CN105948755A - 无压烧结用碳化硅微粉的生产方法 - Google Patents
无压烧结用碳化硅微粉的生产方法 Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 65
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000000843 powder Substances 0.000 title claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 238000001272 pressureless sintering Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 19
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- 238000005554 pickling Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000010298 pulverizing process Methods 0.000 claims description 11
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 239000003595 mist Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 17
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- 230000001105 regulatory effect Effects 0.000 abstract 1
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
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- 238000007789 sealing Methods 0.000 description 2
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- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000010297 mechanical methods and process Methods 0.000 description 1
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Abstract
本发明公开了一种无压烧结用碳化硅微粉的生产方法，属于碳化硅微粉生产技术领域。解决了现有技术先研磨后提纯存在的提纯难和物料收集难的问题，其包括以下步骤：(1)选料；(2)搅拌：将碳化硅微粉加入搅拌桶，加去离子水搅拌；(3)酸洗：将混合酸加入到碳化硅微粉中，搅拌反应；(4)压滤冲洗：将物料脱水、冲洗至物料pH为5‑7；(5)烘干粉碎：将烘干后的物料投入蒸汽动能磨粉碎至物料D50值不大于0.5μm；(6)造粒干燥：将粉碎后的物料加入配料调和后加去离子水调节固液比，待混合均匀后喷雾造粒即可。本发明方法适用于生产无压烧结用碳化硅微粉。
Description
技术领域
本发明涉及一种无压烧结用碳化硅微粉的生产方法，属于碳化硅微粉生产技术领域。
背景技术
随着科学技术的发展，特别是能源、空间技术的高度发展，对材料的要求越来越高，无压烧结碳化硅微粉主要应用于碳化硅陶瓷，如机械密封件、防弹板、装甲板、轴承、轴套、换热器、蜂窝陶瓷等。这就要求材料必须具有耐高温、抗腐蚀、耐磨损等优越性能，才能在比较苛刻的工作环境中使用。由于碳化硅无压烧结陶瓷材料具有抗氧化性强、耐磨性能好、硬度高、热稳定性好、高温强度大、热膨胀系数小、热导率大以及抗热震和耐化学腐蚀等优良特性，因此其已成为尖端科学的重要组成部分，受到普遍重视。
碳化硅陶瓷是近二十几年才开始发展的新材料，但由于其具有特别优良的高强度、高硬度、耐腐蚀、耐高温性能，因此很快得到了开发应用，大量应用于石油化工、冶金机械、航空航天、微电子、汽车、钢铁等领域，并日益显示出其他特种陶瓷所无法比拟的优点。现有的无压烧结碳化硅制品专用碳化硅微粉的生产方法主要有两种：悬浮法和研磨法。这两种方法的缺点是工作效率低，用水量大，生产成本高，物料提纯、收集难度大，跑料严重。
2014年1月29日公开的申请号为201310507885.X的中国发明专利“亚微米级碳化硅微粉的酸洗提纯方法”，该工艺为亚微米级超细粉的提纯，由于颗粒细，在实际操作过程中会出现超细粉收集难度大，跑料严重的现象。申请号为2009102565123，名称为“无压烧结碳化硅制品专用碳化硅微粉及其生产方法”的中国专利，采用先提纯后研磨的方法，对提纯好的物料运用立式砂磨机研磨，在实际生产研磨过程中立式砂磨机的内壁聚氨酯会对物料造成污染。
