CN103739015A - Antimony-tin oxide with conductive and flame retardant effect and preparation method thereof - Google Patents
Antimony-tin oxide with conductive and flame retardant effect and preparation method thereof Download PDFInfo
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- CN103739015A CN103739015A CN201310239953.9A CN201310239953A CN103739015A CN 103739015 A CN103739015 A CN 103739015A CN 201310239953 A CN201310239953 A CN 201310239953A CN 103739015 A CN103739015 A CN 103739015A
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- CN
- China
- Prior art keywords
- tin
- antimony oxide
- preparation
- antimony
- fire retardation
- Prior art date
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Links
- 238000002360 preparation method Methods 0.000 title claims description 7
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 title abstract 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title abstract 2
- 230000000694 effects Effects 0.000 title abstract 2
- 239000003063 flame retardant Substances 0.000 title abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 239000000376 reactant Substances 0.000 claims abstract description 6
- 239000000084 colloidal system Substances 0.000 claims abstract description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- XXLJGBGJDROPKW-UHFFFAOYSA-N antimony;oxotin Chemical compound [Sb].[Sn]=O XXLJGBGJDROPKW-UHFFFAOYSA-N 0.000 claims description 14
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000012046 mixed solvent Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000007790 solid phase Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical compound [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000006250 one-dimensional material Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing an antimony-tin oxide with conductive and flame retardant effects. Anhydrous ethanol and N,N-dimethyl formamide are used as solvents, tin salt, antimonic salt and polyvinylpyrrolidone are prepared to be a mixed solution, pH value of the solution is regulated to precipitate to form colloid or fluid suspension; solvent heat reaction of the reactant colloid or fluid suspension are carried out in a reactor, and a solid phase substance is collected and washed with water and anhydrous ethanol, to obtain the antimony-tin oxide of a SnxSbyOz one-dimensional micro-nano phase. The method is simple in technology, does not need complex technology and equipment, and is easy for industrialization production.
Description
Technical field
The present invention relates to a kind of preparation method with conduction fire retardation tin-antimony oxide, belong to inorganic materials and functional materials fabricating technology field.
Technical background
SnO
2it is N-shaped semiconductor material with wide forbidden band, because of its special air-sensitive, printing opacity and conductive characteristic, become and prepare gas sensor, the ideal material of transparency electrode, thus at aspects such as structure gas sensor, photodiode, flat-panel monitor and thin-film solar cells, be widely used.But pure SnO
2resistance conventionally higher, general by SnO
2in mix a small amount of Sb, In or Pb plasma reduce SnO
2resistivity and keep its good visible light transmissivity, doping SnO
2with its good optics, electric property and high chemical stability, be widely used in the fields such as solar cell, liquid-crystal display, electroluminescent.
One-dimensional material has more superior physics and electric property than zero dimension and two-dimensional material, to SnO
2one-dimentional structure adulterates, and can improve electric transmission and photon excitation efficiency, improves SnO
2the gas sensitization degree of material sensors etc.
The invention provides a kind of simple method successfully prepare length-to-diameter ratio high there is Sn
xsb
yo
zthe tin-antimony oxide of one-dimensional micro-nanometer thing phase.
Summary of the invention
One-dimensional micro-nanometer tin-antimony oxide of the present invention makes by solvent thermal synthesis method.The method suitability extensively, mild condition, technique be simple, is easy to suitability for industrialized production.
The method that the present invention prepares one-dimensional micro-nanometer tin-antimony oxide comprises the following steps:
The mixing solutions of configuration pink salt, antimonic salt and polyvinylpyrrolidone, regulates pH under agitation condition, reactant is separated out and form colloid or suspension.Dehydrated alcohol and DMF are made solvent, and the volume ratio of dehydrated alcohol and DMF is 1:20-1:2, and pink salt and antimonic salt concentration concentration are 0.01-0.5molL
-1, antimony tin mol ratio is 1:100-5:1, and polyvinylpyrrolidone concentration is 0.10-10 g/L, and pH is 8-14.
Then reactant colloid or suspension have been transferred in teflon-lined closed reactor, at 80-200 ℃ of reaction 4-24 hour, finally, by gained solid product water and absolute ethanol washing, remove water-soluble substances, can obtain one-dimensional micro-nanometer tin-antimony oxide.
The prepared one-dimensional micro-nanometer tin-antimony oxide of the present invention, mean diameter is 10 μ m, mean length is 100 μ m.
specific implementation method
Below by embodiment, the invention will be further described.
