CN1686645A - Method of preparing nano-bronze powder using electric deposition - Google Patents

Method of preparing nano-bronze powder using electric deposition Download PDF

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Publication number
CN1686645A
CN1686645A CN 200510049663 CN200510049663A CN1686645A CN 1686645 A CN1686645 A CN 1686645A CN 200510049663 CN200510049663 CN 200510049663 CN 200510049663 A CN200510049663 A CN 200510049663A CN 1686645 A CN1686645 A CN 1686645A
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copper
negative electrode
electric deposition
preparing nano
bronze powder
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CN1305618C (en
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黄德欢
李宗全
夏志平
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黄德欢
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Abstract

A process for preparing copper nanoparticles by electric deposition method includes dissolving Cu salt in distilled water, adding sulfuric acid, polyvinyl pyrrolidone and sodium laurysulfate, putting copper plates as positive and negative electrodes in said solution, applying pulse DC to deposit copper nanoparticles on the negative electrode, taking the copper nanoparticles, washing and vacuum drying.

Description

The method of preparing nano-bronze powder using electric deposition
Technical field
The present invention relates to prepare the method for copper nanoparticle, specifically, belong to the method for preparing nano-bronze powder using electric deposition.
Background technology
The lubricated oil additive of nanometer copper particle conduct can increase substantially the lubricating ability and the usefulness of lubricating oil, is with a wide range of applications.Usually prepare copper nanoparticle with inert gas evaporation-condensation method, chemical reduction method, its characteristics are respectively arranged, at production cost, respectively there is its deficiency the aspects such as influence of environment.Prepare the advantage that copper nanoparticle can be taken into account inert gas evaporation-condensation method, chemical reduction method with electrodeposition process, help preparing copper nanoparticle.
Summary of the invention
The object of the present invention is to provide a kind of method with preparing nano-bronze powder using electric deposition.
The method of preparing nano-bronze powder using electric deposition of the present invention, its step is as follows:
1) add mantoquita in distilled water, compound concentration is the copper salt solution of 0.1~1.0mol/L, treat mantoquita dissolving after, every liter adds strong acid 2~10ml, polyvinylpyrrolidone 10~30g, lauryl sodium sulfate 1~20g;
2) be positive and negative electrode with the copper coin, be seated in set by step 1) in the solution of preparation, feed the pulse direct current electric current, current density is 5~80mA/cm 2, the pulse duration is 0.01~15 second, depositing nano copper powder on negative electrode;
3) copper nanoparticle that deposits on the negative electrode is taken off, and clean with distilled water and ethanol;
4) copper nanoparticle after will cleaning gets final product in 40~80 ℃ of following vacuum drying.
Among the present invention, said mantoquita can be copper sulphate or copper chloride, and said strong acid is sulfuric acid or hydrochloric acid.
Preparation technology of the present invention is simple, and cost is low, and control the nucleation of crystal grain and grow up by the pulse duration, thus the size of control copper particle, the granularity of nanometer copper is 10 to 100nm.Because the influence of surfactant, nanometer copper particle loosely attached on the negative electrode, are easy to collect.This method water is economized, and helps environmental protection.
Description of drawings
Fig. 1 is the X-ray diffractogram of the copper nanoparticle that makes of embodiment 1, and the particle diameter of copper particle is 70nm;
Fig. 2 is the X-ray diffractogram of the copper nanoparticle that makes of embodiment 2, and the particle diameter of copper particle is 75nm;
Fig. 3 is the X-ray diffractogram of the copper nanoparticle that makes of embodiment 3, and the particle diameter of copper particle is 75nm.
The specific embodiment
Embodiment 1
1) add copper sulphate in distilled water, compound concentration is the copper-bath of 0.5mol/L, treat copper sulphate dissolving after, every liter of solution adds sulfuric acid 3ml, polyvinylpyrrolidone 15g, lauryl sodium sulfate 1g;
2) be positive and negative electrode with the copper coin, be seated in set by step 1) in the solution of preparation, feed the pulse direct current electric current, current density is 25mA/cm 2, the pulse duration is 4 seconds, depositing nano copper powder on negative electrode;
3) copper nanoparticle that deposits on the negative electrode is taken off, clean 3 times with ethanol with distilled water, back earlier;
4) copper nanoparticle after will cleaning is put into vacuum drying chamber, 70 ℃ dry down, obtain copper nanoparticle.Fig. 1 is the X-ray diffractogram of the nanometer copper that makes, and the particle diameter of copper particle is 70nm.
Embodiment 2
1) add copper sulphate in distilled water, compound concentration is the copper-bath of 0.5mol/L, treat copper sulphate dissolving after, every liter of solution adds sulfuric acid 5ml, polyvinylpyrrolidone 1g, lauryl sodium sulfate 10g;
2) be positive and negative electrode with the copper coin, be seated in set by step 1) in the solution of preparation, feed the pulse direct current electric current, current density is 15mA/cm 2, the pulse duration is 4 seconds, depositing nano copper powder on negative electrode;
3) copper nanoparticle that deposits on the negative electrode is taken off, clean 3 times with ethanol with distilled water, back earlier;
4) copper nanoparticle after will cleaning is put into vacuum drying chamber, 70 ℃ dry down, obtain copper nanoparticle.Fig. 2 is the X-ray diffractogram of the nanometer copper that makes, and the particle diameter of copper particle is 75nm.
Embodiment 3
1) add copper chloride in distilled water, compound concentration is the copper chloride solution of 0.5mol/L, treat copper chloride dissolving after, every liter of solution adds hydrochloric acid 3ml, polyvinylpyrrolidone 15g, lauryl sodium sulfate 1g; 2) be positive and negative electrode with the copper coin, be seated in set by step 1) in the solution of preparation, feed the pulse direct current electric current, current density is 20mA/cm 2, the pulse duration is 6 seconds, depositing nano copper powder on negative electrode;
3) copper nanoparticle that deposits on the negative electrode is taken off, clean 3 times with ethanol with distilled water, back earlier;
4) copper nanoparticle after will cleaning is put into vacuum drying chamber, 70 ℃ dry down, obtain copper nanoparticle.Fig. 3 is the X-ray diffractogram of the nanometer copper that makes, and the particle diameter of copper particle is 75nm.

