CN113649589A - Preparation method of spherical indium tin alloy nano powder based on organic system - Google Patents
Preparation method of spherical indium tin alloy nano powder based on organic system Download PDFInfo
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- stannic chloride
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- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910001128 Sn alloy Inorganic materials 0.000 title claims abstract description 44
- 239000011858 nanopowder Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 37
- BDWFYHUDXIDTIU-UHFFFAOYSA-N ethanol;propane-1,2,3-triol Chemical compound CCO.OCC(O)CO BDWFYHUDXIDTIU-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 26
- 239000002270 dispersing agent Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 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
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims abstract description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 39
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 21
- 229910052738 indium Inorganic materials 0.000 claims description 14
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 14
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 14
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 14
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 13
- 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 12
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- -1 monobutyl stannic chloride Chemical compound 0.000 claims description 8
- 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
- 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 4
- QMYLPCBJHHGADW-UHFFFAOYSA-N diethyl(methyl)indigane Chemical compound CC[In](C)CC QMYLPCBJHHGADW-UHFFFAOYSA-N 0.000 claims description 4
- 229940080236 sodium cetyl sulfate Drugs 0.000 claims description 4
- GGHPAKFFUZUEKL-UHFFFAOYSA-M sodium;hexadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCOS([O-])(=O)=O GGHPAKFFUZUEKL-UHFFFAOYSA-M 0.000 claims description 4
- OTRPZROOJRIMKW-UHFFFAOYSA-N triethylindigane Chemical compound CC[In](CC)CC OTRPZROOJRIMKW-UHFFFAOYSA-N 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
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
- 229910000337 indium(III) sulfate Inorganic materials 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
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical group [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 3
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 239000011668 ascorbic acid Substances 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
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 claims description 2
- JKNHZOAONLKYQL-UHFFFAOYSA-K tribromoindigane Chemical compound Br[In](Br)Br JKNHZOAONLKYQL-UHFFFAOYSA-K 0.000 claims description 2
- 239000000956 alloy Substances 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 22
- 229910045601 alloy Inorganic materials 0.000 description 16
- 239000002245 particle Substances 0.000 description 12
- 239000006185 dispersion Substances 0.000 description 4
- 101150096185 PAAS gene Proteins 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 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 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- RJGHQTVXGKYATR-UHFFFAOYSA-L dibutyl(dichloro)stannane Chemical compound CCCC[Sn](Cl)(Cl)CCCC RJGHQTVXGKYATR-UHFFFAOYSA-L 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- PIMYDFDXAUVLON-UHFFFAOYSA-M chloro(triethyl)stannane Chemical compound CC[Sn](Cl)(CC)CC PIMYDFDXAUVLON-UHFFFAOYSA-M 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Images
Classifications
-
- 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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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 preparation method of spherical indium tin alloy nano powder based on an organic system, belonging to the technical field of indium tin alloy material preparation. Dissolving indium chloride and a tin precursor in deionized water to obtain an indium tin saturated precursor solution, adding the indium tin saturated precursor solution into an ethanol-glycerol system, uniformly stirring, adding a dispersing agent, uniformly stirring to obtain a reaction system, adding a reducing agent into the reaction system, reacting for 1-3 min under the stirring condition, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain the spherical indium tin alloy nano powder. The indium tin alloy nano powder is spherical and nearly spherical, is simple and safe to operate, low in production cost and easy to wash, and can be applied to industrial production.
Description
Technical Field
The invention relates to a preparation method of spherical indium tin alloy nano powder based on an organic system, belonging to the technical field of indium tin alloy material preparation.
Background
The indium tin solder has good stability and plasticity and low melting point, and has excellent conductivity and fatigue resistance, so that the indium tin solder is widely applied to the field of electronic packaging.
The method for producing indium tin alloy powder mainly comprises a chemical reduction method, an atomization method, an electrochemical method and the like, and the traditional preparation method is the chemical reduction method, a reducing agent is usually added into salt or acid containing metal indium and tin in the preparation process, indium tin alloy is prepared due to the interaction of atomic diffusion and Ostwald and the like in the process, and finally, the nano indium tin alloy powder is obtained through washing, drying and the like. However, glycerol has high viscosity during the separation process, and the separation is relatively difficult, and needs to be washed with water and absolute ethyl alcohol for many times.
Disclosure of Invention
The invention provides a preparation method of spherical indium tin alloy nano powder based on an organic system, aiming at the problem that the nano indium tin alloy powder with high purity and uniform granularity is difficult to obtain In the preparation of indium tin alloy powder In the prior art, and spherical indium tin alloy (In3Sn and InSn4) nano powder with the granularity of 20-120nm is prepared by reducing an indium tin precursor by adopting a reducing agent In the organic system.
