CN113773088A - 一种莫来石结合SiC磨料的制备方法 - Google Patents
一种莫来石结合SiC磨料的制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 105
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 104
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 50
- 238000003756 stirring Methods 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 21
- 239000008187 granular material Substances 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 229910052593 corundum Inorganic materials 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 8
- 229940009827 aluminum acetate Drugs 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052682 stishovite Inorganic materials 0.000 claims description 8
- 229910052905 tridymite Inorganic materials 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000009825 accumulation Methods 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 abstract 2
- 239000000654 additive Substances 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010297 mechanical methods and process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
本发明提供了一种莫来石结合SiC磨料的制备方法，属于磨料制备及纳米复合材料领域。具体制备步骤为：将碳化硅微粉加入到乙醇水溶液中，超声搅拌1~2h；制备莫来石溶胶，将SiC微粉的乙醇水溶液加入，超声搅拌1~2h，干燥后得到莫来石包覆碳化硅颗粒；接着加入PVA混合均匀，密封静置后，进行制粒，干燥后得到均匀大小的SiC颗粒；将这些碳化硅颗粒在1200~1500℃下进行热处理2~3h，得到粒度再造的莫来石结合SiC磨料。本发明通过纳米莫来石和PVA作为添加剂，一方面解决了SiC颗粒过小而无法使用的问题；另一方面少量纳米莫来石的加入，降低了烧结温度，节约了能源。这种莫来石结合的SiC磨料，有尖锐的棱角，磨削性能优良，很好的解决了颗粒过小的SiC微粉再利用的问题。
Description
技术领域
本发明属于磨料制备及纳米复合材料领域，特别是涉及一种莫来石结合SiC磨料的制备方法。
背景技术
碳化硅的结晶结构属于具有较好稳定性的典型共价键结构，稳定性良好，在自然界中几乎不存在纯净的碳化硅化合物。碳化硅因为其良好的超硬性能，在磨料磨具领域得到了广泛的应用，可制备成各种磨削用的砂轮、砂布、砂纸或是作磨料直接应用。
碳化硅的粒度对于其本身的应用有着极其重要的影响。超细粉体粒度再造有多种方法，常用的机械法有球磨法、搅拌球磨法、气流磨法、振动磨粉碎法、机械冲击粉碎法和砂磨粉碎法。物理化学方法有超声波法、氧化腐蚀结合球磨工艺、氢氧化钠腐蚀法等。机械法成本低，工艺简单，产量高，但存在一定的环境污染，粉体纯度不高；物理化学法工序复杂，成本高，产量低。但是在碳化硅的制备过程中，往往会产生许多超细碳化硅微粉，这些碳化硅微粉因粒度过细不能得到有效利用，造成了生产成本升高和一定的环境污染。
