CN108129157A - 石英纤维增强的石英材料及其制备方法 - Google Patents
石英纤维增强的石英材料及其制备方法 Download PDFInfo
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 238000009768 microwave sintering Methods 0.000 abstract description 8
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Abstract
本发明涉及石英纤维增强的石英材料及其制备方法，所述方法包括如下步骤：将晶须状和非晶须状石英纤维依次用无水乙醇和浓硝酸浸泡，然后用过滤水冲洗，再蒸馏、干燥；将其超声处理，然后用二氧化碳激光照射，再过筛；再与石英材料混合并微波烧结，再用酚醛树脂浸渍；最后高温烧结。本发明的石英材料的制备方法，采用二氧化碳激光法使纤维和晶须融合，融合得到的产物既具有纤维增强材料的韧性，又具有较高的抗热震性。微波烧结技术能使被加热体达到均匀的温度，促进致密化，且烧结温度较真空烧结低，减少了方石英的析出。致密化处理时，酚醛树脂填补材料表面的孔隙，减材料比表面积并且具有耐湿热性，可增加材料的使用时间。
Description
技术领域
本发明属于材料技术领域，具体涉及一种石英纤维增强的石英材料及其制备方法。
背景技术
石英材料具有低热膨胀系数、电导率和较高的机械强度、耐热温度、耐冲击性等众多优良性质，在众多领域都有应用。但是在高温烧结时，石英会转变成热膨胀系数较大的方石英，并且表面产生孔隙，使其脆性增大，易断裂。使用晶须增韧时，虽能提高材料的断裂韧性，但会降低材料的抗热震性。
发明内容
本发明的一个目的在于提出一种石英纤维增强的石英材料的制备方法。
本发明的石英纤维增强的石英材料的制备方法，包括如下步骤：S101：将晶须状和非晶须状石英纤维用无水乙醇浸泡2h～3h，然后用浓硝酸浸泡2h～3h，然后用过滤水冲洗，再在100℃～120℃下蒸馏，然后干燥；S102：将所述步骤S101处理过的石英纤维与石英晶须超声处理，然后用二氧化碳激光照射，再将其过分子筛并收集过筛后的物料，得到融合的石英纤维和石英晶须；S103：将所述步骤S102得到的产物与石英材料按照质量比为1：(20～30)混合，然后微波烧结20h～30h，得到增强材料；S104：在80℃～90℃温度下，用酚醛树脂浸渍所述增强材料5h～10h，然后抽真空并保持真空条件继续浸渍2h～3h，再将浸渍后的增强材料静置并冷却至室温；S105：将所述步骤S104得到的产物在70℃/h～80℃/h的速率升温至750℃～800℃并保温20h～25h，然后以350℃/h～400℃/h的速率升温至1000℃～1100℃并保温5h～10h，再冷却至室温，得到石英纤维增强的石英材料。
本发明的石英纤维增强的石英材料的制备方法，制备过程中采用二氧化碳激光法使纤维和晶须融合，融合得到的产物既具有纤维增强材料的韧性，又具有较高的抗热震性。微波烧结技术能使被加热体达到均匀的温度，促进致密化，且烧结温度较真空烧结低，减少了方石英的析出。致密化处理时，酚醛树脂填补材料表面的孔隙，减材料比表面积并且具有耐湿热性，可增加材料的使用时间。
另外，根据本发明上述实施例的石英纤维增强的石英材料的制备方法，还可以具有如下附加的技术特征：
进一步地，在所述步骤S101中，浓硝酸的浓度为96％～97％。
进一步地，在所述步骤S101中，用过滤水冲洗3次～5次。
进一步地，在所述步骤S101中，干燥温度为50℃～80℃，干燥时间为5h～10h。
进一步地，在所述步骤S102中，所述分子筛的大小为100目～200目。
进一步地，在所述步骤S102中，将其过分子筛并收集过筛后的物料，然后重新过分子筛，并重复此过筛操作30次～40次。
