CN101890506B - Method for preparing nano-copper - Google Patents
Method for preparing nano-copper Download PDFInfo
- Publication number
- CN101890506B CN101890506B CN 201010244071 CN201010244071A CN101890506B CN 101890506 B CN101890506 B CN 101890506B CN 201010244071 CN201010244071 CN 201010244071 CN 201010244071 A CN201010244071 A CN 201010244071A CN 101890506 B CN101890506 B CN 101890506B
- Authority
- CN
- China
- Prior art keywords
- copper
- sediment
- nanometer
- gained
- centrifugal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Abstract
The invention relates to a method for preparing nano-copper. The method comprises the following steps of: dispersing a copper precursor into the liquid paraffin serving as a solvent and a reducing agent; adding a surfactant into the liquid paraffin with stirring; performing heat treatment for 2 to 4 hours in an atmosphere of N2 protective gas or no protective gas; standing; centrifuging to obtain a product; and alternately washing the product by using petroleum ether, distilled water or absolute ethyl alcohol to obtain the nano-copper. The nano-copper powder prepared by using the method has the advantages of particle sizes of less than 50 nm, uniform distribution, difficult oxidation, high dispersibility in polar solvents or non-polar solvents, cheap raw materials, low energy consumption, simple process equipment and easy large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of Nanometer Copper, especially a kind of particle diameter is less than the preparation method of 50nm copper powders may.
Background technology
It is little that nanometer technology copper and compound thereof have size, specific area reaches greatly the characteristics such as quantum size effect and macro quanta tunnel effect, make it not only can be used as catalyst and directly apply to chemical industry, also can be used for making electrocondution slurry (conducting resinl, magnetic-conductive adhesive), " super moulding " steel, gas sensor, advanced lubrication oil additive, also be high conductivity, the indispensable basic material of high-intensity nanometer copper material simultaneously.Therefore the research of relevant copper preparations of nanomaterials, performance and application at home and abroad receives much attention in recent years.The preparation method that Nanometer Copper is commonly used has electric radiation method, gas phase steam method, mechanochemical reaction, solvent-thermal method, thermal decomposition method, chemical reduction method etc.Although wherein Radiation Synthesis Method preparation technology is simple, granularity is easily controlled, productive rate is high, particle generates and protection such as can realize synchronously at the advantage, the product that obtains is in the dispersoid state, collects very difficultly, is difficult for scale.Solvent-thermal method working pressure device requires height to device materials, and condition is relatively harsh, is difficult for extension and generates.Mechanochemical reaction technique is simple, can prepare compound, nanometer metal ceramic composite etc. between the solid solution, nano metal of the refractory metal that other conventional methods are difficult to prepare, mutual insoluble system, but it is inhomogeneous that shortcoming is crystal, easily introduces impurity in the mechanical milling process.Plasma method equipment is simple, easy to operate, speed of production is fast, almost can prepare any simple metal nano powder, but energy consumption is large, and the high temperature bottom electrode is easy to fusing or steam and pollution products.Thermal decomposition method is with respect to additive method, quicker, economic and cleaning, but realize control technology to particle diameter and pattern is that all right ripe, also have distance from commercial Application.General chemical reduction method can obtain by the selection of technological parameter and reducing agent the product of different-grain diameter; but used reducing agent is generally ascorbic acid, formaldehyde, hypophosphites, boron hydride, hydrazine hydrate etc.; perhaps poisonous, perhaps expensive, be unfavorable for large-scale production.Prepare the method for Nanometer Copper and reduce the mantoquita predecessor with the hydroperoxyl radical that atoleine is produced when the Pintsch process; not only have the atoleine raw material cheap and easy to get also reusable, do not need special reaction unit; equipment is simple; with low cost; granularity, pattern are easily controlled; and product generates and prevents from reuniting and realize synchronously, and the advantage such as large-scale production very easily has important theory significance and use value to the application of further expansion Nanometer Copper material.
Summary of the invention
Cost was high when the present invention was intended to solve chemical method and prepares Nanometer Copper, and is poisonous and be not easy to the difficult problem of large-scale production, and a kind of easy, high yield, low cost are provided, environmental friendliness and be easy to the preparation method of the stabilized nanoscale copper of large-scale production.
The present invention realizes that above-mentioned purpose is to realize by following measures:
A kind of preparation method of Nanometer Copper is characterized in that the method specifically may further comprise the steps:
The mantoquita predecessor directly is dispersed in the atoleine, under agitation adds surfactant, then at N
2Protection is lower or do not have the protective gas existence lower, heat-treats 3-8h.
