CN113121222A - 一种钛酸钡粉体制备方法 - Google Patents
一种钛酸钡粉体制备方法 Download PDFInfo
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- CN113121222A CN113121222A CN202110361043.2A CN202110361043A CN113121222A CN 113121222 A CN113121222 A CN 113121222A CN 202110361043 A CN202110361043 A CN 202110361043A CN 113121222 A CN113121222 A CN 113121222A
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- barium
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- barium titanate
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- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 63
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000000843 powder Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000010936 titanium Substances 0.000 claims abstract description 50
- 238000002485 combustion reaction Methods 0.000 claims abstract description 44
- 239000002245 particle Substances 0.000 claims abstract description 39
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 33
- 229910052788 barium Inorganic materials 0.000 claims abstract description 31
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 239000011812 mixed powder Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 239000004576 sand Substances 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000011268 mixed slurry Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000001694 spray drying Methods 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 23
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 8
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-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
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003985 ceramic capacitor Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 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 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229920001817 Agar Polymers 0.000 claims description 2
- 229920000936 Agarose Polymers 0.000 claims description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 239000008272 agar Substances 0.000 claims description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 2
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 2
- 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 2
- 239000003989 dielectric material Substances 0.000 claims description 2
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 claims description 2
- 229960001826 dimethylphthalate Drugs 0.000 claims description 2
- OPGYRRGJRBEUFK-UHFFFAOYSA-L disodium;diacetate Chemical compound [Na+].[Na+].CC([O-])=O.CC([O-])=O OPGYRRGJRBEUFK-UHFFFAOYSA-L 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 2
- -1 polypropylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 235000017454 sodium diacetate Nutrition 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- 235000021317 phosphate Nutrition 0.000 claims 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims 1
- 229920000642 polymer Polymers 0.000 abstract description 8
- 239000012071 phase Substances 0.000 abstract description 6
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 abstract description 5
- 238000003746 solid phase reaction Methods 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 10
- 230000007547 defect Effects 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 238000003837 high-temperature calcination Methods 0.000 description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910001422 barium ion Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229910003080 TiO4 Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000010835 comparative analysis Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- BEGBSFPALGFMJI-UHFFFAOYSA-N ethene;sodium Chemical group [Na].C=C BEGBSFPALGFMJI-UHFFFAOYSA-N 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
本发明涉及一种钛酸钡粉体制备方法,具体地,其包括以下步骤:1)采用钛源与钡源作为反应原料,将其分别进行砂磨预处理,直至钛源与钡源的平均粒径均达到200nm以下,且钛源与钡源中钛与钡的摩尔比在1:0.95‑1.05之间;然后进行混合砂磨;获得混合原料;2)将步骤1)中处理好的钛源与钡源混合,向混合原料中添加溶剂、分散剂以及助燃剂;混合均匀获得混合浆料;对上述混合浆料进行砂磨与喷雾干燥,获得混合粉体;3)对步骤2)获得的混合粉体进行高温煅烧,获得钛酸钡粉体。本发明基于固相反应原理和高分子聚合物分解包覆,使得钛酸钡粉体产物的粒径更小更均匀,且四方相比例更高。
Description
技术领域
本发明属于材料化学领域,具体涉及一种钛酸钡粉体制备方法。
背景技术
钛酸钡由于具有相对较高的室温介电常数、相对较高的居里温度及不含引起严重环境污染的重金属元素,是当前制备X7R、X8R等系列多层陶瓷电容器(MLCC)的最佳原料。当前,MLCC器件的小型化制备要求钛酸钡粉体粒径进在一步降低的同时,还要具有相对较高的四方度。
