CN116041071A - 一种高熵氮化物/塞隆复合陶瓷及其制备方法和应用 - Google Patents
一种高熵氮化物/塞隆复合陶瓷及其制备方法和应用 Download PDFInfo
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- 150000004767 nitrides Chemical class 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 43
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- 239000011812 mixed powder Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000007731 hot pressing Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 5
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- 229910052723 transition metal Inorganic materials 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 239000004677 Nylon Substances 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 7
- 229920001778 nylon Polymers 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
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- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
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- 150000001875 compounds Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 6
- 238000002390 rotary evaporation Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
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- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
本发明属于陶瓷技术领域，公开了一种高熵氮化物/塞隆复合陶瓷及其制备方法和应用，所述复合陶瓷中塞隆陶瓷的分子式为β‑Si6‑ zAlzOzN8‑z，z＝0.5～1.5；所述高熵氮化物/塞隆复合陶瓷是将高熵氮化物粉体、Si3N4粉体、AlN粉体、Al2O3粉体和Y2O3粉体加入乙醇和Si3N4球进行球磨混料，干燥后过筛，获得混合粉体；将混合粉体在保护气氛下加以30～80MPa轴向压力，升温至1700～1850℃热压烧结制得。本发明的高熵氮化物/塞隆复合陶瓷具有高硬度、高韧性、高耐磨性，可应用在陶瓷刀具领域中。
Description
技术领域
本发明属于结构陶瓷技术领域，具体地，涉及一种高熵氮化物/塞隆复合陶瓷及其制备方法和应用。
背景技术
高熵氮化物是由第Ⅳ族(Ti、Zr、Hf)、第Ⅴ族(V、Nb、Ta)、第Ⅵ族(Cr、Mo、W)过渡金属元素按等摩尔比组成的氮化物。高熵氮化物比过渡金属一元氮化物具有更高的硬度和韧性(参见ScientificReports,2020,10:19874)。塞隆陶瓷具有高硬度、高强度、耐磨损、抗氧化性和良好的抗热冲击与机械冲击性能，塞隆陶瓷被广泛应用于陶瓷刀具领域。塞隆陶瓷作为刀具材料使用时，通常添加TiN作为增强相，提高韧性和耐磨性等。但含TiN增强相的塞隆陶瓷刀具在切削高温合金等难加工材料时，切削寿命较短，需要进一步提升塞隆陶瓷的硬度、韧性和耐磨性。
