CN100369816C - Synthesis process of nanometer silver sulfide/copper sulfide in controlled shape - Google Patents
Synthesis process of nanometer silver sulfide/copper sulfide in controlled shape Download PDFInfo
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- CN100369816C CN100369816C CNB2006100102886A CN200610010288A CN100369816C CN 100369816 C CN100369816 C CN 100369816C CN B2006100102886 A CNB2006100102886 A CN B2006100102886A CN 200610010288 A CN200610010288 A CN 200610010288A CN 100369816 C CN100369816 C CN 100369816C
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- silver sulfide
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Abstract
The synthesis process of nanometer silver sulfide/copper sulfide in controlled shape relates to shape controlling synthesis technology of silver sulfide/copper sulfide in nanometer structure. The present invention aims at lowering the synthesis temperature of silver sulfide/copper sulfide, and raising the yield and structure controllability. The technological scheme is that under magnetic stirring, silver nitrate or copper chloride solution of 6-15 mmol/L concentration is drop-by-drop added into sodium thiosulfate solution of 9-52.5 mmol/L concentration, cetyl trimethyl ammonium bromide in 2.0-3.5 mmol is then added into the solution, the solution is stirred strongly at 30-60 deg.c for 30 min, acid is added to regulate pH to 1-5, and through further heating at the same temperature for 1-8 hr and natural cooling, the product is obtained.
Description
Technical field
The present invention relates to the shape control synthetic technology of a kind of silver sulfide or copper sulphide nano structure.
Background technology
At present, both at home and abroad about the report of silver sulfide (or copper sulfide) nanostructured synthetic technology seldom.In the synthetic technology of having reported, substantially all be under higher temperature (more than 100 ℃), to carry out, synthetic silver sulfide (or cupric sulfide) nanostructure is single simultaneously, and productive rate very low (20～30%).Control 10 pieces of documents of report sum less than of synthetic technology for the shape of silver sulfide and copper sulphide nano structure, and be only limited to the shape control of zero-dimension nano crystallization powder.
Summary of the invention
Purpose of the present invention mainly be to reduce silver sulfide (or cupric sulfide) synthesis temperature, improve the controllability of its productive rate and structure.Structure control is not limited to the crystallization powder shape control of zero dimension, and has realized the shape control at zero dimension, a peacekeeping two-dimensional nanostructure.This technology has extremely important versatility simultaneously, synthesizes for the shape control of other nanostructures to have great directive significance.
Above-mentioned purpose of the present invention is implemented by following technical solution: under magnetic agitation, be that 6～15mmol/L silver nitrate or copper chloride solution dropwise join in the hypo solution that concentration is 9～52.5mmol/L with concentration, the mixed solution cumulative volume of hypo solution and silver nitrate or copper chloride is 100ml, and control molar concentration ratio is Na
2S
2O
3: AgNO
3Or CuCl
2=1.5～3.5, add then 2.0～3.5mmol softex kw in above-mentioned mixed liquor, strong agitation 30min under 30～60 ℃ of temperature, the pH value that adds again acid-conditioning solution is 1～5, equality of temperature continues heating 1～8h, naturally cool off product.
The present invention at first forms complex; Secondly add the template that to have an effect with complex; Add at last another and make the unsettled material of complex, reduce its decomposition temperature.This method does not need complicated technology and expensive equipment, only needs the laboratory common instruments such as magnetic stirring apparatus, buret and beaker, can realize the shape control to silver sulfide (or copper sulfide) nanostructured.Temperature of reaction of the present invention is below 60 ℃, and productive rate can reach more than 90%, has characteristics such as temperature of reaction is low, productive rate is high, controllable shapes, has overcome low etc. the deficiency of the single and productive rate of temperature height, the structure of bibliographical information fully.
Embodiment
The specific embodiment one: present embodiment is prepared as follows silver sulfide/copper sulphide nano structure: under magnetic agitation, be 6～15mmol/L silver nitrate (or copper chloride) solution with concentration, dropwise joining concentration is in 9～52.5mmol/L hypo solution, its cumulative volume is 100ml, molar concentration ratio Na
2S
2O
3: AgNO
3(CuCl
2)=1.5～3.5, add then 2.0～3.5mmol softex kw (CTAB) in above-mentioned mixed liquor, under 30～60 ℃ of temperature, strong agitation 30min, CTAB is all dissolved, the pH that adds again acid-conditioning solution is in 1～5, and equality of temperature continues heating 1～8h, naturally cool off product.
By regulating Na
2S
2O
3, AgNO
3(CuCl
2) and the proportionate relationship of CTAB, just can synthesize square, ellipse, spherical nano particle; Square, circular chain nanometer rods; Nanobelt and nanometer film.
