CN105503177A - 一种电子陶瓷材料的制备方法 - Google Patents
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000010936 titanium Substances 0.000 claims abstract description 8
- -1 zirconium alkoxide Chemical class 0.000 claims abstract description 8
- 238000007669 thermal treatment Methods 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000000919 ceramic Substances 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 3
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 claims description 3
- JXLWTLZBAJWNSG-UHFFFAOYSA-N CCCC[Ti] Chemical compound CCCC[Ti] JXLWTLZBAJWNSG-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- PWHCIQQGOQTFAE-UHFFFAOYSA-L barium chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Ba+2] PWHCIQQGOQTFAE-UHFFFAOYSA-L 0.000 claims description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 2
- AMGRXJSJSONEEG-UHFFFAOYSA-L strontium dichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Sr]Cl AMGRXJSJSONEEG-UHFFFAOYSA-L 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 2
- 229920001223 polyethylene glycol Polymers 0.000 claims 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 abstract description 8
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052726 zirconium Inorganic materials 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 4
- 159000000009 barium salts Chemical class 0.000 abstract description 3
- 159000000008 strontium salts Chemical class 0.000 abstract description 3
- 229910052719 titanium Inorganic materials 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 230000007935 neutral effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 2
- 239000012065 filter cake Substances 0.000 abstract 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 230000007062 hydrolysis Effects 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
- 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 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- ZMPHUNYTNBVSHC-UHFFFAOYSA-N [Zr].[Ti].[Sr].[Ba] Chemical compound [Zr].[Ti].[Sr].[Ba] ZMPHUNYTNBVSHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 230000007073 chemical hydrolysis Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 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
- 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
- C04B35/46—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 titanium oxides or titanates
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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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- 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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- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
Abstract
本发明公开了一种电子陶瓷材料的制备方法，该制备方法是：在一定量浓盐酸中，搅拌条件下，缓慢依次加入有机锆醇盐、钛醇盐、无机钡盐和无机锶盐，经搅拌，发生水解、聚合反应制得溶液A；在一定量水中加入表面活性剂和分散剂，搅拌制得溶液B；将溶液A倒入溶液B中，静置陈化一段时间后，调节pH值至中性，得到复合溶液C；溶液C经过滤得到湿滤渣D和滤液E，湿滤渣D中加入少量滤液E,转移至反应釜中，控温静置一段时间后，待反应釜中溶液冷却至室温，过滤得到湿滤饼F；湿滤饼F经干燥、热处理得到结构有序的电子陶瓷材料。本发明通过化学制备技术以及热处理工艺，制备了含氧化锆、氧化钛、氧化钡、氧化锶的电子陶瓷材料。
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、氧化钡、氧化锶的电子陶瓷材料的制备方法。
背景技术
陶瓷材料具有诸多优点，如美观大方、耐酸碱、耐高温、应用领域广泛等。电子陶瓷是陶瓷工业中重要的一类，具有独特的介电性、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，例如：钛酸钡是一种钙钛矿型介电材料，被誉为电子陶瓷产业的支柱。
