CN105601276A - 一种电子陶瓷复合材料的制备方法 - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 239000000919 ceramic Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 239000010936 titanium Substances 0.000 claims abstract description 11
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- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 6
- HIEHAIZHJZLEPQ-UHFFFAOYSA-M sodium;naphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 HIEHAIZHJZLEPQ-UHFFFAOYSA-M 0.000 claims abstract description 6
- 150000001621 bismuth Chemical class 0.000 claims abstract description 4
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 4
- 150000003746 yttrium Chemical class 0.000 claims abstract description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 10
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical group C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 8
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 8
- JXLWTLZBAJWNSG-UHFFFAOYSA-N CCCC[Ti] Chemical compound CCCC[Ti] JXLWTLZBAJWNSG-UHFFFAOYSA-N 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 5
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 4
- 229910009523 YCl3 Inorganic materials 0.000 claims description 4
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 claims description 4
- 230000036571 hydration Effects 0.000 claims description 4
- 238000006703 hydration reaction Methods 0.000 claims description 4
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 claims description 4
- BEDFIBPNPHRGDO-UHFFFAOYSA-N yttrium;hydrate Chemical compound O.[Y] BEDFIBPNPHRGDO-UHFFFAOYSA-N 0.000 claims description 4
- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical class C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical class [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims 1
- XGZRAKBCYZIBKP-UHFFFAOYSA-L disodium;dihydroxide Chemical compound [OH-].[OH-].[Na+].[Na+] XGZRAKBCYZIBKP-UHFFFAOYSA-L 0.000 claims 1
- 229910052727 yttrium Inorganic materials 0.000 claims 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical class [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 24
