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CN116496103B - 一种高强度、低密度碳化硅及其制备方法和应用 - Google Patents

一种高强度、低密度碳化硅及其制备方法和应用 Download PDF

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CN116496103B
CN116496103B CN202310745155.7A CN202310745155A CN116496103B CN 116496103 B CN116496103 B CN 116496103B CN 202310745155 A CN202310745155 A CN 202310745155A CN 116496103 B CN116496103 B CN 116496103B
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CN116496103A (zh
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叶明亮
柴杰
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Chengdu Ultra Pure Applied Materials Co.,Ltd.
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Abstract

本发明涉及结构陶瓷材料技术领域，具体涉及一种高强度、低密度碳化硅及其制备方法和应用。本发明公开了一种高强度、低密度碳化硅及其制备方法和应用，高强度、低密度碳化硅的制备方法，包括以下步骤：在碳化硅基材上覆盖石墨粉作为待烧结样品；将待烧结样品进行真空煅烧，经反应烧结获得高强度、低密度碳化硅。本发明制备获得的碳化硅材料具有高强度、低密度的优异性能，为SiC材料反射镜体系提供新的方向和思路。

Description

一种高强度、低密度碳化硅及其制备方法和应用
技术领域
本发明涉及结构陶瓷材料技术领域，具体涉及一种高强度、低密度碳化硅及其制备方法和应用。
背景技术
碳化硅作为一种重要的结构陶瓷材料，凭借其优异的高温力学强度、高硬度、高弹性模量、高耐磨性、高导热、耐腐蚀性等性能，广泛应用于各个行业领域。
一般根据制备方法不同，可以大致把碳化硅分为反应烧结碳化硅、无压烧结碳化硅、热等静压碳化硅、重结晶碳化硅、其他碳化硅等五类。其中，反应烧结制备的碳化硅虽然烧结收缩尺寸很小，但是其含硅（硅的熔点：1420℃）量较高，一般在12%左右，导致强度较低且高温使用环境受限（最高使用温度在1300℃左右）；无压烧结制备的碳化硅，虽然强度较高、能耐高温（最高使用温度在1600℃左右），但密度较大，一般在3.14g/cm3左右，且烧结收缩很大，一般在20%左右，不利于反射镜的复杂结构和轻量化设计。
目前，国内外SiC材料反射镜体系主要有两种：其一，反应烧结SiC胚体+CVD SiC涂层；其二，无压烧结SiC胚体+CVD SiC涂层。为了更好的设计SiC反射镜，拓展SiC材料在反射镜行业的应用前景，本发明开发了一种高强度、低密度碳化硅的制备方法，来解决SiC材料在反射镜行业的一些应用问题。
发明内容
本发明所要解决的技术问题是：常规的反应烧结方法和无压烧结方法无法同时兼顾强度和密度性能，本发明提供了解决上述问题的一种高强度、低密度碳化硅及其制备方法和应用，为SiC材料反射镜体系提供新的方向和思路。
本发明通过下述技术方案实现：
一种高强度、低密度碳化硅的制备方法，包括以下步骤：在碳化硅基材上覆盖石墨粉作为待烧结样品；将待烧结样品进行真空煅烧，经反应烧结获得高强度、低密度碳化硅。
本发明反应原理为：在真空高温（1700~1800℃）下，碳化硅基材中的游离硅（硅的熔点为1410℃）会挥发至基材表面，其中一部分硅与石墨发生反应生产SiC；另一部分硅挥发至真空中。最后，由于基材中游离硅的挥发和反应，导致基材内部形成一些细小孔洞，表面形成致密化层，最终造成了基材密度降低，强度增大。
进一步可选地，所述石墨粉的覆盖厚度为1 cm~3 cm。
本发明通过优化石墨粉的覆盖厚度，提高反应效率，保证产品质量。覆盖厚度低于1 cm时，不利于在反应烧结碳化硅基材表面形成一层致密的碳化硅和硅复合层，覆盖厚度大于3 cm时，通过热传导理论，不利于反应烧结碳化硅基材中硅的挥发。
进一步可选地，所述碳化硅基材的密度为3.02 g/cm3~3.05 g/cm3。
碳化硅基材为商用反应烧结碳化硅，该所述密度为一般反应烧结碳化硅的密度。
进一步可选地，所述石墨粉的粒径为300 nm~500 nm。
粒径过高，活性不够，不能与表面处硅发生高温反应生产SiC；粒径过低，成本较高。
进一步可选地，反应烧结温度为1700 ℃~1800 ℃。
进一步可选地，煅烧工艺包括：
升温到1700 ℃~1800 ℃时保温3 h~5 h；
保温结束后降温至800 ℃~1000 ℃后随炉冷却。
进一步可选地，升温速度为3 ℃/min ~8 ℃/min；保温结束后降温速率为1 ℃/min ~3 ℃/min。
一种高强度、低密度碳化硅，采用上述的一种高强度、低密度碳化硅的制备方法制备获得。
一种高强度、低密度碳化硅的应用，高强度、低密度碳化硅由上述的一种高强度、低密度碳化硅的制备方法制备获得，用于在反射镜领域。
