CN116332653B - 一种高性能氮化铝陶瓷材料及其制备方法 - Google Patents
一种高性能氮化铝陶瓷材料及其制备方法 Download PDFInfo
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 45
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 54
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 28
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 17
- 229910010093 LiAlO Inorganic materials 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- 229910001593 boehmite Inorganic materials 0.000 claims description 15
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 15
- 238000005121 nitriding Methods 0.000 claims description 15
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 15
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 7
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 4
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 239000001263 FEMA 3042 Substances 0.000 claims description 2
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 229940105329 carboxymethylcellulose Drugs 0.000 claims description 2
- 239000008098 formaldehyde solution Substances 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 2
- 235000015523 tannic acid Nutrition 0.000 claims description 2
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 2
- 229940033123 tannic acid Drugs 0.000 claims description 2
- 229920002258 tannic acid Polymers 0.000 claims description 2
- 229920006029 tetra-polymer Polymers 0.000 claims description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims 1
- 238000000748 compression moulding Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 description 7
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000004873 anchoring Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910002706 AlOOH Inorganic materials 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- -1 acrylic ester Chemical class 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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Abstract
本发明涉及陶瓷材料领域,具体为一种高性能氮化铝陶瓷材料及其制备方法,由以下重量份原料制备而成:氮化铝纳米粉80‑100份、烧结助剂6‑12份、增塑剂1‑2份、粘结剂5‑10份、分散剂0.5‑1份,本发明所制备的氮化铝陶瓷材料具有极佳的力学性能和导热性能,综合性能优良,应用前景广泛。
Description
技术领域
本发明涉及陶瓷材料领域,具体为一种高性能氮化铝陶瓷材料及其制备方法。
背景技术
氮化铝陶瓷具有高的热导率,较低的介电常数和介电损耗,与硅、砷化镓等一些半导体相匹配的热膨胀系数,被认为是新一代高性能陶瓷基板、电子封装等散热器件的首选材料。
氮化铝陶瓷是由氮化铝粉体烧结而成的,高纯度氮化铝粉末是制备高性能氮化铝陶瓷的必要前提,影响氮化铝陶瓷性能的主要因素有氮化铝粉体的性能、粉体改性方式、粉末烧结工艺等,其中,氮化铝粉末的性能是决定氮化铝陶瓷制备工艺和质量的关键,由于氮化铝粉末易在空气中发生水解,氧杂质在烧结过程中扩散进入氮化铝晶格,造成氮化铝陶瓷导热性能的降低。
发明内容
发明目的:针对上述技术问题,本发明提出了一种高性能氮化铝陶瓷材料及其制备方法。
所采用的技术方案如下:
一种高性能氮化铝陶瓷材料,由以下重量份原料制备而成:
氮化铝纳米粉80-100份、烧结助剂6-12份、增塑剂1-2份、粘结剂5-10份、分散剂0.5-1份。
进一步地,所述氮化铝纳米粉的制备方法如下:
将苯酚加热融化后,加入氢氧化钠溶液,搅拌均匀,再加入甲醛溶液,升温至65-75℃,搅拌反应20-40min后加入勃姆石溶胶,继续搅拌反应20-40min,冷却至室温,用稀盐酸将反应体系的pH调节至7-8,静置24-48h得到凝胶,真空干燥至恒重后进行高温氮化处理,最后与超分散剂混合球磨、干燥即可。
进一步地,所述勃姆石溶胶的制备方法如下:
将异丙醇铝、水混合升温至60-80℃搅拌1-2h,再加入硝酸,升温至回流反应2-4h,冷却至室温静置24-48h即可。
进一步地,高温氮化处理具体操作如下:
将真空干燥至恒重后的凝胶研磨成粉,一段升温至1000-1050℃,保温反应2-4h,再通入氮气,在氮气氛围下二段升温至1500-1580℃,保温反应10-15h,再降温至550-600℃,保温反应2-4h后,恢复室温即可。
进一步地,所述超分散剂为磺酸盐、丙烯酸、丙烯酸酯和磷酸组成的四元共聚物。
进一步地,所述烧结助剂包括LiAlO2、Y2O3和La2O3,所述LiAlO2、Y2O3和La2O3的质量比为3-6:1:1。
进一步地,所述增塑剂为邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二丁酯或邻苯二甲酸二乙酯中的至少一种。
进一步地,所述粘结剂为聚乙烯醇水溶液。
进一步地,所述分散剂为焦磷酸钠、聚丙烯酸钠、六偏磷酸钠、羧甲基纤维素、鞣酸中的至少一种。
本发明还提供了一种高性能氮化铝陶瓷材料的制备方法:
氮气保护下,氮化铝纳米粉、烧结助剂、增塑剂、分散剂混合球磨后干燥,加入粘结剂造粒,所得粒料放入模具中进行压制成型,得到粗坯,粗坯升温至500-600℃保温1-3h,通入氮气置换空气,再升温至1680-1950℃烧结2-4h,随炉冷却至室温即可。
本发明的有益效果:
