CN105503198B - 氮化硅材料及其制备方法 - Google Patents
氮化硅材料及其制备方法 Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 85
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 26
- 239000002002 slurry Substances 0.000 claims abstract description 26
- -1 aluminium silicon lithium magnesium Chemical compound 0.000 claims abstract description 24
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 24
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 235000013312 flour Nutrition 0.000 claims abstract description 20
- 239000011812 mixed powder Substances 0.000 claims abstract description 20
- 239000012298 atmosphere Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- WPKYZIPODULRBM-UHFFFAOYSA-N azane;prop-2-enoic acid Chemical compound N.OC(=O)C=C WPKYZIPODULRBM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000000462 isostatic pressing Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 239000003595 mist Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000012010 growth Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 241001070941 Castanea Species 0.000 description 2
- 235000014036 Castanea Nutrition 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005255 carburizing Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007773 growth pattern Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000000626 liquid-phase infiltration Methods 0.000 description 1
- 238000005058 metal casting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
本发明公开了一种氮化硅材料及其制备方法，包括将硅粉、石墨粉、钇铝硅锂镁化合物和氮化硅粉混合，得到混合粉末；然后向所述混合粉末中加入聚乙烯醇水溶液、丙烯酸铵水溶液和水，配成料浆；将所述料浆球磨后造粒，然后成型为坯体；将所述坯体干燥后放入微波气氛烧结炉进行烧结，烧结后得到所述氮化硅材料。通过本发明制备得到的氮化硅材料属于高纯，由于材料中更是包含了优质的氮化硅晶须，所以可以达到比氮化硅理想性能还要优越的性能，应用效果和应用领域得到了质的提升。
Description
技术领域
本发明涉及氮化硅材料技术领域，特别是涉及一种氮化硅晶须增强型高纯氮化硅材料及其制备方法。
背景技术
随着社会的发展，科技的进步，氮化硅材料在大众生活、工业生产中越来越受到重视和广泛的应用，如快速热水器中的加热片、金属铸造中的升液管、保护管等产品，采用氮化硅材料制备均体现出了极大的优势。但是现有技术生产的氮化硅材料基本含量在90％左右，因其添加的其它改性或助烧材料本身的性能有限，导致材料的综合性能未能达到氮化硅材料的理想水平。
发明内容