发明内容
为了解决上述现有技术存在的不足，本发明目的在于提供一种高熵氮化物/塞隆复合陶瓷。
本发明另一目的在于提供一种上述高熵氮化物/塞隆复合陶瓷的制备方法。
本发明再一目的在于提供一种上述高熵氮化物/塞隆复合陶瓷的应用。
本发明的目的通过下述技术方案来实现：
一种高熵氮化物/塞隆复合陶瓷，所述复合陶瓷中塞隆陶瓷的分子式为β-Si6- zAlzOzN8-z，z＝0.5～1.5；所述高熵氮化物/塞隆复合陶瓷是将高熵氮化物粉体、Si3N4粉体、AlN粉体、Al2O3粉体和Y2O3粉体加入乙醇和Si3N4球进行球磨混料，干燥后过筛，获得混合粉体；将混合粉体在保护气氛下加以30～80MPa轴向压力，升温至1700～1850℃热压烧结制得。
优选地，所述的高熵氮化物粉体是由等摩尔比的第Ⅳ族过渡金属元素、第Ⅴ族过渡金属元素和第Ⅵ族过渡金属元素中五种以上元素组成的氮化物。
更为优选地，所述第Ⅳ族过渡金属元素为Ti、Zr、Hf；所述第Ⅴ族过渡金属元素为V、Nb、Ta；所述第Ⅵ族过渡金属元素为Cr、Mo、W。
优选地，所述的高熵氮化物粉体的粒径为0.05～2μm，纯度为97％以上；所述Si3N4粉体的粒径为0.1～2μm，纯度为98％以上；所述AlN粉体的粒径为0.1～2μm，纯度为98％以上；所述Al2O3粉体的粒径为0.1～2μm，纯度为98％以上；所述Y2O3粉的粒径为0.1～2μm，纯度为98％以上。
优选地，所述塞隆陶瓷的原料中Y2O3粉体的添加量为1～3wt.％。
优选地，所述的高熵氮化物/塞隆复合陶瓷中高熵氮化物和塞隆陶瓷质量比为(1～4):(6～9)。
优选地，所述筛的孔径为100～200目；所述升温至1700～1850℃的速率为10～50℃/min，所述热压烧结的时间为30～180min；所述保护气氛为氮气或氩气。
优选地，所述高熵氮化物/塞隆复合陶瓷的致密度为95～100％。
所述的高熵氮化物/塞隆复合陶瓷制备方法，包括以下具体步骤：
S1.将高熵氮化物粉体、Si3N4粉体、AlN粉体、Al2O3粉体、Y2O3粉体置于尼龙球磨罐中，加入乙醇和Si3N4球行球磨混料，干燥后获得混合粉体；
S2.将混合粉体装入石墨模具中，在氮气或氩气气氛下，加以30～80MPa轴向压力，以10～50℃/min速率升温至1700～1850℃热压烧结30～180min，制得高熵氮化物/塞隆复合陶瓷。
所述的高熵氮化物/塞隆复合陶瓷在刀具领域中的应用。
本发明的塞隆陶瓷的反应式为：
(2-z/3)Si3N4+(z/3)AlN+(z/3)Al2O3→β-Si6-zAlzOzN8-z；z＝0.5-1.5。
与现有技术相比，本发明具有以下有益效果：
1.本发明的高熵氮化物/塞隆复合陶瓷比传统塞隆陶瓷具有更高的硬度、更高的韧性和更好的耐磨性。
2.本发明的高熵氮化物/塞隆复合陶瓷具有比传统TiN增强塞隆刀具更优的切削性能，可应用在切削刀具领域，用来切削石材、钢铁材料、有色金属、铝合金、高温合金等。
具体实施方式
下面结合实施例对本发明做进一步详细的描述，但本发明的实施方式不限于此。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.10wt％的高熵氮化物粉体(Ti0.2Zr0.2Hf0.2Nb0.2Ta0.2)N(粒径0.5μm)；塞隆陶瓷为β-Si5.1Al0.9O0.9N7.1，通过1.7mol.％Si3N4(粒径0.2μm，纯度99wt.％)、0.3mol.％AlN(粒径为0.5μm，纯度99wt.％)和0.3mol.％Al2O3(粒径300nm，纯度99wt.％)进行原料配比；1wt.％Y2O3(粒径500nm，纯度99wt.％)。将上述混合粉料置于尼龙球磨罐中，加入乙醇和Si3N4球作为球磨介质，球料质量比为4:1，球磨时间为12h，转速为300r/min，球磨旋转蒸发干燥后过100目筛，获得混合粉体；
