CN114195510A - 一种纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉及其制备方法 - Google Patents
一种纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉及其制备方法 Download PDFInfo
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- CN114195510A CN114195510A CN202111625561.7A CN202111625561A CN114195510A CN 114195510 A CN114195510 A CN 114195510A CN 202111625561 A CN202111625561 A CN 202111625561A CN 114195510 A CN114195510 A CN 114195510A
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- magnesium
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- calcium titanate
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- 239000000919 ceramic Substances 0.000 title claims abstract description 54
- 239000000843 powder Substances 0.000 title claims abstract description 52
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000012545 processing Methods 0.000 claims abstract description 8
- 230000001788 irregular Effects 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 47
- 239000002243 precursor Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 150000001875 compounds Chemical class 0.000 claims description 23
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 18
- 239000011777 magnesium Substances 0.000 claims description 18
- 229910052749 magnesium Inorganic materials 0.000 claims description 18
- 229940091250 magnesium supplement Drugs 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 15
- 239000011575 calcium Substances 0.000 claims description 14
- 229910052791 calcium Inorganic materials 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- 239000004094 surface-active agent Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 159000000003 magnesium salts Chemical class 0.000 claims description 8
- 239000012046 mixed solvent Substances 0.000 claims description 8
- 239000002105 nanoparticle Substances 0.000 claims description 8
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 7
- 239000001095 magnesium carbonate Substances 0.000 claims description 7
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 7
- 230000002572 peristaltic effect Effects 0.000 claims description 7
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 7
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- 159000000007 calcium salts Chemical class 0.000 claims description 4
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical compound [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 claims description 4