有鉴于此，本发明的目的在于提出一种氮化硅材料及其制备方法，以提高氮化硅材料的综合性能。
本发明提供的氮化硅材料的制备方法包括以下步骤：
将硅粉、石墨粉、钇铝硅锂镁化合物和氮化硅粉混合，得到混合粉末；
然后向所述混合粉末中加入聚乙烯醇水溶液、丙烯酸铵水溶液和水，配成料浆；
将所述料浆球磨后造粒，然后成型为坯体；
将所述坯体干燥后放入微波气氛烧结炉进行烧结，烧结后得到所述氮化硅材料。
在本发明的一些实施例中，在所述混合粉末中，所述硅粉、石墨粉、钇铝硅锂镁化合物和氮化硅粉所占质量百分数分别为1～3％、1～3％、2～4％以及90～96％。
在本发明的一些实施例中，在所述料浆中，所述硅粉、石墨粉、钇铝硅锂镁化合物、氮化硅粉的总质量占料浆的45～60％。
在本发明的一些实施例中，采用干压或等静压成型方法，80～300MPa压力下成型得到坯体。
在本发明的一些实施例中，所述将所述坯体干燥后放入微波气氛烧结炉进行烧结的步骤包括：
先通氩气保护，升温至1300～1400℃，保温1～5h；
然后将气氛置换为氮气保护，继续升温至1600～1700℃，保温1～5h。
在本发明的一些实施例中，所述微波气氛烧结炉的升温速度为1～5℃/min。
在本发明的一些实施例中，所述钇铝硅锂镁化合物的制备方法包括以下步骤：
将Li2O、Al2O3、Y2O3、MgO和SiO2粉末混合，然后压成圆片；
将所述圆片升温加热至750～850℃，保温2～4h；
再继续升温加热至950～1150℃，保温2～4h，即得到3LiYO2·2LiAlSiO4·(0.1～0.5)MgO的复合化合物。
在本发明的一些实施例中，所述圆片的厚度为2～6mm，所述圆片的升温速度为2～10℃/min。
在本发明的一些实施例中，所述聚乙烯醇水溶液的质量浓度为1～2％，所述丙烯酸铵水溶液的质量浓度为0.8～1.2％。
本发明还提供一种氮化硅材料，所述氮化硅材料根据上述氮化硅材料的制备方法制备得到。
从上面的所述可以看出，本发明提供的氮化硅材料的制备方法采用原位合成烧结方法，该方法是建立在硅粉先碳化、后氮化的双还原机制与微波加热机制配合的基础上，坯体在氩气气氛下微波加热至1300～1400℃时，硅与石墨剧烈吸收微波，发生碳化反应，生成碳化硅，这个时候生成的碳化硅吸收微波能力很强，但氮化硅基础材料在这个温度段吸收微波能力较差且已经产生了较高的强度但没有发生收缩，所以这个时段的碳化硅就像是火栗一样夹杂在氮化硅坯体材料之中，不是很稳定，反应活性较高；当替换成氮气气氛后，加热至1600～1700℃时，不稳定的碳化硅在催化剂(钇铝硅锂镁化合物)的作用下快速反应生成了优质的氮化硅晶须，其反应的机理是液相生长原理，且在微波环境下，其晶须生成方式进化为显著的液相螺旋生长方式，在1600～1700℃温度下，原氮化硅配方材料与原位合成的优质氮化硅晶须结合，保温1～5h，最终得出高纯的性能优良的氮化硅产品。
附图说明
图1为采用本发明实施例的制备方法制备得到的氮化硅材料的X射线衍射图谱；
图2为采用本发明实施例的制备方法制备得到的氮化硅材料的断面SEM照片。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明白，以下结合具体实施例，并参照附图，对本发明进一步详细说明。
实施例1
在本发明的一个实施例中，本发明提供的氮化硅材料的制备方法包括以下步骤：
1)将Li2O、Al2O3、Y2O3、MgO和SiO2粉末均匀混合，然后压成5mm厚的圆片；在空气中以5℃/min的升温速度将圆片加热至800℃，保温3.5h；然后再以8℃/min的升温速度继续加热至1100℃，保温3h，即得到3LiYO2·2LiAlSiO4·0.2MgO的复合化合物。
2)将硅粉(纯度>99.99％)、石墨粉(纯度>99.9％)、通过步骤1)制得的钇铝硅锂镁化合物和氮化硅粉(α相>93％)混合均匀，得到混合粉末。进一步地，在所述混合粉末中，所述硅粉、石墨粉、钇铝硅锂镁化合物和氮化硅粉所占质量百分数分别为2.2％、2.5％、3％和92.3％。
3)向所述混合粉末中加入质量浓度为1.5％的聚乙烯醇水溶液、质量浓度为1.0％的丙烯酸铵水溶液和蒸馏水，配成50wt％的料浆。需要说明的是，所述50wt％的料浆是指所述硅粉、石墨粉、钇铝硅锂镁化合物、氮化硅粉的总质量占料浆的50％。
4)将所述料浆球磨20h后喷雾造粒，用干压成型方法，120～150MPa压力下成型为坯体。