发明内容
为了解决碳化硅生产应用中的问题，本发明将莫来石溶胶和PVA作为结合剂，提供了一种莫来石结合SiC磨料的制备方法。
具体的，本发明提供的一种莫来石结合SiC磨料的制备方法，按照具体如下步骤实施：
S1：称取一定量的碳化硅微粉，在超声搅拌的条件下将S2中的碳化硅微粉加入到乙醇的水溶液中，持续搅拌1~2h至充分分散，无水乙醇的水溶液中无水乙醇与水的体积比在1~3：1，取用无水乙醇的体积与碳化硅微粉的质量比为0.2~1ml：1g；
S2：制备莫来石溶胶，莫来石的化学式为3Al2O3·2SiO2，莫来石与SiC微粉的质量比在5%~15%之间；
S21：制备Al2O3溶胶，根据S2中莫来石的量确定Al2O3溶胶的用量，称取对应量的乙酸铝，与10~15ml无水乙醇混合，用磁力搅拌器搅拌20~30min，然后缓慢加入稀硝酸调节PH值至2~4，溶胶均匀透明，然后在磁力搅拌器上搅拌1~2h，得到Al2O3溶胶；
S22：制备SiO2溶胶，根据S2中莫来石的量确定SiO2溶胶的用量，将对应量的正硅酸乙酯与10~15ml的无水乙醇混合，用磁力搅拌器搅拌15~25min，然后缓慢加入冰醋酸溶液调节PH值至1~3，溶胶均匀透明，最后在磁力搅拌器上均匀搅拌1~2h，得到SiO2溶胶；
S23：在磁力搅拌的条件下，将S21中的Al2O3溶胶缓慢倒入S22的SiO2溶胶中，用磁力搅拌器搅拌0.5~1h，至均匀混合后，得到莫来石溶胶；
S3：在超声搅拌的条件下，将S1中的SiC微粉，缓慢加入到S23的莫来石溶胶中，持续搅拌1~2h至充分分散，然后在80~100℃干燥6~8h，得到均匀混合的莫来石包覆SiC微粉；
S4：将PVA加入到S3的SiC微粉中，PVA的质量与S3中莫来石包覆SiC微粉的质量百分比为3%~5%，机械搅拌1~2h，混合均匀后，密封静置5~10h后得到SiC微粉混合料；
S5：将S4中混合均匀后的粉料倒入制粒机中进行制粒，得到大小均匀，粒度范围为20~200μm的SiC颗粒，在90~100℃下干燥1~2h，得到湿度适当的SiC颗粒；
S6：将S5中处理后的碳化硅颗粒放入高温炉中进行烧结，在1200~1500℃下进行热处理2~3h，然后得到粒度再造的莫来石结合SiC磨料；
优选地，S1中所用SiC微粉粒度为0.5~3μm。
优选地，S2中所用莫来石的量与SiC微粉的质量比在5%~15%之间。
优选地，S5中制粒得到的SiC颗粒的粒度范围为20~200μm。
优选地，S6中，SiC颗粒的烧结温度为1200~1500℃。
上述方法制备得到的粒度再造的莫来石结合碳化硅磨料，形状保持性和自锐性良好。
上述方法制备得到的粒度再造的莫来石结合碳化硅磨料，应用广泛，特别是在堆积磨料砂带、固结磨料线锯、精密磨削、以及用于制作结构陶瓷等方面的应用。
本发明的技术方案具有如下有益效果：
本发明首先提供了一种莫来石结合SiC磨料的制备方法，利用纳米莫来石溶胶和PVA作为结合剂，解决了碳化硅微粉由于粒度过细而无法利用的问题。并且纳米莫来石溶胶的加入，降低了烧结温度，而且粒度再造后的SiC磨料颗粒表面粗造，有尖锐的棱角，磨削性能优良，在保留了SiC优良使用性能的同时，还具有很好的强度，并且实现了废物利用，降低了SiC的生产成本，也减少了环境污染。本发明提供的莫来石结合SiC磨料的制备方法，也可以很好的应用到其他种类的微粉磨料中，具有很好的实用性。
具体实施方式
下面结合具体实施例对本发明作进一步说明，本领域技术人员应该明了实施例是为了更好地理解本发明的技术方案，能予以实施，不应视为对本发明的限定。
