CN116588976A - 一种锑酸锰粉体、其制备方法和应用 - Google Patents
一种锑酸锰粉体、其制备方法和应用 Download PDFInfo
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- 239000011572 manganese Substances 0.000 title claims abstract description 73
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 72
- 239000000843 powder Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 54
- 238000001035 drying Methods 0.000 claims abstract description 52
- 239000002904 solvent Substances 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 230000005496 eutectics Effects 0.000 claims abstract description 30
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 28
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims abstract description 21
- 235000019743 Choline chloride Nutrition 0.000 claims abstract description 21
- 229960003178 choline chloride Drugs 0.000 claims abstract description 21
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 20
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- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 10
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229940093474 manganese carbonate Drugs 0.000 claims abstract description 9
- 235000006748 manganese carbonate Nutrition 0.000 claims abstract description 9
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 9
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 9
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims abstract description 9
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
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- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 claims description 30
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
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- 229910010293 ceramic material Inorganic materials 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000002019 doping agent Substances 0.000 abstract description 3
- 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 2
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- 238000001816 cooling Methods 0.000 description 18
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- 238000011068 loading method Methods 0.000 description 7
- SNBDGFZQPKCZTO-UHFFFAOYSA-N propanedioic acid;hydrochloride Chemical compound Cl.OC(=O)CC(O)=O SNBDGFZQPKCZTO-UHFFFAOYSA-N 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- VYWQTJWGWLKBQA-UHFFFAOYSA-N [amino(hydroxy)methylidene]azanium;chloride Chemical compound Cl.NC(N)=O VYWQTJWGWLKBQA-UHFFFAOYSA-N 0.000 description 6
- AXJDEHNQPMZKOS-UHFFFAOYSA-N acetylazanium;chloride Chemical compound [Cl-].CC([NH3+])=O AXJDEHNQPMZKOS-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 229910000464 lead oxide Inorganic materials 0.000 description 3
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- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