- 210000003298 dental enamel Anatomy 0.000 claims description 4
- UHNWOJJPXCYKCG-UHFFFAOYSA-L magnesium oxalate Chemical compound [Mg+2].[O-]C(=O)C([O-])=O UHNWOJJPXCYKCG-UHFFFAOYSA-L 0.000 claims description 4
- 229920003023 plastic Polymers 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- FNAQSUUGMSOBHW-UHFFFAOYSA-H calcium citrate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O FNAQSUUGMSOBHW-UHFFFAOYSA-H 0.000 claims description 3
- 239000001354 calcium citrate Substances 0.000 claims description 3
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 229960005336 magnesium citrate Drugs 0.000 claims description 3
- 239000004337 magnesium citrate Substances 0.000 claims description 3
- 235000002538 magnesium citrate Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- -1 organic acid magnesium salt Chemical class 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 235000013337 tricalcium citrate Nutrition 0.000 claims description 3
- PLSARIKBYIPYPF-UHFFFAOYSA-H trimagnesium dicitrate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O PLSARIKBYIPYPF-UHFFFAOYSA-H 0.000 claims description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 125000005233 alkylalcohol group Chemical group 0.000 claims description 2
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 2
- 229910001385 heavy metal Inorganic materials 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- 229940095060 magnesium tartrate Drugs 0.000 claims description 2
- MUZDLCBWNVUYIR-ZVGUSBNCSA-L magnesium;(2r,3r)-2,3-dihydroxybutanedioate Chemical compound [Mg+2].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O MUZDLCBWNVUYIR-ZVGUSBNCSA-L 0.000 claims description 2
- JESHZQPNPCJVNG-UHFFFAOYSA-L magnesium;sulfite Chemical compound [Mg+2].[O-]S([O-])=O JESHZQPNPCJVNG-UHFFFAOYSA-L 0.000 claims description 2
- 229910001453 nickel ion Inorganic materials 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims 1
- 238000009210 therapy by ultrasound Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 26
- 239000012071 phase Substances 0.000 description 24
- 239000007789 gas Substances 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 2
- 238000002083 X-ray spectrum Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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- 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
- C04B35/462—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 based on titanates
