CN116041071B - 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 59
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 43
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- 239000011812 mixed powder Substances 0.000 claims abstract description 24
- 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 6
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 27
- 229910052723 transition metal Inorganic materials 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- 239000004677 Nylon Substances 0.000 claims description 7
- 229920001778 nylon Polymers 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 6
- 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
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 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
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
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- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 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 (8)
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；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；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)。
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。
3.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。
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，所述塞隆陶瓷的原料中Y2O3粉体的添加量为1～3wt.％。
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。
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，所述高熵氮化物/塞隆复合陶瓷的致密度为95～100％。
7.根据权利要求1～6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。
8.权利要求1～6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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