上述的一种高强度、低密度碳化硅的制备方法在制备反射镜材料中的应用。
本发明具有如下的优点和有益效果：
1、本发明通过优化反应烧结方法，制备获得的得到的碳化硅基材比常规反应烧结碳化硅材料的四点抗弯强度提高了10%；此外，得到的碳化硅基材的密度为2.6 g/cm3~2.8g/cm3，得到的碳化硅基材的游离硅含量为5~8%，是一种高强度、低密度的碳化硅材料，可适用于反射镜领域，为SiC反射镜体系材料提供一种新的方向和思路。为碳化硅在反射镜行业拓宽了应用方向。
2、本发明提供的制备方法，工艺简单，生产成本低。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明白，下面结合实施例，对本发明作进一步的详细说明，本发明的示意性实施方式及其说明仅用于解释本发明，并不作为对本发明的限定。
实施例1
本实施例提供了一种高强度、低密度碳化硅，由如下制备方法获得：
步骤1，将反应烧结碳化硅基材放置于石墨坩埚中，用石墨粉对其进行覆盖。其中，覆盖的厚度为1.5 cm；碳化硅基材的密度为，3.03 g/cm3；石墨粉的粒径为450 nm。
步骤2，将装有反应烧结碳化硅基材的石墨坩埚放于真空烧结炉中煅烧。煅烧工艺为升温速度为5 ℃/min，升温到1700 ℃时保温3 h；保温结束后进行以2 ℃/min进行降温，降温至1000℃后随炉冷却。
实施例2
本实施例提供了一种高强度、低密度碳化硅，由如下制备方法获得：
步骤1，将反应烧结碳化硅基材放置于石墨坩埚中，用石墨粉对其进行覆盖。其中，覆盖的厚度为2 cm；碳化硅基材的密度为，3.04 g/cm3；石墨粉的粒径为400 nm。
步骤2，将装有反应烧结碳化硅基材的石墨坩埚放于真空烧结炉中煅烧。煅烧工艺为升温速度为8 ℃/min，升温到1750 ℃时保温4 h；保温结束后进行以3 ℃/min进行降温，降温至1000℃后随炉冷却。
实施例3
本实施例提供了一种高强度、低密度碳化硅，由如下制备方法获得：
步骤1，将反应烧结碳化硅基材放置于石墨坩埚中，用石墨粉对其进行覆盖。其中，覆盖的厚度为3 cm；碳化硅基材的密度为，3.04 g/cm3；石墨粉的粒径为350 nm。
步骤2，将装有反应烧结碳化硅基材的石墨坩埚放于真空烧结炉中煅烧。煅烧工艺为升温速度为5 ℃/min，升温到1800 ℃时保温3 h；保温结束后进行以3 ℃/min进行降温，降温至1000℃后随炉冷却。
对比例1
本案例提供了一种碳化硅材料，由如下制备方法获得：
步骤1，将反应烧结碳化硅基材放置于石墨坩埚中，用石墨粉对其进行覆盖。其中，覆盖的厚度为3 cm；碳化硅基材的密度为，3.04 g/cm3；石墨粉的粒径为1μm。
步骤2，将装有反应烧结碳化硅基材的石墨坩埚放于真空烧结炉中煅烧。煅烧工艺为升温速度为5 ℃/min，升温到1800 ℃时保温3 h；保温结束后进行以3 ℃/min进行降温，降温至1000℃后随炉冷却。
对比例2
本案例提供了一种碳化硅材料，由如下制备方法获得：
步骤1，将反应烧结碳化硅基材放置于石墨坩埚中，用石墨粉（粒径范围为10~50μm）对其进行覆盖。其中，覆盖的厚度为3 cm；碳化硅基材的密度为，3.03 g/cm3；石墨粉的粒径为30 μm。
步骤2，将装有反应烧结碳化硅基材的石墨坩埚放于真空烧结炉中煅烧。煅烧工艺为升温速度为5 ℃/min，升温到1800 ℃时保温3 h；保温结束后进行以3 ℃/min进行降温，降温至1000℃后随炉冷却。
对比例3
本案例提供了一种碳化硅材料，由如下制备方法获得：
步骤1，将反应烧结碳化硅基材放置于石墨坩埚中，用石墨粉对其进行覆盖。其中，覆盖的厚度为3 cm；碳化硅基材的密度为，3.05 g/cm3；石墨粉的粒径为350 nm。
步骤2，将装有反应烧结碳化硅基材的石墨坩埚放于真空烧结炉中煅烧。煅烧工艺为升温速度为5 ℃/min，升温到1600 ℃时保温3 h；保温结束后进行以3 ℃/min进行降温，降温至1000℃后随炉冷却。
对比例4
本案例提供了一种碳化硅材料，由如下制备方法获得：
步骤1，将反应烧结碳化硅基材放置于石墨坩埚中，用石墨粉对其进行覆盖。其中，覆盖的厚度为3 cm；碳化硅基材的密度为，3.05 g/cm3；石墨粉的粒径为350 nm。
步骤2，将装有反应烧结碳化硅基材的石墨坩埚放于真空烧结炉中煅烧。煅烧工艺为升温速度为5 ℃/min，升温到1500 ℃时保温3 h；保温结束后进行以3 ℃/min进行降温，降温至1000℃后随炉冷却。
一、样品性能测试方法：
1、强度测试：采用GB/T 6569精细陶瓷弯曲强度试验方法标准，测试样品的四点抗弯强度。
2、密度测试：采用GB/T 25995精细陶瓷密度和显气孔率试验方法，测试样品的密度。
3、游离硅测试：采用GB/T 3045碳化硅化学分析方法，测试样品游离硅的含量。
二、样品性能测试结果：
表1 样品性能测试结果
综上，本发明通过合理设计石墨粉的覆盖厚度、碳化硅基材的密度、石墨粉的粒径等相关参数，可获得同时兼具低密度、高强度的碳化硅材料，且游离硅含量相对较低。
以上所述的具体实施方式，对本发明的目的、技术方案和有益效果进行了进一步详细说明，所应理解的是，以上所述仅为本发明的具体实施方式而已，并不用于限定本发明的保护范围，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (6)