本发明提供了一种高性能氮化铝陶瓷材料,通过溶胶凝胶-高分子聚合过程,制备出碳源和铝源混合均匀的前驱体,高温煅烧后AlOOH原位转化的Al2O3颗粒均匀分散在树脂原位碳化形成的碳基体中,该体系一方面抑制了先驱体勃姆石和氧化铝粒子的长大,另一方面阻碍了氧化铝的相转变,使得氮化反应直接由γ-Al2O3开始,并在高温氮化处理时完全反应为纳米尺寸的氮化铝,超分散剂中的锚固基团能通过离子键、共价键、氢键及范德华力等相互作用以单点或多点锚固的形式牢固吸附于氮化铝纳米粉表面,可以有效阻碍水分子或氧分子对氮化铝粉体的表面侵蚀,避免造成缺陷,LiAlO2、Y2O3和La2O3组成的烧结助剂与与氮化铝粉末表面的氧化铝反应,形成低熔物,产生液相,利用液相传质促进烧结,提高材料的致密度,还能与氧杂质反应,降低氮化铝晶格的氧含量,起到纯化晶格的作用,相比于单一烧结助剂,更能有效提高致密度和热导率,本发明所制备的氮化铝陶瓷材料具有极佳的力学性能和导热性能,综合性能优良,应用前景广泛。
附图说明
图1为本发明实施例1所制备氮化铝陶瓷材料的微观形貌图。
具体实施方式
实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。本发明未提及的技术均参照现有技术。
实施例1:
一种高性能氮化铝陶瓷材料,由以下重量份原料制备而成:
氮化铝纳米粉95份、LiAlO25份、Y2O31份、La2O31份、邻苯二甲酸二丁酯1.5份、5wt%聚乙烯醇水溶液8份、聚丙烯酸钠1份。
其中,氮化铝纳米粉的制备方法如下:
将408g异丙醇铝、3600mL水混合升温至75℃搅拌2h,再加入12mL硝酸,升温至回流反应2h,冷却至室温静置36h得到勃姆石溶胶,将188g苯酚加热至融化后,加入40mL 20wt%氢氧化钠水溶液,搅拌20min,再加入31mL 37%甲醛水溶液,升温至70℃,搅拌反应30min后将制备得到的勃姆石溶胶加入,继续搅拌反应30min,冷却至室温,用稀盐酸将反应体系的pH调节至7-8,静置48h得到凝胶,将其置于烘箱中50℃真空干燥至恒重后进行高温氮化处理,高温氮化处理前将凝胶研磨成粉,于马弗炉中一段升温至1050℃,保温反应3h,再通入氮气,在氮气氛围下二段升温至1580℃,保温反应12h,再降温至5800℃,保温反应4h后,恢复室温,与超分散剂HC323(磺酸盐、丙烯酸、丙烯酸酯和磷酸组成的四元共聚物)混合球磨2h后干燥即可。
上述高性能氮化铝陶瓷材料的制备方法:
氮气保护下,氮化铝纳米粉、LiAlO2、Y2O3、La2O3、邻苯二甲酸二丁酯、聚丙烯酸钠混合球磨后干燥,加入5wt%聚乙烯醇水溶液造粒,所得粒料放入模具中35MPa下压制成型,得到粗坯,粗坯升温至600℃保温2h,通入氮气置换空气,再升温至1900℃烧结3h,随炉冷却至室温即可。
实施例2:
一种高性能氮化铝陶瓷材料,由以下重量份原料制备而成:
氮化铝纳米粉100份、LiAlO25份、Y2O31份、La2O31份、邻苯二甲酸二丁酯2份、5wt%聚乙烯醇水溶液10份、聚丙烯酸钠1份。
其中,氮化铝纳米粉的制备方法如下:
将408g异丙醇铝、3600mL水混合升温至80℃搅拌2h,再加入12mL硝酸,升温至回流反应4h,冷却至室温静置48h得到勃姆石溶胶,将188g苯酚加热至融化后,加入40mL 20wt%氢氧化钠水溶液,搅拌20min,再加入31mL 37%甲醛水溶液,升温至75℃,搅拌反应40min后将制备得到的勃姆石溶胶加入,继续搅拌反应40min,冷却至室温,用稀盐酸将反应体系的pH调节至7-8,静置48h得到凝胶,将其置于烘箱中50℃真空干燥至恒重后进行高温氮化处理,高温氮化处理前将凝胶研磨成粉,于马弗炉中一段升温至1050℃,保温反应4h,再通入氮气,在氮气氛围下二段升温至1580℃,保温反应15h,再降温至600℃,保温反应4h后,恢复室温,与超分散剂HC323(磺酸盐、丙烯酸、丙烯酸酯和磷酸组成的四元共聚物)混合球磨2h后干燥即可。
上述高性能氮化铝陶瓷材料的制备方法:
氮气保护下,氮化铝纳米粉、LiAlO2、Y2O3、La2O3、邻苯二甲酸二丁酯、聚丙烯酸钠混合球磨后干燥,加入5wt%聚乙烯醇水溶液造粒,所得粒料放入模具中35MPa下压制成型,得到粗坯,粗坯升温至600℃保温3h,通入氮气置换空气,再升温至1950℃烧结4h,随炉冷却至室温即可。