A preparation method of spherical indium tin alloy nano powder based on an organic system comprises the following specific steps:
(1) dissolving an indium precursor and a tin precursor in deionized water to obtain an indium tin saturated precursor solution;
(2) adding the indium tin saturated precursor solution obtained in the step (1) into an ethanol-glycerol system, uniformly stirring, adding a dispersing agent, and uniformly stirring to obtain a reaction system;
(3) adding a reducing agent into the reaction system in the step (2), reacting for 1-3 min under the condition of stirring, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain spherical indium tin alloy nano powder;
the indium precursor in the step (1) is indium chloride, indium bromide, indium sulfate, indium sulfide, triethylindium, dimethylethylindium, diethylmethylindium, dimethylethylindium or diethylmethylindium; the tin precursor is stannous sulfate, stannic sulfate, stannous chloride, stannic chloride, dibutyltin 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 or monophenyl stannic chloride;
the molar ratio of indium to tin in the indium tin saturated precursor solution in the step (1) is 1:9-9: 1;
the molar ratio of ethanol to glycerol in the ethanol-glycerol system in the step (2) is 1:0.5-5, and the volume ratio of indium tin saturated precursor solution to the ethanol-glycerol system is 1: 1-5;
the dispersing agent in the step (2) is PVP (polyvinylpyrrolidone), SDS (sodium cetyl sulfate) or PAAS (sodium polyacrylate), and the adding amount of the dispersing agent is 0.1-0.3 g/L;
the reducing agent in the step (3) is one or more of sodium borohydride, hydrazine hydrate, potassium borohydride and ascorbic acid, and the adding amount of the reducing agent is 1.0-1.5 mol/L.
The invention has the beneficial effects that:
(1) the reducing agent of the invention is used for reducing In an organic system3+、Sn2+Ion reduction, nucleation and growth are carried out under the combined action of diffusion and Ostwald curing to form spherical indium tin alloy nano powder;
(2) in an organic system, the glycerol hydroxyl-OH has dispersibility and stability inoxidizability, so that the spherical indium tin alloy nano powder has uniform particle size distribution and narrow particle size distribution range, and the oxidation of the indium tin alloy is prevented.
(3) In the invention, because the glycerol has certain dispersibility and stability, In generated immediately under high-speed rotation3Sn and InSn4Will be wrapped by glycerol, which inhibits the growth of particles and obtains nano indium-tin alloy particles with better dispersity and uniform particle size.
Drawings
FIG. 1 is a scanning electron microscope (magnification of 50000 times) of the nano spherical indium tin alloy powder of example 1;
fig. 2 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 preparation method of spherical indium tin alloy nano powder based on an organic system comprises the following specific steps:
(1) dissolving triethyl indium and stannous sulfate in deionized water to obtain indium tin saturated precursor solution; wherein the molar ratio of indium to tin in the indium tin saturated precursor solution is 1: 1;
(2) under the conditions of room temperature and the stirring speed of 5000r/min, adding the indium tin saturated precursor solution obtained in the step (1) into an ethanol-glycerol system, uniformly stirring, adding a dispersant PVP, and uniformly stirring to obtain a reaction system; wherein the molar ratio of ethanol to glycerol in the ethanol-glycerol system is 1:1, the volume ratio of the indium tin saturated precursor solution to the ethanol-glycerol system is 1:1, and the addition amount of the dispersant PVP is 0.12 g/L;
(3) adding a reducing agent sodium borohydride into the reaction system in the step (2), reacting for 1min under the condition of stirring, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain spherical indium tin alloy nano powder; wherein the addition amount of the reducing agent sodium borohydride is 1.0 mol/L;
the scanning electron microscope image of the indium tin nano alloy powder in this embodiment is shown in fig. 1, and it can be known from fig. 1 that the indium tin nano alloy powder is spherical and nearly spherical, the particle size is 20-80nm, and the dispersion is uniform; as can be seen from the XRD pattern of the nano indium tin nano alloy powder shown In FIG. 2, compared with In3Sn (PDF #04-004-7736) InSn4(PDF #04-003-2161), no impurity peak is generated;
in the indium tin nano alloy powder of the embodiment, In3Sn accounts for 78.10 wt%, and InSn4 accounts for 21.90 wt%.
