CN113042745A - Method for preparing nano indium tin alloy powder by wet chemical method - Google Patents
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- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000000843 powder Substances 0.000 title claims abstract description 74
- 229910001128 Sn alloy Inorganic materials 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000000126 substance Substances 0.000 title claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 45
- 229910052738 indium Inorganic materials 0.000 claims abstract description 26
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 18
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims abstract description 6
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 23
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- -1 monobutyl stannic chloride Chemical compound 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- JMMJWXHSCXIWRF-UHFFFAOYSA-N ethyl(dimethyl)indigane Chemical compound CC[In](C)C JMMJWXHSCXIWRF-UHFFFAOYSA-N 0.000 claims description 5
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 4
- QMYLPCBJHHGADW-UHFFFAOYSA-N diethyl(methyl)indigane Chemical compound CC[In](C)CC QMYLPCBJHHGADW-UHFFFAOYSA-N 0.000 claims description 4
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 4
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 229910000337 indium(III) sulfate Inorganic materials 0.000 claims description 3
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 3
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 claims description 3
- JKNHZOAONLKYQL-UHFFFAOYSA-K tribromoindigane Chemical compound Br[In](Br)Br JKNHZOAONLKYQL-UHFFFAOYSA-K 0.000 claims description 3
- OTRPZROOJRIMKW-UHFFFAOYSA-N triethylindigane Chemical compound CC[In](CC)CC OTRPZROOJRIMKW-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 235000010290 biphenyl Nutrition 0.000 claims description 2
- 239000004305 biphenyl Substances 0.000 claims description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000956 alloy Substances 0.000 abstract description 31
- 239000002245 particle Substances 0.000 abstract description 10
- 238000005406 washing Methods 0.000 abstract description 6
- 150000001298 alcohols Chemical class 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 description 28
- 239000000243 solution Substances 0.000 description 25
- 229910052718 tin Inorganic materials 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 239000002270 dispersing agent Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 239000007983 Tris buffer Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YMLFYGFCXGNERH-UHFFFAOYSA-K butyltin trichloride Chemical compound CCCC[Sn](Cl)(Cl)Cl YMLFYGFCXGNERH-UHFFFAOYSA-K 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SNMVRZFUUCLYTO-UHFFFAOYSA-N n-propyl chloride Chemical compound CCCCl SNMVRZFUUCLYTO-UHFFFAOYSA-N 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 description 1
Images
Classifications
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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
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
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. Dissolving an indium precursor and a tin precursor in deionized water to obtain an indium tin precursor solution; adding a reducing agent into the indium tin precursor solution, reacting under the stirring condition, simultaneously dropwise adding alcohols 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 nano indium-tin alloy powder is spherical and nearly spherical, and the particle size is 40-200 nm. The method has the advantages of simple and safe operation, low production cost and easy washing, and can be applied to industrial production.
Description
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. A method for preparing nano indium tin alloy powder by a wet chemical method is characterized by comprising 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.
2. The method for preparing nano indium tin alloy powder by the wet chemical method according to claim 1, which is characterized in that: 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.
3. The method for preparing nano indium tin alloy powder according to the wet chemical method of claim 1 or 2, which is characterized in that: 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.
4. The method for preparing nano indium tin alloy powder by the wet chemical method according to claim 1, which is characterized in that: the indium accounts for 10-90% of the mass of the nano indium tin alloy powder as 100%.
5. The method for preparing nano indium tin alloy powder by the wet chemical method according to claim 1, which is characterized in that: and (3) the reducing agent in the step (2) is one or more of sodium borohydride, hydrazine hydrate, potassium borohydride and ascorbic acid.
6. The method for preparing nano indium tin alloy powder according to the wet chemical method of claim 1 or 5, which is characterized in that: the reaction temperature in the step (2) is 0-40 ℃.
7. The method for preparing nano indium tin alloy powder by the wet chemical method according to claim 1, which is characterized in that: the alcohol in the step (2) is one or more of absolute ethyl alcohol, methanol, ethylene glycol, 1-propanol, 1-butanol, 1-pentanol, 2-propanol and 2-butanol.
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| CN113649589A (en) * | 2021-08-18 | 2021-11-16 | 昆明理工大学 | Preparation method of spherical indium tin alloy nano powder based on organic system |
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