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CN113042745A - Method for preparing nano indium tin alloy powder by wet chemical method - Google Patents

Method for preparing nano indium tin alloy powder by wet chemical method Download PDF

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CN113042745A
CN113042745A CN202110267400.9A CN202110267400A CN113042745A CN 113042745 A CN113042745 A CN 113042745A CN 202110267400 A CN202110267400 A CN 202110267400A CN 113042745 A CN113042745 A CN 113042745A
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indium
tin
alloy powder
nano
indium tin
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邓华铭
胡劲
段云彪
王开军
郭一飞
王雷
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Kunming University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

本发明涉及一种湿化学法制备纳米铟锡合金粉的方法，属于铟锡合金材料技术领域。本发明将铟前驱体和锡前驱体溶解于去离子水中得到铟锡前驱体溶液；将还原剂加入到铟锡前驱体溶液中并在搅拌条件下反应，同时滴加醇类至溶液呈灰色，固液分离，固体依次经无水乙醇和去离子水清洗，真空干燥即得纳米铟锡合金粉。本发明纳米铟锡合金粉为球形和近球形，粒径为40‑200nm。本发明方法的操作简单安全，生产成本低，易于洗涤，可应用于工业化生产。The invention relates to a method for preparing nano-indium-tin alloy powder by a wet chemical method, and belongs to the technical field of indium-tin alloy materials. In the invention, the indium and tin precursors are dissolved in deionized water to obtain the indium-tin precursor solution; the reducing agent is added to the indium-tin precursor solution and reacts under stirring conditions, and alcohols are added dropwise until the solution turns gray, The solid-liquid separation is performed, the solid is washed with absolute ethanol and deionized water in turn, and dried in vacuum to obtain nano-indium tin alloy powder. The nano-indium tin alloy powder of the present invention is spherical or nearly spherical, and the particle size is 40-200 nm. The method of the invention has the advantages of simple and safe operation, low production cost, easy washing, and can be applied to industrialized production.