本发明中使用的所有技术和科学术语与本技术领域技术人员通常理解的意义相同。下列实施例中如无特别说明所采用的方法均为常规方法，所采用的原料均为市售分析纯原料。均不作为对本发明的限定，本技术领域的技术人员还可以根据对现有技术的掌握及本发明的记载，使用相似的方法，设备，材料来重复实施本发明。
下面就本发明的技术方案进行具体的举例说明。
实施例1
一种莫来石结合SiC磨料的制备方法，其特征在于，具体实施步骤如下：
S1：称取30g的碳化硅微粉，在超声搅拌的条件下将S2中的碳化硅微粉加入到30ml乙醇的水溶液中，持续搅拌1~2h至充分分散，无水乙醇的水溶液中无水乙醇与水的体积比在1.5：1，取用无水乙醇的体积与碳化硅微粉的质量比为1ml：1g；
S2：制备莫来石溶胶，莫来石的化学式为3Al2O3·2SiO2，莫来石与SiC微粉的质量比为10%；
S21：制备Al2O3溶胶，根据S2中莫来石的量确定Al2O3溶胶的用量，将对应量的乙酸铝与15ml无水乙醇混合，用磁力搅拌器搅拌30min，然后缓慢加入稀硝酸调节PH值至3，溶胶均匀透明，然后在磁力搅拌器上搅拌2h，得到Al2O3溶胶；
S22：制备SiO2溶胶，根据S2中莫来石的量确定SiO2溶胶的用量，将对应量的正硅酸乙酯与15ml的无水乙醇混合，用磁力搅拌器搅拌25min，然后缓慢加入冰醋酸溶液调节PH值至2，溶胶均匀透明，最后在磁力搅拌器上均匀搅拌2h，得到SiO2溶胶；
S23：在磁力搅拌的条件下，将S21中的Al2O3溶胶缓慢倒入S22的SiO2溶胶中，用磁力搅拌器搅拌1h，至均匀混合后，得到莫来石溶胶；
S3：在超声搅拌的条件下，将S1中的SiC微粉，缓慢加入到S23的莫来石溶胶中，持续搅拌2h至混合均匀，然后在80℃干燥6h，得到均匀混合的莫来石包覆SiC微粉；
S4：将PVA加入到S3的SiC微粉中，PVA的质量与S3中莫来石包覆SiC微粉的质量百分比为5%，机械搅拌1h，混合均匀后，密封静置10h后得到SiC微粉混合料；
S5：将S4中混合均匀后的粉料倒入制粒机中进行制粒，得到大小均匀，粒度为30μm的SiC颗粒，在90~100℃下干燥1h，得到湿度适当的SiC颗粒；
S6：将S5中处理后的碳化硅颗粒放入高温炉中进行烧结，在1300℃下进行热处理3h，然后得到粒度再造的莫来石结合SiC磨料。
实施例2
一种莫来石结合SiC磨料的制备方法，具体实施步骤如下：
S1：称取30g的碳化硅微粉，在超声搅拌的条件下将S2中的碳化硅微粉加入到30ml乙醇的水溶液中，持续搅拌2h至充分分散，无水乙醇的水溶液中无水乙醇与水的体积比在2：1，取用无水乙醇的体积与碳化硅微粉的质量比为1ml：1g；
S2：制备莫来石溶胶，莫来石的化学式为3Al2O3·2SiO2，莫来石与SiC微粉的质量比为13%；
S21：制备Al2O3溶胶，根据S2中莫来石的量确定Al2O3溶胶的用量，将对应量的乙酸铝与15ml无水乙醇混合，用磁力搅拌器搅拌30min，然后缓慢加入稀硝酸调节PH值至3，溶胶均匀透明，然后在磁力搅拌器上搅拌2h，得到Al2O3溶胶；
S22：制备SiO2溶胶，根据S2中莫来石的量确定SiO2溶胶的用量，将对应量的正硅酸乙酯与15ml的无水乙醇混合，用磁力搅拌器搅拌20min，然后缓慢加入冰醋酸溶液调节PH值至2，溶胶均匀透明，最后在磁力搅拌器上均匀搅拌2h，得到SiO2溶胶；
S23：在磁力搅拌的条件下，将S21中的Al2O3溶胶缓慢倒入S22的SiO2溶胶中，用磁力搅拌器搅拌1h，至均匀混合后，得到莫来石溶胶；
S3：在超声搅拌的条件下，将S1中的SiC微粉，缓慢加入到S23的莫来石溶胶中，持续搅拌1h至混合均匀，然后在80℃干燥6h，得到均匀混合的莫来石包覆SiC微粉；
S4：将PVA加入到S3的SiC微粉中，PVA的质量与S3中莫来石包覆SiC微粉的质量百分比为5%，机械搅拌1h，混合均匀后，密封静置10h后得到SiC微粉混合料；
S5：将S4中混合均匀后的粉料倒入制粒机中进行制粒，得到大小均匀，粒度范围为45μm的SiC颗粒，在90℃下干燥1h，得到湿度适当的SiC颗粒；