电子陶瓷可分为绝缘陶瓷、介电陶瓷、压电陶瓷、磁性陶瓷和传感器陶瓷等，各种陶瓷材料通常存在介电常数低、不耐高温、温度稳定性能差等缺陷，这不仅和电子陶瓷本身组份有关，还与制备工艺息息相关。CN102701738A采用物理混合球磨，制备了一种复合二氧化钛、氧化锆、氧化钙、钛酸镁等多种组份的电子陶瓷材料。
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。
发明内容
本发明的目的在于：提供一种电子陶瓷材料的制备方法。结合化学工艺，制备结构有序、性能优异的含氧化锆、氧化钛、氧化钡及氧化锶电子陶瓷材料。
本发明的技术解决方案是：在一定量浓盐酸中，搅拌条件下，缓慢依次加入有机锆醇盐、钛醇盐、无机钡盐和无机锶盐，经搅拌，发生水解、聚合反应制得溶液A；在一定量水中加入表面活性剂和分散剂，搅拌制得溶液B；将溶液A倒入溶液B中，静置陈化一段时间后，调节pH值至中性，得到复合溶液C；溶液C经过滤得到湿滤渣D和滤液E，湿滤渣D中加入少量滤液E,转移至反应釜中，控温静置一段时间后，待反应釜中溶液冷却至室温，过滤得到湿滤饼F；湿滤饼F经干燥、热处理得到结构有序的电子陶瓷材料。
本发明与现有技术相比，其显著优点：其一、该电子陶瓷材料在化学制备过程中，通过在强酸性条件下，有机锆醇盐及钛醇盐与无机钡盐及锶盐之间的化学水解、聚合反应，形成稳定的钛锆钡锶基复合前驱体，结合热处理工艺，制备了含氧化锆、氧化钛、氧化钡及氧化锶的电子陶瓷材料；其二、该化学制备技术可推广用于制备其他多组份、多功能复合电子陶瓷材料。
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材料
步骤1：在250mL质量浓度为36.5%的浓盐酸HCl中，搅拌时，缓慢加入100g正丁醇钛Ti(OC4H9)4、28.2g质量浓度为80%的正丁醇锆Zr(OC4H9)4、7.2g二水合氯化钡BaCl2·2H2O、3.9g六水合氯化锶SrCl2·6H2O，搅拌时间控制2h，得到溶液A；
步骤2：在100mL去离子水中，加入30g表面活性剂十二烷基苯磺酸钠和10g分散剂聚乙二醇-2000PEG-2000，搅拌3h，制得溶液B；
步骤3：将溶液A倒入溶液B中，静置陈化24h，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；
步骤4：复合溶液C经过滤得到湿滤渣D和滤液E，湿滤渣D中加入100mL滤液E,转移至1L反应釜中，控温150oC,静置12h后，待反应釜中溶液冷却至室温，过滤得到湿滤饼F；
步骤5：湿滤饼F经110oC干燥12h,1100oC热处理4h得到结构有序的电子陶瓷材料。
实施例2：依以下步骤制备电子陶瓷材料
步骤1：在250mL质量浓度为36.5%的浓HCl中，搅拌时，缓慢加入100gTi(OC4H9)4、56.4g质量浓度为80%的Zr(OC4H9)4、21.6gBaCl2·2H2O、11.7gSrCl2·6H2O，搅拌时间控制4h，得到溶液A；
步骤2：在100mL去离子水中，加入50g十二烷基苯磺酸钠和20gPEG-6000，搅拌6h，制得溶液B；
步骤3：将溶液A倒入溶液B中，静置陈化48h，采用质量浓度为30%的NaOH溶液调节pH值至中性，得到复合溶液C；
步骤4：复合溶液C经过滤得到湿滤渣D和滤液E，湿滤渣D中加入150mL滤液E,转移至1L反应釜中，控温180oC,静置8h后，待反应釜中溶液冷却至室温，过滤得到湿滤饼F；
步骤5：湿滤饼F经150oC干燥8h,900oC热处理8h得到结构有序的电子陶瓷材料。
实施例3：依以下步骤制备电子陶瓷材料
步骤1：在250mL质量浓度为36.5%的浓HCl中，搅拌时，缓慢加入100gTi(OC4H9)4、40g质量浓度为80%的Zr(OC4H9)4、15gBaCl2·2H2O、8gSrCl2·6H2O，搅拌时间控制3h，得到溶液A；
步骤2：在100mL去离子水中，加入40g十二烷基苯磺酸钠和15gPEG-4000，搅拌5h，制得溶液B；
步骤3：将溶液A倒入溶液B中，静置陈化36h，采用质量浓度为30%的NaOH溶液调节pH值至中性，得到复合溶液C；
步骤4：复合溶液C经过滤得到湿滤渣D和滤液E，湿滤渣D中加入120mL滤液E,转移至1L反应釜中，控温160oC,静置10h后，待反应釜中溶液冷却至室温，过滤得到湿滤饼F；
步骤5：湿滤饼F经120oC干燥10h,1000oC热处理10h得到结构有序的电子陶瓷材料。
Claims (3)
1.一种电子陶瓷材料的制备方法，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、无机二水合氯化钡BaCl2·2H2O及六水合氯化锶SrCl2·6H2O，经搅拌，时间控制2h-4h，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十二烷基苯磺酸钠和分散剂聚乙二醇PEG，搅拌3h-6h，制得溶液B；将溶液A倒入溶液B中，静置陈化24h-36h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经过滤得到湿滤渣D和滤液E，湿滤渣D中加入少量滤液E,转移至反应釜中，控温150oC-180oC，静置8h-12h后，待反应釜中溶液冷却至室温，过滤得到湿滤饼F；湿滤饼F经110oC-150oC干燥8h-12h、热处理，温度控制900oC-1100oC，时间控制8h-12h，得到结构有序的电子陶瓷材料。
2.根据权利要求1所述的一种电子陶瓷材料的制备方法，其特征在于：所述的溶液A中Zr(OC4H9)4、BaCl2·2H2O及SrCl2·6H2O分别占Ti(OC4H9)4的摩尔比为20%-40%、10%-30%及5%-15%。
3.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：所述的表面活性剂十二烷基苯磺酸钠占Ti(OC4H9)4的质量比例为30%-50%，分散剂PEG，分子量可选2000、4000及6000，其添加量占Ti(OC4H9)4的质量比例为10%-20%。
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| CN108484109A (zh) * | 2018-06-24 | 2018-09-04 | 龚娟 | 一种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 |
| CN113582582A (zh) * | 2021-07-30 | 2021-11-02 | 湖南省新化县林海陶瓷有限公司 | 一种宽工作温区的电子陶瓷复合基片的制备工艺 |
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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 |
| CN108484109A (zh) * | 2018-06-24 | 2018-09-04 | 龚娟 | 一种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 |
| CN113582582A (zh) * | 2021-07-30 | 2021-11-02 | 湖南省新化县林海陶瓷有限公司 | 一种宽工作温区的电子陶瓷复合基片的制备工艺 |
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