CN110156468A - 一种ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺 - Google Patents

一种ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺 Download PDF

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CN110156468A
CN110156468A CN201910339931.7A CN201910339931A CN110156468A CN 110156468 A CN110156468 A CN 110156468A CN 201910339931 A CN201910339931 A CN 201910339931A CN 110156468 A CN110156468 A CN 110156468A
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zirconium
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吴恒
刘长青
常小靖
伍媛婷
王秀峰
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Gongyi Van Research Yihui Composite Material Co Ltd
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Abstract

本发明公开了一种ZrC‑ZrB2‑SiC陶瓷复合粉体的前驱体转化法制备工艺，以八水氧氯化锆，硼酸，正硅酸乙酯，葡萄糖为起始原料，以无水乙醇和去离子水为溶剂。其中，原料物质的量硼酸：八水氧氯化锆：正硅酸乙酯为1‑5:1:0.5‑5，质量比葡萄糖：正硅酸乙酯＝1‑4:1。分别配制锆前驱体溶液，硼酸溶液、正硅酸乙酯溶液以及葡萄糖溶液，将各溶液混合均匀得到硼硅锆前驱体溶液；将硼硅锆前驱体溶液烘干后，在氩气气氛保护下，1450‑1600℃热处理1‑2h，得到ZrC‑ZrB2‑SiC陶瓷粉体。所制备的陶瓷粉体粒径均一，平均粒径约150nm。本发明具有工艺简单，周期短，能耗低，成本低的特点，所得到的陶瓷相粒度均匀细小，纯度高。