A, leave standstill, centrifugal, discard supernatant liquor and collect solid.
B, with gained solid benzinum among the B, distilled water and absolute ethyl alcohol alternately washing to obtain powder solid be copper nano-particle.
The mantoquita predecessor can be the crystal salt of Kocide SD, basic copper carbonate, copper nitrate, Schweinfurt green and copper sulphate among the present invention, also can be the aqueous solution of the crystal salt of copper nitrate, Schweinfurt green and copper sulphate, the complex that the hydrolysis of ethanol solution and corresponding salt, the colloid of alcoholysis or corresponding salt and part form.
Surfactant can be Span-80, Tween-80, Tween-85, PVP, PVA, PEG600, CTAB, SDS, acrylamide, oleyl amine, the single or composite use such as oleamide.
Can be diethanol amine with the part of mantoquita complexing, triethanolamine, the schiff bases that ethylenediamine or these amine and salicylide form, DMF, catechol, amion acetic acid, ortho-aminobenzoic acid, o-aminophenol etc., also can be that other contain N, the organic ligand of O coordination center, or wherein one or more mating reaction.
The mol ratio of mantoquita and atoleine is: 1: 25～1: 120;
The mol ratio of mantoquita and surfactant is: 200: 1～2: 1;
The mol ratio of mantoquita and part is: 1: 4～1: 6;
The preparation method of a kind of Nanometer Copper of the present invention adopts technique scheme, take mantoquita as raw material, take atoleine as solvent with reducing agent, after treatment, uses benzinum, distilled water or absolute ethanol washing again, makes Nanometer Copper at air drying.Raw materials used cheap and easy to get, simple process, equipment is simple, with low cost, productive rate is higher.Prepared nano copper particle particle diameter is evenly distributed, gained Nanometer Copper powder granularity through Instrument measuring all less than 50nm, and in air, be difficult for oxidation, can stable dispersion in industrial polarity, the nonpolar organic-inorganic solvents such as lube base oil and benzotrichloride, benzene, benzinum, absolute ethyl alcohol, distilled water, be fit to large-scale industrial production, have widely industrial use.
Description of drawings
Fig. 1 is the XRD figure of product of the present invention;
Fig. 2 is the SEM figure of product of the present invention;
Fig. 3 is the TEM figure of product of the present invention.
The specific embodiment
For a better understanding of the present invention, describe by following examples.
Embodiment 1
Predecessor is that mantoquita prepares Nanometer Copper, carries out in accordance with the following steps:
(1) with the copper nitrate of 0.01mol (commercially available, analyze pure, molecular formula Cu (NO
3)
23H
2O), grind below 100 orders, add in the 150ml atoleine while stir, add 20ml span-80, stir 1h;
(2) until copper nitrate in mixed liquor, be uniformly dispersed be the blue-green clear emulsion after, pour the 500ml three-neck flask into, logical N
2, continue to stir, slowly be warmed up to 300 ℃, keep 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
The preparation of Nanometer Copper, carry out in accordance with the following steps:
(1) with the Kocide SD of 0.01mol (commercially available, analyze pure, molecular formula Cu (OH)
2), grind below 100 orders, add in the 150ml atoleine while stir, add 20ml span-80, stir 1h;
(2) until copper nitrate in mixed liquor, be uniformly dispersed be the blue-green clear emulsion after, pour the 500ml three-neck flask into, logical N
2, continue to stir, slowly be warmed up to 300 ℃, keep 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 3
Predecessor is that copper salt solution prepares Nanometer Copper, carries out in accordance with the following steps:
(1) with the copper nitrate of 0.01mol (commercially available, analyze pure, molecular formula Cu (NO
3)
23H
2O), be dissolved in the absolute ethyl alcohol that 20ml contains 1.0g PVA, add Tween 85 on one side and stirs and add in the 150ml atoleine adding 20mlspan-80, stirring 1h;
(2) until copper nitrate in mixed liquor, be uniformly dispersed be the blue-green clear emulsion after, pour the 500ml three-neck flask into, logical N
2, continue to stir, slowly be warmed up to 300 ℃, keep 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 4
The preparation of Nanometer Copper, carry out in accordance with the following steps:
(1) with the copper nitrate of 0.01mol (commercially available, analyze pure, molecular formula Cu (NO
3)
23H
2O), be dissolved in the distilled water that 20ml contains 1.0g SDS and CTAB, add in the 150ml atoleine while stir, add 5ml span-80, stir 1h;
(2) until copper nitrate in mixed liquor, be uniformly dispersed be the blue-green clear emulsion after, pour the 500ml three-neck flask into, logical N
2, continue to stir, slowly be warmed up to 300 ℃, keep 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 5