进一步地，在所述步骤S102中，超声时间为0.5h～1h。
进一步地，在所述步骤S102中，用二氧化碳激光照射的方式具体为：首先用近红外脉冲激光预处理0.5h～1h，再用波长为10μm～11μm的二氧化碳激光照射0.5h～1h。
进一步地，在所述步骤S104中，抽真空的速率为100mL/min～200mL/min。
本发明的另一个目的在于提出所述方法制备的石英纤维增强的石英材料。
本发明的附加方面和优点将在下面的描述中部分给出，部分将从下面的描述中变得明显，或通过本发明的实践了解到。
具体实施方式
下面详细描述本发明的实施例，所述实施例是示例性的，旨在用于解释本发明，而不能理解为对本发明的限制。
实施例1
实施例1提出了一种石英纤维增强的石英材料，其制备方法包括如下步骤：
(1)将晶须状和非晶须状石英纤维用无水乙醇浸泡2h，然后用浓度为97％的浓硝酸浸泡2h，然后用过滤水冲洗5次，再在100℃下蒸馏，然后在80℃温度下干燥5h。
(2)将所述步骤(1)处理过的石英纤维与石英晶须超声处理1h，然后用近红外脉冲激光预处理0.5h，再用波长为11μm的二氧化碳激光照射0.5h，再将其过200目的分子筛并收集过筛后的物料，然后重新过分子筛，并重复此过筛操作30次，得到融合的石英纤维和石英晶须。
(3)将所述步骤(2)得到的产物与石英材料按照质量比为1：30混合，然后微波烧结20h，得到增强材料。
(4)在90℃温度下，用酚醛树脂浸渍所述增强材料5h，然后按照200mL/min的速率抽真空并保持真空条件继续浸渍2h，再将浸渍后的增强材料静置并冷却至室温。
(5)将所述步骤(4)得到的产物在80℃/h的速率升温至750℃并保温25h，然后以350℃/h的速率升温至1100℃并保温5h，再冷却至室温，得到石英纤维增强的石英材料。
实施例2
实施例2提出了一种石英纤维增强的石英材料，其制备方法包括如下步骤：
(1)将晶须状和非晶须状石英纤维用无水乙醇浸泡3h，然后用浓度为96％的浓硝酸浸泡3h，然后用过滤水冲洗3次，再在120℃下蒸馏，然后在50℃温度下干燥10h。
(2)将所述步骤(1)处理过的石英纤维与石英晶须超声处理0.5h，然后用近红外脉冲激光预处理1h，再用波长为10μm的二氧化碳激光照射1h，再将其过100目的分子筛并收集过筛后的物料，然后重新过分子筛，并重复此过筛操作40次，得到融合的石英纤维和石英晶须。
(3)将所述步骤(2)得到的产物与石英材料按照质量比为1：20混合，然后微波烧结30h，得到增强材料。
(4)在80℃温度下，用酚醛树脂浸渍所述增强材料10h，然后按照100mL/min的速率抽真空并保持真空条件继续浸渍3h，再将浸渍后的增强材料静置并冷却至室温。
(5)将所述步骤(4)得到的产物在70℃/h的速率升温至800℃并保温20h，然后以400℃/h的速率升温至1000℃并保温10h，再冷却至室温，得到石英纤维增强的石英材料。
实施例3
实施例3提出了一种石英纤维增强的石英材料，其制备方法包括如下步骤：
(1)将晶须状和非晶须状石英纤维用无水乙醇浸泡2.5h，然后用浓度为96％的浓硝酸浸泡2.5h，然后用过滤水冲洗4次，再在110℃下蒸馏，然后在65℃温度下干燥7h。
(2)将所述步骤(1)处理过的石英纤维与石英晶须超声处理0.8h，然后用近红外脉冲激光预处理0.8h，再用波长为10μm的二氧化碳激光照射0.7h，再将其过150目的分子筛并收集过筛后的物料，然后重新过分子筛，并重复此过筛操作35次，得到融合的石英纤维和石英晶须。
(3)将所述步骤(2)得到的产物与石英材料按照质量比为1：25混合，然后微波烧结25h，得到增强材料。
(4)在85℃温度下，用酚醛树脂浸渍所述增强材料7h，然后按照150mL/min的速率抽真空并保持真空条件继续浸渍2.5h，再将浸渍后的增强材料静置并冷却至室温。