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- 229910001928 zirconium oxide Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- OOBNORVQFIAGPT-UHFFFAOYSA-N antimony manganese Chemical compound [Mn].[Sb] OOBNORVQFIAGPT-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- 238000001000 micrograph Methods 0.000 description 2
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- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization 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
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
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- 239000003292 glue Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
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- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
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- 231100000053 low toxicity Toxicity 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
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- 238000010899 nucleation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
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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
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- 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
- C04B35/491—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 based on lead zirconates and lead titanates, e.g. PZT
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Abstract
本发明公开了一种锑酸锰粉体、其制备方法和应用,属于无机材料制备技术领域。本发明将摩尔比为1.8~2.2:1的锰源和锑源经球磨烘干后,按照氢键受体与锰源摩尔比0.5~1:1加入低共熔溶剂,混合均匀后烘干、粉碎,最后经过700‑800℃固相烧结、粉碎、洗涤和烘干,得到亚微米级纯相锑酸锰粉体;所述锰源为二氧化锰,碳酸锰,硝酸锰中的一种或几种,锑源为三氧化二锑、五氧化二锑中的一种或两种;所述低共熔溶剂是以氯化胆碱作为氢键受体,以丙二酸、尿素、乙酰胺中的一种作为氢键供体。本发明方法所制备的锑酸锰粉体,为标准的四方相晶体结构,粒度均匀、单分散性好,适合作为大功率压电陶瓷材料的掺杂物使用。
Description
技术领域
本发明属于无机材料制备技术领域,更具体地说,涉及一种锑酸锰粉体、其制备方法和应用。
背景技术
压电陶瓷作为结构简单,便于制作,小型化、高速度、低功耗、高可靠性的电子元器件,在现代光机电产品中占有十分重要的地位。随着电子器件越来越高的集成化,多功能化和功率化的要求,传统的压电陶瓷已不能满足现代产品的需求,而是对大功率压电陶瓷的需求越来越大,就大功率而言,往往要求陶瓷材料具备以下性能(1)优良的压电性能(2)材料在交变的环境温度或长期使用过程中性能稳定;(3)材料在谐振状态下能够承受大的电功率。因此提高压电陶瓷性能参数是开发大功率压电陶瓷材料的关键。为了寻求更高性能的压电陶瓷材料,通常在陶瓷原料中添加掺杂物来提高陶瓷材料的压电性能参数,以保证压电陶瓷片在大功率条件下能正常稳定的工作。本专利旨在提供一种掺杂物(锑酸锰)的制备方法。
在现有的技术资料中对亚微米级纯相锑酸锰制备方法的记录较少,中国专利文献CN 102139924 B公开了利用水热法合成锑酸锰的方法,但其中水合肼属于高毒类化学品,在实验过程中对人体有伤害,此外根据专利结果,使用该方法制备出的锑酸锰粉体结晶度不高,粒度不均匀,且粒径较大(10-20μm)(参见其说明书附图1-2),不适合用于大功率压电陶瓷材料的掺杂物使用。并且水热法在反应过程中对工艺要求较苛刻,对反应物有诸多限制,反应产物较多为多相混合物,难以分离,且过程中容易出现副反应造成实验结果不理想。
发明内容
针对现有技术存在的上述缺陷,本发明所要解决的技术问题在于提供一种亚微米级纯相锑酸锰粉体。本发明所要解决的另一技术问题在于提供前述锑酸锰粉体制备方法。本发明最后所要解决的技术问题在于提供前述锑酸锰粉体的具体应用,特别是在制备大功率型压电陶瓷中的应用。
为了解决上述技术问题,本发明所采用的技术方案如下:
一种锑酸锰粉体制备方法,具体包括如下步骤:
将锰源和锑源混合后,加入球磨助剂球磨、烘干,得到粉料,将粉料与低共熔溶剂混匀得到料浆,烘干料浆得到前驱体粉料,将前驱体粉料破碎后,经过高温烧结、离心洗涤和干燥,即得锑酸锰粉体。
在一些实施例中,所述锰源为二氧化锰、碳酸锰、硝酸锰中的一种,所述锑源为三氧化二锑或五氧化二锑。
在一些实施例中,所述锰源与锑源的摩尔比为1.8~2.2:1。
在一些实施例中,所述低共熔溶剂,以氯化胆碱作为氢键受体,以丙二酸、尿素、乙酰胺中的一种作为氢键供体,以水作为溶剂。
在一些实施例中,为达到最佳技术效果,所述低共熔溶剂中氢键受体与氢键供体摩尔比为:0.5~1.5。
优选地,所述的锑酸锰粉体制备方法,氢键受体与锰源摩尔比为0.5~1:1。