实施例3:
一种高性能氮化铝陶瓷材料,由以下重量份原料制备而成:
氮化铝纳米粉80份、LiAlO25份、Y2O31份、La2O31份、邻苯二甲酸二丁酯1份、5wt%聚乙烯醇水溶液5份、聚丙烯酸钠0.5份。
其中,氮化铝纳米粉的制备方法如下:
将408g异丙醇铝、3600mL水混合升温至60℃搅拌1h,再加入12mL硝酸,升温至回流反应2h,冷却至室温静置24h得到勃姆石溶胶,将188g苯酚加热至融化后,加入40mL 20wt%氢氧化钠水溶液,搅拌20min,再加入31mL 37%甲醛水溶液,升温至65℃,搅拌反应20min后将制备得到的勃姆石溶胶加入,继续搅拌反应20min,冷却至室温,用稀盐酸将反应体系的pH调节至7-8,静置24h得到凝胶,将其置于烘箱中50℃真空干燥至恒重后进行高温氮化处理,高温氮化处理前将凝胶研磨成粉,于马弗炉中一段升温至1000℃,保温反应2h,再通入氮气,在氮气氛围下二段升温至1500℃,保温反应10h,再降温至550℃,保温反应2h后,恢复室温,与超分散剂HC323(磺酸盐、丙烯酸、丙烯酸酯和磷酸组成的四元共聚物)混合球磨2h后干燥即可。
上述高性能氮化铝陶瓷材料的制备方法:
氮气保护下,氮化铝纳米粉、LiAlO2、Y2O3、La2O3、邻苯二甲酸二丁酯、聚丙烯酸钠混合球磨后干燥,加入5wt%聚乙烯醇水溶液造粒,所得粒料放入模具中35MPa下压制成型,得到粗坯,粗坯升温至500℃保温1h,通入氮气置换空气,再升温至1680℃烧结2h,随炉冷却至室温即可。
实施例4:
一种高性能氮化铝陶瓷材料,由以下重量份原料制备而成:
氮化铝纳米粉100份、LiAlO25份、Y2O31份、La2O31份、邻苯二甲酸二丁酯1份、5wt%聚乙烯醇水溶液10份、聚丙烯酸钠0.5份。
其中,氮化铝纳米粉的制备方法如下:
将408g异丙醇铝、3600mL水混合升温至80℃搅拌1h,再加入12mL硝酸,升温至回流反应4h,冷却至室温静置24h得到勃姆石溶胶,将188g苯酚加热至融化后,加入40mL 20wt%氢氧化钠水溶液,搅拌20min,再加入31mL 37%甲醛水溶液,升温至75℃,搅拌反应20min后将制备得到的勃姆石溶胶加入,继续搅拌反应40min,冷却至室温,用稀盐酸将反应体系的pH调节至7-8,静置24h得到凝胶,将其置于烘箱中50℃真空干燥至恒重后进行高温氮化处理,高温氮化处理前将凝胶研磨成粉,于马弗炉中一段升温至1050℃,保温反应2h,再通入氮气,在氮气氛围下二段升温至1580℃,保温反应10h,再降温至600℃,保温反应2h后,恢复室温,与超分散剂HC323(磺酸盐、丙烯酸、丙烯酸酯和磷酸组成的四元共聚物)混合球磨2h后干燥即可。
上述高性能氮化铝陶瓷材料的制备方法:
氮气保护下,氮化铝纳米粉、LiAlO2、Y2O3、La2O3、邻苯二甲酸二丁酯、聚丙烯酸钠混合球磨后干燥,加入5wt%聚乙烯醇水溶液造粒,所得粒料放入模具中35MPa下压制成型,得到粗坯,粗坯升温至600℃保温1h,通入氮气置换空气,再升温至1950℃烧结2h,随炉冷却至室温即可。
实施例5:
一种高性能氮化铝陶瓷材料,由以下重量份原料制备而成:
氮化铝纳米粉80份、LiAlO25份、Y2O31份、La2O31份、邻苯二甲酸二丁酯2份、5wt%聚乙烯醇水溶液5份、聚丙烯酸钠1份。
其中,氮化铝纳米粉的制备方法如下:
将408g异丙醇铝、3600mL水混合升温至60℃搅拌2h,再加入12mL硝酸,升温至回流反应2h,冷却至室温静置48h得到勃姆石溶胶,将188g苯酚加热至融化后,加入40mL 20wt%氢氧化钠水溶液,搅拌20min,再加入31mL 37%甲醛水溶液,升温至65℃,搅拌反应40min后将制备得到的勃姆石溶胶加入,继续搅拌反应20min,冷却至室温,用稀盐酸将反应体系的pH调节至7-8,静置48h得到凝胶,将其置于烘箱中50℃真空干燥至恒重后进行高温氮化处理,高温氮化处理前将凝胶研磨成粉,于马弗炉中一段升温至1000℃,保温反应4h,再通入氮气,在氮气氛围下二段升温至1500℃,保温反应15h,再降温至550℃,保温反应4h后,恢复室温,与超分散剂HC323(磺酸盐、丙烯酸、丙烯酸酯和磷酸组成的四元共聚物)混合球磨2h后干燥即可。