(5)将所述步骤(4)得到的产物在75℃/h的速率升温至750℃并保温23h，然后以375℃/h的速率升温至1050℃并保温8h，再冷却至室温，得到石英纤维增强的石英材料。
本发明的石英纤维增强的石英材料的制备方法，制备过程中采用二氧化碳激光法使纤维和晶须融合，融合得到的产物既具有纤维增强材料的韧性，又具有较高的抗热震性。微波烧结技术能使被加热体达到均匀的温度，促进致密化，且烧结温度较真空烧结低，减少了方石英的析出。致密化处理时，酚醛树脂填补材料表面的孔隙，减材料比表面积并且具有耐湿热性，可增加材料的使用时间。
在本说明书的描述中，参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不必须针对的是相同的实施例或示例。而且，描述的具体特征、结构、材料或者特点可以在任一个或多个实施例或示例中以合适的方式结合。此外，在不相互矛盾的情况下，本领域的技术人员可以将本说明书中描述的不同实施例或示例以及不同实施例或示例的特征进行结合和组合。
尽管上面已经示出和描述了本发明的实施例，可以理解的是，上述实施例是示例性的，不能理解为对本发明的限制，本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。
Claims (10)
1.一种石英纤维增强的石英材料的制备方法，其特征在于，包括如下步骤：
S101：将晶须状和非晶须状石英纤维用无水乙醇浸泡2h～3h，然后用浓硝酸浸泡2h～3h，然后用过滤水冲洗，再在100℃～120℃下蒸馏，然后干燥；
S102：将所述步骤S101处理过的石英纤维与石英晶须超声处理，然后用二氧化碳激光照射，再将其过分子筛并收集过筛后的物料，得到融合的石英纤维和石英晶须；
S103：将所述步骤S102得到的产物与石英材料按照质量比为1：(20～30)混合，然后微波烧结20h～30h，得到增强材料；
S104：在80℃～90℃温度下，用酚醛树脂浸渍所述增强材料5h～10h，然后抽真空并保持真空条件继续浸渍2h～3h，再将浸渍后的增强材料静置并冷却至室温；
S105：将所述步骤S104得到的产物在70℃/h～80℃/h的速率升温至750℃～800℃并保温20h～25h，然后以350℃/h～400℃/h的速率升温至1000℃～1100℃并保温5h～10h，再冷却至室温，得到石英纤维增强的石英材料。
2.根据权利要求1所述的石英纤维增强的石英材料的制备方法，其特征在于，在所述步骤S101中，浓硝酸的浓度为96％～97％。
3.根据权利要求1所述的石英纤维增强的石英材料的制备方法，其特征在于，在所述步骤S101中，用过滤水冲洗3次～5次。
4.根据权利要求1所述的石英纤维增强的石英材料的制备方法，其特征在于，在所述步骤S101中，干燥温度为50℃～80℃，干燥时间为5h～10h。
5.根据权利要求1所述的石英纤维增强的石英材料的制备方法，其特征在于，在所述步骤S102中，所述分子筛的大小为100目～200目。
6.根据权利要求1所述的石英纤维增强的石英材料的制备方法，其特征在于，在所述步骤S102中，将其过分子筛并收集过筛后的物料，然后重新过分子筛，并重复此过筛操作30次～40次。
7.根据权利要求1所述的石英纤维增强的石英材料的制备方法，其特征在于，在所述步骤S102中，超声时间为0.5h～1h。
8.根据权利要求1所述的石英纤维增强的石英材料的制备方法，其特征在于，在所述步骤S102中，用二氧化碳激光照射的方式具体为：首先用近红外脉冲激光预处理0.5h～1h，再用波长为10μm～11μm的二氧化碳激光照射0.5h～1h。
9.根据权利要求1所述的石英纤维增强的石英材料的制备方法，其特征在于，在所述步骤S104中，抽真空的速率为100mL/min～200mL/min。
10.权利要求1-9任一项所述方法制备的石英纤维增强的石英材料。
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