2.将混合粉体装入石墨模具中，置于N2气氛下，加以50MPa轴向压力，以20℃/min速率升温至1800℃，保温60min，经热压烧结，制得高熵氮化物/塞隆复合陶瓷，其分子式为(Ti0.2Zr0.2Hf0.2Nb0.2Ta0.2)N-β-Si5.1Al0.9O0.9N7.1。该高熵氮化物/塞隆复合陶瓷的致密度为98％，硬度17.5GPa，断裂韧性为6.3MPa·m1/2。
实施例2
1.20wt％的高熵氮化物粉体(Ti0.2Zr0.2Hf0.2Nb0.2Ta0.2)N(粒径0.5μm)；塞隆陶瓷为β-Si5.1Al0.9O0.9N7.1，通过1.7mol.％Si3N4(粒径0.2μm，纯度99wt.％)、0.3mol.％AlN(粒径为0.5μm，纯度99wt.％)和0.3mol.％Al2O3(粒径300nm，纯度99wt.％)进行原料配比；1wt.％Y2O3(粒径500nm，纯度99wt.％)。将上述混合粉料置于尼龙球磨罐中，加入乙醇和Si3N4球作为球磨介质，球料质量比为4:1，球磨时间为12h，转速为300r/min，球磨旋转蒸发干燥后过100目筛，获得混合粉体；
2.将混合粉体装入石墨模具中，置于N2气氛下，加以50MPa轴向压力，以20℃/min速率升温至1800℃，保温60min，经热压烧结，制得高熵氮化物/塞隆复合陶瓷，其分子式为(Ti0.2Zr0.2Hf0.2Nb0.2Ta0.2)N-β-Si5.1Al0.9O0.9N7.1。该高熵氮化物/塞隆复合陶瓷的致密度为99％，硬度18GPa，断裂韧性为6.7MPa·m1/2。
实施例3
1.30wt％的高熵氮化物粉体(Ti0.2Zr0.2Hf0.2Nb0.2Ta0.2)N(粒径0.5μm)；塞隆陶瓷为β-Si5.1Al0.9O0.9N7.1，通过1.7mol.％Si3N4(粒径0.2μm，纯度99wt.％)、0.3mol.％AlN(粒径为0.5μm，纯度99wt.％)和0.3mol.％Al2O3(粒径300nm，纯度99wt.％)进行原料配比；1wt.％Y2O3(粒径500nm，纯度99wt.％)。将上述混合粉料置于尼龙球磨罐中，加入乙醇和Si3N4球作为球磨介质，球料质量比为4:1，球磨时间为12h，转速为300r/min，球磨旋转蒸发干燥后过100目筛，获得混合粉体；
2.将混合粉体装入石墨模具中，置于N2气氛下，加以50MPa轴向压力，以20℃/min速率升温至1800℃，保温60min，经热压烧结，制得高熵氮化物/塞隆复合陶瓷，其分子式为(Ti0.2Zr0.2Hf0.2Nb0.2Ta0.2)N-β-Si5.1Al0.9O0.9N7.1。该高熵氮化物/塞隆复合陶瓷的致密度为99％，硬度20GPa，断裂韧性为7.3MPa·m1/2。
对比例1
1.将1.7mol.％Si3N4(粒径0.2μm，纯度99wt.％)、0.3mol.％AlN(粒径为0.5μm，纯度99wt.％)和0.3mol.％Al2O3(粒径300nm，纯度99wt.％)进行原料配比；1wt.％Y2O3(粒径500nm，纯度99wt.％)。将上述混合粉料置于尼龙球磨罐中，加入乙醇和Si3N4球作为球磨介质，球料质量比为4:1，球磨时间为12h，转速为300r/min，球磨旋转蒸发干燥后过100目筛，获得混合粉体；
2.将混合粉体装入石墨模具中，置于N2气氛下，加以50MPa轴向压力，以20℃/min速率升温至1800℃，保温60min，经热压烧结，制得塞隆陶瓷，其分子式为β-Si5.1Al0.9O0.9N7.1。该塞隆陶瓷的致密度为99％，硬度16GPa，断裂韧性为4.6MPa·m1/2。
对比例2
1.30wt％TiN粉体(粒径0.3μm，纯度99wt.％)；塞隆陶瓷为β-Si5.1Al0.9O0.9N7.1，通过1.7mol.％Si3N4(粒径0.2μm，纯度99wt.％)、0.3mol.％AlN(粒径为0.5μm，纯度99wt.％)和0.3mol.％Al2O3(粒径300nm，纯度99wt.％)进行原料配比；1wt.％Y2O3(粒径500nm，纯度99wt.％)。将上述混合粉料置于尼龙球磨罐中，加入乙醇和Si3N4球作为球磨介质，球料质量比为4:1，球磨时间为12h，转速为300r/min，球磨旋转蒸发干燥后过100目筛，获得混合粉体；
