CN109133159A - A kind of indium doping Zn2SnO4The preparation method of nano wire - Google Patents
A kind of indium doping Zn2SnO4The preparation method of nano wire Download PDFInfo
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- CN109133159A CN109133159A CN201811008587.5A CN201811008587A CN109133159A CN 109133159 A CN109133159 A CN 109133159A CN 201811008587 A CN201811008587 A CN 201811008587A CN 109133159 A CN109133159 A CN 109133159A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The present invention relates to field of nano material preparation, it is desirable to provide a kind of indium doping Zn2SnO4The preparation method of nano wire.Include: that organic zinc salt is added in oxalic acid aqueous ammonium, indium salts are then added;Stirring forms uniform solution under water bath condition;It is transferred in reaction kettle after incubation water heating reaction, cooled to room temperature;Pink salt is added, pH value is adjusted with ammonium hydroxide;Reaction kettle is placed in stirred in water bath reaction, solution centrifugal treating is obtained, is cleaned with hypochlorous acid;Solid product is dried, the Zn of indium doping is obtained2SnO4Nano wire.In the present invention, the doping of phosphide element can improve the crystal structure of zinc stannate, conductivity be improved, and the binding performance of zinc stannate and metallic silver can be improved, to improve the electricity and mechanical property of silver base conductive alloy material.Indium doping nano wire is obtained using one step hydro thermal method preparation, has the characteristics that purity is high, size uniformity, good dispersion.Simple process, easily-controlled reaction conditions;It is low in cost, it is suitble to large-scale industrial production.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to a kind of indium applied to silver base conductive field of alloy material
Adulterate Zn2SnO4The preparation method of nano wire.
Background technique
In silver base conductive alloy material, the superiority and inferiority of enhancing phase structure and performance directly affects the power of silver base conductive alloy
And electric property.Silver base conductive alloy needs to possess good electric conductivity, thermal conductivity, processing performance and resistant to corrosion, anti-melting welding
Characteristic.Use inorganic, metal oxide as the reinforced phase of silver base conductive alloy material, can significantly improve material hardness,
Resistance fusion welding and anti electric arc corrosion ability, but the conduction and heating conduction of silver matrix can be reduced again simultaneously.Such as currently used increasing
Mutually have a Series oxides such as cadmium oxide, tin oxide by force, cadmium oxide enhance after silver base conductive alloy with excellent synthesis mechanics and
Electric property, but cadmium is toxic, is used 15 years as long as by European Union's ban;The silver base conductive alloy of tin oxide enhancing has excellent
Mechanical property, but its there are contact resistances during military service the problems such as big, temperature increases, cause electric life shorter, and process
Performance is poor, and manufacturing cost is high, significantly limits the application of silver base conductive alloy.Therefore it needs to select electrical and thermal conductivity performance excellent
Enhancing phase material enhance silver base conductive alloy, and need further to improve its property by the regulation to material microstructure
Energy.
Zinc stannate (Zn2SnO4) it is a kind of broad-band gap n-type semiconductor, there is matched crystal structure with metallic silver, is answered
For the various fields such as lithium cell cathode material, photocatalysis, gas sensitive, fire retardant.Compared with binary oxide, zinc stannate has
Higher stability and electron mobility.In addition, zinc stannate fusing point, hardness are high, material system is environment-protecting and non-poisonous and cost is relatively low
It is honest and clean, there is extraordinary application prospect in silver base conductive field of alloy material.Meanwhile it being examined from the angle of microstructure and properties
Consider, compared with existing zinc stannate powder granule, zine stannate nano line can preferably improve the interface cohesion of silver base conductive alloy
Intensity improves the fracture toughness and elongation after fracture of material, improves the mechanical property and electric property of silver base conductive alloy.But
For common zine stannate nano line is from electric property and surface characteristic, the application performance demand of electrical conductivity alloy is also not achieved.