1.一种高强度、低密度碳化硅的制备方法，其特征在于，包括以下步骤：
在碳化硅基材上覆盖石墨粉作为待烧结样品；
将待烧结样品进行真空煅烧，经反应烧结获得高强度、低密度碳化硅；
所述石墨粉的覆盖厚度为1 cm~3 cm；
所述碳化硅基材的密度为3.02 g/cm3~3.05 g/cm3；
所述石墨粉的粒径为300 nm~500 nm；
反应烧结温度为1700 ℃~1800 ℃。
2.根据权利要求1所述的一种高强度、低密度碳化硅的制备方法，其特征在于，煅烧工艺包括：
升温到1700 ℃~1800 ℃时保温3 h~5 h；
保温结束后降温至800 ℃~1000 ℃后随炉冷却。
3.根据权利要求2所述的一种高强度、低密度碳化硅的制备方法，其特征在于，升温速度为3 ℃/min ~8 ℃/min；保温结束后降温速率为1 ℃/min ~3 ℃/min。
4.一种高强度、低密度碳化硅，其特征在于，采用权利要求1至3任一项所述的一种高强度、低密度碳化硅的制备方法制备获得。
5.一种高强度、低密度碳化硅的应用，高强度、低密度碳化硅由权利要求1至3任一项所述的一种高强度、低密度碳化硅的制备方法制备获得，其特征在于，用于在反射镜领域。
6.权利要求1至3任一项所述的一种高强度、低密度碳化硅的制备方法在制备反射镜材料中的应用。
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