S6：将S5中处理后的碳化硅颗粒放入高温炉中进行烧结，在1350℃下进行热处理3h，然后得到粒度再造的莫来石结合SiC磨料；
实施例1，实施例2制得的莫来石结合碳化硅磨料工艺稳定，质量可靠，性能优良。例如我们分被选取了实施例1和实施例2中所制备的粒度为30μm，45μm的莫来石结合碳化硅颗粒，制备了SiC陶瓷磨具，对硅晶圆进行磨削加工，加工后合金的表面非常均匀，其粗糙度分别达到0.18μm，0.24μm；为了对照选用市售的SiC陶瓷磨具，加工后的硅晶圆表面粗糙度较大，最小仅为0.4μm；并且本发明制备的纳米结合的碳化硅陶瓷磨具的磨削效率更高，磨削损耗更小。
以上所述实施例仅是为充分说明本发明而所举的较佳的实施例，其保护范围不限于此。本技术领域的技术人员在本发明基础上所作的等同替代或变换，均在本发明的保护范围之内，本发明的保护范围以权利要求书为准。
Claims (7)
1.一种莫来石结合SiC磨料的制备方法，其特征在于，具体实施步骤如下：
S1：称取一定量的碳化硅微粉，在超声搅拌的条件下将S2中的碳化硅微粉加入到乙醇的水溶液中，持续搅拌1~2h至充分分散，无水乙醇的水溶液中无水乙醇与水的体积比在1~3：1，取用无水乙醇的体积与碳化硅微粉的质量比为0.2~1ml：1g；
S2：制备莫来石溶胶，莫来石的化学式为3Al2O3·2SiO2，莫来石与SiC微粉的质量比在5%~15%之间；
S21：制备Al2O3溶胶，根据S2中莫来石的量确定Al2O3溶胶的用量，将对应量的乙酸铝与10~15ml无水乙醇混合，用磁力搅拌器搅拌20~30min，然后缓慢加入稀硝酸调节PH值至2~4，溶胶均匀透明，然后在磁力搅拌器上搅拌1~2h，得到Al2O3溶胶；
S22：制备SiO2溶胶，根据S2中莫来石的量确定SiO2溶胶的用量，将对应量的正硅酸乙酯与10~15ml的无水乙醇混合，用磁力搅拌器搅拌15~25min，然后缓慢加入冰醋酸溶液调节PH值至1~3，溶胶均匀透明，最后在磁力搅拌器上均匀搅拌1~2h，得到SiO2溶胶；
S23：在磁力搅拌的条件下，将S21中的Al2O3溶胶缓慢倒入S22的SiO2溶胶中，用磁力搅拌器搅拌0.5~1h，至均匀混合后，得到莫来石溶胶；
S3：在超声搅拌的条件下，将S1中的SiC微粉，缓慢加入到S23的莫来石溶胶中，持续搅拌1~2h至充分分散，然后在80~100℃干燥6~8h，得到均匀混合的莫来石包覆SiC微粉；
S4：将PVA加入到S3的SiC微粉中，PVA的质量与S3中莫来石包覆SiC微粉的质量百分比为3%~5%，机械搅拌1~2h，混合均匀后，密封静置5~10h后得到SiC微粉混合料；
S5：将S4中混合均匀后的粉料倒入制粒机中进行制粒，得到大小均匀，粒度范围为20~200μm的SiC颗粒，在90~100℃下干燥1~2h，得到湿度适当的SiC颗粒；
S6：将S5中处理后的碳化硅颗粒放入高温炉中进行烧结，在1200~1500℃下进行热处理2~3h，然后得到粒度再造的莫来石结合SiC磨料。
2.根据权利要求1所述的莫来石结合SiC磨料的制备方法，其特征在于，S1中所用SiC微粉粒度为0.5~3μm。
3.根据权利要求1所述的莫来石结合SiC磨料的制备方法，其特征在于，S2中所用莫来石的量与SiC微粉的质量比在5%~15%之间。
4.根据权利要求1所述的莫来石结合SiC磨料的制备方法，其特征在于，S5中制粒得到的SiC颗粒的粒度范围为20~200μm。
5.根据权利要求1所述的莫来石结合SiC磨料的制备方法，其特征在于，S6中，SiC颗粒的热处理温度为1200~1500℃。
6.一种莫来石结合SiC磨料，其特征在于，由权利要求1~5任一所述的方法制备获得。
7.根据权利要求6所述的莫来石结合SiC磨料，其特征在于，可应用在堆积磨料砂带、固结磨料线锯、精密磨削、以及用于制作结构陶瓷等方面。
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