Description

一种ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺
技术领域
本发明属于无机非金属材料技术领域，涉及超高温陶瓷原料粉体的制备，特别涉及一种ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺。
背景技术
一直以来ZrB2陶瓷因为自身的优异性能一直是科学家研究的热点，具有低密度、高熔点、高比模量、抗烧蚀、物理稳定性和热化学稳定性好等特点，是超高温陶瓷材料极具潜力的一种材料。由于单相ZrB2抗氧化性差，在热冲击条件下固有的脆性和有限的烧结性影响其在超高温领域的应用。如今越来越多的研究者将工作重心放在了ZrB2基复相陶瓷粉体研究上。研究表明，通过调控微观结构和组分制备ZrC-ZrB2-SiC复相陶瓷粉体因具备更宽的抗氧化区间表现出优异的抗氧化和高温力学性能。这是因为SiC可以改善ZrB2烧结性，抗氧化性性和机械性能；ZrC是另一种合适的材料，可以加入到ZrB2中作为烧结助剂以及增强剂，极大地提高了材料的致密性。
目前制备ZrC-ZrB2-SiC陶瓷粉体常用的方法有：(1)机械球法，即将Zr粉、Si粉、B4C和碳源通过球磨进行均匀混合，但在球磨过程中原料粉体易被氧化，原料本身含有氧杂质，反应温度过低，原位反应不充分，导致生成物中易引入氧化物相。(2)熔盐法，可极大的降低合成温度，但熔盐温度和加入还原剂的量对ZrC-ZrB2-SiC陶瓷粉体的合成影响很大，合成的复合粉体中ZrC-ZrB2-SiC含量低，很难制备出纯ZrC-ZrB2-SiC陶瓷粉体。(3)自蔓延高温合成法，该方法利用反应物之间高的反应热通过自传导使反应快速发生，当反应物一旦被点燃，反应会一直进行直到反应完全，反应过程很难控制；而且最终产物会含有一些金属杂质，需要通过萃取洗掉杂质后才能使用。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺。
为了实现上述目的，本发明采用的技术方案是：
一种ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺，包括：
步骤1)，在持续磁力搅拌的情况下，将八水氧氯化锆溶于无水乙醇中，滴加双氧水，配制成均一透明的溶液，即锆前驱体溶液；将硼酸溶于无水乙醇中，水浴加热至完全溶解，配制硼酸溶液；将正硅酸乙酯溶于无水乙醇中配制正硅酸乙酯溶液；将葡萄糖溶于去离子水，制得葡萄糖溶液；
步骤2)，在持续磁力搅拌的情况下，依次将所述正硅酸乙酯溶液、硼酸溶液、葡萄糖溶液加入到锆前驱体溶液中，制得硼硅锆前驱体溶液；
步骤3)，将所述硼硅锆前驱体溶液烘干后放置于石墨坩埚中，在氩气气氛保护下，在1450-1600℃热处理1-2h，得到ZrC-ZrB2-SiC陶瓷粉体。
所述硼酸、八水氧氯化锆和正硅酸乙酯的物质的量之比为1-5:1:0.5-5，所述葡萄糖和正硅酸乙酯的质量比为1-4:1。
所制备的氧氯化锆前驱体溶液的浓度为0.08-0.26g/mL,双氧水与氧氯化锆前驱体溶液的体积比为1:10-15，硼酸溶液的浓度为0.016-0.082g/mL，正硅酸乙酯溶液的浓度为0.023-0.23g/mL，葡萄糖溶液的浓度为0.006-0.024g/mL。
所述水浴加热的温度为40-80℃。
由于采用上述技术方案，本发明将廉价易得的可溶性锆源、硅源和碳源在分子水平上均匀混合，缩短了反应时间，降低了陶瓷相的形成温度，因而，具有能耗低，周期短，成本低的特点，且所制备的陶瓷粉体陶瓷相分布均匀，粒径细小均一，平均粒径约150nm，纯度高，无杂质相。
附图说明
图1是具体实施例1中所制备的ZrC-ZrB2-SiC陶瓷复合粉体的XRD谱图。
图2为本发明实施案例1所制备的ZrC-ZrB2-SiC陶瓷复合粉体的SEM照片。
具体实施方式
下面结合附图和具体实施方式对本发明做进一步描述，并非对其保护范围的限制。
实施例1
一种ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺，具体流程如下：
(1)步骤一：按物质的量比为硼酸：八水氧氯化锆：正硅酸乙酯＝4:1:2，质量比葡萄糖：正硅酸乙酯＝2.5:1，分别称取八水氧氯化锆，硼酸，正硅酸乙酯，葡萄糖备用。
(2)步骤二：持续磁力搅拌的情况下，将氧氯化锆溶于无水乙醇中，滴加双氧水，配制成均一透明的溶液，即锆前驱体溶液。将硼酸溶于无水乙醇中，水浴加热至完全溶解，配制硼酸溶液。将正硅酸乙酯溶于无水乙醇中配制正硅酸乙酯溶液。将葡萄糖溶于去离子水，制得葡萄糖溶液。在持续磁力搅拌的情况下，依次将正硅酸乙酯溶液、硼酸溶液、葡萄糖溶液加入到锆前驱体溶液中，制得硼硅锆前驱体溶液。
(3)步骤三：将步骤二得到的硼硅锆前驱体溶液，在烘干后放置于石墨坩埚中，在氩气气氛保护下，在1500℃下热处理2h，得到ZrC-ZrB2-SiC陶瓷粉体。
实施例2
一种ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺，除下述热处理温度不同外，其余同实施例1.
本实施例中：称取的原料物质的量比为硼酸：八水氧氯化锆：正硅酸乙酯＝4:1:3，质量比葡萄糖：正硅酸乙酯＝2:1；热处理温度为1600℃。
实施例3
一种ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺，除下述保温时间不同外，其余同实施例1.
本实施例中：称取的原料物质的量比为硼酸：八水氧氯化锆：正硅酸乙酯＝3:1:2，质量比葡萄糖：正硅酸乙酯＝2:1；保温2h。
从图1中可以看出，采用本发明的制备工艺所制备的复合陶瓷粉体的物相组成为纯的ZrC、ZrB2和SiC，晶化度高，未见其他杂质相存在。
从图2可以看出，采用本发明的制备工艺所制备的复合陶瓷粉体，陶瓷相为不规则的颗粒状，粒径尺寸均一，平粒径约150nm。

Claims (4)