Description

Method for preparing nano indium tin alloy powder by wet chemical method
Technical Field
The invention relates to a method for preparing nano indium tin alloy powder by a wet chemical method, belonging to the technical field of indium tin alloy materials.
Background
The indium tin solder has good stability and plasticity and lower melting point, and is widely applied in the field of electronic packaging due to excellent conductivity, fatigue resistance and the like.
The conventional preparation method is a chemical reduction method, and the preparation process usually comprises adding a reducing agent into a salt or acid containing metal indium and tin, reducing to prepare indium and tin simple substances, combining the stripped indium and tin to form an alloy, and finally washing, drying and the like to obtain the nano indium-tin alloy powder. Reducing agents, stabilizing agents, dispersing agents and the like are often added in the reduction process, and are difficult to remove in subsequent treatment, and the nano indium tin alloy powder with high purity and uniform particle size is difficult to obtain.
Disclosure of Invention
The invention provides a method for preparing nano indium tin alloy powder by a wet chemical method, aiming at the problems that reducing agents, stabilizing agents and dispersing agents are difficult to remove In the subsequent treatment In the chemical reduction method In the prior art and nano indium tin alloy powder with high purity and uniform granularity is difficult to obtain3Sn, namely obtaining indium tin alloy in one step, wherein the grain size of the nano indium tin alloy powder is 40-200 nm; pure In can be prepared by the proportioning of indium and tin3Sn。
A method for preparing nano indium tin alloy powder by a wet chemical method comprises the following specific steps:
(1) dissolving an indium precursor and a tin precursor in deionized water to obtain an indium tin precursor solution;
(2) adding a reducing agent into the indium tin precursor solution obtained in the step (1), reacting under stirring, simultaneously dropwise adding alcohol until the solution is gray, carrying out solid-liquid separation, sequentially cleaning the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain the nano indium tin alloy powder.
The indium precursor in the step (1) is one or more of indium chloride, indium bromide, indium sulfate, indium sulfide, triethylindium, dimethylethylindium, diethylmethylindium, dimethylethylindium and diethylmethylindium.
The tin precursor is one or more of stannous sulfate, stannic sulfate, stannous chloride, stannic chloride, dibutyl stannic chloride, monobutyl stannic chloride, triethyl stannic chloride, triphenyl stannic chloride, tributyl stannic chloride, tripropyl stannic chloride, diphenyl stannic chloride, tetrabutyl stannic chloride, dioctyl stannic chloride and mono-phenyl stannic chloride.
The indium accounts for 10-90% of the mass of the nano indium tin alloy powder as 100%.
The reducing agent in the step (2) is one or more of sodium borohydride, hydrazine hydrate, potassium borohydride and ascorbic acid.
The reaction temperature in the step (2) is 0-40 ℃.
The alcohol in the step (2) is one or more of absolute ethyl alcohol, methanol, glycol, 1-propanol, 1-butanol, 1-pentanol, 2-propanol and 2-butanol.
The invention has the beneficial effects that:
(1) the invention utilizes a reducing agent to lead In of indium tin precursor solution to be In3+、Sn2+Ions are directly reduced into In and Sn atoms, and the metal atoms which are just reduced belong to active metal atoms, so that nucleation and growth are easy to realize, and an alloy is formed;
(2) the process of the invention forms In and InSn In the absence of added alcohol4On the basis of (1), adding alcohol to promote In the alloy3Sn is formed;
(3) in the reaction process of the invention, impurities such as a dispersing agent and the like are not introduced, and the obtained nano indium tin alloy powder is spherical or spheroidal, and has uniform particle size distribution and high purity.
Drawings
FIG. 1 is a scanning electron microscope (80000 times magnification) of the spherical ITO powder of example 1;
FIG. 2 is a scanning electron microscope image (magnification 200000 times) of the spherical ITO powder of example 1;
fig. 3 is an XRD pattern of the nano spherical indium tin alloy powder of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a method for preparing nano indium tin alloy powder by a wet chemical method comprises the following specific steps:
(1) dissolving an indium precursor (indium chloride) and a tin precursor (stannous sulfate) in deionized water to obtain an indium tin precursor solution;
(2) adding a reducing agent (sodium borohydride) into the indium tin precursor solution obtained in the step (1) at the temperature of 10 ℃ and the stirring speed of 500r/min for reaction, simultaneously dropwise adding absolute ethyl alcohol until the solution is gray, carrying out solid-liquid separation, sequentially washing the solid with the absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain nano indium tin alloy powder; the indium accounts for 45 percent based on the mass of the nano indium tin alloy powder as 100 percent;
the scanning electron microscope images of the nano indium tin nano alloy powder of the embodiment are shown in fig. 1-2, and it can be seen from fig. 1-2 that the nano indium tin nano alloy powder has a particle size of 40-200nm and is uniformly dispersed; as can be seen In FIG. 3, the XRD pattern of the nano indium tin nano alloy powder shows that no impurity peak exists when In3Sn (PDF #04-004-7736) and InSn4(PDF #04-003-2161) are compared.
Example 2: a method for preparing nano indium tin alloy powder by a wet chemical method comprises the following specific steps:
(1) dissolving an indium precursor (triethylindium) and a tin precursor (stannous chloride) in deionized water to obtain an indium tin precursor solution;
(2) adding a reducing agent (potassium borohydride) into the indium tin precursor solution obtained in the step (1) at the temperature of 0 ℃ and the stirring speed of 700r/min for reaction, simultaneously dropwise adding ethylene glycol until the solution is gray, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain nano indium tin alloy powder; the indium accounts for 50 percent based on the mass of the nano indium tin alloy powder as 100 percent;