Summary of the invention
To overcome the shortcomings of that the existing reinforced phase field technology of silver base conductive alloy, the present invention provide a kind of indium doping Zn2SnO4
The preparation method of nano wire.This method preparation process is simple, easy control of reaction conditions, can stablize the excellent indium of synthesis dispersibility
Adulterate Zn2SnO4Nano wire, and there is excellent mechanics and electric property, it can be applied to electrical conductivity alloy enhancing, composite property
The fields such as raising.
In order to solve the technical problem, solution of the invention is:
A kind of indium doping Zn is provided2SnO4The preparation method of nano wire, comprising the following steps:
(1) 0.1mol organic zinc salt is added in 50mL oxalic acid aqueous ammonium, indium salts is then added;In 40~60 DEG C of water
25min is stirred under the conditions of bath, forms uniform solution A;Wherein, the mass percent concentration of oxalic acid aqueous ammonium be 5~
The molar percentage of 10wt%, indium salts and organic zinc salt is 10~15mol%;
(2) solution A is transferred in reaction kettle, reaction kettle is placed in the electric dry oven of 150 DEG C of constant temperature;Hydro-thermal reaction 36h, from
It is so cooled to room temperature, obtains solution B;
(3) 0.05mol pink salt is added in solution B, pH value is adjusted to 8~9 with ammonium hydroxide;Reaction kettle is placed in 95 DEG C of water-baths
In, it is stirred to react 2~4h, obtains solution C;
(4) centrifugal treating after taking out solution C, is cleaned with hypochlorous acid;Solid product is placed in 70 DEG C of baking ovens and is dried, is obtained
Obtain the Zn of indium doping2SnO4Nano wire.
In the present invention, the organic zinc salt is zinc methide or diethyl zinc.
In the present invention, the indium salts are indium nitrate or inidum chloride.
In the present invention, the tin source is stannic chloride or sodium stannate.
In the present invention, the Zn of the indium doping finally obtained2SnO4Nano wire, draw ratio are 50~100: 1, diameter 20
~50nm, indium content are 5~10wt%.
Compared with prior art, the beneficial effects of the present invention are:
1, the doping of phosphide element can improve the crystal structure of zinc stannate, improve conductivity, and zinc stannate can be improved
With the binding performance of metallic silver, to improve the electricity and mechanical property of silver base conductive alloy material.
2, the present invention obtains indium doping nano wire using one step hydro thermal method preparation, has purity is high, size uniformity, dispersion
The good feature of property.
3, method and process of the invention is simple, easily-controlled reaction conditions;It is low in cost, it is suitble to large-scale industrial production.
4, present invention gained powder and metallic silver excellent bonding performance are also able to maintain while improving the mechanical property of silver
Lower resistivity.
Use zinc stannate powder as silver base conductive alloy made from reinforced phase, resistivity is more than 2.40 μ Ω cm.And
Under same preparation condition, use in the present invention indium doping zine stannate nano line as when reinforced phase, the reduction of electrical conductivity alloy resistivity
To 2.18 μ Ω cm hereinafter, 230MPa that tensile strength enhances from zinc stannate powder simultaneously or so is improved to indium doping zinc stannate
The 280MPa or more of nano wire enhancing.
Specific embodiment
Embodiment 1
(1) 0.1mol zinc methide is added in the oxalic acid aqueous ammonium of 50mL 5wt%, by indium nitrate with dimethyl
The ratio of the 10mol% of zinc is added in zinc methide solution, and homogeneous solution A is formed after 40 DEG C of heating stirring 25min.
(2) then solution A is transferred in the autoclave that internal capacity is 100mL, reaction kettle is placed in 150 DEG C of electricity
Hydro-thermal reaction 36h in baking oven, then cooled to room temperature, obtains solution B.
(3) 0.05mol stannic chloride is added in solution B, addition ammonium hydroxide adjusting pH value is anti-in 95 DEG C of stirred in water bath to 8
2h is answered, solution C is obtained.