传统的水热法是在高压反应釜中,可溶性钡源与钛源在碱性溶液中经高压反应合成钛酸钡。尽管通过水热法能够比较容易地制备出纳米及亚微米级、高四方相钛酸钡粉体,但是水热反应机制不可避免的在钛酸钡中引入较多羟基及质子缺陷,从而在MLCC中诱导较多的氧空位缺陷及载流子,导致器件老化性能显著降低。
传统的固相法是将碳酸钡与二氧化钛的混合粉体在马弗炉中经高温煅烧获得。相比而言,通过固相反应、经高温煅烧制备的钛酸钡粉体,具有相对较高结晶度,无羟基缺陷,能够显著降低MLCC中氧空位诱导的漏电流。同时,相比水热制备方法,固相法合成钛酸钡具有设备要求低、生产安全性高、生产成本低等优点。然而,由于粉体堆积引起受热不均,以及钛酸钡晶粒经过长时间升温及高温煅烧,导致晶粒粒径显著增大、粒径分布较宽及晶粒团聚,影响其在微型MLCC中的应用。这也是当前钛酸钡固相法制备工艺中亟需解决的问题。
发明内容
为了解决上述固相法制备钛酸钡粉体粒径过大的问题,获得高四方相、小粒径、缺陷少的钛酸钡粉体,本发明一个方面提供了一种钛酸钡粉体的制备方法,包括以下步骤:
1)采用钛源与钡源作为反应原料,将其分别进行砂磨预处理,直至钛源与钡源的平均粒径均达到200nm以下,且钛源与钡源的Ba/Ti摩尔比在1:0.95-1.05之间;然后将处理好的钛源与钡源混合,并进行砂磨处理,获得混合原料;
2)向步骤1)获得的混合原料中添加溶剂、分散剂以及助燃剂;混合均匀获得混合浆料;对上述混合浆料进行砂磨与喷雾干燥,直至混合粉体比表面积为5-50m2/g;
3)对步骤2)获得的混合粉体进行高温煅烧,获得钛酸钡粉体,其中,煅烧温度为1000-1060度,保温时间为60-180分钟。
在本发明的技术方案中,步骤1)中所述的钛源选自二氧化钛、氢氧化钛。
在本发明的技术方案中,步骤1)中所述的钡源选自碳酸钡、氧化钡、氢氧化钡。
在本发明的技术方案中,步骤1)中钛源和钡源中钛与钡的摩尔比为1:0.993-1.0045。
在本发明的技术方案中,步骤1)中所述的钛源与钡源的纯度为98%以上,经过砂磨预处理的钛源与钡源的平均粒径不大于200nm。
进一步地,经过砂磨预处理的钛源与钡源的平均粒径分别为80-120nm。例如为90nm、100nm、110nm、120nm。
在本发明的技术方案中,步骤2)中使用的溶剂为水或有机溶剂,优选地,有机溶剂选自无水乙醇、甲苯、甲基乙基酮、醋酸乙酯。
在本发明的技术方案中,步骤2)中使用的分散剂选自六偏磷酸钠、硅酸钠、碳酸钠、柠檬酸钠、乙二胺四乙酸钠、二乙酸钠。
在本发明的技术方案中,步骤2)中分散剂的用量为0.01wt%-0.1wt%。例如为0.02wt%、0.03wt%、0.04wt%、0.05wt%、0.06wt%、0.07wt%、0.08wt%、0.09wt%、0.1wt%。
在本发明的技术方案中,步骤2)中所述的助燃剂为聚乙二醇、聚乙烯醇、聚丙烯、聚苯乙烯、聚乙酸乙酯、聚甲基丙烯酸甲酯、硬脂酸、油酸、邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、琼脂、琼脂糖、甲基纤维素、硅酸钠溶液中的一种或多种组合。
在本发明的技术方案中,步骤2)中助燃剂的添加量为钛源含量的1wt%-10wt%,优选为1wt%-6wt%。例如为2wt%、3wt%、4wt%、5wt%。
在本发明的技术方案中,所述的混合粉体为经过砂磨均匀混合分散并经喷雾干燥的由钛源、钡源、分散剂、助燃剂组成的混合粉体,混合粉体中钡和钛的摩尔比为1:0.993-1.0045。
在本发明的技术方案中,所述的混合粉体比表面积为8-15m2/g,优选9-11m2/g,更优选为10m2/g。
在本发明的技术方案中,所述的高温煅烧升温速率为5-20度/分钟,煅烧温度为1030-1060度,保温时间为100-150分钟,对混合粉体进行热处理的方式。
本发明另一个方面提供了由上述方法制备的获得钛酸钡粉体。
在本发明的技术方案中,所述的钛酸钡粉体平均粒径为90-220nm、晶格参数c/a比为1.009以上、Ba/Ti离子摩尔比为0.992-1.006。
在一些具体的实施例中,所述的钛酸钡粉体的平均粒径为100nm、110nm、120nm、130nm、140nm、150nm、160nm、170nm、180nm、190nm、200nm、210nm或他们之间的任意数值。
在一些具体的实施例中,,所述的钛酸钡粉体的晶格参数c/a比为1.0090、1.0091、1.0092、1.0093、1.0094、1.0095、1.0096、1.0097、1.0098、1.0099、1.0091、1.010。
本发明另一个方面提供了本发明的钛酸钡粉体作为介电材料的用途。
优选地,钛酸钡粉体用于制备电子元器件的用途,更优选地,电子元器件为多层陶瓷电容器。
有益效果
