CN114436667A - 一种增加氮化硅韧性的制备方法 - Google Patents
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 49
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 229910007948 ZrB2 Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- 238000007731 hot pressing Methods 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000207199 Citrus Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006355 external stress Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011361 granulated particle Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种增加氮化硅韧性的制备方法，涉及一种氮化硅制备方法，由于氮化硅脆性一直是限制氮化硅陶瓷应用的最大问题，所以本申请包括以下步骤：S1、制备原材料，在α‑Si3N4和β‑Si3N4中添加SiC晶须和Si3N4短纤维；S2、原材料倒入密闭搅拌器内搅拌，在搅拌器中加入SiC晶须、Si3N4短纤维和PVA，对所述密闭搅拌器加热保温直至密闭搅拌器内的温度维持80‑100℃，对所述密闭搅拌器通气1‑2h；S3、调节助烧剂用量成分；S4、对步骤S2中所得成品造粒；S5、对S4中的颗粒成品高温烧结，加入步骤S3中调制的助烧剂，本申请通过对氮化硅制作方式的改进，能够使得制备的样品由普通氮化硅陶瓷断裂韧性5.2MPa·m1/2，提高至断裂韧性为7.82MPa·m1/2，从而有效地提高氮化硅的韧性。
Description
技术领域
本发明涉及一种氮化硅制备方法，具体是一种增加氮化硅韧性的制备方法。
背景技术
氮化硅陶瓷材料具有优异的高温强度和耐环境性，其有热震性好、耐腐蚀、摩擦系数小、热膨胀系数小的特点，它在冶金和热加工工业上被广泛用于测温热电偶套管、铸模、柑涡、烧舟、马弗炉炉膛、燃烧嘴、发热体夹具、炼铝炉炉衬、铝液导管、铝包内衬、铝电解槽衬里、热辐射管、高温鼓风机、阀门等；但其脆性一直是限制氮化硅陶瓷应用的最大问题。
发明内容
本发明的目的在于提供一种增加氮化硅韧性的制备方法，以解决上述背景技术中提出的问题。
为实现上述目的，本发明提供如下技术方案：
一种增加氮化硅韧性的制备方法，包括以下步骤：
S1、制备原材料，在α-Si3N4和β-Si3N4中添加SiC晶须和Si3N4短纤维；
S2、原材料倒入密闭搅拌器内搅拌，对所述密闭搅拌器加热保温直至密闭搅拌器内的温度维持80-100℃，对所述密闭搅拌器通气1-2h；
S3、调节助烧剂用量成分；
S4、对步骤S2中所得成品造粒；
S5、对S4中的颗粒成品高温烧结，加入步骤S3中调制的助烧剂。
作为本发明进一步的方案：所述步骤S1中的原材料还包括ZrB2、氧化锆、氧化铈分散剂和PVA。
作为本发明再进一步的方案：所述步骤S1中的原材料的各个组分配比分别为：α-Si3N4 (1-10份)、β-Si3N4(70-80份)、SiC晶须(1-10份)、Si3N4短纤维(1-10份)、ZrB2 (1-10份)、氧化锆(1-5份)和氧化铈分散剂(1-5份)。
作为本发明再进一步的方案：所述步骤S1中加入的SiC晶须和Si3N4短纤维比例为1： 3。
作为本发明再进一步的方案：所述步骤S2中的密闭搅拌器上设置有出气孔和进气孔。
作为本发明再进一步的方案：所述步骤S3中助烧剂用量成分配比为：ZrB2：ZrO2：CeO2为1:3:5。
作为本发明再进一步的方案：所述步骤S4中成品造粒尺径分为三种，造粒球体大颗粒粒径为：130-200μm，造粒球体中颗粒粒径：80-120μm，造粒球体小颗粒粒径：40-60μm。
作为本发明再进一步的方案：所述步骤S4中的成品造粒水分率为：1％-2％。
作为本发明再进一步的方案：所述步骤S5中高温烧结条件为，在烧结温度达到1300-1600℃时，充氮气(0.3-0.5MPa)。
作为本发明再进一步的方案：所述步骤S5中的高温烧结方式是：采用热压烧结工艺和放电等离子烧结工艺结合。
与现有技术相比，本发明的有益效果是：本申请通过对氮化硅制作方式的改进，能够使得制备的样品由普通氮化硅陶瓷断裂韧性5.2MPa·m1/2，提高至断裂韧性为7.82MPa·m1/2，，从而有效地提高氮化硅的韧性。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明实施例中，一种增加氮化硅韧性的制备方法，包括步骤S1，首先需要准备原材料及限定原材料的组分，其中需要加入α-Si3N4(1-10份)、β-Si3N4(70-80份)、SiC 晶须(1-10份)、Si3N4短纤维(1-10份)、ZrB2(1-10份)、氧化锆(1-5份)、氧化铈分散剂(1-5份)，PVA(聚乙烯醇)和去水离子若干份，在本实施例中，需要将加入的 SiC晶须和Si3N4短纤维的配置比例限定为1：3；