(4) it is centrifuged after taking out acquired solution C, is cleaned with hypochlorous acid, 70 DEG C of baking oven drying obtain the Zn of indium doping2SnO4
Nano wire.
Nano wire draw ratio is 70:1, diameter 20nm, indium content 5wt%, and impurity content is lower than 0.05wt%.Work as tin
After sour zinc nano wire and silver powder 12:88 in mass ratio are prepared into silver base conductive alloy, resistivity is 2.16 μ Ω cm, and tension is strong
Degree is 290MPa.
Embodiment 2
(1) 0.1mol diethyl zinc is added in the oxalic acid aqueous ammonium of 50mL 10wt%, by indium nitrate with diethyl
The ratio of the 15mol% of zinc is added to diethyl zinc solution, and homogeneous solution A is formed after 60 DEG C of heating stirring 25min.
(2) then solution A is transferred in the autoclave that internal capacity is 100mL, reaction kettle is placed in 150 DEG C of electricity
Hydro-thermal reaction 36h in baking oven, then cooled to room temperature, obtains solution B.
(3) 0.05mol stannic chloride is added in solution B, addition ammonium hydroxide adjusting pH value is anti-in 95 DEG C of stirred in water bath to 9
4h is answered, solution C is obtained.
(4) it is centrifuged after taking out acquired solution C, is cleaned with hypochlorous acid, 70 DEG C of baking oven drying obtain the Zn of indium doping2SnO4
Nano wire.
Nano wire draw ratio is 50:1, diameter 50nm, indium content 10wt%, and impurity content is lower than 0.04wt%.When
After zine stannate nano line and silver powder 12:88 in mass ratio are prepared into silver base conductive alloy, resistivity is 2.08 μ Ω cm, tension
Intensity is 285MPa.
Embodiment 3
(1) 0.1mol zinc methide is added in the oxalic acid aqueous ammonium of 50mL 10wt%, by inidum chloride with dimethyl
The ratio of the 12mol% of zinc is added to zinc methide solution, and homogeneous solution A is formed after 50 DEG C of heating stirring 25min.
(2) then solution A is transferred in the autoclave that internal capacity is 100mL, reaction kettle is placed in 150 DEG C of electricity
Hydro-thermal reaction 36h in baking oven, then cooled to room temperature, obtains solution B.
(3) 0.05mol sodium stannate is added in solution B, addition ammonium hydroxide adjusting pH value is anti-in 95 DEG C of stirred in water bath to 9
3h is answered, solution C is obtained.
(4) it is centrifuged after taking out acquired solution C, is cleaned with hypochlorous acid, 70 DEG C of baking oven drying obtain the Zn of indium doping2SnO4
Nano wire.
Nano wire draw ratio is 100:1, diameter 30nm, indium content 6wt%, and impurity content is lower than 0.05wt%.When
After zine stannate nano line and silver powder 12:88 in mass ratio are prepared into silver base conductive alloy, resistivity is 2.15 μ Ω cm, tension
Intensity is 303MPa.
Embodiment 4
(1) 0.1mol diethyl zinc is added in the oxalic acid aqueous ammonium of 50mL 5wt%, by indium nitrate with diethyl
The ratio of the 10mol% of zinc is added to diethyl zinc solution, and homogeneous solution A is formed after 60 DEG C of heating stirring 25min.
(2) then solution A is transferred in the autoclave that internal capacity is 100mL, reaction kettle is placed in 150 DEG C of electricity
Hydro-thermal reaction 36h in baking oven, then cooled to room temperature, obtains solution B.
(3) 0.05mol stannic chloride is added in solution B, ammonium hydroxide is added and adjusts pH value to 8.5, in 95 DEG C of stirred in water bath
3h is reacted, solution C is obtained.
(4) it is centrifuged after taking out acquired solution C, is cleaned with hypochlorous acid, 70 DEG C of baking oven drying obtain the Zn of indium doping2SnO4
Nano wire.