the particle size of the nano indium tin nano alloy powder is 40-120nm, and the nano indium tin nano alloy powder is uniformly dispersed; compared with the XRD patterns of the nano indium tin nano alloy powder In In3Sn (PDF #04-004-7736) and InSn4(PDF #04-003-2161), the nano indium tin nano alloy powder has no impurity peaks.
Example 3: a method for preparing nano indium tin alloy powder by a wet chemical method comprises the following specific steps:
(1) dissolving an indium precursor (indium sulfate) and a tin precursor (stannic chloride) in deionized water to obtain an indium tin precursor solution;
(2) adding a reducing agent (ascorbic acid) into the indium tin precursor solution obtained in the step (1) at the temperature of 5 ℃ and the stirring speed of 700r/min for reaction, simultaneously dropwise adding 2-propanol until the solution is gray, carrying out solid-liquid separation, sequentially cleaning the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain nano indium tin alloy powder; the indium accounts for 50 percent based on the mass of the nano indium tin alloy powder as 100 percent;
the particle size of the nano indium tin nano alloy powder is 50-180nm, and the nano indium tin nano alloy powder is uniformly dispersed; compared with the XRD patterns of the nano indium tin nano alloy powder In In3Sn (PDF #04-004-7736) and InSn4(PDF #04-003-2161), the nano indium tin nano alloy powder has no impurity peaks.
Example 4: a method for preparing nano indium tin alloy powder by a wet chemical method comprises the following specific steps:
(1) dissolving an indium precursor (dimethyl ethyl indium) and a tin precursor (monobutyl tin chloride) in deionized water to obtain an indium tin precursor solution;
(2) adding a reducing agent (hydrazine hydrate) into the indium tin precursor solution obtained in the step (1) at the temperature of 15 ℃ and the stirring speed of 550r/min for reaction, simultaneously dropwise adding methanol until the solution is gray, carrying out solid-liquid separation, sequentially cleaning the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain nano indium tin alloy powder; the indium accounts for 50 percent based on the mass of the nano indium tin alloy powder as 100 percent;
the nano indium tin nano alloy powder has the particle size of 60-170nm and is uniformly dispersed; compared with the XRD patterns of the nano indium tin nano alloy powder In In3Sn (PDF #04-004-7736) and InSn4(PDF #04-003-2161), the nano indium tin nano alloy powder has no impurity peaks.
Example 5: a method for preparing nano indium tin alloy powder by a wet chemical method comprises the following specific steps:
(1) dissolving an indium precursor (indium sulfide) and a tin precursor (tin sulfate) in deionized water to obtain an indium tin precursor solution;
(2) adding a reducing agent (sodium borohydride) into the indium tin precursor solution obtained in the step (1) at the temperature of 10 ℃ and the stirring speed of 650r/min for reaction, simultaneously dropwise adding absolute ethyl alcohol until the solution is gray, carrying out solid-liquid separation, sequentially washing the solid with the absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain nano indium tin alloy powder; the indium accounts for 55 percent based on the mass of the nano indium tin alloy powder as 100 percent;
the particle size of the nano indium tin nano alloy powder is 80-190nm, and the nano indium tin nano alloy powder is uniformly dispersed; compared with the XRD patterns of the nano indium tin nano alloy powder In In3Sn (PDF #04-004-7736) and InSn4(PDF #04-003-2161), the nano indium tin nano alloy powder has no impurity peaks.
Example 6: a method for preparing nano indium tin alloy powder by a wet chemical method comprises the following specific steps:
(1) indium precursor (dimethylethylium indium) and tin precursor (tris)Propyl chlorideTin melting) is dissolved in deionized water to obtain indium tin precursor solution;
(2) adding a reducing agent (sodium borohydride) into the indium tin precursor solution obtained in the step (1) at the temperature of 30 ℃ and the stirring speed of 600r/min for reaction, simultaneously dropwise adding absolute ethyl alcohol until the solution is gray, carrying out solid-liquid separation, sequentially washing the solid with the absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain nano indium tin alloy powder; the indium accounts for 50 percent based on the mass of the nano indium tin alloy powder as 100 percent;
the particle size of the nano indium tin nano alloy powder is 60-200nm, and the nano indium tin nano alloy powder is uniformly dispersed; compared with the XRD patterns of the nano indium tin nano alloy powder In In3Sn (PDF #04-004-7736) and InSn4(PDF #04-003-2161), the nano indium tin nano alloy powder has no impurity peaks.
Example 7: a method for preparing nano indium tin alloy powder by a wet chemical method comprises the following specific steps:
(1) dissolving an indium precursor (indium bromide) and a tin precursor (stannous sulfate) in deionized water to obtain an indium tin precursor solution;
(2) adding a reducing agent (sodium borohydride) into the indium tin precursor solution obtained in the step (1) at the temperature of 20 ℃ and the stirring speed of 700r/min for reaction, simultaneously dropwise adding propanol until the solution is gray, carrying out solid-liquid separation, sequentially cleaning the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain nano indium tin alloy powder; the indium accounts for 60 percent based on the mass of the nano indium tin alloy powder as 100 percent;
the particle size of the nano indium tin nano alloy powder is 40-150nm, and the nano indium tin nano alloy powder is uniformly dispersed; compared with the XRD patterns of the nano indium tin nano alloy powder In In3Sn (PDF #04-004-7736) and InSn4(PDF #04-003-2161), the nano indium tin nano alloy powder has no impurity peaks.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.