The specific embodiment two: present embodiment is take the synthetic method of silver sulfide nano cubic as example: with 50mlAgNO
3(20mmol/L) solution dropwise joins 50mlNa
2S
2O
3(44mmol/L) in the solution, under magnetic agitation, add 3mmolCTAB in above-mentioned mixed liquor, 30～40 ℃ of lower stirring 30min that continue all dissolve CTAB, use 1mol/LHNO
3The pH=1 of accent mixed liquor～2.5, equality of temperature heating 2～3h, naturally cooling, centrifugation, the carbon disulfide washing, drying namely gets product.
The specific embodiment three: present embodiment is take the synthetic method of the circular chain nanometer rods of silver sulfide as example: with 50mlAgNO
3(20mmol/L) solution dropwise joins 50mlNa
2S
2O
3(in 48～60mmol/L) solution, under magnetic agitation, add 3mmolCTAB in above-mentioned mixed liquor, 30～40 ℃ of lower stirring 30min that continue all dissolve CTAB, use 1mol/LHNO
3The pH=2 of accent mixed liquor～3, equality of temperature heating 1.5～3.5h, naturally cooling, centrifugation, the carbon disulfide washing, drying namely gets product.
The specific embodiment four: present embodiment is take the synthetic method of silver sulfide nanobelt as example: with 50mlAgNO
3(20mmol/L) solution dropwise joins 50mlNa
2S
2O
3(40mmol/L) in the solution, under magnetic agitation, add 3mmolCTAB in above-mentioned mixed liquor, 25～40 ℃ of lower stirring 30min that continue all dissolve CTAB, use 1mol/LHNO
3The pH=1.5 of accent mixed liquor～3, equality of temperature heating 1.0～3.5h, naturally cooling, centrifugation, the carbon disulfide washing, drying namely gets product.
The specific embodiment five: present embodiment is take the synthetic method of copper sulphide nano cube as example: with 50mlCuCl
2(20mmol/L) solution dropwise joins 50mlNa
2S
2O
3(44mmol/L) in the solution, under magnetic agitation, add 3mmolCTAB in above-mentioned mixed liquor, 30～40 ℃ of lower stirring 30min that continue all dissolve CTAB, use 1mol/LHNO
3The pH=1 of accent mixed liquor～2.5, equality of temperature heating 2～3h, naturally cooling, centrifugation, the carbon disulfide washing, drying namely gets product.
The specific embodiment six: present embodiment is take the synthetic method of the square chain nanometer rods of copper sulfide as example: with 50mlCuCl
2(20mmol/L) solution dropwise joins 50mlNa
2S
2O
3(in 48～60mmol/L) solution, under magnetic agitation, add 3mmolCTAB in above-mentioned mixed liquor, 30～40 ℃ of lower stirring 30min that continue all dissolve CTAB, use 1mol/LHNO
3The pH=2 of accent mixed liquor～3, equality of temperature heating 1.5～3.5h, naturally cooling, centrifugation, the carbon disulfide washing, drying namely gets product.
The specific embodiment seven: present embodiment is take the synthetic method of copper sulphide nano film as example: with 50mlCuCl
2(20mmol/L) solution dropwise joins 50mlNa
2S
2O
3(40mmol/L) in the solution, under magnetic agitation, add 3mmolCTAB in above-mentioned mixed liquor, 25～40 ℃ of lower stirring 30min that continue all dissolve CTAB, use 1mol/LHNO
3The pH=1.5 of accent mixed liquor～3, equality of temperature heating 1.0～3.5h, naturally cooling, centrifugation, the carbon disulfide washing, drying namely gets product.
Claims (4)
1. the shape of silver sulfide/copper sulphide nano structure is controlled synthetic method, it is characterized in that described method is: under magnetic agitation, be that 6～15mmol/L silver nitrate or copper chloride solution dropwise join in the hypo solution that concentration is 9～52.5mmol/L with concentration, the mixed solution cumulative volume of hypo solution and silver nitrate or copper chloride is 100ml, and control molar concentration ratio is Na
2S
2O
3: AgNO
3Or CuCl
2=1.5～3.5, add then 2.0～3.5mmol softex kw in above-mentioned mixed liquor, strong agitation 30min under 30～60 ℃ of temperature, the pH value that adds again acid-conditioning solution is 1～5, equality of temperature continues heating 1～8h, naturally cool off product.
2. the shape of silver sulfide according to claim 1/copper sulphide nano structure control synthetic method is characterized in that described Na
2S
2O
3With AgNO
3Or CuCl
2Molar concentration rate be 2.2.