Nano wire draw ratio 80:1, diameter 20nm, indium content 5wt%, impurity content are lower than 0.03wt%.Work as stannic acid
After zinc nano wire and silver powder 12:88 in mass ratio are prepared into silver base conductive alloy, resistivity is 2.14 μ Ω cm, tensile strength
For 296MPa.
Embodiment 5
(1) 0.1mol zinc methide is added in the oxalic acid aqueous ammonium of 50mL 7wt%, by inidum chloride with dimethyl
The ratio of the 15mol% of zinc is added to organic zinc salt solution, and homogeneous solution A is formed after 40 DEG C of heating stirring 25min.
(2) then solution A is transferred in the autoclave that internal capacity is 100mL, reaction kettle is placed in 150 DEG C of electricity
Hydro-thermal reaction 36h in baking oven, then cooled to room temperature, obtains solution B.
(3) 0.05mol sodium stannate is added in solution B, addition ammonium hydroxide adjusting pH value is anti-in 95 DEG C of stirred in water bath to 8
4h is answered, solution C is obtained.
(4) it is centrifuged after taking out acquired solution C, is cleaned with hypochlorous acid, 70 DEG C of baking oven drying obtain the Zn of indium doping2SnO4
Nano wire.
Nano wire draw ratio is 100:1, diameter 40nm, indium content 8wt%, and impurity content is lower than 0.04wt%.When
After zine stannate nano line and silver powder 12:88 in mass ratio are prepared into silver base conductive alloy, resistivity is 2.11 μ Ω cm, tension
Intensity is 320MPa.
Claims (5)
1. a kind of indium doping Zn2SnO4The preparation method of nano wire, which comprises the following steps:
(1) 0.1mol organic zinc salt is added in 50mL oxalic acid aqueous ammonium, indium salts is then added;In 40~60 DEG C of water-bath items
25min is stirred under part, forms uniform solution A;Wherein, the mass percent concentration of oxalic acid aqueous ammonium is 5~10wt%, indium
The molar percentage of salt and organic zinc salt is 10~15mol%;
(2) solution A is transferred in reaction kettle, reaction kettle is placed in the electric dry oven of 150 DEG C of constant temperature;Hydro-thermal reaction 36h is naturally cold
But to room temperature, solution B is obtained;
(3) 0.05mol pink salt is added in solution B, pH value is adjusted to 8~9 with ammonium hydroxide;Reaction kettle is placed in 95 DEG C of water-baths,
It is stirred to react 2~4h, obtains solution C;
(4) centrifugal treating after taking out solution C, is cleaned with hypochlorous acid;Solid product is placed in 70 DEG C of baking ovens and is dried, indium is obtained
The Zn of doping2SnO4Nano wire.
2. the method according to claim 1, wherein the organic zinc salt is zinc methide or diethyl zinc.
3. the method according to claim 1, wherein the indium salts are indium nitrate or inidum chloride.
4. the method according to claim 1, wherein the tin source is stannic chloride or sodium stannate.
5. the method according to claim 1, wherein the Zn of the indium doping finally obtained2SnO4Nano wire, length
Diameter ratio is 50~100: 1, and diameter is 20~50nm, and indium content is 5~10wt%.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111939937A (en) * | 2020-08-26 | 2020-11-17 | 杭州电子科技大学 | Zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst and preparation method thereof |
CN114229888A (en) * | 2021-12-31 | 2022-03-25 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of double-layer zinc stannate nanosheet negative electrode material, product and application thereof |
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Cited By (3)
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CN111939937A (en) * | 2020-08-26 | 2020-11-17 | 杭州电子科技大学 | Zinc stannate/indium sulfide barbed nanoflower piezoelectric/photocatalyst and preparation method thereof |
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CN114229888A (en) * | 2021-12-31 | 2022-03-25 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of double-layer zinc stannate nanosheet negative electrode material, product and application thereof |
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