在一些实施例中,所述球磨过程中,锰源和锑源:球:球磨助剂的质量比为1:2~2.2:1,转速设置200-450r/min,球磨3-9h。
优选地,所述球磨助剂为无水乙醇。
优选地,为便于操作和达到最佳效果,将粉料与低共熔溶剂混匀过程中,控制料浆整体粘度为100-500mPa•s。
在一些实施例中,前驱体粉料破碎后过60目-100目网筛。
在一些实施例中,高温烧结具体条件为:置于密闭的高温烧结炉中,以3-5℃/min的升温速率达到700-800℃,保温2-4h。
任一所述的方法制备得到的产品。
所述的产品在制备压电陶瓷中的应用,具体地,是作为压电陶瓷材料的掺杂物使用。
优选地,所述的应用中,所述压电陶瓷为大功率型压电陶瓷。
相比于现有技术,本发明的有益效果为:
(1)本发明通过在制备锑酸锰的高温烧结过程中加入低共熔溶剂,提高反应物之间的扩散速率,减小晶胞畸变,控制生成的晶粒尺寸及形貌。并且能够有效降低反应温度,减少烧结时间,促进固相反应中生成物的结晶成核,提高生成物粉体的结晶度。反应结束后经高速离心后再水洗即可将杂质离子去除,保证生成粉料的纯度不受影响;
(2)本发明采用高能球磨与固相烧结相结合的方法,形成具有一定级配的亚微米级颗粒。与水热法相比该工艺路径短,条件易控制,生产效率高,且使用低毒性不挥发、易制备的新型绿色溶剂,高效环保,有利于工业化生产;
(3)根据x射线衍射分析出本发明制备的锑酸锰粉体为纯相晶体结构,根据晶胞参数值分析为标准的四方相结构,图像中衍射峰尖锐,表明该粉体的结晶度高。通过激光粒度仪测试,粉料基本为亚微米级粒群,呈单分散性,能均匀渗杂基体,保证压电陶瓷片的致密性,从而使压电陶瓷获得更优性能。
附图说明
图1为本发明实施例1中制备的锑酸锰粉体的xrd测试图;
图2为本发明实施例1中制备的锑酸锰粉体的扫描电镜图;
图3为本发明实施例1中制备的锑酸锰粉体的粒度分布数据图;
图4为本发明对照组1中制备的含有较多杂相的锑酸锰粉体xrd测试图;
图5为本发明对照组1中制备的粒度分布不均的锑酸锰粉体扫描电镜图;
图6为本发明对照组1中制备的粒度分布不均的锑酸锰粉体粒度分布图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面结合具体实施例对本发明进一步进行描述。以下实施例中如无特殊说明,所用的技术手段均为本领域技术人员所熟知的常规手段。以下所述比例均为摩尔比,特殊情况另有说明,使用的药品纯度均不低于化学纯。以下实施例中使用的球磨设备可为立式行星球磨机,可采用玛瑙球,氧化铝球,钢球或氧化锆球进行球磨,例如,将直径为3mm、5mm、10mm的三种氧化锆球以(2-4):(3-6):(1-3)重量配比进行球磨。
实施例1:将1mol五氧化二锑与2mol二氧化锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置260r/min,球磨8h过滤烘干,与氯化胆碱-丙二酸(1:1)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为2mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以3℃/min的速率升温至700℃,保温4h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,结果如图1-3所示,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例2:将1mol三氧化二锑与2mol碳酸锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置320r/min,球磨6h过滤烘干,与氯化胆碱-尿素(1.5:1)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1mol),烘干,装入密闭的坩埚送入箱式高温烧结炉中,以4℃/min的速率升温至800℃,保温2h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例3:将1mol五氧化二锑与2mol硝酸锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置400r/min,球磨4h过滤烘干,与氯化胆碱-乙酰胺(1:1.5)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.5mol),烘干,装入密闭的坩埚送入箱式高温烧结炉中,以5℃/min的速率升温至780℃,保温2.5h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例4:将1mol五氧化二锑与1.8mol碳酸锰的摩尔比混合,按照料:球:酒精=1:2.1:1的比例置于球磨罐中,转速设置280r/min,球磨8h过滤烘干,与氯化胆碱-乙酰胺(1:2)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.5mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以3℃/min的速率升温至750℃,保温3.5h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例5:将1mol三氧化二锑与1.8mol二氧化锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置350r/min,球磨6h过滤烘干,与氯化胆碱-尿素(1:1)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1mol),烘干,装入密闭的坩埚送入箱式高温烧结炉中,以4℃/min的速率升温至720℃,保温4h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例6:将1mol三氧化二锑与1.8mol硝酸锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置450r/min,球磨3h过滤烘干,与氯化胆碱-丙二酸(1:2)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.8mol),烘干,装入密闭的坩埚送入箱式高温烧结炉中,以5℃/min的速率升温至800℃,保温3h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