3. the shape of silver sulfide according to claim 1/copper sulphide nano structure control synthetic method is characterized in that described Na
2S
2O
3With AgNO
3Or CuCl
2Molar concentration rate be 2.0.
4. the shape of silver sulfide according to claim 1/copper sulphide nano structure control synthetic method is characterized in that described Na
2S
2O
3With AgNO
3Or CuCl
2Molar concentration rate be 2.4～3.0.
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| CNB2006100102886A CN100369816C (en) | 2006-07-14 | 2006-07-14 | Synthesis process of nanometer silver sulfide/copper sulfide in controlled shape |
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|---|---|---|---|
| CNB2006100102886A CN100369816C (en) | 2006-07-14 | 2006-07-14 | Synthesis process of nanometer silver sulfide/copper sulfide in controlled shape |
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|---|---|
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| CN100369816C true CN100369816C (en) | 2008-02-20 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580266B (en) * | 2009-03-23 | 2010-12-01 | 哈尔滨工程大学 | Preparation method of CuS hierarchical structure nano material |
| CN101927345B (en) * | 2010-09-23 | 2012-01-04 | 湖南科技大学 | Method for preparing core-shell gold nanoparticles and detecting concentration of silver ions |
| CN102557108A (en) * | 2011-11-23 | 2012-07-11 | 陕西科技大学 | Monodisperse annular copper sulfide microcrystal prepared by ultrasonic auxiliary microwave hydrothermal method |
| CN102557107A (en) * | 2011-11-23 | 2012-07-11 | 陕西科技大学 | Method for preparing flower-shaped copper sulfide (CuS) nanocrystal |
| CN102716755B (en) * | 2012-07-17 | 2014-02-19 | 哈尔滨师范大学 | Preparation method of silver sulfide/zinc sulfide compound semiconductor photocatalyst with ultraviolet light catalytic activity |
| CN104176764B (en) * | 2014-09-02 | 2016-04-13 | 辽宁科技大学 | A kind of preparation method being self-assembled into ring-type nano-copper sulfide |
| CN104709936B (en) * | 2014-12-09 | 2016-08-24 | 西南交通大学 | A kind of preparation method of lim solid sulfuration copper ball |
| AT520597B1 (en) * | 2017-10-30 | 2020-09-15 | Hauser Thomas | Material comprising a precious metal phase |
| CN109054812B (en) * | 2018-08-24 | 2021-06-22 | 南京邮电大学 | Method for preparing near-infrared two-region fluorescent silver sulfide quantum dots in water phase |
| CN112366311B (en) * | 2020-09-29 | 2021-10-08 | 杭州职业技术学院 | Carbon-assembled copper sulfide hollow nanocube honeycomb material and preparation and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004108598A1 (en) * | 2003-06-05 | 2004-12-16 | National University Of Singapore | A method of preparing metal chalcogenide particles |
| CN1704843A (en) * | 2004-05-31 | 2005-12-07 | 中国科学院理化技术研究所 | Silver sulfide nano particle sensibilizer, its preparing method and use |
| CN1709798A (en) * | 2004-06-18 | 2005-12-21 | 中国科学院兰州化学物理研究所 | Method for preparing silver sulfide semiconductor nano particle |
| US20060039850A1 (en) * | 2004-04-20 | 2006-02-23 | Samsung Electronics Co., Ltd. | Method for manufacturing metal sulfide nanocrystals using thiol compound as sulfur precursor |
-
2006
- 2006-07-14 CN CNB2006100102886A patent/CN100369816C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004108598A1 (en) * | 2003-06-05 | 2004-12-16 | National University Of Singapore | A method of preparing metal chalcogenide particles |
| US20060039850A1 (en) * | 2004-04-20 | 2006-02-23 | Samsung Electronics Co., Ltd. | Method for manufacturing metal sulfide nanocrystals using thiol compound as sulfur precursor |
| CN1704843A (en) * | 2004-05-31 | 2005-12-07 | 中国科学院理化技术研究所 | Silver sulfide nano particle sensibilizer, its preparing method and use |
| CN1709798A (en) * | 2004-06-18 | 2005-12-21 | 中国科学院兰州化学物理研究所 | Method for preparing silver sulfide semiconductor nano particle |
Non-Patent Citations (2)
| Title |
|---|
| 半导体硫化银纳米晶的控制合成与光学性能研究. 杨小红.安徽教育学院学报，第23卷第3期. 2005 * |
| 银、铜硫化物纳米球的活性模板合成及其光学性能研究. 刘金库等.功能材料，第35卷第6期. 2004 * |
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