Example 2: a preparation method of spherical indium tin alloy nano powder based on an organic system comprises the following specific steps:
(1) dissolving indium chloride and stannous chloride in deionized water to obtain indium tin saturated precursor solution; wherein the molar ratio of indium to tin in the indium tin saturated precursor solution is 1: 4;
(2) under the conditions of room temperature and the stirring speed of 5000r/min, adding the indium tin saturated precursor solution obtained in the step (1) into an ethanol-glycerol system, uniformly stirring, adding a dispersant PVP, and uniformly stirring to obtain a reaction system; wherein the molar ratio of ethanol to glycerol in the ethanol-glycerol system is 1:1, the volume ratio of the indium tin saturated precursor solution to the ethanol-glycerol system is 1:2, and the addition amount of the dispersant PVP is 0.2 g/L;
(3) adding a reducing agent sodium borohydride into the reaction system in the step (2), reacting for 2min under the condition of stirring, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain spherical indium tin alloy nano powder; wherein the addition amount of the reducing agent sodium borohydride is 1.2 mol/L;
the indium tin nano alloy powder in the embodiment is spherical and approximately spherical, has the particle size of 30-80nm and is uniformly dispersed;
in the indium tin nano alloy powder of the embodiment, In3Sn accounts for 8.77 wt%, and InSn4 accounts for 91.23 wt%.
Example 3: a preparation method of spherical indium tin alloy nano powder based on an organic system comprises the following specific steps:
(1) dissolving dimethyl ethyl indium and tin sulfate in deionized water to obtain indium tin saturated precursor solution; wherein the molar ratio of indium to tin in the indium tin saturated precursor solution is 1: 1;
(2) under the conditions of room temperature and the stirring speed of 5000r/min, adding the indium tin saturated precursor solution obtained in the step (1) into an ethanol-glycerol system, uniformly stirring, adding a dispersant PVP, and uniformly stirring to obtain a reaction system; wherein the molar ratio of ethanol to glycerol in the ethanol-glycerol system is 1:3, the volume ratio of the indium tin saturated precursor solution to the ethanol-glycerol system is 1:5, and the addition amount of the dispersing agent SDS is 0.10 g/L;
(3) adding a reducing agent hydrazine hydrate into the reaction system in the step (2), reacting for 3min under the condition of stirring, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain spherical indium tin alloy nano powder; wherein the addition amount of the reducing agent hydrazine hydrate is 1.5 mol/L;
the indium tin nano alloy powder is spherical and approximately spherical, the particle size is 40-120nm, and the dispersion is uniform;
in the indium tin nano alloy powder of the embodiment, In3Sn accounts for 70.11 wt%, and InSn4 accounts for 29.89 wt%.
Example 4: a preparation method of spherical indium tin alloy nano powder based on an organic system comprises the following specific steps:
(1) dissolving indium sulfate and dibutyl tin chloride in deionized water to obtain indium tin saturated precursor solution; wherein the molar ratio of indium to tin in the indium tin saturated precursor solution is 1: 1;
(2) under the conditions of room temperature and the stirring speed of 5000r/min, adding the indium tin saturated precursor solution obtained in the step (1) into an ethanol-glycerol system, uniformly stirring, adding a dispersing agent PAAS, and uniformly stirring to obtain a reaction system; wherein the molar ratio of ethanol to glycerol in the ethanol-glycerol system is 1:3, the volume ratio of the indium tin saturated precursor solution to the ethanol-glycerol system is 1:3, and the addition amount of the dispersing agent PAAS is 0.13 g/L;
(3) adding a reducing agent hydrazine hydrate into the reaction system in the step (2), reacting for 1.5min under the condition of stirring, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain spherical indium tin alloy nano powder; wherein the addition amount of the reducing agent hydrazine hydrate is 1.2 mol/L;
the indium tin nano alloy powder in the embodiment is spherical and approximately spherical, has the particle size of 60-100nm and is uniformly dispersed;
in the indium tin nano alloy powder of the embodiment, In3Sn accounts for 69.80 wt%, and InSn4 accounts for 30.20 wt%.
Example 5: a preparation method of spherical indium tin alloy nano powder based on an organic system comprises the following specific steps:
(1) dissolving indium chloride and tin sulfate in deionized water to obtain indium tin saturated precursor solution; wherein the molar ratio of indium to tin in the indium tin saturated precursor solution is 3: 1;
(2) under the conditions of room temperature and the stirring speed of 5000r/min, adding the indium tin saturated precursor solution obtained in the step (1) into an ethanol-glycerol system, uniformly stirring, adding a dispersant PVP, and uniformly stirring to obtain a reaction system; wherein the molar ratio of ethanol to glycerol in the ethanol-glycerol system is 1:2, the volume ratio of the indium tin saturated precursor solution to the ethanol-glycerol system is 1:4, and the addition amount of the dispersant PVP is 0.15 g/L;
(3) adding a reducing agent hydrazine hydrate into the reaction system in the step (2), reacting for 1.8min under the condition of stirring, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain spherical indium tin alloy nano powder; wherein the addition amount of the reducing agent hydrazine hydrate is 1.1 mol/L;
the indium tin nano alloy powder in the embodiment is spherical and nearly spherical, has the particle size of 30-100nm and is uniformly dispersed;
in the indium tin nano alloy powder of the embodiment, In3Sn accounts for 96.29 wt%, and InSn4 accounts for 3.71 wt%.