Predecessor is that colloid prepares Nanometer Copper, carries out according to following steps:
(1) with the Schweinfurt green of 0.02mol (commercially available, analyze pure, molecular formula Cu (CH
3COO)
2H
2O) be dissolved in the 15ml absolute ethyl alcohol, add the 1.0g oleamide, in 45 ℃ of water-baths, stir lower reaction 2h, namely get colloid;
(2) with gained colloid in (1), aging 1-3d changes in the 200ml atoleine, is warming up to gradually 200 ℃, reaction 5h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 6
Predecessor is the preparation Nanometer Copper of the complex compound of mantoquita, carries out according to the following steps:
(1) with the copper sulphate of 0.02mol (commercially available, analyze pure, molecular formula CuSO
45H
2O), be dissolved in the 20ml absolute ethyl alcohol, 45 ℃ of water-baths, under the magnetic agitation, the concentrated ammonia liquor titration becomes glue;
(2) gained colloid in (1) is added in the 150ml atoleine, add 1ml Span-80,20ml PEG600, N
2Protection is lower, and mechanical agitation is warming up to 200 ℃ gradually, heat treatment 5h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each 5 times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 7
Predecessor is the preparation Nanometer Copper of the complex compound of mantoquita, carries out according to the following steps:
(1) with the copper sulphate of 0.02mol (commercially available, analyze pure, molecular formula CuSO
45H
2O) be dissolved in the 20ml distilled water that contains 1.0g PVP, it is about 8 that NaOH transfers PH, becomes glue;
(2) gained colloid in (1) is added in the 150ml atoleine, add 2ml Tween-80, unprotect gas exists lower, and mechanical agitation is warming up to 250 ℃ gradually, heat treatment 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each 3 times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 8
Predecessor is the preparation Nanometer Copper of mantoquita complex compound, carries out according to the following steps:
(1) with the Schweinfurt green of 0.01mol (commercially available, analyze pure, molecular formula CH
3COO)
2H2O) be dissolved in the 20ml absolute methanol, add again 0.02mol by the Schiff base ligand of salicylide and ethylenediamine preparation, fully stirring and dissolving.
(2) gained colloid in (1) is added in the 150ml atoleine, add 3ml Span-85, N
2Protection is lower, and mechanical agitation is warming up to 250 ℃ gradually, heat treatment 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 9
Predecessor is the preparation Nanometer Copper of mantoquita complex compound, carries out according to the following steps:
(1) the 0.04mol ortho-aminobenzoic acid is dissolved in the 20ml absolute ethyl alcohol, stir lower add the copper nitrate that contains 0.01mol (commercially available, analyze pure, molecular formula Cu (NO
3)
23H
2O) 20ml distilled water, 35 ℃ of water-baths become glue.
(2) gained colloid in (1) is added in the 100ml atoleine, add the 2ml oleyl amine, N
2Protection is lower, and mechanical agitation is warming up to 225 ℃ gradually, heat treatment 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 10
Predecessor is the preparation Nanometer Copper of mantoquita complex compound, carries out according to the following steps:
(1) 0.04mol o-aminophenol and 0.02mol amion acetic acid are dissolved in the 30ml absolute ethyl alcohol, stir lower add the copper nitrate that contains 0.01mol (commercially available, analyze pure, molecular formula Cu (NO
3)
23H
2O) 20ml distilled water, 35 ℃ of water-baths become glue.
(2) gained colloid in (1) is added in the 150ml atoleine, add the 2g oleamide, N
2Protection is lower, and mechanical agitation is warming up to 250 ℃ gradually, heat treatment 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 4 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 11
Predecessor is the preparation Nanometer Copper of mantoquita complex compound, carries out according to the following steps:
(1) 0.04mol o-aminophenol and 0.02mol amion acetic acid are dissolved in the 30ml absolute ethyl alcohol, stir lower add the copper nitrate that contains 0.01mol (commercially available, analyze pure, molecular formula Cu (NO
3)
23H
2O) 20ml distilled water, 35 ℃ of water-baths become glue.
(2) gained colloid in (1) is added in the 100ml atoleine, add the 2g oleamide, N
2Protection is lower, and mechanical agitation is warming up to 250 ℃ gradually, heat treatment 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 5 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 12
Predecessor is the preparation Nanometer Copper of mantoquita complex compound, carries out according to the following steps:
(1) with the copper nitrate of 0.02mol (commercially available, analyze pure, molecular formula Cu (NO
3)
23H
2O) be dissolved in 8.3ml DMF.
