CN116924811B - 一步法生产高纯六硼化硅的工艺 - Google Patents
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- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 16
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- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
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Abstract
一种一步法生产高纯六硼化硅的工艺，以二氧化硅、硼酐、碳化硼和石墨粉为原料粉，加入粘合剂和镁粉，在真空球磨机中，混料，用400t油压机压成圆柱形块体；将圆柱形块体装入真空电阻烧结炉的石墨坩埚中，抽真空至0‑5Pa，开始升温，升温功率为130kw/h，温度升至1200℃，开始反应，继续抽真空，真空度降至3Pa‑5Pa后，继续保温2小时，停电随炉降温，得到高纯六硼化硅。优点是：以二氧化硅、硼酐、碳化硼、石墨粉为原料，原材料成本低，摆脱了用单质合成的高成本生产工艺，将原料经压块后真空烧制，一步完成，工艺条件简单、可控，生产成本低，获得的六硼化硅产品纯度高，适合工业化生产。
Description
技术领域
本发明涉及一种一步法生产高纯六硼化硅的工艺。
背景技术
六硼化硅是富硼化合物陶瓷中材料中的一种，具有富硼化合物陶瓷的高硬度特性，并且还具有优异的电学性能，广泛应用于微波器件、平板显示、真空维纳器件领域。六硼化硅已经应用于航天、军工领域，如六硼化硅用于高超声速飞行器的表面防热复合涂层，该复合涂层能够加快高速飞行器表明散热。
目前，六硼化硅的制备方法主要是气相沉积法和硼单质和硅单质烧结法。气相沉积法操作步骤繁琐，生产原料污染性风险性大，不适合工业化生产。单质烧结法由原料硼单质价格昂贵；CN 106082250A公开了“一种六硼化硅粉末制备方法”，步骤是：将平均粒度＜10μm硅粉和＜20μm的硼粉按配比称重，球磨混合均匀，装入陶瓷坩埚，装入合成炉，通入氩气并滴入SiCl4，加热到1500-1600℃，冷却后球磨得到所需的SiB6粉末。该方法能制备化学纯度高、物相纯净的单相SiB6粉末。但以单质硼粉为原料，生产成本高，且对原料硅粉和硼粉的细度要求较高。
为降低原料成本，CN112125315A公开了“一种低成本高纯六硼化硅生产工艺”，该工艺以三氧化二硼和硼氢化钾为原料，还原得到硼粉，与外加原料硅粉，通过自蔓延法生产高纯六硼化硅。具有原料成本低，节约能源，且产品纯度高的优点。但该工艺为降低成本，先以三氧化二硼和硼氢化钾还原制备硼粉，然后，再与硅粉反应制备高纯六硼化硅，需分两步完成，工艺相对繁琐。
发明内容
本发明要解决的技术问题是提供了一种一步法生产高纯六硼化硅的工艺，工艺简单可控，一步法合成，生产成本低，获得的六硼化硅产品纯度高，可以大规模工业化生产。
本发明的技术方案是：
一种一步法生产高纯六硼化硅的工艺，其具体步骤如下：
(1)混料
以二氧化硅、硼酐、碳化硼和石墨粉为原料粉，其中，二氧化硅与硼酐的摩尔比为1:(1-3)，二氧化硅与碳化硼的摩尔比为1:1，二氧化硅与石墨粉的摩尔比为1:(4-6)，加入粘合剂和镁粉，放入10L的真空球磨机中，混料2-4小时，得到混合物料；
(2)压块
将混合物料按照每份0.8kg称重，用400t油压机压成圆柱形块体；
(3)制备高纯六硼化硅
将步骤(2)压制的圆柱形块体装入真空电阻烧结炉的石墨坩埚中，抽真空至0-5Pa，开始升温，升温功率为130kw/h，温度升至1200℃，开始反应，继续抽真空，真空度降至3Pa-5Pa后，继续保温2小时，停电随炉降温，得到高纯六硼化硅(SiB6)。
进一步的，二氧化硅粉纯度为99.9％，硼酐的纯度为99.8％，碳化硼的纯度为99.5％，石墨粉纯度为99.99％。
进一步的，二氧化硅粉粒度为600目，硼酐的粒度为800目，碳化硼的粒度为400目，石墨粉的粒度为800目。
进一步的，加入的粘合剂为羧甲基纤维素，每1kg原料粉加入羧甲基纤维素3g。
进一步的，每1kg原料粉加入镁粉10g。
进一步的，真空球磨机中球磨时，每次装料量为3kg-5kg。
本发明的有益效果：
以二氧化硅、硼酐、碳化硼、石墨粉为原料，原材料成本低，摆脱了用单质合成的高成本生产工艺，将原料经压块后真空烧制，一步完成，工艺条件简单、可控，生产成本低，获得的六硼化硅产品纯度高，可以工业化生产。
附图说明
图1是本发明生产的六硼化硅电镜图像；
图2是本发明生产的六硼化硅的X射线衍射图谱。
具体实施方式
通过下面的实施例可以更详细的解释本发明，本发明并不局限于下面的实施例。
实施例1
二氧化硅粉纯度为99.9％，粒度为600目，