Example 6: a preparation method of spherical indium tin alloy nano powder based on an organic system comprises the following specific steps:
(1) dissolving triethyl indium and triethyl tin chloride in deionized water to obtain indium tin saturated precursor solution; wherein the molar ratio of indium to tin in the indium tin saturated precursor solution is 3: 1;
(2) under the conditions of room temperature and the stirring speed of 5000r/min, adding the indium tin saturated precursor solution obtained in the step (1) into an ethanol-glycerol system, uniformly stirring, adding a dispersant PVP, and uniformly stirring to obtain a reaction system; wherein the molar ratio of ethanol to glycerol in the ethanol-glycerol system is 1:1, the volume ratio of the indium tin saturated precursor solution to the ethanol-glycerol system is 1:3, and the addition amount of the dispersant PVP is 0.25 g/L;
(3) adding a reducing agent hydrazine hydrate into the reaction system in the step (2), reacting for 1.5min under the condition of stirring, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain spherical indium tin alloy nano powder; wherein the addition amount of the reducing agent hydrazine hydrate is 1.2 mol/L;
the indium tin nano alloy powder in the embodiment is spherical and nearly spherical, the particle size is 20-60nm, and the dispersion is uniform;
in the indium tin nano alloy powder of the embodiment, In3Sn accounts for 95.32 wt%, and InSn4 accounts for 4.68 wt%.
Example 7: a preparation method of spherical indium tin alloy nano powder based on an organic system comprises the following specific steps:
(1) dissolving indium chloride and tin sulfate in deionized water to obtain indium tin saturated precursor solution; wherein the molar ratio of indium to tin in the indium tin saturated precursor solution is 3: 1;
(2) under the conditions of room temperature and the stirring speed of 5000r/min, adding the indium tin saturated precursor solution obtained in the step (1) into an ethanol-glycerol system, uniformly stirring, adding a dispersant PVP, and uniformly stirring to obtain a reaction system; wherein the molar ratio of ethanol to glycerol in the ethanol-glycerol system is 1:2, the volume ratio of the indium tin saturated precursor solution to the ethanol-glycerol system is 1:4, and the addition amount of the dispersant PVP is 0.18 g/L;
(3) adding a reducing agent hydrazine hydrate into the reaction system in the step (2), reacting for 2.0min under the condition of stirring, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain spherical indium tin alloy nano powder; wherein the addition amount of the reducing agent hydrazine hydrate is 1.2 mol/L;
the indium tin nano alloy powder is spherical and approximately spherical, the particle size is 40-90nm, and the dispersion is uniform;
in the indium tin nano alloy powder of the embodiment, In3Sn accounts for 95.48 wt%, and InSn4 accounts for 4.52 wt%.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (6)
1. A preparation method of spherical indium tin alloy nano powder based on an organic system 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 saturated precursor solution;
(2) adding the indium tin saturated precursor solution obtained in the step (1) into an ethanol-glycerol system, uniformly stirring, adding a dispersing agent, and uniformly stirring to obtain a reaction system;
(3) and (3) adding a reducing agent into the reaction system in the step (2), reacting for 1-3 min under the condition of stirring, carrying out solid-liquid separation, sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain the spherical indium tin alloy nano powder.
2. The method for preparing spherical indium tin alloy nanopowder based on organic system according to claim 1, wherein: the indium precursor in the step (1) is indium chloride, indium bromide, indium sulfate, indium sulfide, triethylindium, dimethylethylindium, diethylmethylindium, dimethylethylindium or diethylmethylindium; the tin precursor is 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 or monophenyl stannic chloride.
3. The method for preparing spherical indium tin alloy nanopowder based on organic system according to claim 1 or 2, wherein: the mol ratio of indium to tin in the indium tin saturated precursor solution in the step (1) is 1:9-9: 1.
4. The method for preparing spherical indium tin alloy nanopowder based on organic system according to claim 1, wherein: and (2) the molar ratio of ethanol to glycerol in the ethanol-glycerol system is 1:0.5-5, and the volume ratio of the indium tin saturated precursor solution to the ethanol-glycerol system is 1: 1-5.
5. The method for preparing spherical indium tin alloy nanopowder based on organic system according to claim 1, wherein: the dispersing agent in the step (2) is polyvinylpyrrolidone, sodium cetyl sulfate or sodium polyacrylate, and the addition amount of the dispersing agent is 0.1-0.3 g/L.
6. The method for preparing spherical indium tin alloy nanopowder based on organic system according to claim 1, wherein: and (3) the reducing agent is one or more of sodium borohydride, hydrazine hydrate, potassium borohydride and ascorbic acid, and the addition amount of the reducing agent is 1.0-1.5 mol/L.
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| CN113042745A (en) * | 2021-03-12 | 2021-06-29 | 昆明理工大学 | Method for preparing nano indium tin alloy powder by wet chemical method |
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