上述高性能氮化铝陶瓷材料的制备方法:
氮气保护下,氮化铝纳米粉、LiAlO2、Y2O3、La2O3、邻苯二甲酸二丁酯、聚丙烯酸钠混合球磨后干燥,加入5wt%聚乙烯醇水溶液造粒,所得粒料放入模具中35MPa下压制成型,得到粗坯,粗坯升温至500℃保温3h,通入氮气置换空气,再升温至1680℃烧结4h,随炉冷却至室温即可。
对比例1:
与实施例1基本相同,区别在于,用市售氮化铝纳米粉(清河县安迪金属材料有限公司)代替本发明中氮化铝纳米粉。
对比例2:
与实施例1基本相同,区别在于,不加入烧结助剂。
对比例3:
与实施例1基本相同,区别在于,烧结助剂中不含LiAlO2。
对比例4:
与实施例1基本相同,区别在于,不经过超分散剂HC323球磨处理。
性能测试:
以本发明实施例1-5及对比例1-4中所制备氮化铝陶瓷材料作为试样;
利用电子式万能试验机对试样进行弯曲强度测试;
采用布氏硬度计对试样的硬度进行测试;
采用激光热导仪对试样的热导率进行测试;
测试结果如下表1所示:
表1:
由上表1可知,本发明所制备的氮化铝陶瓷材料具有极佳的力学性能和导热性能,综合性能优良,应用前景广泛。
以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (6)
1.一种高性能氮化铝陶瓷材料,其特征在于,由以下重量份原料制备而成:
氮化铝纳米粉80-100份、烧结助剂6-12份、增塑剂1-2份、粘结剂5-10份、分散剂0.5-1份;
所述氮化铝纳米粉的制备方法如下:
将苯酚加热融化后,加入氢氧化钠溶液,搅拌均匀,再加入甲醛溶液,升温至65-75℃,搅拌反应20-40min后加入勃姆石溶胶,继续搅拌反应20-40min,冷却至室温,用稀盐酸将反应体系的pH调节至7-8,静置24-48h得到凝胶,真空干燥至恒重后进行高温氮化处理,最后与超分散剂混合球磨、干燥即可;
高温氮化处理具体操作如下:
将真空干燥至恒重后的凝胶研磨成粉,一段升温至1000-1050℃,保温反应2-4h,再通入氮气,在氮气氛围下二段升温至1500-1580℃,保温反应10-15h,再降温至550-600℃,保温反应2-4h后,恢复室温即可;
所述勃姆石溶胶的制备方法如下:
将异丙醇铝、水混合升温至60-80℃搅拌1-2h,再加入硝酸,升温至回流反应2-4h,冷却至室温静置24-48h即可;
所述烧结助剂包括LiAlO2、Y2O3和La2O3,所述LiAlO2、Y2O3和La2O3的质量比为3-6:1:1。
2.如权利要求1所述的高性能氮化铝陶瓷材料,其特征在于,所述超分散剂为磺酸盐、丙烯酸、丙烯酸酯和磷酸组成的四元共聚物。
3.如权利要求1所述的高性能氮化铝陶瓷材料,其特征在于,所述增塑剂为邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二丁酯或邻苯二甲酸二乙酯中的至少一种。
4.如权利要求1所述的高性能氮化铝陶瓷材料,其特征在于,所述粘结剂为聚乙烯醇水溶液。
5.如权利要求1所述的高性能氮化铝陶瓷材料,其特征在于,所述分散剂为焦磷酸钠、聚丙烯酸钠、六偏磷酸钠、羧甲基纤维素、鞣酸中的至少一种。
6.一种如权利要求1-5中任一项所述的高性能氮化铝陶瓷材料的制备方法,其特征在于,氮气保护下,氮化铝纳米粉、烧结助剂、增塑剂、分散剂混合球磨后干燥,加入粘结剂造粒,所得粒料放入模具中进行压制成型,得到粗坯,粗坯升温至500-600℃保温1-3h,通入氮气置换空气,再升温至1680-1950℃烧结2-4h,随炉冷却至室温即可。
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