2.将混合粉体装入石墨模具中，置于N2气氛下，加以50MPa轴向压力，以20℃/min速率升温至1800℃，保温60min，经热压烧结，制得TiN/塞隆复合陶瓷，其分子式为TiN-β-Si5.1Al0.9O0.9N7.1。该TiN/塞隆复合陶瓷的致密度为99％，硬度17.3GPa，断裂韧性为6.8MPa·m1/2。
综上可知，本发明的高熵氮化物/塞隆复合陶瓷的致密度为98％以上，硬度17.5～20GPa，断裂韧性为6.3～7.3MPa·m1/2。其硬度和韧性比对比例1的塞隆陶瓷明显提高，对比例2的TiN/塞隆复合陶瓷断裂韧性和硬度均较好，但都不及本发明的高熵氮化物/塞隆复合陶瓷。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (10)
1.一种高熵氮化物/塞隆复合陶瓷，其特征在于，所述复合陶瓷中塞隆陶瓷的分子式为β-Si6-zAlzOzN8-z，z＝0.5～1.5；所述高熵氮化物/塞隆复合陶瓷是将高熵氮化物粉体、Si3N4粉体、AlN粉体、Al2O3粉体和Y2O3粉体加入乙醇和Si3N4球进行球磨混料，干燥后过筛，获得混合粉体；将混合粉体在保护气氛下加以30～80MPa轴向压力，升温至1700～1850℃热压烧结制得。
2.根据权利要求1所述的高熵氮化物/塞隆复合陶瓷，其特征在于，所述的高熵氮化物粉体是由等摩尔比的第Ⅳ族过渡金属元素、第Ⅴ族过渡金属元素和第Ⅵ族过渡金属元素中五种以上元素组成的氮化物。
3.根据权利要求2所述的高熵氮化物/塞隆复合陶瓷，其特征在于，所述第Ⅳ族过渡金属元素为Ti、Zr、Hf；所述第Ⅴ族过渡金属元素为V、Nb、Ta；所述第Ⅵ族过渡金属元素为Cr、Mo、W。
4.根据权利要求1所述的高熵氮化物/塞隆复合陶瓷，其特征在于，所述的高熵氮化物粉体的粒径为0.05～2μm，纯度为97％以上；所述Si3N4粉体的粒径为0.1～2μm，纯度为98％以上；所述AlN粉体的粒径为0.1～2μm，纯度为98％以上；所述Al2O3粉体的粒径为0.1～2μm，纯度为98％以上；所述Y2O3粉的粒径为0.1～2μm，纯度为98％以上。
5.根据权利要求1所述的高熵氮化物/塞隆复合陶瓷，其特征在于，所述塞隆陶瓷的原料中Y2O3粉体的添加量为1～3wt.％。
6.根据权利要求1所述的高熵氮化物/塞隆复合陶瓷，其特征在于，所述的高熵氮化物/塞隆复合陶瓷中高熵氮化物和塞隆陶瓷质量比为(1～4):(6～9)。
7.根据权利要求1所述的高熵氮化物/塞隆复合陶瓷，其特征在于，所述筛的孔径为100～200目；所述升温至1700～1850℃的速率为10～50℃/min，所述热压烧结的时间为30～180min；所述保护气氛为氮气或氩气。
8.根据权利要求1所述的高熵氮化物/塞隆复合陶瓷，其特征在于，所述高熵氮化物/塞隆复合陶瓷的致密度为95～100％。
9.根据权利要求1～8任一项所述的高熵氮化物/塞隆复合陶瓷制备方法，其特征在于，包括以下具体步骤：
S1.将高熵氮化物粉体、Si3N4粉体、AlN粉体、Al2O3粉体、Y2O3粉体置于尼龙球磨罐中，加入乙醇和Si3N4球行球磨混料，干燥后获得混合粉体；
S2.将混合粉体装入石墨模具中，在氮气或氩气气氛下，加以30～80MPa轴向压力，以10～50℃/min速率升温至1700～1850℃热压烧结30～180min，制得高熵氮化物/塞隆复合陶瓷。
10.权利要求1～8任一项所述的高熵氮化物/塞隆复合陶瓷在刀具领域中的应用。
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4547470A (en) * | 1983-04-25 | 1985-10-15 | Mitsubishi Kinzoku Kabushiki Kaisha | Sialon-base ceramic materials excellent in wear resistance |
| JPS63201063A (ja) * | 1987-02-12 | 1988-08-19 | 日立金属株式会社 | セラミツクヒ−タ及びその製造方法 |
| JPH0450167A (ja) * | 1990-06-15 | 1992-02-19 | Toshiba Corp | 分散強化型複合セラミックス及び分散強化型複合セラミックス製造用複合粒子の製造方法 |