5)将所述坯体干燥后放入微波气氛烧结炉进行烧结，先通氩气(纯度>99.99％)保护，以3℃/min的升温速度升至1350℃，保温4h，然后将气氛置换为氮气(纯度>99.99％)保护，以4/min的升温速度升至1650℃，保温3h，即得到氮化硅材料。
实施例2
在本发明的另一个实施例中，本发明提供的氮化硅材料的制备方法包括以下步骤：
1)将Li2O、Al2O3、Y2O3、MgO和SiO2粉末均匀混合，然后压成4.5mm厚的圆片；在空气中以3.5℃/min的升温速度将圆片加热至830℃，保温2h；然后再以6.5℃/min的升温速度继续加热至970℃，保温4h，即得到3LiYO2·2LiAlSiO4·0.3MgO的复合化合物。
2)将硅粉(纯度>99.99％)、石墨粉(纯度>99.9％)、通过步骤1)制得的钇铝硅锂镁化合物和氮化硅粉(α相>93％)混合均匀，得到混合粉末。进一步地，在所述混合粉末中，所述硅粉、石墨粉、钇铝硅锂镁化合物和氮化硅粉所占质量百分数分别为3％、1.5％、2.6％和92.9％。
3)向所述混合粉末中加入质量浓度为1.2％的聚乙烯醇水溶液、质量浓度为1.2％的丙烯酸铵水溶液和蒸馏水，配成56wt％的料浆。需要说明的是，所述56wt％的料浆是指所述硅粉、石墨粉、钇铝硅锂镁化合物、氮化硅粉的总质量占料浆的56％。
4)将所述料浆球磨18h后喷雾造粒，用等静压成型方法，250～300MPa压力下成型为坯体。
5)将所述坯体干燥后放入微波气氛烧结炉进行烧结，先通氩气(纯度>99.99％)保护，以5℃/min的升温速度升至1380℃，保温3.5h，然后将气氛置换为氮气(纯度>99.99％)保护，以3/min的升温速度升至1620℃，保温4h，即得到氮化硅材料。
实施例3
在本发明的又一个实施例中，本发明提供的氮化硅材料的制备方法包括以下步骤：
1)将Li2O、Al2O3、Y2O3、MgO和SiO2粉末均匀混合，然后压成3mm厚的圆片；在空气中以10℃/min的升温速度将圆片加热至840℃，保温3.5h；然后再以3℃/min的升温速度继续加热至960℃，保温4h，即得到3LiYO2·2LiAlSiO4·0.5MgO的复合化合物。
2)将硅粉(纯度>99.99％)、石墨粉(纯度>99.9％)、通过步骤1)制得的钇铝硅锂镁化合物和氮化硅粉(α相>93％)混合均匀，得到混合粉末。进一步地，在所述混合粉末中，所述硅粉、石墨粉、钇铝硅锂镁化合物和氮化硅粉所占质量百分数分别为1.4％、2.6％、4％和92％。
3)向所述混合粉末中加入质量浓度为2.0％的聚乙烯醇水溶液、质量浓度为0.8％的丙烯酸铵水溶液和蒸馏水，配成48wt％的料浆。需要说明的是，所述48wt％的料浆是指所述硅粉、石墨粉、钇铝硅锂镁化合物、氮化硅粉的总质量占料浆的48％。
4)将所述料浆球磨15h后喷雾造粒，用干压成型方法，250～280MPa压力下成型为坯体。
5)将所述坯体干燥后放入微波气氛烧结炉进行烧结，先通氩气(纯度>99.99％)保护，以1.5℃/min的升温速度升至1400℃，保温4h，然后将气氛置换为氮气(纯度>99.99％)保护，以3/min的升温速度升至1690℃，保温2h，即得到氮化硅材料。
实施例4
在本发明的另一个实施例中，本发明提供的氮化硅材料的制备方法包括以下步骤：
1)将Li2O、Al2O3、Y2O3、MgO和SiO2粉末均匀混合，然后压成2mm厚的圆片；在空气中以5℃/min的升温速度将圆片加热至755℃，保温4h；然后再以10℃/min的升温速度继续加热至1050℃，保温2h，即得到3LiYO2·2LiAlSiO4·0.4MgO的复合化合物。
2)将硅粉(纯度>99.99％)、石墨粉(纯度>99.9％)、通过步骤1)制得的钇铝硅锂镁化合物和氮化硅粉(α相>93％)混合均匀，得到混合粉末。进一步地，在所述混合粉末中，所述硅粉、石墨粉、钇铝硅锂镁化合物和氮化硅粉所占质量百分数分别为2％、2.5％、4％和91.5％。
3)向所述混合粉末中加入质量浓度为1％的聚乙烯醇水溶液、质量浓度为1.1％的丙烯酸铵水溶液和蒸馏水，配成52wt％的料浆。需要说明的是，所述52wt％的料浆是指所述硅粉、石墨粉、钇铝硅锂镁化合物、氮化硅粉的总质量占料浆的52％。
4)将所述料浆球磨10h后喷雾造粒，用等静压成型方法，190～210MPa压力下成型为坯体。
5)将所述坯体干燥后放入微波气氛烧结炉进行烧结，先通氩气(纯度>99.99％)保护，以1℃/min的升温速度升至1330℃，保温4.5h，然后将气氛置换为氮气(纯度>99.99％)保护，以3.5/min的升温速度升至1610℃，保温5h，即得到氮化硅材料。