例7:将1mol五氧化二锑与1.9mol二氧化锰的摩尔比混合,按照料:球:酒精=1:2.2:1的比例置于球磨罐中,转速设置350r/min,球磨5h过滤烘干,与氯化胆碱-尿素(1:1.5)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.9mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以3℃/min的速率升温至720℃,保温4h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例8:将1mol五氧化二锑与1.9mol碳酸锰的摩尔比混合,按照料:球:酒精=1:2.1:1的比例置于球磨罐中,转速设置400r/min,球磨4h过滤烘干,与氯化胆碱-乙酰胺(1:1.2)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.6mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以3℃/min的速率升温至750℃,保温3.5h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例9:将1mol三氧化二锑与1.9mol二氧化锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置350r/min,球磨4h过滤烘干,与氯化胆碱-丙二酸(1.5:1)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.2mol),烘干,装入密闭的坩埚送入箱式高温烧结炉中,以5℃/min的速率升温至800℃,保温3h,冷却后将其粉碎,离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例10:将1mol五氧化二锑与2.1mol硝酸锰的摩尔比混合,按照料:球:酒精=1:2.2:1的比例置于球磨罐中,转速设置400r/min,球磨4h过滤烘干,与氯化胆碱-丙二酸(1:1.5)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.6mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以4℃/min的速率升温至780℃,保温2.5h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例11:将1mol五氧化二锑与2.1mol二氧化锰的摩尔比混合,按照料:球:酒精=1:2.1:1的比例置于球磨罐中,转速设置350r/min,球磨5h过滤烘干,与氯化胆碱-尿素(1:2)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.2mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以4℃/min的速率升温至720℃,保温4h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例12:将1mol三氧化二锑与2.1mol碳酸锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置300r/min,球磨6h过滤烘干,与氯化胆碱-乙酰胺(1.5:1)的低共熔溶剂加去离子水搅拌均匀(其中氯化胆碱为1.8mol),烘干,装入密闭的坩埚送入箱式高温烧结炉中,以5℃/min的速率升温至800℃,保温3h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例13:将1mol五氧化二锑与2.2mol二氧化锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置320r/min,球磨5h过滤烘干,与氯化胆碱-丙二酸(1:1.2)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为2.2mol),烘干,装入密闭的坩埚中送入箱式高温烧结炉中,以3℃/min的速率升温至800℃,保温2.5h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例14:将1mol三氧化二锑与2.2mol二氧化锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置250r/min,球磨9h过滤烘干,与氯化胆碱-乙酰胺(1:1)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.5mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以3℃/min的速率升温至800℃,保温3h,冷却后心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
实施例15:将1mol五氧化二锑与2.2mol硝酸锰的摩尔比混合,按照料:球:酒精=1:2.2:1的比例置于球磨罐中,转速设置420r/min,球磨3h过滤烘干,与氯化胆碱-尿素(1:1.2)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.1mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以5℃/min的速率升温至780℃,保温3h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实施例得到了亚微米级纯相锑酸锰粉体。
对照组1:将1mol五氧化二锑与2mol二氧化锰的摩尔比混合,按照料:球:酒精=1:2:1的比例置于球磨罐中,转速设置350r/min,球磨5h过滤烘干,装入密闭的坩埚送入箱式高温烧结炉,以3℃/min的速率升温至800℃,保温3h,冷却后将其粉碎,离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,结果如图4-6所示,表明本实验得到有较多杂相的锑酸锰粉体。