| JP2003267787A (ja) * | 2002-03-12 | 2003-09-25 | Toshiba Tungaloy Co Ltd | β´−サイアロン基セラミックス工具およびその製造方法 |
| US20130298474A1 (en) * | 2010-12-22 | 2013-11-14 | Sandvik Intellectual Property Ab | Cutting tool made of sialon based material |
| CN111423236A (zh) * | 2020-03-22 | 2020-07-17 | 华南理工大学 | 一种（Hf0.25Ti0.25Zr0.25W0.25）N高熵陶瓷粉体及其制备方法 |
| CN113402279A (zh) * | 2021-03-29 | 2021-09-17 | 广东工业大学 | 一种长棒状β-SiAlON增韧的高熵碳化物陶瓷及其制备方法和应用 |
| CN113943162A (zh) * | 2021-10-20 | 2022-01-18 | 西北工业大学 | 一种α-SiAlON高熵透明陶瓷材料及其制备方法 |
| CN115340387A (zh) * | 2022-09-06 | 2022-11-15 | 中国有色桂林矿产地质研究院有限公司 | 一种含高熵陶瓷相的氮化硼超硬材料及其制备方法和应用 |
-
2022
- 2022-12-28 CN CN202211695379.3A patent/CN116041071B/zh active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4547470A (en) * | 1983-04-25 | 1985-10-15 | Mitsubishi Kinzoku Kabushiki Kaisha | Sialon-base ceramic materials excellent in wear resistance |
| JPS63201063A (ja) * | 1987-02-12 | 1988-08-19 | 日立金属株式会社 | セラミツクヒ−タ及びその製造方法 |
| JPH0450167A (ja) * | 1990-06-15 | 1992-02-19 | Toshiba Corp | 分散強化型複合セラミックス及び分散強化型複合セラミックス製造用複合粒子の製造方法 |
| JP2003267787A (ja) * | 2002-03-12 | 2003-09-25 | Toshiba Tungaloy Co Ltd | β´−サイアロン基セラミックス工具およびその製造方法 |
| US20130298474A1 (en) * | 2010-12-22 | 2013-11-14 | Sandvik Intellectual Property Ab | Cutting tool made of sialon based material |
| CN111423236A (zh) * | 2020-03-22 | 2020-07-17 | 华南理工大学 | 一种（Hf0.25Ti0.25Zr0.25W0.25）N高熵陶瓷粉体及其制备方法 |
| CN113402279A (zh) * | 2021-03-29 | 2021-09-17 | 广东工业大学 | 一种长棒状β-SiAlON增韧的高熵碳化物陶瓷及其制备方法和应用 |
| CN113943162A (zh) * | 2021-10-20 | 2022-01-18 | 西北工业大学 | 一种α-SiAlON高熵透明陶瓷材料及其制备方法 |
| CN115340387A (zh) * | 2022-09-06 | 2022-11-15 | 中国有色桂林矿产地质研究院有限公司 | 一种含高熵陶瓷相的氮化硼超硬材料及其制备方法和应用 |
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