- 235000011121 sodium hydroxide Nutrition 0.000 abstract description 8
- -1 titanium alkoxide Chemical class 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000416 bismuth oxide Inorganic materials 0.000 abstract description 4
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 229910052726 zirconium Inorganic materials 0.000 abstract description 2
- 239000012065 filter cake Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 6
- 150000004002 naphthaldehydes Chemical class 0.000 description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 6
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- DJOYTAUERRJRAT-UHFFFAOYSA-N 2-(n-methyl-4-nitroanilino)acetonitrile Chemical compound N#CCN(C)C1=CC=C([N+]([O-])=O)C=C1 DJOYTAUERRJRAT-UHFFFAOYSA-N 0.000 description 1
- 229910021523 barium zirconate Inorganic materials 0.000 description 1
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- GEZAXHSNIQTPMM-UHFFFAOYSA-N dysprosium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Dy+3].[Dy+3] GEZAXHSNIQTPMM-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
Abstract
本发明公开了一种电子陶瓷复合材料的制备方法，该制备方法是：在一定量浓盐酸中，搅拌条件下，缓慢依次加入有机钛醇盐、锆醇盐、无机钇盐和无机铋盐，经搅拌发生水解、聚合反应制得溶液A；同时，在水浴条件下，一定量去离子水中加入表面活性剂萘磺酸钠和分散剂聚甲醛萘磺酸钠盐，搅拌制得溶液B；在水浴条件下，将溶液A倒入溶液B中，静置反应、陈化，采用液碱调节pH值至中性，得到复合溶液C；溶液C经离心分离，得到湿滤饼D，经干燥、热处理得到结构有序的电子陶瓷复合材料。本发明结合化学制备技术和热处理技术，制备了结构有序、性能优异的含氧化锆、氧化钛、氧化钇及氧化铋的电子陶瓷复合材料。
Description
技术领域
本发明属于陶瓷材料制备技术，特别是一种含氧化锆、氧化钛、氧化钇、氧化铋的电子陶瓷复合材料的制备方法。
背景技术
电子陶瓷材料在陶瓷工业中占据了重要的地位，具有很多特性，如介电性、压电性、磁性、半导体性、绝缘性等，在电容器、集成电路、电子元件等诸多领域具有广泛用途。CN102120697A报道了一种采用氧化镝、氧化钇、锆酸钙改性锆酸钡基陶瓷电容器材料。CN103964847A报道了一种片式多层陶瓷电容器用低损耗微波介质陶瓷材料，通过氧化铌、氧化钽、氧化锌、氧化锆复合而成。
大多数电子陶瓷材料的制备方法均采用物理混合、煅烧处理，这会导致陶瓷材料中各组分相容性不好，无法发挥各组分间的协调功能，因此无法达到预期的效果。化学制备技术是一种将无机材料与有机材料复合的一种有效技术，具有低成本、可调控多种复合材料功能及组份、适于批量生产等诸多优势，涉及无机材料、有机材料、复合材料等众多领域。CN102531579A采用固相法获得了陶瓷介质材料。
发明内容
本发明的目的在于：提供一种电子陶瓷复合材料的制备方法。采用化学制备技术与热处理技术相结合，制备结构有序、性能优异的含氧化锆、氧化钛、氧化钇及氧化铋的电子陶瓷复合材料。
本发明的技术解决方案是：在一定量浓盐酸中，搅拌条件下，缓慢依次加入有机钛醇盐、锆醇盐、无机钇盐和无机铋盐，经搅拌发生水解、聚合反应制得溶液A；同时，在水浴条件下，一定量去离子水中加入表面活性剂萘磺酸钠和分散剂聚甲醛萘磺酸钠盐，搅拌制得溶液B；在水浴条件下，将溶液A倒入溶液B中，静置反应、陈化，采用液碱调节pH值至中性，得到复合溶液C；溶液C经离心分离，得到湿滤饼D，经干燥、热处理得到结构有序的电子陶瓷复合材料。