参见图1，为采用本发明实施例的制备方法制备得到的氮化硅材料的X射线衍射图谱，从图中可以看出，采用本发明提供的方法制备得到的氮化硅材料纯度极高(纯度>99％)。将该氮化硅材料在六合集团铝液池中应用80天后测试材料成分，仍然保持高纯及高性能。
由此可见，本发明提供的氮化硅材料的制备方法以钇铝硅锂镁化合物作为原料，其作用是：1、大幅降低氮化硅材料的烧结温度，提高液相浸润的质量，增加氮化硅材料的致密度；2、烧结过程中，随着高温保温时间的延长，该化合物逐渐析出晶界，排出材料之外，不对材料体纯度产生影响；3、在原位合成氮化硅晶须的反应中充当了重要的催化剂角色，加速了氮化硅晶须的生成。图2为采用本发明实施例的制备方法制备得到的氮化硅材料的断面SEM照片，从图中可以看出氮化硅晶须增强作用明显。
本发明提供的氮化硅材料的制备方法采用原位合成烧结方法，该方法是建立在硅粉先碳化、后氮化的双还原机制与微波加热机制配合的基础上，坯体在氩气气氛下微波加热至1300～1400℃时，硅与石墨剧烈吸收微波，发生碳化反应，生成碳化硅，这个时候生成的碳化硅吸收微波能力很强，但氮化硅基础材料在这个温度段吸收微波能力较差且已经产生了较高的强度但没有发生收缩，所以这个时段的碳化硅就像是火栗一样夹杂在氮化硅坯体材料之中，不是很稳定，反应活性较高；当替换成氮气气氛后，加热至1600～1700℃时，不稳定的碳化硅在催化剂(钇铝硅锂镁化合物)的作用下快速反应生成了优质的氮化硅晶须，其反应的机理是液相生长原理，且在微波环境下，其晶须生成方式进化为显著的液相螺旋生长方式，在1600～1700℃温度下，原氮化硅配方材料与原位合成的优质氮化硅晶须结合，保温1～5h，最终得出高纯的性能优良的氮化硅产品。
与现有技术相比，通过本发明制备得到的氮化硅材料属于高纯(纯度>99％)，远远高于现有技术。由于材料中更是包含了优质的氮化硅晶须，所以可以达到比氮化硅理想性能还要优越的性能，应用效果和应用领域得到了质的提升。本发明的氮化硅材料致密度>99％，抗弯强度>900MPa，材料断裂韧性>8.5MPam2，材料试样(Ф10×50mm)进行1200℃—>冷水的实验可达30以上不破裂，性能指标远远高于现有技术生产的氮化硅材料。
所属领域的普通技术人员应当理解：以上任何实施例的讨论仅为示例性的，并非旨在暗示本公开的范围(包括权利要求)被限于这些例子；在本发明的思路下，以上实施例或者不同实施例中的技术特征之间也可以进行组合，步骤可以以任意顺序实现，并存在如上所述的本发明的不同方面的许多其它变化，为了简明它们没有在细节中提供。因此，凡在本发明的精神和原则之内，所做的任何省略、修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (4)
1.一种氮化硅材料的制备方法，其特征在于，包括以下步骤：
将硅粉、石墨粉、钇铝硅锂镁化合物和氮化硅粉混合，得到混合粉末；在所述混合粉末中，所述硅粉、石墨粉、钇铝硅锂镁化合物和氮化硅粉所占质量百分数分别为1～3％、1～3％、2～4％以及90～96％；
然后向所述混合粉末中加入聚乙烯醇水溶液、丙烯酸铵水溶液和水，配成料浆；在所述料浆中，所述硅粉、石墨粉、钇铝硅锂镁化合物、氮化硅粉的总质量占料浆的45～60％；
将所述料浆球磨后造粒，然后采用干压或等静压成型方法，80～300MPa压力下成型得到坯体；
将所述坯体干燥后放入微波气氛烧结炉进行烧结，所述微波气氛烧结炉的升温速度为1～5℃/min，先通氩气保护，升温至1300～1400℃，保温1～5h，然后将气氛置换为氮气保护，继续升温至1600～1700℃，保温1～5h，烧结后得到所述氮化硅材料；
其中，所述钇铝硅锂镁化合物的制备方法包括以下步骤：
将Li2O、Al2O3、Y2O3、MgO和SiO2粉末混合，然后压成圆片；
将所述圆片升温加热至750～850℃，保温2～4h；
再继续升温加热至950～1150℃，保温2～4h，即得到3LiYO2·2LiAlSiO4·(0.1～0.5)MgO的复合化合物。
2.根据权利要求1所述的氮化硅材料的制备方法，其特征在于，所述圆片的厚度为2～6mm，所述圆片的升温速度为2～10℃/min。
3.根据权利要求1所述的氮化硅材料的制备方法，其特征在于，所述聚乙烯醇水溶液的质量浓度为1～2％，所述丙烯酸铵水溶液的质量浓度为0.8～1.2％。
4.一种氮化硅材料，其特征在于，所述氮化硅材料根据权利要求1～3中任意一项所述的氮化硅材料的制备方法制备得到。
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