CN106007687A - 一种采用高压相变法制备纳米多晶柯石英的方法 - Google Patents
一种采用高压相变法制备纳米多晶柯石英的方法 Download PDFInfo
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Abstract
本发明涉及一种纳米多晶柯石英的制备技术。采用微晶、纳米晶α‑SiO2作为初始材料，经净化除杂后，不添加除去离子水以外的任何粘结剂，装配烧结单元，直接经高温超高压烧结制备纳米多晶柯石英材料。这种纳米多晶柯石英材料物相单一，晶粒大小均匀，且不会发生团聚现象和晶粒在高温下异常长大。这使得本发明成功解决采用纳米原料时发生团聚和晶粒异常长大的难题。
Description
技术领域
本发明涉及一种以微晶α-SiO2为原料，通过预压成型，利用压机产生高温超高压制备纳米多晶柯石英的方法，属于无机材料领域。
背景技术
陶瓷材料多属于共价键化合物，在高压高温或常压高温条件下，一般存在多种相变，部分陶瓷材料的高压高温相可以在常压条件下截获；陶瓷材料常压高温下的相变大多数也可在高压高温下发生，且可被常温常压截获。因此，以大颗粒陶瓷粉晶为初始材料利用高压相变可制备多种纳米陶瓷多晶。现有纳米多晶陶瓷的制备多以纳米粉末为初始材料，纳米粉末存在团聚、吸附、难以分散的问题制约了烧结所得多晶材料的力学性能。如何抑制纳米晶粒在高温烧结过程中的长大，使其保持纳米特性与烧结体高致密度，是纳米多晶材料制备面临的技术难题。
本项目将采用微晶、纳米晶α-SiO2为初始相来解决纳米初始粉末存在的团聚、吸附以及难以分散的问题；利用高压可以抑制原子的长程扩散从进而抑制晶粒的长大来解决常压高温烧结纳米多晶材料过程中的晶粒长大问题。
石英是一种广泛存在于自然界中的矿物,在地球的表面含量非常高，是各种硅酸盐矿物的重要组成部分，为石英族矿物。石英石英有多种同质变体，常压下有七种晶型：α-石英、β-石英、α-鳞石英、β1-鳞石英、β-鳞石英、α-方石英和β-方石英。在高压下石英也有多种变体，柯石英是石英的第一个高压变体，属单斜晶系，密度为
3.01g/cm3。高压下，可发生石英–柯石英–斯石英–CaCl2结构超斯石英–α-PbO2结构超斯石英的相变。α-SiO2在 ~3GPa 左右发生相变可形成柯石英，本发明将以微晶、纳米晶α-SiO2为初始材料利用高压相变制备纳米柯石英多晶，通过比较采用纳米晶α-SiO2、微晶α-SiO2为初始材料在高压下通过相变合成柯石英多晶力学性能的差异，优化出高硬度、高韧性纳米柯石英多晶的制备途径。
直接利用微晶、纳米晶α-SiO2原料，在高温超高压下制备高性能柯石英多晶块体材料的的报道还尚未出现。
发明内容
本发明的目的是为了克服采用纳米初始粉末利用高压相变制备纳米多晶时纳米初始粉末存在的团聚、吸附以及难以分散的问题。公开了一种以微晶、纳米晶粉末为原料，通过预压成型，在高温超高压条件下制备高性能纳米多晶柯石英材料的方法。
本发明所述制备高性能纳米多晶柯石英的方法按照如下步骤进行：
一、原料处理，将微晶、纳米晶α-SiO2原料用无水乙醇清洗，120℃烘干，加适量去离子水作为粘结剂，预压成型，把成型样品放入烘箱中干燥，。
二、装配烧结单元：打磨和抛光包裹的金属材料，进行去油、超声波清洗、红外烘干。把预压成型的微晶、纳米晶α-SiO2原料放入金属杯中，再次预压成型，然后装入高压合成装置的样品腔。
三、高温高压烧结：烧结压力为3-16GPa,保压的同时进行加温，烧结温度为700-2000℃，保温1-50分钟。保温完毕后迅速降温，然后开始降压。
四、取出合成腔体内的样品，进行打磨、抛光。以得到柯石英多晶体。
本发明的优点在于：
本发明的纳米多晶柯石英材料，采用纯相的微晶、纳米晶α-SiO2微粉为原料，采用高温高压相变法烧结而成。且样品中不含其它杂质，利用高压使原料破碎成均匀的晶粒，高温使多晶体的晶粒不断长大，而同时高压条件又对这种晶粒的不断长大有所抑制。从而得到纯度较高、物相均一的柯石英多晶体。
本发明是利用高温超高压的相变条件下制备纳米柯石英多晶材料。具有相变速度快，压力和温度条件容易控制等优点。
下面通过附图和具体实施方式对本发明做进一步说明，但并不意味着对本发明保护范围的限制。
附图说明
附图1烧结单元装配图。
具体实施方式
下面通过实施例对本发明进行具体的描述，有必要在此指出的是本实施例只对于本发明进行进一步说明，不能理解为对本发明保护范围的限制，该领域的技术熟练人员可以根据上述本发明的内容作出一些非本质的改进和调整。
实施例1：选用平均粒径为10μm的微晶α-SiO2微粉，按照本发明所示工艺流程制备纳米多晶柯石英材料。原料处理：将微晶α-SiO2原料用无水乙醇搅拌清洗，待其沉降，倒去上部液体，把α-SiO2微粉放入烘箱中120℃烘干。加适量的去离子水作为粘结剂，使α-SiO2微粉具有一定的湿度，预压成型，把成型样品放入烘箱中干燥，出去最为粘结剂的去离子水。