- C04B35/465—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 based on titanates based on alkaline earth metal titanates
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
本发明涉及一种纯晶相高平质因数纳米尺寸钛酸镁钙钙陶瓷粉材料及其制备方法，该材料是一种呈现不规则形状纯晶相结构的纳米尺寸的钛酸镁钙钙纳米陶瓷粉，材料颗粒尺寸为60‑150nm，干燥粉碎处理以后粒度D50小于200nm，比表面积1‑30m2/g，加工烧结后的陶瓷器件具有超高的品质因数，介电常数在20‑40范围内可调。与现有技术相比，本发明的制备过程操作简便，不需要额外的复杂条件和复杂设备，常温常压下搅拌就可以发生反应，而且其实用的原料便宜易得，从而使材料的制备成本相对较低，颗粒粒度尺寸较小而且制备的钛酸镁钙可以用作制作电子陶瓷器件、滤波器陶瓷器件等多种用途。
Description
技术领域
本发明属于材料制备技术领域，具体涉及一种粒度D50小于200nm、纯晶相纳米尺寸钛酸镁钙陶瓷粉及其制备方法。
背景技术
钛酸镁钙基陶瓷是日常生活中常见的一种具有良好应用性能的介电陶瓷材料，具有比较好的介电稳定性，已经被广泛地应用于电子信息、生活用品、生物医药等诸多领域。但是随着应用领域的扩展和性能指标的提升，对钛酸镁钙基陶瓷材料性能要求也越来越高，特别是介电常数和品质因数指标，往往要求介电常数稳定和高的品质因数。因此钛酸镁钙陶瓷粉体的性能是决定将来加工所得滤波介电陶瓷产品的根本因素，制备出具有特殊优异性能的钛酸镁钙基陶瓷粉材料已经成为材料界研究热点。控制其晶相结构、尺寸和形貌可以改善其机械性能、热烧结性能。在介电滤波陶瓷器件加工过程中钛酸镁钙陶瓷粉体的纯度、颗粒大小、晶相、表面结构和形貌等特性直接决定了陶瓷器件加工的良品率和后续的使用性能。有关高性能的钛酸镁钙纳米陶瓷粉体的制备是现在的研究热点和技术难点。但是现有常见固相法制备方法得到的钛酸镁钙陶瓷粉体颗粒往往比较大，即使颗粒尺寸可以达到纳米级，但是产品干燥处理以后总是使其发生团聚严重或晶相不纯，极大限制了钛酸镁钙陶瓷材料的开发与应用。高质量的具有特定介电常数的纳米级钛酸镁钙基陶瓷粉体的制备及其结构控制是决定钛酸镁钙基陶瓷应用的关键技术难题。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种粒度D50小于200nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉材料及其制备方法。
本发明的目的可以通过以下技术方案来实现：一种纯晶相高品质因数纳米尺寸钛酸镁钙基粉体材料，其特征在于，该材料是一种呈现不规则形状纯晶相结构的纳米尺寸的钛酸镁钙纳米陶瓷粉，材料颗粒尺寸为60-150nm，干燥粉碎处理以后粒度D50小于200nm，D90小于300nm，比表面积1-30m2/g，加工烧结后的陶瓷器件具有超高的品质因数，介电常数在20-40范围内可调，表观密度为3.0-4.0g/cm3。
本发明提出的一种粒度D50小于200nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉材料的制备方法：首先将不溶于水的含镁化合物前躯体、含钙化合物前驱体和一定量表面活性剂分散与水和有机醇的混合溶液中，将钛的氯化物溶液缓慢引入上述混合溶液中，进行在液相反应过程，经过后续的离心、洗涤、干燥和焙烧处理得到纯晶相纳米尺寸钛酸镁钙陶瓷粉，然后再经过气体粉磨处理就可以得到粒度D50小于200nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉材料。具体步骤如下：
(1)将一定量的不溶于水的含镁化合物前躯体、含钙化合物前驱体和表面活性剂溶解到水和有机醇混合溶剂(水与有机醇的体积比为1:0.1～1)中，超声分散，机械搅拌下得到悬浊液，将此溶液记做溶液A。
(2)称取一定量的钛的氯化物溶解于一定体积的去离子水溶液中，将其记做溶液B。
(3)采用蠕动泵分别以正加、反加或并流方式将溶液A和溶液B均匀混合，室温下发生反应，然后继续搅拌1-2天，得到白色凝胶，离心分离得到沉淀产物，洗涤，干燥、焙烧，最后将得到的固体粉末样品经过气态粉磨处理，即得到粒度D50小于200nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉材料。
本发明中，不溶于水的含镁化合物前驱体和含钙化合物前驱体经过超声分散形成悬浊液，由于钛的氯化物会剧烈水解产生出酸性很强的氯化氢，可以有效促进含镁混合物溶解生成镁离子和钙离子，而钛的氯化物水解产生出来的钛酸，又可以和镁离子或钙离子发生沉淀反应，发生沉淀-溶解-沉淀的复杂过程，表面活性剂的存在可以减弱溶胶颗粒之间的相互作用和改变相应沉淀的表面状态，有效防止沉淀颗粒之间团聚的发生，而且对钛酸镁钙晶相具有有效的调控作用。因此经过比较简单的处理过程就可以得到粒度D50小于200nm、纯晶相高品质因数纳米尺寸的钛酸镁钙陶瓷粉材料。
溶液A和溶液B形成的反应体系中不溶于水的含镁化合物前驱体的浓度是1-15wt％；含钙化合物前驱体的质量浓度为0.5-10％；不溶于水的含镁化合物前驱体与含钛氯化物的质量比为0.5-2.5：1；反应温度可在室温条件下，即随着季节变换控制范围在0-40℃。
所述的不溶于水的含镁化合物前驱体是不溶于水和有机醇的无机镁盐或者有机酸镁盐类；所述的所述的镁盐前驱体为碳酸镁、草酸镁、柠檬酸镁、酒石酸镁、亚硫酸镁、氢氧化镁中的一种或几种；
所述的含钙化合物前驱体是无机钙盐、有机酸钙盐或者含钙的氢氧化物类，例如碳酸钙、草酸钙、柠檬酸钙、氯化钙、硝酸钙、氢氧化钙中的一种或几种；