对照组2:将1mol三氧化二锑与1.7mol硝酸锰的摩尔比混合,按照料:球:酒精=1:1.9:1的比例置于球磨罐中,转速设置400r/min,球磨4h过滤烘干,与氯化胆碱-丙二酸(1:1)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为1.5mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以3℃/min的速率升温至700℃,保温4h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实验得到有较多杂相且粒度分布不均的锑酸锰粉体。
对照组3:将1mol五氧化二锑与2.3mol二氧化锰的摩尔比混合,按照料:球:酒精=1:1.9:1的比例置于球磨罐中,转速设置450r/min,球磨2.5h过滤烘干,与氯化胆碱-尿素(1:1)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为2mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以3℃/min的速率升温至750℃,保温4h,冷却后离心洗涤,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实验得到有较多杂相且粒度分布不均的锑酸锰粉体。
对照组4:将1mol三氧化二锑与2.1mol碳酸锰的摩尔比混合,按照料:球:酒精=1:1.9:1的比例置于球磨罐中,转速设置400r/min,球磨3.5h过滤烘干,与氯化胆碱-丙二酸(2:1)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为2mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以3℃/min的速率升温至650℃,保温4h,冷却离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实验得到有较多杂相且粒度分布不均的锑酸锰粉体。
对照组5:将1mol五氧化二锑与2mol二氧化锰的摩尔比混合,按照料:球:酒精=1:2.3:1的比例置于球磨罐中,转速设置280r/min,球磨8h过滤烘干,与氯化胆碱-乙酰胺(1.5:1)的低共熔溶剂混合搅拌均匀(其中氯化胆碱为2.2mol),烘干,装入密闭的坩埚送入箱式高温烧结炉,以4℃/min的速率升温至700℃,保温3h,冷却后离心洗涤,在80℃下干燥后,经过xrd测试、扫描电镜观察和粒度分布测试,表明本实验得到有较多杂相且粒度分布不均的锑酸锰粉体。
实施例16:亚微米级纯相锑酸锰在压电陶瓷制备中的应用
将上述实施例1-15中制备好的亚微米级纯相锑酸锰与氧化铅,氧化锆和二氧化钛根据化学式Pb(Mn1/3Sb2/3)x(Zr0.47Ti0.48)(1-x)/0.95O3按照x=0.01-0.10化学计量比称量混合后置于球磨罐中,混料烘干,按照固相合成法制备合成陶瓷粉,造粒压制陶瓷坯片,然后排胶烧结研磨处理,得到标准陶瓷测试片(φ12*1mm),烧银极化,于室温静置24h后测试性能:d33=340-360pC/N,εr=1550-1650,tanδ=0.2-0.3%,Qm=1200,具体见表1。
对照组6:将二氧化锰(或碳酸锰、硝酸锰)和三氧化二锑(或五氧化二锑)与氧化铅,氧化锆和二氧化钛按照与实施例16相同的计量比和制备方法得到锰锑掺杂的压电陶瓷,于室温静置 24h 后使用与实施例16同样方法测试性能:d33=310-350pC/N,εr=1400-1600,tanδ=0.3-0.5%,Qm=1000,与实施例16相比,采用传统的氧化物混合方法掺杂会导致压电性能降低,机械品质因数降低,具体见表1,该结果表明对照组6不能很好应用于大功率型压电陶瓷。
对照组7:将上述对照组1-5中制备的粒径较大且尺寸不均一的纯相锑酸锰与氧化铅,氧化锆和二氧化钛按照与实施例16相同的计量比和制备方法得到锰锑掺杂的压电陶瓷,于室温静置24h后使用与实施例16同样方法测试性能:d33=320-340pC/N,εr=1300-1500,tanδ=0.4-0.6%,Qm=900,与实施例相比,使用粒径较大且尺寸不均一的纯相锑酸锰进行掺杂会导致压电性能降低,机械品质因数降低,具体见表1,该结果表明对照组7不能很好应用于大功率型压电陶瓷。
表1 压电陶瓷性能测试结果
申请人声明,以上所述仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,所属技术领域的技术人员应该明了,任何属于本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,均落在本发明的保护范围和公开范围之内。
Claims (14)
1.一种锑酸锰粉体制备方法,其特征在于,具体包括如下步骤:
将锰源和锑源混合后,加入球磨助剂球磨、烘干,得到粉料,将粉料与低共熔溶剂混匀得到料浆,烘干料浆得到前驱体粉料,将前驱体粉料破碎后,经过高温烧结、离心洗涤和干燥,即得锑酸锰粉体。
2.根据权利要求1所述的锑酸锰粉体制备方法,其特征在于,所述锰源为二氧化锰、碳酸锰、硝酸锰中的一种,所述锑源为三氧化二锑或五氧化二锑。
3.根据权利要求1所述的锑酸锰粉体制备方法,其特征在于,所述锰源与锑源的摩尔比为1.8~2.2:1。
4.根据权利要求1所述的锑酸锰粉体制备方法,其特征在于,所述低共熔溶剂,以氯化胆碱作为氢键受体,以丙二酸、尿素、乙酰胺中的一种作为氢键供体,以水作为溶剂。
5.根据权利要求4所述的锑酸锰粉体制备方法,其特征在于,所述低共熔溶剂中氢键受体与氢键供体摩尔比为0.5~1.5:1。
6.根据权利要求5所述的锑酸锰粉体制备方法,其特征在于,所述氢键受体与锰源摩尔比为0.5~1:1。
7.根据权利要求1所述的锑酸锰粉体制备方法,其特征在于,所述锰源和锑源:球:球磨助剂的质量比为1:2~2.2:1,转速设置200-450r/min,球磨3-9h。
8.根据权利要求7所述的锑酸锰粉体制备方法,其特征在于,所述球磨助剂为无水乙醇。
9.根据权利要求1所述的锑酸锰粉体制备方法,其特征在于,将粉料与低共熔溶剂混匀过程中,控制料浆整体粘度为100-500mPa·s。
10.根据权利要求1所述的锑酸锰粉体制备方法,其特征在于,前驱体粉料破碎后再过60目-100目网筛。
11.根据权利要求1所述的锑酸锰粉体制备方法,其特征在于,高温烧结具体条件为:置于密闭的高温烧结炉中,以3-5℃/min的升温速率达到700-800℃,保温2-4h。
12.权利要求1-11任一所述的方法制备得到的产品。
13.权利要求12所述的产品在制备压电陶瓷中的应用。
14.根据权利要求13所述的应用,其特征在于,所述压电陶瓷为大功率型压电陶瓷。
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