本发明与现有技术相比，其显著优点：其一、该电子陶瓷复合材料通过化学制备技术，复合了锆钛钇铋四种元素，结合热处理工艺，制备了含氧化锆、氧化钛、氧化钇及氧化铋的电子陶瓷复合材料；其二、该化学制备技术成本低廉，适于工业化生产，制得的电子复合材料纯度高、性能优异。
具体实施方式
下面结合具体实施例进一步说明本发明的技术解决方案，这些实施例不能理解为是对技术解决方案的限制。
实施例1：依以下步骤制备电子陶瓷复合材料
步骤1：在300mL质量浓度为36.5%的浓盐酸HCl中，开动搅拌，缓慢加入100g正丁醇钛Ti(OC4H9)4、42.3g质量浓度为80%的正丁醇锆Zr(OC4H9)4、5.6g六水合硝酸钇Y(NO3)3·6H2O、7.1g五水合硝酸铋Bi(NO3)3·5H2O，搅拌时间控制4h，得到溶液A；
步骤2：在60oC水浴条件下，将20g表面活性剂2-萘磺酸钠和3g分散剂聚萘甲醛磺酸钠盐加入到100mL去离子水中，搅拌2h，制得溶液B；
步骤3：在60oC水浴条件下，将溶液A倒入溶液B中，静置反应、陈化24h，采用质量浓度30%的液碱NaOH溶液调节pH值至中性，得到复合溶液C；
步骤4：溶液C经离心分离，得到湿滤饼D，经110oC，12h烘干、1100oC热处理12h,得到结构有序的电子陶瓷复合材料。
实施例2：依以下步骤制备电子陶瓷复合材料
步骤1：在300mL质量浓度为36.5%的浓盐酸HCl中，开动搅拌，缓慢加入100g正丁醇钛Ti(OC4H9)4、98.7g质量浓度为80%的正丁醇锆Zr(OC4H9)4、16.8g六水合硝酸钇Y(NO3)3·6H2O、21.4g五水合硝酸铋Bi(NO3)3·5H2O，搅拌时间控制6h，得到溶液A；
步骤2：在80oC水浴条件下，将40g表面活性剂2-萘磺酸钠和5g分散剂聚萘甲醛磺酸钠盐加入到100mL去离子水中，搅拌4h，制得溶液B；
步骤3：在80oC水浴条件下，将溶液A倒入溶液B中，静置反应、陈化48h，采用质量浓度30%的液碱NaOH溶液调节pH值至中性，得到复合溶液C；
步骤4：溶液C经离心分离，得到湿滤饼D，经150oC，8h烘干、1300oC热处理8h,得到结构有序的电子陶瓷复合材料。
实施例3：依以下步骤制备电子陶瓷复合材料
步骤1：在300mL质量浓度为36.5%的浓盐酸HCl中，开动搅拌，缓慢加入100g正丁醇钛Ti(OC4H9)4、60g质量浓度为80%的正丁醇锆Zr(OC4H9)4、10g六水合硝酸钇Y(NO3)3·6H2O、15g五水合硝酸铋Bi(NO3)3·5H2O，搅拌时间控制5h，得到溶液A；
步骤2：在70oC水浴条件下，将30g表面活性剂2-萘磺酸钠和4g分散剂聚萘甲醛磺酸钠盐加入到100mL去离子水中，搅拌3h，制得溶液B；
步骤3：在70oC水浴条件下，将溶液A倒入溶液B中，静置反应、陈化36h，采用质量浓度30%的液碱NaOH溶液调节pH值至中性，得到复合溶液C；
步骤4：溶液C经离心分离，得到湿滤饼D，经120oC，10h烘干、1200oC热处理10h,得到结构有序的电子陶瓷复合材料。
实施例4：依以下步骤制备电子陶瓷复合材料
步骤1：在300mL质量浓度为36.5%的浓盐酸HCl中，开动搅拌，缓慢加入100g正丁醇钛Ti(OC4H9)4、42.3g质量浓度为80%的正丁醇锆Zr(OC4H9)4、4.4g六水合氯化钇YCl3·6H2O、4.6g氯化铋BiCl3，搅拌时间控制4h，得到溶液A；
步骤2：在80oC水浴条件下，将40g表面活性剂1-萘磺酸钠和5g分散剂聚萘甲醛磺酸钠盐加入到100mL去离子水中，搅拌2h，制得溶液B；；
步骤3：同实施例1；
步骤4：同实施例1。
实施例5：依以下步骤制备电子陶瓷复合材料
步骤1：在300mL质量浓度为36.5%的浓盐酸HCl中，开动搅拌，缓慢加入100g正丁醇钛Ti(OC4H9)4、98.7g质量浓度为80%的正丁醇锆Zr(OC4H9)4、13.2g六水合氯化钇YCl3·6H2O、13.86g氯化铋BiCl3，搅拌时间控制6h，得到溶液A；
步骤2：在80oC水浴条件下，将40g表面活性剂1-萘磺酸钠和5g分散剂聚萘甲醛磺酸钠盐加入到100mL去离子水中，搅拌4h，制得溶液B；
步骤3：同实施例2；
步骤4：同实施例2。
实施例6：依以下步骤制备电子陶瓷复合材料
步骤1：在300mL质量浓度为36.5%的浓盐酸HCl中，开动搅拌，缓慢加入100g正丁醇钛Ti(OC4H9)4、60g质量浓度为80%的正丁醇锆Zr(OC4H9)4、8g六水合氯化钇YCl3·6H2O、8g氯化铋BiCl3，搅拌时间控制5h，得到溶液A；
步骤2：在70oC水浴条件下，将30g表面活性剂1-萘磺酸钠和4g分散剂聚萘甲醛磺酸钠盐加入到100mL去离子水中，搅拌3h，制得溶液B；
步骤3：同实施例3；
步骤4：同实施例3。
Claims (5)