Claims (7)

1.一种湿化学法制备纳米铟锡合金粉的方法，其特征在于，具体步骤如下：1. a method for preparing nano-indium tin alloy powder by wet chemical method, is characterized in that, concrete steps are as follows: (1)将铟前驱体和锡前驱体溶解于去离子水中得到铟锡前驱体溶液；(1) Dissolving the indium precursor and the tin precursor in deionized water to obtain an indium-tin precursor solution; (2)将还原剂加入到步骤(1)铟锡前驱体溶液中并在搅拌条件下反应，同时滴加醇类至溶液呈灰色，固液分离，固体依次经无水乙醇和去离子水清洗，真空干燥即得纳米铟锡合金粉。(2) adding a reducing agent to the indium tin precursor solution in step (1) and reacting under stirring conditions, while adding alcohols dropwise until the solution turns gray, the solid-liquid is separated, and the solid is sequentially washed with absolute ethanol and deionized water , and vacuum drying to obtain nano-indium tin alloy powder. 2.根据权利要求1所述湿化学法制备纳米铟锡合金粉的方法，其特征在于：步骤(1)铟前驱体为氯化铟、溴化铟、硫酸铟、硫化铟、三乙基铟、二甲基乙基铟、二乙基甲基铟、二甲基乙基铟、二乙基甲基铟中的一种或多种。2 . The method for preparing nano-indium tin alloy powder by wet chemical method according to claim 1 , wherein the indium precursor in step (1) is indium chloride, indium bromide, indium sulfate, indium sulfide, and triethylindium. 3 . , one or more of dimethyl ethyl indium, diethyl methyl indium, dimethyl ethyl indium, and diethyl methyl indium. 3.根据权利要求1或2所述湿化学法制备纳米铟锡合金粉的方法，其特征在于：锡前驱体为硫酸亚锡、硫酸锡、氯化亚锡、四氯化锡、二丁基氯化锡、单丁基氯化锡、三乙基氯化锡、三苯基氯化锡、三丁基氯化锡、三丙基氯化锡、二苯基氯化锡、四丁基锡、二辛基氯化锡和单、苯基氯化锡中的一种或多种。3. the method for preparing nano-indium tin alloy powder by wet chemical method according to claim 1 and 2 is characterized in that: tin precursor is stannous sulfate, tin sulfate, stannous chloride, tin tetrachloride, dibutyl Tin Chloride, Monobutyl Tin Chloride, Triethyl Tin Chloride, Triphenyl Tin Chloride, Tributyl Tin Chloride, Tripropyl Tin Chloride, Diphenyl Tin Chloride, Tetrabutyl Tin Chloride, Diphenyl Tin Chloride One or more of octyl tin chloride and mono, phenyl tin chloride. 4.根据权利要求1所述湿化学法制备纳米铟锡合金粉的方法，其特征在于：以纳米铟锡合金粉的质量为100％计，铟占10～90％。4 . The method for preparing nano-indium-tin alloy powder by wet chemical method according to claim 1 , wherein the indium accounts for 10-90% based on the mass of the nano-indium-tin alloy powder as 100%. 5 . 5.根据权利要求1所述湿化学法制备纳米铟锡合金粉的方法，其特征在于：步骤(2)还原剂为硼氢化钠、水合肼、硼氢化钾、抗坏血酸的一种或多种。5 . The method for preparing nano-indium tin alloy powder by wet chemical method according to claim 1 , wherein the reducing agent in step (2) is one or more of sodium borohydride, hydrazine hydrate, potassium borohydride and ascorbic acid. 6 . 6.根据权利要求1或5所述湿化学法制备纳米铟锡合金粉的方法，其特征在于：步骤(2)反应温度为0-40℃。6 . The method for preparing nano-indium tin alloy powder by wet chemical method according to claim 1 or 5 , wherein the reaction temperature in step (2) is 0-40° C. 7 . 7.根据权利要求1所述湿化学法制备纳米铟锡合金粉的方法，其特征在于：步骤(2)醇类为无水乙醇、甲醇、乙二醇、1-丙醇、1-丁醇、1-戊醇、2-丙醇、2-丁醇中的一种或多种。7. The method for preparing nano-indium tin alloy powder by wet chemical method according to claim 1, characterized in that: the alcohols in step (2) are absolute ethanol, methanol, ethylene glycol, 1-propanol, 1-butanol , one or more of 1-pentanol, 2-propanol and 2-butanol.
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Application publication date: 20210629