所述的钛氯化物为四氯化钛、三氯化钛、氯氧化钛中的一种或几种一种或几种；
所述的表面活性剂主要是非离子型的高分子聚合物；所述的表面活性剂为聚乙二醇、PVP、聚丙烯酸、聚醚、F127中的一种或几种；含镁化合物前驱体与表面活性剂的质量比为10:0.2～1。
所述的有机醇为液态直链烷基醇或者其异构体醇；所述的有机醇是乙醇、甲醇、丙醇、异丙醇、正丁醇、苯甲醇中的一种或几种。
所述的水为经过水净化处理得到的水，其中重金属离子、铁、钴、镍离子低于ppm以下。
所述的溶液A和溶液B的盛放容器和反应容器为玻璃容器、有机塑料容器或陶瓷搪瓷容器，包括玻璃烧瓶、玻璃烧杯、表面皿、锥形瓶、广口瓶、称量瓶、试管、量杯、塑料烧杯、陶瓷反应釜、搪瓷反应釜、离心管中的一种或几种。
步骤(3)中的离心分离的离心转速在4000-10000rpm，每次离心时间5-10min。
步骤(3)中的洗涤选用的溶剂为水、甲醇、乙醇、异丙醇中的一种或几种。
步骤(3)中的干燥处理选用的温度范围为70–120℃；焙烧处理选用的温度范围为700-1200℃，焙烧时间为3-10h，采用的气氛为空气气氛，需要空压机不断鼓入空气。
固体粉末样品经过气态粉磨处理所选用的设备为气流粉碎机，功率为5KW，经过旋风分离器收集粉末产品，空气压缩机功率为80KW，为粉碎提供10.0Mpa压缩空气。
与现有技术相比，本发明通过在水和有机醇的混合溶剂中不溶于水的含镁化合物前驱体和含钙化合物前驱体经过与钛的氯化物会剧烈水解产生出酸性很强的氯化氢发生反应，而后又与钛酸发生沉淀反应，发生沉淀-溶解-沉淀的复杂过程，在此反应体系中有机醇起到至关重要的作用，它的存在不仅可以减弱溶胶颗粒之间的相互作用，还可以改变相应沉淀的表面状态，从而防止沉淀颗粒之间团聚的发生，此外对钛酸镁钙晶相结构进行有效的调控，而后续经过气态粉碎技术可以有效解除产品中颗粒团聚，有效控制产品中的粒度分布，与传统的钛酸镁钙陶瓷粉体合成方法相比，该发明方法可控性强，过程简单、操作方便、成本低廉。而且整个制备反应过程是在室温静态条件下进行,节能环保所得纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉具有不规则的颗粒形貌，表面凹凸不平，而且颗粒分散性良好，颗粒度均匀，粒度尺寸较小，具有广阔的应用前景，特别是在电子信息产业陶瓷器件加工领域。
附图说明
图1本制备方法得到的粒度D50小于200nm、纯晶相高品质因数纳米尺寸的钛酸镁钙陶瓷粉体特征透射电子显微镜(TEM)图，由实施例1制得。
图2单分散的粒度D50小于200nm、纯晶相高品质因数纳米尺寸的钛酸镁钙陶瓷粉体特征大角X射线谱图，由实施例1制得。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。
实施例1
将10g碳酸镁、0.5g碳酸钙和1.0g PEG-10000用500ml水和乙醇混合溶剂(水与有机醇的体积比为1:0.1)溶解，搅拌半个小时以后将100ml含有40g四氯化钛溶液通过蠕动泵加入上述溶液，搅拌12h以后，将生成的凝胶溶液产物在11000rpm转速下离心5分钟分离得到凝胶，然后用水和乙醇各清洗两次以后，在空气中80℃干燥12h以后，经过1100℃煅烧4小时后，再经过气体压力为8.0MPa气态粉碎仪处理，旋风分离器收集得到的粉末样品，可以得到D50为70nm、纯晶相纳米尺寸钛酸镁钙陶瓷粉体，介电常数测试结果为20.6，品质因数可以达到110000。其形貌和特性见图1-图2所示。
实施例2
将10g草酸镁、1g氯化钙和1.0g PEG-40000用500ml水和乙醇混合溶剂溶解(水与有机醇的体积比为1:0.1)，搅拌半个小时以后将100ml含有50g氯氧化钛水溶液通过蠕动泵加入上述溶液，搅拌12h以后，将生成的凝胶溶液产物在11000rpm转速下离心5分钟分离得到凝胶，然后用水和乙醇各清洗两次以后，在空气中110℃干燥12小时以后，经过900℃煅烧4小时后，可以得到D50为90nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉体。
实施例3
将10g碳酸镁、1g碳酸钙和1.0g PEG-10000用500ml水和乙醇混合溶剂(水与有机醇的体积比为1:0.2)溶解，搅拌半个小时以后采用蠕动泵将上述溶液慢慢滴加到400ml含有80g三氯化钛水溶液，搅拌12h以后，将生成的凝胶溶液产物在8000rpm转速下离心5分钟分离得到凝胶，然后用水和乙醇各清洗两次以后，在空气中100℃干燥12小时以后，经过1000℃煅烧4小时后，再经过气体压力为1.0MPa气态粉碎仪处理，旋风分离器收集得到的粉末样品，可以得到D50为105nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉体。
实施例4
将10g碳酸镁、2g氢氧化钙和2.0g P123用500ml水和乙醇混合溶剂(水与有机醇的体积比为1:0.1)溶解，搅拌半个小时以后采用蠕动泵将上述溶液慢慢滴加到400ml含有60g三氯化钛水溶液，搅拌12h以后，将生成的凝胶溶液产物在8000rpm转速下离心5分钟分离得到凝胶，然后用水和乙醇各清洗两次以后，在空气中100℃干燥12小时以后，经过1000℃煅烧4小时后，再经过气体压力为1.0MPa气态粉碎仪处理，旋风分离器收集得到的粉末样品，可以得到D50为130nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉体。
实施例5
一种粒度D50小于200nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉体制备方法具体步骤如下：