包括步骤S2，准备一个密闭搅拌器，其中在本实施例中的密闭搅拌器为80-100L的容量，其中密闭搅拌器是可以进行搅拌的，将原材料加入密闭搅拌器内进行搅拌，同时设置密闭搅拌器的加热到80-100℃后进行保温，随后往密闭搅拌器内部通气，通气时间为 1-2h，其中通入的气体可以是空气也可以是氮气或者其余惰性气体，在本实施例中在密闭搅拌器上设置出气孔和进气孔，并在进气孔上加入40-50个管道气流进行通气操作，直至 SiC晶须和Si3N4短纤维均匀分散在Si3N4的基体中，形成混合后的原材料；
包括步骤S3，调节助烧剂的成分和成分的用量，即在本实施例中采用ZrB2、ZrO2和CeO2，并且其配比为1:3:5；
包括步骤S4，对步骤S2中混合好的原材料进行造粒，并对造粒的球体尺寸进行限定，其中造粒球体大颗粒粒径为130-200μm，造粒球体中颗粒粒径为80-120μm，造粒球体小颗粒粒径为40-60μm且对造粒形成的颗粒水分率进行限定，限定在1％-2％；
包括步骤S5，对造粒后的原材料进行高温烧结，并加入步骤S3中的助烧剂，即以ZrB2、ZrO2、CeO2为烧结助剂，当温度达到1300-1600℃时，充氮气(0.3-0.5MPa)保护，防止SiC、Si3N4晶须氧化，本申请中采用的是热压烧结工艺和放电等离子烧结工艺相结合的烧结方式对氮化硅样品进行烧结，这样促进了第二相ZrB2的引入，ZrB2的引入使得α-Si3N4转化β-Si3N4相变，可抵消外加应力，阻止裂纹扩展达到增韧的目的，经最终的实验可得，使用该方法进行增韧，制备的样品由普通氮化硅陶瓷断裂韧性5.2MPa·m1/2，提高至断裂韧性为7.82MPa·m1/2。
作为本申请的进一步实施例，在步骤S4和步骤S5之间还存在步骤Sn，其中步骤Sn是将步骤S4得到的颗粒使用方形模具进行压制，将颗粒压制到一定的条件后形成致密的毛坯，在本实施例中，压成边长为120mm的正方形，在此过程中实用的压力是35MP，保压时间为20min。
由于常见的增韧方式有连续纤维增韧、短切纤维/晶须增韧、颗粒增韧、相变增韧、纳米增韧等，其中相变增韧和纳米增韧属于自增韧，取决于陶瓷材料本身固有的特性和形貌，通过各种形貌的增强体(纤维、颗粒、晶须等)增强的陶瓷基复合材料能极大地改善陶瓷基体的断裂韧性。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。
Claims (10)
1.一种增加氮化硅韧性的制备方法，其特征在于，包括以下步骤：
S1、制备原材料，在α-Si3N4和β-Si3N4中添加SiC晶须和Si3N4短纤维；
S2、原材料倒入密闭搅拌器内搅拌，对所述密闭搅拌器加热保温直至密闭搅拌器内的温度维持80-100℃，对所述密闭搅拌器通气1-2h；
S3、调节助烧剂用量成分；
S4、对步骤S2中所得成品造粒；
S5、对S4中的颗粒成品高温烧结，加入步骤S3中调制的助烧剂。
2.根据权利要求1所述的增加氮化硅韧性的制备方法，其特征在于，所述步骤S1中的原材料还包括ZrB2、氧化锆、氧化铈分散剂和PVA。
3.根据权利要求2所述的增加氮化硅韧性的制备方法，其特征在于，所述步骤S1中的原材料的各个组分配比分别为：α-Si3N4(1-10份)、β-Si3N4(70-80份)、SiC晶须(1-10份)、Si3N4短纤维(1-10份)、ZrB2(1-10份)、氧化锆(1-5份)和氧化铈分散剂(1-5份)。
4.根据权利要求1所述的增加氮化硅韧性的制备方法，其特征在于，所述步骤S1中加入的SiC晶须和Si3N4短纤维比例为1：3。
5.根据权利要求1所述的增加氮化硅韧性的制备方法，其特征在于，所述步骤S2中的密闭搅拌器上设置有出气孔和进气孔。
6.根据权利要求1所述的增加氮化硅韧性的制备方法，其特征在于，所述步骤S3中助烧剂用量成分配比为：ZrB2：ZrO2：CeO2为1:3:5。
7.根据权利要求1所述的增加氮化硅韧性的制备方法，其特征在于，所述步骤S4中成品造粒尺径分为三种，造粒球体大颗粒粒径为：130-200μm，造粒球体中颗粒粒径：80-120μm，造粒球体小颗粒粒径：40-60μm。
8.根据权利要求1所述的增加氮化硅韧性的制备方法，其特征在于，所述步骤S4中的成品造粒水分率为：1％-2％。
9.根据权利要求1所述的增加氮化硅韧性的制备方法，其特征在于，所述步骤S5中高温烧结条件为，在烧结温度达到1300-1600℃时，充氮气(0.3-0.5MPa)。
10.根据权利要求1所述的增加氮化硅韧性的制备方法，其特征在于，所述步骤S5中的高温烧结方式是：采用热压烧结工艺和放电等离子烧结工艺结合。
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4886767A (en) * | 1986-11-21 | 1989-12-12 | Kabushiki Kaisha Toshiba | Silicon nitride-ceramic and a manufacturing method therof |
| CN1058950A (zh) * | 1990-08-15 | 1992-02-26 | 陶氏化学公司 | 一种自增强氮化硅陶瓷体及其制备方法 |
| US5401450A (en) * | 1991-12-20 | 1995-03-28 | Nissan Motor Co., Ltd | β-silicon nitride sintered body and method of producing same |