(2) gained solution in (1) is added in the 100ml atoleine, add 2ml Span80, unprotect gas exists lower, and mechanical agitation is warming up to 250 ℃ gradually, heat treatment 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 5 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 13
Predecessor is the preparation Nanometer Copper of mantoquita complex compound, carries out according to the following steps:
(1) with the copper nitrate of 0.02mol (commercially available, analyze pure, molecular formula Cu (NO
3)
23H
2O) be dissolved in the 15ml diethylamine.
(2) gained solution in (1) is added in the 100ml atoleine, unprotect gas exists lower, and mechanical agitation is warming up to 250 ℃ gradually, heat treatment 4h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 5 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Embodiment 14
Predecessor is the preparation Nanometer Copper of mantoquita complex compound, carries out according to the following steps:
(1) with the copper nitrate of 0.02mol (commercially available, analyze pure, molecular formula Cu (NO
3)
23H
2O) be dissolved in the 15ml triethanolamine.
(2) gained solution in (1) is added in the 100ml atoleine, it is lower to add the existence of 5ml Span-80 unprotect gas, and mechanical agitation is warming up to 250 ℃ gradually, heat treatment 3h;
(3) with (2) products therefrom centrifugation, discard upper strata oil, stay sediment;
(4) (3) gained sediment is used first petroleum ether 5 times, centrifugal, stay sediment;
(5) (4) gained sediment is alternately washed each three times with distilled water and absolute ethyl alcohol, centrifugal;
(6) (5) gained sediment is at room temperature natural drying, namely the nanometer powder particle diameter of system is less than the Nanometer Copper of 50nm.
Claims (2)
1. the preparation method of a Nanometer Copper, its method is as follows;
Take atoleine as solvent with reducing agent, the mantoquita predecessor directly is dispersed in the atoleine, under agitation add surfactant; Under nitrogen protection, be warming up to 200-300 ℃ and heat-treat, heat treatment time 3-5h; Again with the product after the above-mentioned heat treatment through leaving standstill, centrifugal and filter, with the alternately washing of benzinum, distilled water, absolute ethyl alcohol, in air drying or 80-100 ℃ of oven dry under nitrogen atmosphere, namely make the copper powders may particle diameter less than the Nanometer Copper of 50nm;
Described mantoquita predecessor is the complex of the crystal salt of the crystal salt alcoholysis gained colloid of copper nitrate, acetic acid copper and copper sulfate or copper nitrate, Schweinfurt green, copper sulphate, described complex is the four ammino copper complex ions that above-mentioned crystal salt and ammoniacal liquor generate, or above-mentioned crystal salt and the formed complex ion of diethylamine, diethanol amine or triethanolamine, or the complex ion of the schiff bases of salicylide and ethylenediamine preparation and the formation of above-mentioned crystal salt.
2. method as claimed in claim 1, its surfactant is Span-80, Tween-80, PVP, PVA, triethanolamine, ethylenediamine, Tween-85, PEG600, SDS, CTAB, acrylamide, oleyl amine, or the single or composite use of oleamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010244071 CN101890506B (en) | 2010-07-31 | 2010-07-31 | Method for preparing nano-copper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010244071 CN101890506B (en) | 2010-07-31 | 2010-07-31 | Method for preparing nano-copper |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101890506A CN101890506A (en) | 2010-11-24 |
| CN101890506B true CN101890506B (en) | 2013-04-24 |
Family
ID=43099938
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010244071 Expired - Fee Related CN101890506B (en) | 2010-07-31 | 2010-07-31 | Method for preparing nano-copper |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101890506B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104668581A (en) * | 2015-03-09 | 2015-06-03 | 浙江工业大学 | Method for preparing copper hollow micro-spheres with solvothermal method |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102371358A (en) * | 2011-11-18 | 2012-03-14 | 复旦大学 | Aqueous-phase preparation method for re-dispersible nano-copper particles |
| CN102557297B (en) * | 2011-12-31 | 2013-10-02 | 重庆重冶铜业有限公司 | Treatment method of waste liquid after cleaning copper plated layer of printed circuit board |
| CN102837004B (en) * | 2012-09-25 | 2015-02-04 | 吉林大学 | Preparation method of polyhedral copper nanoparticle |
| CN103194616B (en) * | 2013-04-08 | 2014-07-30 | 吉林大学 | Method for preparing copper nanocrystalline |