将完全干燥后的样品装入金属杯中，再次预压成型，放入合成腔体内，如图1所示。其中组件主要有保温材料，加热片，加热管，包裹管，包裹片，保温材料，导电电极。利用国产铰链式六面顶压机产生高温高压。高温高压烧结时，烧结压力为12GPa，烧结温度为1200℃。
采用此工艺制备的纳米多晶柯石英材料物相单一，结构均匀，具有较高硬度和致密度，且没有发生采用纳米晶原料所产生的团聚和晶粒异常长大。
Claims (5)
1.采用高压相变法备纳米多晶柯石英的方法，其特征在与：利用高温高压条件，采用微晶、纳米晶α-SiO2作为初始材料，合成出纳米多晶柯石英；包括如下工艺步骤：一、采用纯度较高的微晶、纳米晶α-SiO2作为初始材料；二、对初始材料进行预压成块体处理；三、在高温高压条件下，使α-SiO2转变为柯石英多晶体块体材料。
2.根据权利要求1所述的采用高压相变法制备多晶柯石英的方法，其特征在于：原材料采用微晶、纳米晶α-SiO2为初始材料，原材料的粒径尺寸为4 nm-500 um。
3.根据权利要求1所述的采用高压相变法制备多晶柯石英的方法，其特征在于：原材料采用微晶、纳米晶α-SiO2单相为初始材料，不添加任何烧结助剂、矿化剂。
4.根据权利要求1所述的采用高压相变法制备多晶柯石英的方法，其特征在于：利用压机产生高温超高压条件，使原材料中的六方型α-SiO2相变为纳米结构的单斜型柯石英多晶块体，且晶粒均匀分布在柯石英多晶晶粒中，大面积形成结合紧密、高强度的纳米柯石英多晶，最终烧结成柯石英多晶块体。
5.根据权利要求1所述的采用高压相变法制备多晶柯石英的方法，其特征在于：预压成型的后α-SiO2块体经高温高压烧结，高温高压烧结的压力为1.0—30 Gpa，温度为400—2500℃。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106830902A (zh) * | 2017-03-06 | 2017-06-13 | 河南工业大学 | 一种采用高压相变法制备多晶α‑氧化铝的方法 |
| CN106829968A (zh) * | 2017-03-06 | 2017-06-13 | 河南工业大学 | 一种采用高压相变法制备纳米多晶斯石英的方法 |
| CN110424053A (zh) * | 2019-07-22 | 2019-11-08 | 四川大学 | 一种制备纳米结构块体材料的方法 |
| CN110550942A (zh) * | 2019-09-16 | 2019-12-10 | 陕西理工大学 | 纳米孪晶二氧化硅压电材料的制备方法 |
| CN111718197A (zh) * | 2019-03-20 | 2020-09-29 | 山东工业陶瓷研究设计院有限公司 | 一种薄型石英陶瓷部件及其高效制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106830902A (zh) * | 2017-03-06 | 2017-06-13 | 河南工业大学 | 一种采用高压相变法制备多晶α‑氧化铝的方法 |
| CN106829968A (zh) * | 2017-03-06 | 2017-06-13 | 河南工业大学 | 一种采用高压相变法制备纳米多晶斯石英的方法 |
| CN106829968B (zh) * | 2017-03-06 | 2019-03-22 | 河南工业大学 | 一种采用高压相变法制备纳米多晶斯石英的方法 |
| CN111718197A (zh) * | 2019-03-20 | 2020-09-29 | 山东工业陶瓷研究设计院有限公司 | 一种薄型石英陶瓷部件及其高效制备方法 |
| CN110424053A (zh) * | 2019-07-22 | 2019-11-08 | 四川大学 | 一种制备纳米结构块体材料的方法 |
| CN110424053B (zh) * | 2019-07-22 | 2021-01-15 | 四川大学 | 一种制备纳米结构块体材料的方法 |
| CN110550942A (zh) * | 2019-09-16 | 2019-12-10 | 陕西理工大学 | 纳米孪晶二氧化硅压电材料的制备方法 |
| CN110550942B (zh) * | 2019-09-16 | 2022-03-08 | 陕西理工大学 | 纳米孪晶二氧化硅压电材料的制备方法 |
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