CN106830978B - 一种高纯度的多孔钛硅碳陶瓷制备方法 - Google Patents

一种高纯度的多孔钛硅碳陶瓷制备方法 Download PDF

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CN106830978B
CN106830978B CN201710039810.1A CN201710039810A CN106830978B CN 106830978 B CN106830978 B CN 106830978B CN 201710039810 A CN201710039810 A CN 201710039810A CN 106830978 B CN106830978 B CN 106830978B
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倪东恵
周超兰
李烈军
鲁艳军
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South China University of Technology SCUT
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Abstract

本发明公开了一种高纯度的多孔钛硅碳陶瓷制备方法，包括步骤：1）将钛硅碳粉末与一定粒径的碳酸氢铵颗粒分别按照9:1~6:4的质量比在混粉机中混合6~12h；2）将干燥的混合粉末倒入钢模中，用100~1000MPa压力压制成生坯；3）将生坯置于管式炉中，通以保护气氛氩气，以1~30℃/min的速度逐步升温至1200℃，保温1~5 h后随炉冷却得到高纯多孔钛硅碳陶瓷。本发明提供的制备方法工艺简单，成本低，对制备设备限制较少，利于工业化生产。

Description

一种高纯度的多孔钛硅碳陶瓷制备方法
技术领域
本发明涉及多孔陶瓷的制备领域，具体涉及一种成分稳定、高纯度的多孔钛硅碳陶瓷制备方法。
背景技术
钛硅碳（Ti3SiC2）是一种兼具了陶瓷和金属材料特点的三元碳化物陶瓷。因其具有质轻、热稳定性和化学稳定性好、优良机械加工性等优点，钛硅碳陶瓷被认为具备应用于生物医用材料的潜质。大多数医用移植材料对材料本身孔隙率的可调节性要求比较高，因为可以通过调节材料的孔隙率对医用材料力学性能进行改变，从而实现医用性植入材料与人体自身骨骼的匹配性。
但是到目前为止，关于多钛硅碳的制备方面的报道尚不多，采用不完全烧结法和热等静压法合成出多孔钛硅碳，孔隙率范围为0~55％。该方法的造孔原理是通过烧结过程中Si元素的挥发以及粉末烧结收缩产生的孔洞。利用元素粉可在不同温度下烧结制备出多孔钛硅碳，并发现不同温度下烧结制备的多孔钛硅碳孔隙率不同，但是其在低于1350℃下烧结出的多孔钛硅碳纯度较低，因此上述方法均无法制备出纯度较高且孔隙率和孔结构可控制的多孔钛硅碳。
发明内容
本发明旨在解决的技术问题包括：无压烧结工艺对生产设备要求低，生产成本低廉，产品成分稳定，多孔陶瓷的孔隙率及孔形貌可控性强。
本发明可通过如下技术方案实现：
一种高纯度的多孔钛硅碳陶瓷制备方法，包括步骤：
1）将钛硅碳粉末与一定粒径的碳酸氢铵（NH4HCO3）颗粒分别按照9:1~6:4的质量比在混粉机中混合6~12h；
2）将干燥的混合粉末倒入钢模中，用100~1000MPa压力压制成生坯；
3）将生坯置于管式炉中，通以保护气氛氩气，以1~30℃/min的速度逐步升温至1200℃，保温1~5h后随炉冷却得到高纯多孔钛硅碳陶瓷。
进一步地，步骤1）中所述的碳酸氢铵颗粒的粒径为1~500微米。
进一步地，步骤3）中，所述的以1~30℃/min的速度逐步升温至1200℃，保温1~5 h后随炉冷却的过程具体包括步骤：
31）以1~30℃/min的速度升温至200℃，保温10~60 min以去除碳酸氢铵颗粒；
32）再以1~30℃/min的速度升温到800℃；
33）最后以1~30℃/min的速度升温至1200℃，保温1~5h后随炉冷却。
本发明将钛硅碳粉末与碳酸氢铵（NH4HCO3）造孔剂混合后压制成坯，将生坯在氩气氛的保护下无压烧结制备出孔结构可控的高纯多孔钛硅碳陶瓷。所制备的多孔钛硅碳陶瓷与烧结前成分几乎相同，多孔钛硅碳陶瓷的纯度取决于原料钛硅碳陶瓷粉本身的纯度，该制备方法易于控制多孔陶瓷的纯度。
本发明与现有技术相比具有如下优点：
（1）造孔剂成本低廉、去除容易，在烧结过程中可以直接去除，简化制备步骤。
（2）生产设备简单，烧结工艺简单。
（3）对烧结原料条件限制少，烧结前后产品成分稳定，利于产品的批量化生产。
附图说明
图1为烧结前后的钛硅碳的XRD分析图谱。
图2为碳酸氢铵含量对多孔钛硅碳的孔隙率的影响示意图。
具体实施方式
为更好理解本发明，下面结合附图和实施例对本发明做进一步的说明，但是本发明要求保护的范围并不局限于实施例表示的范围。
实施例1
一种高纯度的多孔钛硅碳陶瓷制备方法，包括步骤：
1）将钛硅碳粉末与经研磨并过筛的粒径为1微米的碳酸氢铵粉末按照9:1的质量比在V型混粉机中混合12h；