本发明基于固相反应原理和高分子聚合物分解包覆,先令钛源、钡源及高分子聚合物均匀混合。在砂磨过程中,介质球相互摩擦进一步降低钛源与钡源颗粒粒径,其颗粒表面存在大量氧空位缺陷。基于离子-偶极子相互作用,钛源与钡源颗粒表面的Ti离子与Ba离子均吸附较多羟基。同时,在砂磨作用下,高分子聚合物通过分子内氢键及分子间电子转移与颗粒表面Ti离子、Ba离子相邻的羟基相连,从而使得Ti源与Ba源颗粒表面均匀包覆高分子聚合物,避免Ba2TiO4、BaTi2O5、Ba6Ti17O40等中间相的产生,进一步促进四方相BaTiO3的生成。
该制备方法完全基于钛酸钡的固相反应机制,不引入羟基或质子缺陷。相比于水热法制备钛酸钡粉体,本发明制备的钛酸钡粉体能够显著提升MLCC器件的老化特性。
本发明相比传统TiO2与BaCO3混合煅烧制备钛酸钡方案,通过添加助燃剂、进行砂磨及喷雾干燥能够在粉体颗粒外形成高分子聚合物包覆壳层,避免粉体烘干过程中的团聚及结块;避免产生Ba2TiO4、BaTi2O5、Ba6Ti17O40等中间产物,所以本发明获得的钛酸钡具有更高的四方度。
本发明采用了更低的煅烧温度,能够控制晶粒粒径生长,所以本发明获得的钛酸钡具有更小粒径。
附图说明
通过结合附图进行的以下描述,本发明的实施例的上述和其它方面、特点和优点将变得更加清楚,附图中:
图1为根据实施例6合成的钛酸钡粉体的X射线衍射(XRD)图谱。
图2为根据实施例6合成的钛酸钡粉体的扫描电子显微镜(SEM)图片。
具体实施方式
为了使本发明的上述目的、特征和优点能够更加明显易懂,下面对本发明的具体实施方式做详细的说明,但不能理解为对本发明的可实施范围的限定。
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图,详细描述本发明实施例中的技术方案。显然,所描述的实施例仅是本发明的一部分实施例,而不是全部的实施例。本领域技术人员可以在不违背本发明内涵的情况下做类似的改进,因此本发明不受下面公开的具体实施例的限制。
考虑到现有商用固相法制备钛酸钡粉体粒径难以进一步降低的问题,本发明提供了一种钛酸钡粉体制备方法。具有以下优势:
在砂磨过程中,介质球相互摩擦进一步降低Ti源与Ba源颗粒粒径,其颗粒表面存在大量氧空位缺陷。基于离子-偶极子相互作用,Ti源与Ba源颗粒表面的Ti离子与Ba离子均吸附较多羟基。同时,在砂磨作用下,助燃剂中的高分子聚合物通过分子内氢键及分子间电子转移与颗粒表面Ti离子、Ba离子相邻的羟基相连,从而使得Ti源与Ba源颗粒表面均匀包覆高分子聚合物,避免Ba2TiO4、BaTi2O5、Ba6Ti17O40等中间相的产生,进一步促进煅烧过程中四方相BaTiO3的生成。
实施例1制备钛酸钡粉体
该钛酸钡粉体制备方法,包括以下步骤:
1)采用TiO2与BaCO3作为反应原料,对其分别进行砂磨预处理。通过激光粒度分析仪测试,获得经砂磨处理的TiO2与BaCO3的平均粒径(d50)分别为95nm与110nm。由于TiO2与BaCO3原料粉体通常达到亚微米或微米级别,需要对TiO2与BaCO3原料进行多级砂磨或球磨处理,使其粒径降至100nm左右。通过分别调节TiO2与BaCO3原料的砂磨时间,使得TiO2与BaCO3粉体平均粒径相近,从而有利于下一步提升粉体混合均匀度。将经过砂磨处理的TiO2与BaCO3混合,二者的摩尔比为1:1,并进行砂磨处理,获得混合原料;
2)取100g步骤1)所得混合原料,向其中添加溶剂无水乙醇100g,分散剂六偏磷酸钠1g,不添加助燃剂,进行砂磨混合获得混合浆料。
3)对第2)步获得的混合浆料,进行喷雾干燥获得混合粉体,混合粉体的比表面积为10m2/g。对混合粉体进行高温煅烧,获得钛酸钡粉体。所述的高温煅烧工艺为,利用马弗炉,设置升温速率为5-20℃/分钟,煅烧温度为1030℃,保温时间为120分钟,对混合粉体进行热处理的方式。
实施例2
实施例2采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的2wt%。
实施例3
实施例3采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的4wt%。
实施例4
实施例4采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的6wt%。
实施例5
实施例5采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的8wt%。
实施例6
实施例6采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的10wt%。
实施例7
实施例7采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的12wt%。
实施例8采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的6wt%,且步骤3)中的煅烧温度为970℃,保温时间为120分钟。
实施例9采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的6wt%,且步骤3)中的煅烧温度为1000℃,保温时间为120分钟。