| CN108907221A (en) * | 2018-06-10 | 2018-11-30 | 江苏经贸职业技术学院 | A kind of synthetic method of copper nano-cluster |
| CN109806913B (en) * | 2019-03-12 | 2022-05-31 | 南京信融环保新材料有限公司 | Denitration catalyst applied to cement plant and preparation method thereof |
| CN110125433A (en) * | 2019-05-05 | 2019-08-16 | 上海交通大学 | A method of preparing copper nanoparticle at room temperature |
| CN110152676B (en) * | 2019-05-21 | 2022-02-18 | 太原理工大学 | Preparation method of anti-sintering metal catalyst |
| CN110153443A (en) * | 2019-07-11 | 2019-08-23 | 中国科学院深圳先进技术研究院 | A kind of copper nanometer sheet and its preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618799A (en) * | 2003-11-21 | 2005-05-25 | 河南大学 | Metal coppor nano-particle and its preparation process and use |
| CN1686648A (en) * | 2005-04-26 | 2005-10-26 | 黄德欢 | Preparation method of nano-bronze powder |
| CN1693204A (en) * | 2005-04-26 | 2005-11-09 | 黄德欢 | Process for preparing nano cuprous oxide powder |
| CN1837288A (en) * | 2005-03-25 | 2006-09-27 | 浙江工业大学 | Temperature sensitive composite materials and preparing process thereof |
-
2010
- 2010-07-31 CN CN 201010244071 patent/CN101890506B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618799A (en) * | 2003-11-21 | 2005-05-25 | 河南大学 | Metal coppor nano-particle and its preparation process and use |
| CN1837288A (en) * | 2005-03-25 | 2006-09-27 | 浙江工业大学 | Temperature sensitive composite materials and preparing process thereof |
| CN1686648A (en) * | 2005-04-26 | 2005-10-26 | 黄德欢 | Preparation method of nano-bronze powder |
| CN1693204A (en) * | 2005-04-26 | 2005-11-09 | 黄德欢 | Process for preparing nano cuprous oxide powder |
Non-Patent Citations (1)
| Title |
|---|
| 樊金串等.表面活性剂对完全液相法制Cu-Zn-Al浆状催化剂结构和性能的影响.<<高等学校化学学报>>.2008,第29卷(第5期),第993-999页. * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104668581A (en) * | 2015-03-09 | 2015-06-03 | 浙江工业大学 | Method for preparing copper hollow micro-spheres with solvothermal method |
| CN104668581B (en) * | 2015-03-09 | 2017-03-08 | 浙江工业大学 | A kind of method that solvent-thermal method prepares copper tiny balloon |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101890506A (en) | 2010-11-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101890506B (en) | Method for preparing nano-copper | |
| CN103934468B (en) | The supercritical water process for thermosynthesizing of nano metal or metal oxide nano particles | |
| CN105798320A (en) | Method for preparing nanometer copper powder at low temperature | |
| CN104014811B (en) | A kind of octreotide acetate that utilizes is for the method for Template preparation coralloid nano cobalt | |
| CN102672199B (en) | Preparation method of silver particle with sheet-strip integrated structural shape | |
| CN103962570A (en) | Preparation method of nickel nanopowder | |
| CN104310458B (en) | A kind of method preparing zinc oxide nano rod | |
| CN103396356B (en) | Spirofluorene copper pyridine micro-nano particle and preparation method thereof | |
| CN111922360B (en) | Preparation method of nano copper powder | |
| CN107498068A (en) | A kind of preparation method of flower-like nanometer copper | |
| CN106623971A (en) | Nano-silver particles for conductive ink and preparation method of nano-silver particles | |
| CN102849774A (en) | Method for preparing nanometer cerium oxide by hydrothermal method | |
| CN108855217B (en) | Preparation method and application of copper-based metal organic framework nano sheet | |
| CN111496266A (en) | Environment-friendly conductive nano copper ink and preparation method thereof | |
| CN105668606B (en) | A kind of preparation method of square nano-sheet cerium oxide | |
| CN104625082A (en) | Nanometer nickel powder preparation method | |
| CN105215347A (en) | A kind of zinc oxide and gold nano grain composite and preparation method thereof | |
| CN103224831B (en) | A kind of electrorheological fluid and preparation method thereof | |
| CN101406963B (en) | Method for preparing nano silver powder | |
| CN104030341B (en) | The preparation method of copper oxide nano material | |
| CN105290414A (en) | Method for synthesizing nano-copper particles | |
| CN104445340A (en) | Method for preparing octahedral cerium oxide self-assembled by nano blocks | |
| CN103950981B (en) | A kind of preparation method of zinc molybdate micro mist | |
| CN103145173B (en) | Preparation method of copper sulphide classified nanometer structure material | |
| CN107043133B (en) | Flower-shaped γ Fe2O3The preparation method of microballoon |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130424 Termination date: 20130731 |