硼酐的纯度为99.8％,粒度为800目，
碳化硼的纯度为99.5％，粒度为400目，
石墨粉纯度为99.99％，粒度为800目。
(1)混料：称取二氧化硅4.81kg、硼酐16.71kg、碳化硼4.42kg、石墨粉5.76kg(摩尔比1:3:1:6)，加入粘合剂95g、镁粉317g，放入10L的真空球磨机中，每次装料5kg，混料3小时，得到混合物料；
(2)压块：将混合物料按每份0.8kg称重，用400t油压机压成圆柱形块体；
(3)制备高纯六硼化硅：将步骤(2)压制的圆柱形块体装入真空电阻烧结炉的石墨坩埚中，抽真空至3Pa开始升温，升温功率130kw/h，温度升至1200℃开始反应，观察炉内压表、真空度表，待数值起伏较大，真空泵加速运转排出产生的大量气体，真空度降至3Pa，继续保温2小时，停电随炉降温，得到高纯六硼化硅(SiB6)，经检测，高纯六硼化硅的纯度为99.69％。
实施例2
二氧化硅粉纯度为99.9％，粒度为600目，
硼酐的纯度为99.8％,粒度为800目，
碳化硼的纯度为99.5％，粒度为400目，
石墨粉纯度为99.99％，粒度为800目。
(1)混料：称取二氧化硅4.81kg、硼酐11.14kg、碳化硼4.42kg、石墨粉4.8kg(摩尔比1:2:1:5)，加入粘合剂75.5g、镁粉251.7g，放入10L的真空球磨机中，每次装料4kg，混料2小时，得到混合物料；
(2)压块：将混合物料按每份0.8kg称重，用400t油压机压成圆柱形块体；
(3)制备高纯六硼化硅：将步骤(2)压制的圆柱形块体装入真空电阻烧结炉的石墨坩埚中，抽真空至4Pa开始升温，升温功率130kw/h，温度升至1200℃开始反应，观察炉内压表、真空度表，待数值起伏较大，真空泵加速运转排出产生的大量气体，真空度降至4Pa，继续保温2小时，停电随炉降温，得到高纯六硼化硅(SiB6)，经检测，高纯六硼化硅的纯度为99.61％。
实施例3
二氧化硅粉纯度为99.9％，粒度为600目，
硼酐的纯度为99.8％,粒度为800目，
碳化硼的纯度为99.5％，粒度为400目，
石墨粉纯度为99.99％，粒度为800目。
(1)混料：称取二氧化硅4.81kg、硼酐5.57kg、碳化硼4.42kg、石墨粉3.84kg(摩尔比1:1:1:4)，加入粘合剂56g、镁粉18.64g，放入10L的真空球磨机中，每次装料3kg，混料4小时，得到混合物料；
(2)压块：将混合物料按每份0.8kg称重，用400t油压机压成圆柱形块体；
(3)制备高纯六硼化硅：将步骤(2)压制的圆柱形块体装入真空电阻烧结炉的石墨坩埚中，抽真空至5Pa开始升温，升温功率130kw/h，温度升至1200℃开始反应，观察炉内压表、真空度表，待数值起伏较大，真空泵加速运转排出产生的大量气体，真空度降至5Pa，继续保温2小时，停电随炉降温，得到高纯六硼化硅(SiB6)，经检测，高纯六硼化硅的纯度为99.55％。
以上仅为本发明的具体实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作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)
1.一种一步法生产高纯六硼化硅的工艺，其特征是，
具体步骤如下：
(1)混料
以二氧化硅、硼酐、碳化硼和石墨粉为原料粉，其中，二氧化硅与硼酐的摩尔比为1:(1-3)，二氧化硅与碳化硼的摩尔比为1:1，二氧化硅与石墨粉的摩尔比为1:(4-6)，加入粘合剂和镁粉，放入10L的真空球磨机中，混料2-4小时，得到混合物料；
(2)压块
将混合物料按照每份0.8kg称重，用400t油压机压成圆柱形块体；
(3)制备高纯六硼化硅
将步骤(2)压制的圆柱形块体装入真空电阻烧结炉的石墨坩埚中，抽真空至0-5Pa，开始升温，升温功率为130kw/h，温度升至1200℃，开始反应，继续抽真空，真空度降至3Pa-5Pa后，继续保温2小时，停电随炉降温，得到高纯六硼化硅。
2.根据权利要求1所述的一步法生产高纯六硼化硅的工艺，其特征是：二氧化硅粉纯度为99.9％，硼酐的纯度为99.8％，碳化硼的纯度为99.5％，石墨粉纯度为99.99％。
3.根据权利要求1所述的一步法生产高纯六硼化硅的工艺，其特征是：二氧化硅粉粒度为600目，硼酐的粒度为800目，碳化硼的粒度为400目，石墨粉的粒度为800目。
4.根据权利要求1所述的一步法生产高纯六硼化硅的工艺，其特征是：加入的粘合剂为羧甲基纤维素，每1kg原料粉加入羧甲基纤维素3g。
5.根据权利要求1所述的一步法生产高纯六硼化硅的工艺，其特征是：每1kg原料粉加入镁粉10g。
6.根据权利要求1所述的一步法生产高纯六硼化硅的工艺，其特征是：真空球磨机中球磨时，每次装料量为3kg-5kg。
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