1.一种ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺，其特征在于，包括：
步骤1)，在持续磁力搅拌的情况下，将八水氧氯化锆溶于无水乙醇中，滴加双氧水，配制得到锆前驱体溶液；将硼酸溶于无水乙醇中，水浴加热至完全溶解，配制硼酸溶液；将正硅酸乙酯溶于无水乙醇中配制正硅酸乙酯溶液；将葡萄糖溶于去离子水，制得葡萄糖溶液；
步骤2)，在持续磁力搅拌的情况下，依次将所述正硅酸乙酯溶液、硼酸溶液、葡萄糖溶液加入到锆前驱体溶液中，制得硼硅锆前驱体溶液；
步骤3)，将所述硼硅锆前驱体溶液烘干后放置于石墨坩埚中，在氩气气氛保护下，在1450-1600℃热处理1-2h，得到ZrC-ZrB2-SiC陶瓷粉体。
2.根据权利要求1所述ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺，其特征在于，所述硼酸、八水氧氯化锆和正硅酸乙酯的物质的量之比为1-5:1:0.5-5，所述葡萄糖和正硅酸乙酯的质量比为1-4:1。
3.根据权利要求1所述ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺，其特征在于，所制备的氧氯化锆前驱体溶液的浓度为0.08-0.26g/mL,双氧水与氧氯化锆前驱体溶液的体积比为1:10-15，硼酸溶液的浓度为0.016-0.082g/mL，正硅酸乙酯溶液的浓度为0.023-0.23g/mL，葡萄糖溶液的浓度为0.006-0.024g/mL。
4.根据权利要求1所述ZrC-ZrB2-SiC陶瓷复合粉体的前驱体转化法制备工艺，其特征在于，所述水浴加热的温度为40-80℃。
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111187075A (zh) * 2020-02-18 2020-05-22 陕西科技大学 一种自分散超细ZrC-SiC陶瓷复合粉体的前驱体转化法制备工艺
CN111253161A (zh) * 2020-01-20 2020-06-09 陕西科技大学 一种SiCf-ZrC-ZrB2陶瓷复合粉体及其制备方法
CN112079650A (zh) * 2020-08-21 2020-12-15 西安理工大学 一种ZrC/ZrB2复相多孔超高温陶瓷的制备方法
CN112174671A (zh) * 2020-10-10 2021-01-05 黑龙江大学 一种耐高温SiZrBOC五元陶瓷的制备方法
CN112174669A (zh) * 2020-10-10 2021-01-05 黑龙江大学 一种溶胶凝胶法合成SiZrBOC陶瓷的制备方法
CN113773090A (zh) * 2021-11-15 2021-12-10 长沙理工大学 一种ZrB2-ZrC-SiC纳米复合陶瓷材料的制备方法
CN113896558A (zh) * 2021-11-10 2022-01-07 航天特种材料及工艺技术研究所 一种高性能热疏导复合材料及其制备方法
CN115504815A (zh) * 2022-10-19 2022-12-23 长沙晶优新材料科技有限公司 一种等离子喷涂制备(C/C)/ZrB2-SiC-LaB6复合涂层材料的方法
CN115849914A (zh) * 2022-10-19 2023-03-28 湘潭大学 一种ZrB2-SiC-LaB6三元超高温纳米复合陶瓷的制备方法

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CN111253161A (zh) * 2020-01-20 2020-06-09 陕西科技大学 一种SiCf-ZrC-ZrB2陶瓷复合粉体及其制备方法
CN111187075A (zh) * 2020-02-18 2020-05-22 陕西科技大学 一种自分散超细ZrC-SiC陶瓷复合粉体的前驱体转化法制备工艺
CN112079650A (zh) * 2020-08-21 2020-12-15 西安理工大学 一种ZrC/ZrB2复相多孔超高温陶瓷的制备方法
CN112174671A (zh) * 2020-10-10 2021-01-05 黑龙江大学 一种耐高温SiZrBOC五元陶瓷的制备方法
CN112174669A (zh) * 2020-10-10 2021-01-05 黑龙江大学 一种溶胶凝胶法合成SiZrBOC陶瓷的制备方法
CN112174671B (zh) * 2020-10-10 2022-07-29 黑龙江大学 一种耐高温SiZrBOC五元陶瓷的制备方法
CN113896558A (zh) * 2021-11-10 2022-01-07 航天特种材料及工艺技术研究所 一种高性能热疏导复合材料及其制备方法
CN113773090A (zh) * 2021-11-15 2021-12-10 长沙理工大学 一种ZrB2-ZrC-SiC纳米复合陶瓷材料的制备方法
CN113773090B (zh) * 2021-11-15 2022-02-18 长沙理工大学 一种ZrB2-ZrC-SiC纳米复合陶瓷材料的制备方法
CN115504815A (zh) * 2022-10-19 2022-12-23 长沙晶优新材料科技有限公司 一种等离子喷涂制备(C/C)/ZrB2-SiC-LaB6复合涂层材料的方法
CN115849914A (zh) * 2022-10-19 2023-03-28 湘潭大学 一种ZrB2-SiC-LaB6三元超高温纳米复合陶瓷的制备方法
CN115504815B (zh) * 2022-10-19 2023-11-03 长沙晶优新材料科技有限公司 一种等离子喷涂制备(C/C)/ZrB2-SiC-LaB6复合涂层材料的方法

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