实施例10采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的6wt%,且步骤3)中的煅烧温度为1060℃,保温时间为120分钟。
实施例11采用与实施例1相同的方法,区别仅在于在步骤2)中还添加了助燃剂,助燃剂为聚乙烯醇,助燃剂的添加量为TiO2含量的6wt%,且步骤3)中的煅烧温度为1080℃,保温时间为120分钟。
对方钛酸钡粉体检测
分别对上述所述的钛酸钡粉体进行平均粒径的检测、计算晶格参数c/a、Ba/Ti离子摩尔比。并对所得的钛酸钡粉体的进行X射线衍射(XRD)检测和扫描电子显微镜(SEM)观察。实验结果见表1-2以及图1-2。
实施例1-11制备的钛酸钡粉体,可实现平均粒径为100-270nm,晶格参数c/a比为1.009以上,产物钛酸钡粉体Ba/Ti离子摩尔比为0.992-1.006。
为了验证助燃剂的添加效果,选择经过砂磨处理、纯度均为99%的钛酸钡(100nm)与二氧化钛(100nm)的作为原料,对其进行砂磨混合处理,并按照表1开展实施例。实施例1-7为验证添加不同含量助燃剂对煅烧钛酸钡粉体的影响;实施例6、8-11为验证不同煅烧温度对煅烧钛酸钡粉体的影响。
对比分析实施例1-7结果可知,针对粉体试样,有效的助燃剂添加量为2-10wt%;对比分析实施例4、7-11可知,针对粉体试样,合适的煅烧温度为1000-1060度。
虽然已经参照特定实施例示出并描述了本发明,但是本领域的技术人员将理解:在不脱离由权利要求及其等同物限定的本发明的精神和范围的情况下,可在此进行形式和细节上的各种变化。
表1实施例1-6具体参数及产物钛酸钡粉体性能
表2实施例1-6产物钛酸钡粉体性能
Claims (10)
1.一种钛酸钡粉体的制备方法,其特征在于,其包括以下步骤:
1)采用钛源与钡源作为反应原料,将其分别进行砂磨预处理,直至钛源与钡源的平均粒径均达到200nm以下,且钛源与钡源的Ba/Ti摩尔比在1:0.95-1.05之间;然后将处理好的钛源与钡源混合,并进行砂磨处理,获得混合原料;
2)向步骤1)获得的混合原料中添加溶剂、分散剂以及助燃剂;混合均匀获得混合浆料;对上述混合浆料进行砂磨与喷雾干燥,直至混合粉体比表面积为5-50m2/g;
3)对步骤2)获得的混合粉体进行高温煅烧,获得钛酸钡粉体,其中,煅烧温度为1000-1060度,保温时间为60-180分钟;
优选地,步骤1)中所述的钛源选自二氧化钛、氢氧化钛;
优选地,步骤1)中所述的钡源选自碳酸钡、氧化钡、氢氧化钡。
2.根据权利要求1所述的钛酸钡粉体的制备方法,其特征在于,步骤1)中钛源和钡源中钛与钡的摩尔比为1:0.993-1.0045。
3.根据权利要求1所述的钛酸钡粉体的制备方法,其特征在于,步骤1)中所述的钛源与钡源的纯度为98%以上,经过砂磨预处理的钛源与钡源的平均粒径不大于200nm。
4.根据权利要求1所述的钛酸钡粉体的制备方法,其特征在于,经过砂磨预处理的钛源与钡源的平均粒径分别为80-120nm。
5.根据权利要求1所述的钛酸钡粉体的制备方法,其特征在于,步骤2)中使用的分散剂选自磷酸盐,优选为六偏磷酸钠、硅酸钠、碳酸钠、柠檬酸钠、乙二胺四乙酸钠、二乙酸钠;
优选地,步骤2)中分散剂的用量为0.01-0.1wt%。
6.根据权利要求1所述的钛酸钡粉体的制备方法,其特征在于,步骤2)中使用的溶剂为水或有机溶剂,优选地,有机溶剂选自无水乙醇、甲苯、甲基乙基酮、醋酸乙酯。
7.根据权利要求1所述的钛酸钡粉体的制备方法,其特征在于,步骤2)中所述的助燃剂为聚乙二醇、聚乙烯醇、聚丙烯、聚苯乙烯、聚乙酸乙酯、聚甲基丙烯酸甲酯、硬脂酸、油酸、邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、琼脂、琼脂糖、甲基纤维素、硅酸钠溶液中的一种或多种组合;
优选地,步骤2)中助燃剂的添加量为钛源含量的1-10wt%,更优选为1-6wt%。
8.根据权利要求1所述的钛酸钡粉体的制备方法,其特征在于,所述的高温煅烧升温速率为5-20度/分钟,煅烧温度为1030-1060度,保温时间为100-150分钟,对混合粉体进行热处理的方式。
9.根据权利要求1-8任一项所述的制备方法获得的钛酸钡粉体;
优选地,所述的钛酸钡粉体平均粒径为90-220nm、晶格参数c/a比为1.009以上、Ba/Ti离子摩尔比为0.992-1.006。
10.根据权利要求9所述的钛酸钡粉体作为介电材料的用途;
优选地,钛酸钡粉体用于制备电子元器件的用途,更优选地,电子元器件为多层陶瓷电容器。