发明内容
本发明的目的在于提供一种无压烧结用碳化硅微粉的生产方法，本方法操作方便，工作效率高，生产成本低。
所述的无压烧结用碳化硅微粉的生产方法，包括以下步骤：
(1)选料：选择D50为5-7μm的碳化硅微粉；
(2)搅拌：将碳化硅微粉加入搅拌桶，并加入去离子水搅拌均匀；
(3)酸洗：将混合酸加入到碳化硅微粉中，搅拌反应15-20小时；
(4)压滤冲洗：将酸洗后的物料送至压滤机内进行脱水，然后用去离子水冲洗，直至物料pH为5-7；
(5)烘干粉碎：将压滤机内的物料取出后放入80-100℃的烘箱内烘干，烘干后将物料投入蒸汽动能磨进行粉碎，至物料D50值不大于0.5μm；
(6)造粒干燥：将粉碎后的物料加入配料调和为混合料，然后加去离子水调节固液比，待混合均匀后喷雾造粒即得所述的无压烧结用碳化硅微粉。
所述的去离子水电导率为5-30μs/cm。
步骤(2)所述的碳化硅微粉和去离子水的质量比为1-3:3-6。
步骤(3)所述的混合酸由氢氟酸、硫酸、硝酸按照2:2:1的质量比混合而成。
步骤(3)所述的混合酸与碳化硅微粉的质量比为5-10:1-3。
步骤(5)所述的蒸汽动能磨的蒸汽压力为30-40MPa，叶轮转速为4000-6000转/分。
步骤(6)所述的配料由B4C、酚醛树脂、乙醇和油酸组成。
步骤(6)所述配料的各组分的质量比为B4C：酚醛树脂：乙醇：油酸为0.2-0.6:0.3-0.8:5-10:0.8-1.3。
步骤(6)所述的物料与配料的质量比为100:1。
步骤(6)所述的混合料与去离子水的质量比为1:0.5-1。
所述方法生产的碳化硅微粉的含量≥98.5％。
与现有技术相比本发明的有益效果是：
本发明方法操作方便，解决了现有技术先研磨后提纯存在的提纯难和物料收集难的问题，本发明先对粗物料提纯，后经无污染蒸汽动能磨粉碎，粉碎过程为物料高速对撞过程，对撞过程是物料本身的对撞，不会掺入任何杂质，可始终保持物料碳化硅含量98.5％以上。本发明方法工作效率高，大大减少了用水量，降低了生产成本，所生产的碳化硅微粉性能稳定，粒度均匀，可广泛应用于生产机械密封件、防弹板、装甲板、轴承、轴套、换热器、蜂窝陶瓷等。
具体实施方式
下面结合具体实施例对本发明做进一步说明。
实施例1
所述的无压烧结用碳化硅微粉的生产方法，包括以下步骤：
(1)选料：选择D50为6μm的碳化硅微粉；
(2)搅拌：将碳化硅微粉加入搅拌桶，并按照碳化硅微粉和去离子水的质量比为1:3的比例加入去离子水搅拌均匀；
(3)酸洗：将由氢氟酸、硫酸、硝酸按照2:2:1的质量比混合而成的混合酸加入到碳化硅微粉中，搅拌反应18小时，其中混合酸与碳化硅微粉的质量比为10:3；
(4)压滤冲洗：将酸洗后的物料送至压滤机内进行脱水，然后用去离子水冲洗，直至物料pH为6；
(5)烘干粉碎：将压滤机内的物料取出后放入90℃的烘箱内烘干，烘干后将物料投入蒸汽压力为35MPa，叶轮转速为5000转/分的蒸汽动能磨进行粉碎，至物料D50值不大于0.5μm；
(6)造粒干燥：将粉碎后的物料加入配料调和为混合料，然后加去离子水调节固液比，待混合均匀后喷雾造粒即得所述的无压烧结用碳化硅微粉，其中配料由B4C、酚醛树脂、乙醇和油酸按照0.4:0.5:7:1的质量比组成，物料与配料的质量比为100:1。
所述的去离子水电导率为20μs/cm。
所述方法生产的碳化硅微粉的含量为99.4％。
实施例2
所述的无压烧结用碳化硅微粉的生产方法，包括以下步骤：
(1)选料：选择D50为5μm的碳化硅微粉；
(2)搅拌：将碳化硅微粉加入搅拌桶，并按照碳化硅微粉和去离子水的质量比为1:6的比例加入去离子水搅拌均匀；
(3)酸洗：将由氢氟酸、硫酸、硝酸按照2:2:1的质量比混合而成的混合酸加入到碳化硅微粉中，搅拌反应15小时，其中混合酸与碳化硅微粉的质量比为10:1；
(4)压滤冲洗：将酸洗后的物料送至压滤机内进行脱水，然后用去离子水冲洗，直至物料pH为5；
(5)烘干粉碎：将压滤机内的物料取出后放入80℃的烘箱内烘干，烘干后将物料投入蒸汽压力为30MPa，叶轮转速为4000转/分的蒸汽动能磨进行粉碎，至物料D50值不大于0.5μm；
(6)造粒干燥：将粉碎后的物料加入配料调和为混合料，然后加去离子水调节固液比，待混合均匀后喷雾造粒即得所述的无压烧结用碳化硅微粉，其中配料由B4C、酚醛树脂、乙醇和油酸按照0.2:0.3:5:0.8的质量比组成，物料与配料的质量比为100:1。
所述的去离子水电导率为5μs/cm。
所述方法生产的碳化硅微粉的含量为99.1％。
实施例3
所述的无压烧结用碳化硅微粉的生产方法，包括以下步骤：
(1)选料：选择D50为7μm的碳化硅微粉；
(2)搅拌：将碳化硅微粉加入搅拌桶，并按照碳化硅微粉和去离子水的质量比为1:1的比例加入去离子水搅拌均匀；
(3)酸洗：将由氢氟酸、硫酸、硝酸按照2:2:1的质量比混合而成的混合酸加入到碳化硅微粉中，搅拌反应20小时，其中混合酸与碳化硅微粉的质量比为5:3；
