式中，Si3N4∶TiN∶Y2O3∶La2O3∶AlN＝(9～11)∶(5.4～6.6)∶(0.8～1.2)∶(0.8～1.2)∶(1.3～1.66)，ZrN的加入量为8～15w.t％。
一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法，Si3N4选用α相含量高于70％粉料，纯度高于97％，平均粒度0.7μm；Y2O3、La2O3和AlN为市售，化学纯；TiN购自合肥凯尔纳米能源科技股份有限公司，纯度为99.2％，平均粒度为20nm；ZrN购自锦州金鑫股份有限公司；将各成分按(9～11)∶()∶(5.4～6.6)∶(0.8～1.2)∶(0.8～1.2)∶(1.3～1.66)的比例称量配料，将配好的料加入酒精在玛瑙研钵中混磨2小时或加入酒精和ZrO2球在聚氨酯筒中球磨1小时后置于空气中干燥；再将干燥好的混合料用不锈钢磨具干压成方块后放入烧结炉中在N2保护气氛中进行烧结，烧结温度为1760℃±25℃，保温时间根据样品的大小可设为1-3h。
利用日本理学D/MAX-RB型X射线衍射仪对烧结进行样品的物相分析，证实样品内含有金属氮化物的固溶体TiZrN2。

Claims (3)

1.一种Si3N4-TiZrN2-TiN复合导电陶瓷，其特征在于：合成该复合导电陶瓷的原料包括：Si3N4、ZrN、TiN、Y2O3、La2O3、AlN；该复合导电陶瓷的的最终产物里包括Si3N4相、TiN相和金属氮化物的固溶体TiZrN2相。
2.如权利要求1所述的一种Si3N4-TiZrN2-TiN复合导电陶瓷，其特征在于：Si3N4∶TiN∶Y2O3∶La2O3∶AlN＝(9～11)∶(5.4～6.6)∶(0.8～1.2)∶(0.8～1.2)∶(1.3～1.66)，ZrN的加入量为8～15w.t％。
3.一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法，其特征在于：包括以下步骤：
(1)配料混合：将Si3N4、TiN、Y2O3、La2O3、AlN以(9～11)∶(5.4～6.6)∶(0.8～1.2)∶(0.8～1.2)∶(1.3～1.66)的比例混合，ZrN的加入量为8～15w.t％，之后在研钵中加入酒精研磨1～3h后干燥；其中，Si3N4的α相含量高于70％，纯度高于97％，粒度为0.6～0.8μm，TiN粒度为18～22nm，ZrN粒度为16～21nm；
(2)成型及烧结：将干燥后的混合料用模具干压成型再经冷等静压后放入烧结炉中在N2保护气氛中进行烧结，烧结温度为1760±25℃，保温时间为1～3h。
CN201610178439.2A 2016-03-18 2016-03-18 一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法 Expired - Fee Related CN105884375B (zh)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN112679211A (zh) * 2021-01-29 2021-04-20 北方民族大学 一种ZrN-镧氧化物复相陶瓷及其无压反应烧结制备方法
CN113121245A (zh) * 2019-12-31 2021-07-16 辽宁省轻工科学研究院有限公司 一种可放电加工的氮化硅基复合导电陶瓷及其制备方法

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