2）将混合粉末倒入钢模中，在CMT5105电子万能试验机上用300MPa压力压制成直径约为20mm，高约为5mm的生坯；
3）将生坯置于管式炉中，用氩气作为保护气氛，以5℃/min的速度升温至200℃，保温40min以去除碳酸氢铵造孔剂，再以5℃/min的速度升温到800℃，最后以2℃/min的速度升温至1200℃，保温2h后随炉冷却，所制备出的多孔钛硅碳陶瓷的孔隙率为39.1%，见图2所示。
实施例2
一种高纯度的多孔钛硅碳陶瓷制备方法，包括步骤：
1）将钛硅碳粉末与经研磨并过筛的粒径为50微米的碳酸氢铵粉末按照8:2的质量比在V型混粉机中混合10h；
2）将混合粉末倒入钢模中，在CMT5105电子万能试验机上用600MPa压力压制成直径约为20mm，高约为5mm的生坯；
3）将生坯置于管式炉中，用氩气作为保护气氛，以5℃/min的速度升温至200℃，保温40min以去除碳酸氢铵造孔剂，再以5℃/min的速度升温到800℃，最后以2℃/min的速度升温至1200℃，保温2h后随炉冷却，所制备出的多孔钛硅碳陶瓷的孔隙率为48.5%。
实施例3
一种高纯度的多孔钛硅碳陶瓷制备方法，包括步骤：
1）将钛硅碳粉末与经研磨并过筛的粒径为75微米的碳酸氢铵粉末按照7:3的质量比在V型混粉机中混合6h；
2）将混合粉末倒入钢模中，在CMT5105电子万能试验机上用1000MPa压力压制成直径约为20mm，高约为5mm的生坯；
3）将生坯置于管式炉中，用氩气作为保护气氛，以5℃/min的速度升温至200℃，保温40min以去除碳酸氢铵造孔剂，再以5℃/min的速度升温到800℃，最后以2℃/min的速度升温至1200℃，保温2h后随炉冷却，所制备出的多孔钛硅碳陶瓷的孔隙率为59.2%。
图1为烧结前后的钛硅碳的XRD分析图谱。如图所示，烧结后多孔钛硅碳块体的XRD图谱与烧结前的钛硅碳粉末的XRD图谱基本一致，未出现新的杂质峰。图2为碳酸氢铵含量对上述实施例1-3所制备出的多孔钛硅碳的孔隙率的影响。
实施例4
一种高纯度的多孔钛硅碳陶瓷制备方法，包括步骤：
1）将钛硅碳粉末与经研磨并过筛的粒径为130微米的碳酸氢铵粉末按照7:3的质量比在V型混粉机中混合6h；
2）将混合粉末倒入钢模中，在CMT5105电子万能试验机上用800MPa压力压制成直径约为20mm，高约为5mm的生坯；
3）将生坯置于管式炉中，用氩气作为保护气氛，以5℃/min的速度升温至200℃，保温40min以去除碳酸氢铵造孔剂，再以5℃/min的速度升温到800℃，最后以2℃/min的速度升温至1200℃，保温2h后随炉冷却，所制备出的多孔钛硅碳陶瓷的孔隙率为62.1%。
实施例5
一种高纯度的多孔钛硅碳陶瓷制备方法，包括步骤：
1）将钛硅碳粉末与经研磨并过筛的粒径为150微米的碳酸氢铵粉末按照9:1的质量比在V型混粉机中混合6h；
2）将混合粉末倒入钢模中，在CMT5105电子万能试验机上用100MPa压力压制成直径约为20mm，高约为5mm的生坯；
3）将生坯置于管式炉中，用氩气作为保护气氛，以1℃/min的速度升温至200℃，保温40min以去除碳酸氢铵造孔剂，再以1℃/min的速度升温到800℃，最后以1℃/min的速度升温至1200℃，保温5h后随炉冷却，所制备出的多孔钛硅碳陶瓷的孔隙率为53.8%。
实施例6
一种高纯度的多孔钛硅碳陶瓷制备方法，包括步骤：
1）将钛硅碳粉末，与经研磨并过筛的粒径为500微米的碳酸氢铵粉末按照6:4的质量比在V型混粉机中混合12h；
2）将混合粉末倒入钢模中，在CMT5105电子万能试验机上用1000MPa压力压制成直径约为20mm，高约为5mm的生坯；
3）将生坯置于管式炉中，用氩气作为保护气氛，以30℃/min的速度升温至200℃，保温40min以去除碳酸氢铵造孔剂，再以30℃/min的速度升温到800℃，最后以30℃/min的速度升温至1200℃，保温1h后随炉冷却，所制备出的多孔钛硅碳陶瓷的孔隙率为63.2%。
本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明权利要求的保护范围之内。

Claims (1)

1.一种高纯度的多孔钛硅碳陶瓷制备方法，其特征在于，包括步骤：
1）将钛硅碳粉末与一定粒径的碳酸氢铵颗粒分别按照9:1~6:4的质量比在混粉机中混合6~12h；所述的碳酸氢铵颗粒的粒径为1~500微米；
2）将干燥的混合粉末倒入钢模中，用100~1000MPa压力压制成生坯；
3）将生坯置于管式炉中，通以保护气氛氩气，以1~30℃/min的速度逐步升温至1200℃，保温1~5h后随炉冷却得到高纯多孔钛硅碳陶瓷；所述的以1~30℃/min的速度逐步升温至1200℃，保温1~5h后随炉冷却的过程具体包括步骤：
1）以1~30℃/min的速度升温至200℃，保温1~5 h以去除碳酸氢铵颗粒；
2）再以1~30℃/min的速度升温到800℃；
3）最后以1~30℃/min的速度升温至1200℃，保温1~5 h后随炉冷却。
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