(4)压滤冲洗：将酸洗后的物料送至压滤机内进行脱水，然后用去离子水冲洗，直至物料pH为7；
(5)烘干粉碎：将压滤机内的物料取出后放入100℃的烘箱内烘干，烘干后将物料投入蒸汽压力为40MPa，叶轮转速为6000转/分的蒸汽动能磨进行粉碎，至物料D50值不大于0.5μm；
(6)造粒干燥：将粉碎后的物料加入配料调和为混合料，然后加去离子水调节固液比，待混合均匀后喷雾造粒即得所述的无压烧结用碳化硅微粉，其中配料由B4C、酚醛树脂、乙醇和油酸按照0.6:0.8:10:1.3的质量比组成，物料与配料的质量比为100:1。
所述的去离子水电导率为30μs/cm。
所述方法生产的碳化硅微粉的含量为98.8％。
Claims (10)
1.一种无压烧结用碳化硅微粉的生产方法，其特征在于包括以下步骤：
(1)选料：选择D50为5-7μm的碳化硅微粉；
(2)搅拌：将碳化硅微粉加入搅拌桶，并加入去离子水搅拌均匀；
(3)酸洗：将混合酸加入到碳化硅微粉中，搅拌反应15-20小时；
(4)压滤冲洗：将酸洗后的物料送至压滤机内进行脱水，然后用去离子水冲洗，直至物料pH为5-7；
(5)烘干粉碎：将压滤机内的物料取出后放入80-100℃的烘箱内烘干，烘干后将物料投入蒸汽动能磨进行粉碎，至物料D50值不大于0.5μm；
(6)造粒干燥：将粉碎后的物料加入配料调和为混合料，然后加去离子水调节固液比，待混合均匀后喷雾造粒即得所述的无压烧结用碳化硅微粉。
2.根据权利要求1所述的无压烧结用碳化硅微粉的生产方法，其特征在于：所述的去离子水电导率为5-30μs/cm。
3.根据权利要求1或2所述的无压烧结用碳化硅微粉的生产方法，其特征在于：步骤(2)所述的碳化硅微粉和去离子水的质量比为1-3:3-6。
4.根据权利要求3所述的无压烧结用碳化硅微粉的生产方法，其特征在于：步骤(3)所述的混合酸由氢氟酸、硫酸、硝酸按照2:2:1的质量比混合而成。
5.根据权利要求4所述的无压烧结用碳化硅微粉的生产方法，其特征在于：步骤(3)所述的混合酸与碳化硅微粉的质量比为5-10:1-3。
6.根据权利要求5所述的无压烧结用碳化硅微粉的生产方法，其特征在于：步骤(5)所述的蒸汽动能磨的蒸汽压力为30-40MPa，叶轮转速为4000-6000转/分。
7.根据权利要求6所述的无压烧结用碳化硅微粉的生产方法，其特征在于：步骤(6)所述的配料由B4C、酚醛树脂、乙醇和油酸组成。
8.根据权利要求7所述的无压烧结用碳化硅微粉的生产方法，其特征在于：步骤(6)所述配料的各组分的质量比为B4C：酚醛树脂：乙醇：油酸为0.2-0.6:0.3-0.8:5-10:0.8-1.3。
9.根据权利要求8所述的无压烧结用碳化硅微粉的生产方法，其特征在于：步骤(6)所述的物料与配料的质量比为100:1。
10.根据权利要求9所述的无压烧结用碳化硅微粉的生产方法，其特征在于：步骤(6)所述的混合料与去离子水的质量比为1:0.5-1。
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| CN108752003A (zh) * | 2018-08-17 | 2018-11-06 | 宁夏和兴碳基材料有限公司 | 碳化硅精细陶瓷用碳化硅微粉的制备方法 |
| CN108892142A (zh) * | 2018-07-24 | 2018-11-27 | 通化宏信研磨材有限责任公司 | 一种亚微米碳化硅超细粉体的提纯方法 |
| CN109851364A (zh) * | 2019-04-18 | 2019-06-07 | 山田研磨材料有限公司 | 一种碳化硅挤出成型生产工艺 |
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| CN108892142B (zh) * | 2018-07-24 | 2021-09-14 | 通化宏信研磨材有限责任公司 | 一种亚微米碳化硅超细粉体的提纯方法 |
| CN108752003A (zh) * | 2018-08-17 | 2018-11-06 | 宁夏和兴碳基材料有限公司 | 碳化硅精细陶瓷用碳化硅微粉的制备方法 |
| CN108752003B (zh) * | 2018-08-17 | 2021-06-22 | 宁夏和兴碳基材料有限公司 | 碳化硅精细陶瓷用碳化硅微粉的制备方法 |
| CN109896860A (zh) * | 2019-04-16 | 2019-06-18 | 山田研磨材料有限公司 | 一种碳化硅注浆成型生产工艺 |
| CN109956755A (zh) * | 2019-04-16 | 2019-07-02 | 山田研磨材料有限公司 | 一种碳化硅挤出成型生产烧结工艺 |
| CN109851364A (zh) * | 2019-04-18 | 2019-06-07 | 山田研磨材料有限公司 | 一种碳化硅挤出成型生产工艺 |
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