(1)将一定量的镁盐前驱体碳酸镁、钙盐前驱体碳酸钙(镁和钙原子比例为10:1)和表面活性剂PVP溶解到水和有机醇乙醇混合溶剂(水与有机醇的体积比为1:0.1)中，机械搅拌下得到悬浊液，将此溶液记做溶液A。
(2)称取一定量的三氯化钛水溶液，将其记做溶液B。镁盐前驱体与三氯化钛水溶液的质量比为0.8：2；
(3)采用蠕动泵分别以正加、反加或并流方式将溶液A和溶液B均匀混合，室温下发生反应，所形成的反应体系中镁盐前驱体的浓度是1wt％，然后继续搅拌1天，得到凝胶溶液，离心分离得到沉淀产物，离心分离的离心转速在5000rpm，每次离心时间10min。采用水洗涤，120℃干燥、1100℃焙烧3h，最后将得到的固体粉末样品经过气态粉磨处理，即得到粒度D50小于200nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉材料。固体粉末样品经过气态粉磨处理所选用的设备为气流粉碎机，功率为5KW，经过旋风分离器收集粉末产品，空气压缩机功率为80KW，为粉碎提供10.0Mpa压缩空气。
Claims (10)
1.一种纯晶相纳米尺寸钛酸镁钙陶瓷粉材料，其特征在于，该材料是一种呈现不规则形状纯晶相结构的纳米尺寸的钛酸镁钙陶瓷粉，材料颗粒尺寸为60-150nm，干燥粉碎处理以后粒度D50小于200nm，比表面积1-30m2/g，加工烧结后的陶瓷器件具有超高的品质因数，介电常数在20-40范围内可调，表观密度为3.0-4.0g/cm3。
2.一种如权利要求1所述的纯晶相高品质因数纳米尺寸的钛酸镁钙陶瓷粉材料的制备方法，其特征在于，包括以下步骤：
(1)将一定量的不溶于水的含镁化合物前驱体、含钙化合物前驱体、表面活性剂溶解到水和有机醇混合溶剂中，超声处理以后机械搅拌下得到悬浊液，将此溶液记做溶液A。
(2)称取一定量的含有钛氯化物溶溶液，将其记做溶液B。
(3)采用蠕动泵分别以正加、反加或并流方式将溶液A和溶液B均匀混合，室温下发生反应，然后继续搅拌1-2天，得到凝胶溶液，离心分离得到沉淀产物，洗涤，干燥、焙烧，最后将得到的固体粉末样品经过气态粉磨处理，即得到粒度D50小于200nm、纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉材料。
3.根据权利要求2所述的纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉材料的制备方法，其特征在于，溶液A和溶液B形成的反应体系中不溶于水的含镁化合物前驱体的质量浓度是1-15wt％；含钙化合物前驱体的质量浓度为0.5-10％；不溶于水的含镁化合物前驱体前驱体与含钛氯化物的质量比为0.5-2.5：1；反应温度范围为0–40℃。
4.根据权利要求2所述的纯晶相纳米尺寸钛酸镁钙陶瓷粉的制备方法，其特征在于，所述的含镁化合物前驱体是不溶于水和有机醇的无机镁盐、有机酸镁盐或者含镁的氢氧化物类，例如碳酸镁、草酸镁、柠檬酸镁等；
所述的含钙化合物前驱体是无机钙盐、有机酸钙盐或者含钙的氢氧化物类，例如碳酸钙、草酸钙、柠檬酸钙、氯化钙、硝酸钙、氢氧化钙等；
所述的表面活性剂主要是非离子型的高分子聚合物；
所述的含钛氯化物主要是四氯化钛、氯氧化钛或者三氯化钛；
所述的有机醇为液态直链烷基醇或者其异构体醇；
所述的水为经过水净化处理得到的水，其中重金属离子、铁、钴、镍离子低于10ppm以下。
5.根据权利要求4所述的纯晶相纳米尺寸钛酸镁钙陶瓷粉的制备方法，其特征在于，所述的镁盐前驱体为碳酸镁、草酸镁、柠檬酸镁、酒石酸镁、亚硫酸镁、氢氧化镁中的一种或几种；
所述的钙盐前驱体为碳酸钙、草酸钙、柠檬酸钙、氯化钙、硝酸钙、氢氧化钙中的一种或几种；
所述的钛氯化物为四氯化钛、三氯化钛、氯氧化钛中的一种或几种一种或几种；
所述的表面活性剂为聚乙二醇、PVP、聚丙烯酸、聚醚、F127中的一种或几种；
所述的有机醇是乙醇、甲醇、丙醇、异丙醇、正丁醇、苯甲醇中的一种或几种。
6.根据权利要求2所述的纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉的制备方法，其特征在于，所述的溶液A和溶液B的盛放容器和反应容器为玻璃容器、有机塑料容器或陶瓷搪瓷容器，包括玻璃烧瓶、玻璃烧杯、表面皿、锥形瓶、广口瓶、称量瓶、试管、量杯、塑料烧杯、陶瓷反应釜、搪瓷反应釜、离心管中的一种或几种。
7.根据权利要求2所述的纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉的制备方法，其特征在于，步骤(3)中的离心分离的离心转速在4000-10000rpm，每次离心时间5-10min。
8.根据权利要求2所述的纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉的制备方法，其特征在于，步骤(3)中的洗涤选用的溶剂为水、甲醇、乙醇、异丙醇中的一种或几种。
9.根据权利要求2所述的纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉的制备方法，其特征在于，步骤(3)中的干燥处理选用的温度范围为70–120℃；焙烧处理选用的温度范围为700-1200℃，焙烧时间为3h-10h，焙烧采用空气气氛，需要空压机不断鼓入空气。
10.根据权利要求2所述的纯晶相高品质因数纳米尺寸钛酸镁钙陶瓷粉的制备方法，其特征在于，固体粉末样品经过气态粉磨处理所选用的设备为气流粉碎机，功率为5KW，经过旋风分离器收集粉末产品，空气压缩机功率为80KW，为粉碎提供10.0Mpa压缩空气。
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