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116639972A (zh) * | 2023-05-29 | 2023-08-25 | 重庆新申世纪新材料科技有限公司 | 一种四方相纳米钛酸钡粉体及其制备方法和应用 |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1130004A1 (en) * | 2000-03-02 | 2001-09-05 | Murata Manufacturing Co., Ltd. | Oxide having perovskite structure, barium titanate, and manufacturing method therefor, dielectric ceramic, and ceramic electronic component |
CN1841588A (zh) * | 2005-03-29 | 2006-10-04 | 三星电机株式会社 | 介电陶瓷粉末的制造方法及多层陶瓷电容器 |
CN105967227A (zh) * | 2016-05-10 | 2016-09-28 | 湖北天瓷电子材料有限公司 | 一种高分子交联网络辅助的钛酸钡固相合成法 |
CN107555987A (zh) * | 2017-09-07 | 2018-01-09 | 安徽中创电子信息材料有限公司 | 一种亚微米级钛酸钡粉体超细微颗粒制备方法 |
CN108217720A (zh) * | 2016-12-15 | 2018-06-29 | 南方科技大学 | 片式多层陶瓷电容器用钛酸钡纳米晶的制备方法 |
CN109796042A (zh) * | 2019-03-11 | 2019-05-24 | 湖北天瓷电子材料有限公司 | 一种加胶制备固相法钛酸钡方法 |
CN111099892A (zh) * | 2020-01-03 | 2020-05-05 | 山东国瓷功能材料股份有限公司 | 一种钛酸钡基两相复合微波介质陶瓷材料及其制备方法 |
-
2021
- 2021-04-02 CN CN202110361043.2A patent/CN113121222A/zh active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1130004A1 (en) * | 2000-03-02 | 2001-09-05 | Murata Manufacturing Co., Ltd. | Oxide having perovskite structure, barium titanate, and manufacturing method therefor, dielectric ceramic, and ceramic electronic component |
CN1841588A (zh) * | 2005-03-29 | 2006-10-04 | 三星电机株式会社 | 介电陶瓷粉末的制造方法及多层陶瓷电容器 |
CN105967227A (zh) * | 2016-05-10 | 2016-09-28 | 湖北天瓷电子材料有限公司 | 一种高分子交联网络辅助的钛酸钡固相合成法 |
CN108217720A (zh) * | 2016-12-15 | 2018-06-29 | 南方科技大学 | 片式多层陶瓷电容器用钛酸钡纳米晶的制备方法 |
CN107555987A (zh) * | 2017-09-07 | 2018-01-09 | 安徽中创电子信息材料有限公司 | 一种亚微米级钛酸钡粉体超细微颗粒制备方法 |
CN109796042A (zh) * | 2019-03-11 | 2019-05-24 | 湖北天瓷电子材料有限公司 | 一种加胶制备固相法钛酸钡方法 |
CN111099892A (zh) * | 2020-01-03 | 2020-05-05 | 山东国瓷功能材料股份有限公司 | 一种钛酸钡基两相复合微波介质陶瓷材料及其制备方法 |
Non-Patent Citations (1)
Title |
---|
赵丽华等: "《分散剂对钛酸钡介电性能的影响》", 《绝缘材料》, no. 1, 20 February 2005 (2005-02-20), pages 24 - 26 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116639972A (zh) * | 2023-05-29 | 2023-08-25 | 重庆新申世纪新材料科技有限公司 | 一种四方相纳米钛酸钡粉体及其制备方法和应用 |
CN116639972B (zh) * | 2023-05-29 | 2024-03-19 | 重庆新申世纪新材料科技有限公司 | 一种四方相纳米钛酸钡粉体及其制备方法和应用 |
CN116639972B9 (zh) * | 2023-05-29 | 2024-04-05 | 重庆新申世纪新材料科技有限公司 | 一种四方相纳米钛酸钡粉体及其制备方法和应用 |
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