WO2019051737A1 - 一种高纯纳米二氧化锡球形粉末的制备方法 - Google Patents

一种高纯纳米二氧化锡球形粉末的制备方法 Download PDF

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Publication number
WO2019051737A1
WO2019051737A1 PCT/CN2017/101794 CN2017101794W WO2019051737A1 WO 2019051737 A1 WO2019051737 A1 WO 2019051737A1 CN 2017101794 W CN2017101794 W CN 2017101794W WO 2019051737 A1 WO2019051737 A1 WO 2019051737A1
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Prior art keywords
purity
spherical powder
tin dioxide
parts
tin
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PCT/CN2017/101794
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English (en)
French (fr)
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孟永辉
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孟永辉
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Publication of WO2019051737A1 publication Critical patent/WO2019051737A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G15/00—Compounds of gallium, indium or thallium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/02—Oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides

Definitions

  • the invention relates to a preparation method of a high-purity nano-tin dioxide spherical powder.
  • Optical, electrical and catalytic properties are widely used in luminescent materials, light absorbing materials, catalyst materials, gas sensing materials, dilute magnetic semiconductor materials, lithium ion battery anode materials and other fields.
  • tin dioxide is also one of the main components of ITO film, which is a heavily doped, high-degenerate n-type semiconductor oxide film due to its low resistivity, high visible light transmittance, and high infrared reflectance. It has the advantages of strong bonding with glass matrix, scratch resistance and good chemical stability. It has been widely used in many fields such as flat panel displays, solar cells, automobile windshields and electronic shielding.
  • the preparation methods of the nano-SnO 2 mainly include a microemulsion method, a vacuum evaporation coacervation method, a hydrothermal synthesis method, a chemical precipitation method, an electrospinning method, a sol-gel method, an oxidation method, and the like.
  • a method for preparing a high-purity nano-tin dioxide spherical powder comprises the steps of: adding 5-15 parts of high-purity metal tin particles to 40-50 parts of ammonium nitrate solution, and then adding an AR-grade nitric acid solution thereto until tin The granules are dissolved to obtain a light yellow slurry. After aging for 20-24 hours, the mixture is washed, washed with deionized water for 3-5 times, dried at 70-80 ° C for 5-7 h, and then calcined at 240-260 ° C for 2-4 h. It is obtained by cooling to room temperature; each raw material is part by weight.
  • the aging is aged for 22 hours.
  • the preparation method it is washed 4 times with deionized water.
  • the preparation method it is dried at 75 ° C for 6 h.
  • calcination is carried out at 250 ° C for 3 h.
  • the method provided by the invention is simple and can obtain nanometer tin dioxide spherical powder with small particle size, narrow distribution range and high purity, and is suitable for industrial production.
  • a method for preparing a high-purity nano-tin dioxide spherical powder comprises the steps of: adding 10 parts of high-purity tin metal particles to 45 parts of ammonium nitrate solution, and then adding an AR-grade nitric acid solution thereto until the tin particles are dissolved, thereby obtaining Light yellow paste, Chen After aging for 22 h, it was washed, washed 4 times with deionized water, dried at 75 ° C for 6 h, then calcined at 250 ° C for 3 h, and cooled to room temperature; each raw material was in parts by weight.
  • a method for preparing a high-purity nano-tin dioxide spherical powder comprises the steps of: adding 5 parts of high-purity tin metal particles to 40 parts of ammonium nitrate solution, and then adding an AR-grade nitric acid solution thereto until the tin particles are dissolved, thereby obtaining Light yellow slurry, after aging for 20 h, it was washed, washed three times with deionized water, dried at 70 ° C for 5 h, then calcined at 240 ° C for 2 h, and cooled to room temperature; each raw material was part by weight.
  • a method for preparing a high-purity nano-tin dioxide spherical powder comprises the steps of: adding 15 parts of high-purity metal tin particles to 50 parts of ammonium nitrate solution, and then adding an AR-grade nitric acid solution thereto until the tin particles are dissolved, thereby obtaining Light yellow slurry, after aging for 24 hours, it was washed, washed 5 times with deionized water, dried at 80 ° C for 7 h, then calcined at 260 ° C for 4 h, and cooled to room temperature; each raw material was part by weight.
  • the method provided by the invention is simple and can obtain nanometer tin dioxide spherical powder with small particle size, narrow distribution range and high purity, and is suitable for industrial production.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

一种高纯纳米二氧化锡球形粉末的制备方法，包括如下步骤：将5-15份高纯金属锡粒加入到40-50份硝酸铵溶液中，再向其中加入AR级硝酸溶液，直到锡粒溶解，得到淡黄色浆料，陈放老化20-24h后，抽虑，用去离子水洗涤3-5次，于70-80℃干燥5-7h，然后在240-260℃煅烧2-4h，冷却至室温即得，各原料均为重量份。方法简便，能够得到粒径小、分布范围窄、纯度高的纳米二氧化锡球形粉，适合工业化生产。