1.一种电子陶瓷复合材料的制备方法，其特征在于，该制备方法是：在一定质量浓度为36.5%的盐酸HCl中，搅拌条件下，缓慢依次加入有机正丁醇钛Ti(OC4H9)4、质量浓度为80%的有机正丁醇锆Zr(OC4H9)4、无机钇盐和无机铋盐，经搅拌，时间控制4h-6h，发生水解、聚合反应制得溶液A；在一定量去离子水中加入表面活性剂萘磺酸钠和分散剂聚甲醛萘磺酸钠盐，水浴控温60oC-80oC，搅拌2h-4h，制得溶液B；在水浴条件下，温度范围控制60oC-80oC，将溶液A倒入溶液B中，静置反应、陈化24h-48h后，采用质量浓度为30%的氢氧化钠NaOH溶液调节pH值至中性，得到复合溶液C；溶液C经离心分离，得到湿滤饼D，经110oC-150oC干燥8h-12h、热处理，温度控制1100oC-1300oC，时间控制8h-12h，得到结构有序的电子陶瓷复合材料。
2.根据权利要求1所述的一种电子陶瓷复合材料的制备方法，其特征在于：所述的无机钇盐任选六水合硝酸钇Y(NO3)3·6H2O或六水合氯化钇YCl3·6H2O，所述的无机铋盐任选五水合硝酸铋Bi(NO3)3·5H2O或氯化铋BiCl3。
3.根据权利要求1所述的一种电子陶瓷复合材料的制备方法，其特征在于：所述的表面活性剂萘磺酸钠可任选1-萘磺酸钠或2-萘磺酸钠。
4.根据权利要求1所述的一种电子陶瓷复合材料的制备方法，其特征在于：溶液A中Zr(OC4H9)4、无机钇盐和无机铋盐分别占Ti(OC4H9)4的摩尔比为30%-70%、5%-15%及5%-15%。
5.根据权利要求1所述的一种电子陶瓷的制备方法，其特征在于：所述的表面活性剂萘磺酸钠和分散剂聚甲醛萘磺酸钠盐分别占Ti(OC4H9)4的质量比为20%-40%和3%-5%。
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106630999A (zh) * | 2016-10-09 | 2017-05-10 | 龚娟 | 一种电子陶瓷材料的制备方法 |
| CN107523172A (zh) * | 2017-10-06 | 2017-12-29 | 南京市雨花台区绿宝工业设计服务中心 | 一种建筑内墙复合涂料的制备方法 |
| CN107721416A (zh) * | 2017-11-23 | 2018-02-23 | 龚娟 | 一种义齿陶瓷材料的制备方法 |
| CN107721415A (zh) * | 2017-11-23 | 2018-02-23 | 龚娟 | 一种复合义齿陶瓷材料及其制备方法 |
| CN108484109A (zh) * | 2018-06-24 | 2018-09-04 | 龚娟 | 一种陶瓷材料的制备方法 |
| CN108640650A (zh) * | 2018-06-24 | 2018-10-12 | 龚娟 | 一种复合陶瓷材料的制备方法 |
| CN108911782A (zh) * | 2018-09-13 | 2018-11-30 | 龚娟 | 一种保温陶瓷材料的制备方法 |
| CN108947485A (zh) * | 2018-09-13 | 2018-12-07 | 龚娟 | 一种日用陶瓷复合材料的制备方法 |
| CN108996989A (zh) * | 2018-09-13 | 2018-12-14 | 龚娟 | 一种保温陶瓷复合材料的制备方法 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291787A (zh) * | 2014-10-14 | 2015-01-21 | 季红军 | 一种复合陶瓷材料及其制备方法 |
-
2015
- 2015-12-30 CN CN201511010697.1A patent/CN105601276B/zh not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291787A (zh) * | 2014-10-14 | 2015-01-21 | 季红军 | 一种复合陶瓷材料及其制备方法 |
Non-Patent Citations (2)
| Title |
|---|
| 沈君权等: "正丁醇钛一乙酸钡水解法合成BaTiO3粉体的研究", 《中国陶瓷》 * |
| 路大勇等: "锶锆共掺杂对钛酸钡陶瓷结构和介电性质的影响", 《东北师大学报（自然科学版）》 * |
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|---|---|---|---|---|
| CN106630999A (zh) * | 2016-10-09 | 2017-05-10 | 龚娟 | 一种电子陶瓷材料的制备方法 |
| CN107523172A (zh) * | 2017-10-06 | 2017-12-29 | 南京市雨花台区绿宝工业设计服务中心 | 一种建筑内墙复合涂料的制备方法 |
| CN107721416A (zh) * | 2017-11-23 | 2018-02-23 | 龚娟 | 一种义齿陶瓷材料的制备方法 |
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