| CN103848639A (zh) * | 2012-11-28 | 2014-06-11 | 大连大友高技术陶瓷有限公司 | 一种氮化硅增韧陶瓷 |
| CN105016738A (zh) * | 2014-04-30 | 2015-11-04 | 广东工业大学 | 氮化硅陶瓷及其制备方法 |
| CN107586136A (zh) * | 2017-10-17 | 2018-01-16 | 广东工业大学 | 一种3d打印氮化硅陶瓷的方法 |
| CN108439996A (zh) * | 2018-05-28 | 2018-08-24 | 江苏东浦精细陶瓷科技股份有限公司 | 一种氮化硅-碳化硅复合材料材料及其制备方法 |
| CN108975921A (zh) * | 2018-08-16 | 2018-12-11 | 南通通州湾新材料科技有限公司 | 一种氮化硅陶瓷的制备方法及其陶瓷覆铜板 |
| CN109206141A (zh) * | 2018-08-27 | 2019-01-15 | 广东工业大学 | 一种高硬高韧氮化硅陶瓷及其制备方法和应用 |
| CN110156476A (zh) * | 2019-04-26 | 2019-08-23 | 广东工业大学 | 一种高硬高韧氮化硅基陶瓷及其制备方法和应用 |
| CN111620711A (zh) * | 2020-05-21 | 2020-09-04 | 贵研铂业股份有限公司 | 一种仿生氮化硅陶瓷材料及其制备方法 |
| CN113185302A (zh) * | 2021-06-10 | 2021-07-30 | 灵石鸿润和新材料有限公司 | 一种风力发电用大尺寸氮化硅陶瓷球及其制备方法和应用 |
-
2021
- 2021-12-20 CN CN202111557682.2A patent/CN114436667A/zh active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4886767A (en) * | 1986-11-21 | 1989-12-12 | Kabushiki Kaisha Toshiba | Silicon nitride-ceramic and a manufacturing method therof |
| CN1058950A (zh) * | 1990-08-15 | 1992-02-26 | 陶氏化学公司 | 一种自增强氮化硅陶瓷体及其制备方法 |
| US5401450A (en) * | 1991-12-20 | 1995-03-28 | Nissan Motor Co., Ltd | β-silicon nitride sintered body and method of producing same |
| CN103848639A (zh) * | 2012-11-28 | 2014-06-11 | 大连大友高技术陶瓷有限公司 | 一种氮化硅增韧陶瓷 |
| CN105016738A (zh) * | 2014-04-30 | 2015-11-04 | 广东工业大学 | 氮化硅陶瓷及其制备方法 |
| CN107586136A (zh) * | 2017-10-17 | 2018-01-16 | 广东工业大学 | 一种3d打印氮化硅陶瓷的方法 |
| CN108439996A (zh) * | 2018-05-28 | 2018-08-24 | 江苏东浦精细陶瓷科技股份有限公司 | 一种氮化硅-碳化硅复合材料材料及其制备方法 |
| CN108975921A (zh) * | 2018-08-16 | 2018-12-11 | 南通通州湾新材料科技有限公司 | 一种氮化硅陶瓷的制备方法及其陶瓷覆铜板 |
| CN109206141A (zh) * | 2018-08-27 | 2019-01-15 | 广东工业大学 | 一种高硬高韧氮化硅陶瓷及其制备方法和应用 |
| CN110156476A (zh) * | 2019-04-26 | 2019-08-23 | 广东工业大学 | 一种高硬高韧氮化硅基陶瓷及其制备方法和应用 |
| CN111620711A (zh) * | 2020-05-21 | 2020-09-04 | 贵研铂业股份有限公司 | 一种仿生氮化硅陶瓷材料及其制备方法 |
| CN113185302A (zh) * | 2021-06-10 | 2021-07-30 | 灵石鸿润和新材料有限公司 | 一种风力发电用大尺寸氮化硅陶瓷球及其制备方法和应用 |
Non-Patent Citations (4)
| Title |
|---|
| WEI-MING GUO: "《rapid communication》", 《RAPID COMMUNICATION》 * |
| 于俊杰: "基于显微结构调控的高硬高韧氮化硅陶瓷的研究", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
| 杜大明: "氮化硅常压烧结研究进展", 《山东陶瓷》 * |
| 裴立宅: "《高技术陶瓷材料》", 31 March 2015 * |
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