Description

一种高纯纳米二氧化锡球形粉末的制备方法 技术领域
本发明涉及一种高纯纳米二氧化锡球形粉末的制备方法。
背景技术
光学、电学以及催化等性能，被广泛用于发光材料、吸光材料、催化剂材料、气敏材料、稀磁半导体材料、锂离子电池负极材料等领域。另外，二氧化锡也是ITO薄膜的主要成分之一，ITO薄膜是一种重掺杂、高简并n型半导体氧化物薄膜，由于其具有低电阻率、高可见光透光率、高红外线区反射率、与玻璃基体结合牢固、抗擦伤、良好的化学稳定性等优点，已经广泛应用于平板显示器、太阳能电池、汽车挡风玻璃以及电子屏蔽等诸多领域。
目前，纳米SnO2的制备方法主要有微乳液法、真空蒸发凝聚法、水热合成法、化学沉淀法、静电纺丝法、溶胶-凝胶法、氧化法等。
发明内容
本发明的目的在于提供一种高纯纳米二氧化锡球形粉末的制备方法。
本发明通过下面技术方案实现：
一种高纯纳米二氧化锡球形粉末的制备方法，包括如下步骤：将5-15份高纯金属锡粒加入到40-50份硝酸铵溶液中，再向其中加入AR级硝酸溶液，直到锡粒溶解，得到淡黄色浆料，陈放老化20-24h后，抽虑，用去离子水洗涤3-5次，于70-80℃干燥5-7h，然后在240-260℃煅烧2-4h，冷却至室温即得；各原料均为重量份。
优选地，所述的制备方法中，陈放老化22h。
优选地，所述的制备方法中，用去离子水洗涤4次。
优选地，所述的制备方法中，于75℃干燥6h。
优选地，所述的制备方法中，在250℃煅烧3h。
本发明技术效果：
本发明提供的方法简便，能够得到粒径小、分布范围窄、纯度高的纳米二氧化锡球形粉，适合工业化生产。
具体实施方式
下面结合实施例具体介绍本发明的实质性内容。
实施例1
一种高纯纳米二氧化锡球形粉末的制备方法，包括如下步骤：将10份高纯金属锡粒加入到45份硝酸铵溶液中，再向其中加入AR级硝酸溶液，直到锡粒溶解，得到淡黄色浆料，陈 放老化22h后，抽虑，用去离子水洗涤4次，于75℃干燥6h，然后在250℃煅烧3h，冷却至室温即得；各原料均为重量份。
实施例2
一种高纯纳米二氧化锡球形粉末的制备方法，包括如下步骤：将5份高纯金属锡粒加入到40份硝酸铵溶液中，再向其中加入AR级硝酸溶液，直到锡粒溶解，得到淡黄色浆料，陈放老化20h后，抽虑，用去离子水洗涤3次，于70℃干燥5h，然后在240℃煅烧2h，冷却至室温即得；各原料均为重量份。
实施例3
一种高纯纳米二氧化锡球形粉末的制备方法，包括如下步骤：将15份高纯金属锡粒加入到50份硝酸铵溶液中，再向其中加入AR级硝酸溶液，直到锡粒溶解，得到淡黄色浆料，陈放老化24h后，抽虑，用去离子水洗涤5次，于80℃干燥7h，然后在260℃煅烧4h，冷却至室温即得；各原料均为重量份。
本发明提供的方法简便，能够得到粒径小、分布范围窄、纯度高的纳米二氧化锡球形粉，适合工业化生产。

Claims (5)

  1. 一种高纯纳米二氧化锡球形粉末的制备方法，其特征在于包括如下步骤：将5-15份高纯金属锡粒加入到40-50份硝酸铵溶液中，再向其中加入AR级硝酸溶液，直到锡粒溶解，得到淡黄色浆料，陈放老化20-24h后，抽虑，用去离子水洗涤3-5次，于70-80℃干燥5-7h，然后在240-260℃煅烧2-4h，冷却至室温即得；各原料均为重量份。
  2. 根据权利要求1所述的制备方法，其特征在于：陈放老化22h。
  3. 根据权利要求1所述的制备方法，其特征在于：用去离子水洗涤4次。
  4. 根据权利要求1所述的制备方法，其特征在于：于75℃干燥6h。
  5. 根据权利要求1所述的制备方法，其特征在于：在250℃煅烧3h。
PCT/CN2017/101794 2017-09-14 2017-09-15 一种高纯纳米二氧化锡球形粉末的制备方法 WO2019051737A1 (zh)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04219315A (ja) * 1990-12-19 1992-08-10 Dowa Mining Co Ltd 酸化インジウム粉の製造方法
JPH05193939A (ja) * 1991-08-30 1993-08-03 Tosoh Corp 酸化インジウム粉末及びｉｔｏ焼結体の製造方法
JPH06227815A (ja) * 1993-02-04 1994-08-16 Fuji Titan Kogyo Kk 導電性微粉末の製造方法
CN1438179A (zh) * 2003-03-14 2003-08-27 中国科学院上海硅酸盐研究所 纳米氧化锡粉体的制备方法
US20070295944A1 (en) * 2002-03-22 2007-12-27 Samsung Corning Co., Ltd. Method for manufacturing high-density indium tin oxide target, methods for preparing tin oxide powder and indium oxide powder used therefor
CN101108743A (zh) * 2006-07-19 2008-01-23 中南大学 一种制备纳米二氧化锡的方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04219315A (ja) * 1990-12-19 1992-08-10 Dowa Mining Co Ltd 酸化インジウム粉の製造方法
JPH05193939A (ja) * 1991-08-30 1993-08-03 Tosoh Corp 酸化インジウム粉末及びｉｔｏ焼結体の製造方法
JPH06227815A (ja) * 1993-02-04 1994-08-16 Fuji Titan Kogyo Kk 導電性微粉末の製造方法
US20070295944A1 (en) * 2002-03-22 2007-12-27 Samsung Corning Co., Ltd. Method for manufacturing high-density indium tin oxide target, methods for preparing tin oxide powder and indium oxide powder used therefor
CN1438179A (zh) * 2003-03-14 2003-08-27 中国科学院上海硅酸盐研究所 纳米氧化锡粉体的制备方法
CN101108743A (zh) * 2006-07-19 2008-01-23 中南大学 一种制备纳米二氧化锡的方法

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