Embodiment 1:
Configuration SnCl
4, SbCl
3with the mixing solutions of polyvinylpyrrolidone, solvent is that volume ratio is dehydrated alcohol and the DMF of 1:2, SnCl
4and SbCl
3concentration be 0.10molL
-1, concentration 5 g/L of polyvinylpyrrolidone.Under the condition constantly stirring, regulator solution pH value is 11, forms suspension.In sealed reactor, be heated to 100 ℃, be incubated 12 hours.Collect the solid matter that reaction generates, after separating, washing, obtain pale powder shape product.Tetragonal spheroidal Sn in product X ray diffraction peaks and standard spectrum storehouse
918sb
109o
2(JCPDS, No.88-2348) coupling; Through scanning electron microscope analysis, be acicular structure, diameter is about 10 μ m, and length is about 100 μ m.
Embodiment 2:
Configuration SnCl
4, SbCl
3with the mixing solutions of polyvinylpyrrolidone, solvent is that volume ratio is dehydrated alcohol and the DMF of 1:2, SnCl
4and SbCl
3concentration be 0.10molL
-1, concentration 5 g/L of polyvinylpyrrolidone.Under the condition constantly stirring, regulator solution pH value is 11, forms suspension.In sealed reactor, be heated to 150 ℃, be incubated 12 hours.Collect the solid matter that reaction generates, after separating, washing, obtain pale powder shape product.Tetragonal spheroidal Sn in product X ray diffraction peaks and standard spectrum storehouse
918sb
109o
2(JCPDS, No.88-2348) coupling; Through scanning electron microscope analysis, be acicular structure, diameter is about 5 μ m, and length is about 20 μ m.
Claims (5)
1. one kind has conduction fire retardation tin-antimony oxide and preparation method thereof, it is characterized in that first pink salt, antimonic salt and polyvinylpyrrolidone being mixed with to mixing solutions, with dehydrated alcohol and N, dinethylformamide is made solvent, under agitation condition, regulate pH again, reactant is separated out and form after colloid or suspension, move in autoclave and react, after collection solid matter water and absolute ethanol washing, can obtain tin-antimony oxide.
2. as claimed in claim 1 have a conduction fire retardation tin-antimony oxide, it is characterized in that: target compound is a kind of containing Sn
xsb
yo
zthe tin-antimony oxide of one-dimensional micro-nanometer thing phase, the representative thing of one-dimensional micro-nanometer thing phase is Sn mutually
918sb
109o
2.
3. the preparation method with conduction fire retardation tin-antimony oxide as claimed in claim 1, is characterized in that: antimonic salt in reactant: pink salt mol ratio is 1:100-5:1.
4. the preparation method with conduction fire retardation tin-antimony oxide as claimed in claim 1, is characterized in that: dehydrated alcohol and DMF are made mixed solvent, and the volume ratio of dehydrated alcohol and DMF is 1:20-1:2.
5. the preparation method with conduction fire retardation tin-antimony oxide as claimed in claim 1, is characterized in that: reactant solution pH value is 8-14.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310239953.9A CN103739015A (en) | 2013-06-18 | 2013-06-18 | Antimony-tin oxide with conductive and flame retardant effect and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310239953.9A CN103739015A (en) | 2013-06-18 | 2013-06-18 | Antimony-tin oxide with conductive and flame retardant effect and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103739015A true CN103739015A (en) | 2014-04-23 |
Family
ID=50496109
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310239953.9A Pending CN103739015A (en) | 2013-06-18 | 2013-06-18 | Antimony-tin oxide with conductive and flame retardant effect and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103739015A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962455A (en) * | 2006-11-11 | 2007-05-16 | 广西民族大学 | Process for preparing multiple ATO nanometer structure |
-
2013
- 2013-06-18 CN CN201310239953.9A patent/CN103739015A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962455A (en) * | 2006-11-11 | 2007-05-16 | 广西民族大学 | Process for preparing multiple ATO nanometer structure |
Non-Patent Citations (2)
| Title |
|---|
| 雷楠楠 等: "聚乙烯吡咯烷酮/溶剂辅助合成SnO2纳米晶体", 《青岛科技大学（自然科学版）》, vol. 34, no. 1, 28 February 2013 (2013-02-28), pages 22 - 27 * |
| 龚圣 等: "溶胶－凝胶法制备纳米锑掺杂氧化锡的团聚消除", 《化工学报》, vol. 62, no. 5, 31 May 2011 (2011-05-31), pages 1460 - 1465 * |
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Application publication date: 20140423 |