Claims (3)

1. the method for preparing nano-bronze powder using electric deposition is characterized in that may further comprise the steps:
1) add mantoquita in distilled water, compound concentration is the copper salt solution of 0.1~1.0mol/L, treat mantoquita dissolving after, every liter adds strong acid 2~10ml, polyvinylpyrrolidone 10~30g, lauryl sodium sulfate 1~20g;
2) be positive and negative electrode with the copper coin, be seated in set by step 1) in the solution of preparation, feed the pulse direct current electric current, current density is 5~80mA/cm 2, the pulse duration is 0.01~15 second, depositing nano copper powder on negative electrode;
3) copper nanoparticle that deposits on the negative electrode is taken off, and clean with distilled water and ethanol;
4) copper nanoparticle after will cleaning gets final product in 40~80 ℃ of following vacuum drying.
2. the method for preparing nano-bronze powder using electric deposition according to claim 1 is characterized in that said mantoquita is copper sulphate or copper chloride.
3. the method for preparing nano-bronze powder using electric deposition according to claim 1 is characterized in that said strong acid is sulfuric acid or hydrochloric acid.
CNB2005100496633A 2005-04-26 2005-04-26 Method of preparing nano-bronze powder using electric deposition Expired - Fee Related CN1305618C (en)

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WO2010107328A1 (en) * 2009-03-20 2010-09-23 Instytut Chemii Przemyslowej Im. Prof Ignacego Moscickiego Method for obtaining copper powders and nanopowders from industrial electrolytes including waste industrial electrolytes
CN101818365B (en) * 2009-09-23 2012-04-04 兰州理工大学 Method for preparing nano stibium powder
CN102978667A (en) * 2012-10-25 2013-03-20 烟台大学 Preparation method for nanometer copper powder through electro-deposition
CN103276412A (en) * 2013-05-29 2013-09-04 辽宁科技大学 Method for preparing copper or nickel powder and electrolysis device based on same
CN103639420A (en) * 2013-11-27 2014-03-19 昆明理工大学 Method for utilizing low co-fusion type ionic liquid electro-deposition to manufacture nanometer copper powder
CN105063664A (en) * 2015-07-24 2015-11-18 山东金宝电子股份有限公司 Additive for producing electrolytic copper powder of uniform particle diameter
CN105097297A (en) * 2014-05-08 2015-11-25 同济大学 Method for preparing high-activity nano-copper oxide serving as super-capacitor electrode material
CN107022772A (en) * 2017-06-20 2017-08-08 广东工业大学 A kind of nano copper slurry and preparation method thereof
CN108315771A (en) * 2018-02-11 2018-07-24 中国工程物理研究院材料研究所 A kind of electrochemical preparation method of sub-nanometer size copper particle elctro-catalyst
CN108468069A (en) * 2018-06-26 2018-08-31 中南大学 A method of copper powder is prepared using green surfactant
CN108517541A (en) * 2018-04-16 2018-09-11 沈阳建筑大学 A kind of electrochemical preparation method of Nanometer Copper powder
CN108677219A (en) * 2018-06-26 2018-10-19 中南大学 A method of superfine cupper powder is prepared using microemulsion
CN108677220A (en) * 2018-06-26 2018-10-19 中南大学 A kind of electrolyte being used to prepare Nano metal powder
CN108728871A (en) * 2018-06-26 2018-11-02 中南大学 A method of copper nanoparticle is prepared using fluorocarbon surfactant
CN108914164A (en) * 2018-08-09 2018-11-30 金陵科技学院 A method of Anti-Oxidation Copper Nanopowders are prepared from contained waste liquid recycling
CN110760892A (en) * 2019-11-15 2020-02-07 清华大学 Method for preparing metal particles by continuous electrochemical deposition

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US4028199A (en) * 1974-08-05 1977-06-07 National Development Research Corporation Method of producing metal powder
SU1090760A1 (en) * 1981-09-01 1984-05-07 Уральский Ордена Трудового Красного Знамени Научно-Исследовательский И Проектный Институт Медной Промышленности "Унипромедь" Method for producing copper powder
US6036839A (en) * 1998-02-04 2000-03-14 Electrocopper Products Limited Low density high surface area copper powder and electrodeposition process for making same
CN1234914C (en) * 2002-11-01 2006-01-04 中国科学院金属研究所 Nano twin crystal copper material with ultrahigh strength and superhigh conductivity as well as preparation method

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CN102362010A (en) * 2009-03-20 2012-02-22 内诺技术有限公司 Method for obtaining copper powders and nanopowders from industrial electrolytes including waste industrial electrolytes
WO2010107328A1 (en) * 2009-03-20 2010-09-23 Instytut Chemii Przemyslowej Im. Prof Ignacego Moscickiego Method for obtaining copper powders and nanopowders from industrial electrolytes including waste industrial electrolytes
EA021884B1 (en) * 2009-03-20 2015-09-30 Нано-Тек Сп. З.О.О. Method for obtaining copper powders and nanopowders from industrial electrolytes including waste industrial electrolytes
CN101818365B (en) * 2009-09-23 2012-04-04 兰州理工大学 Method for preparing nano stibium powder
CN102978667B (en) * 2012-10-25 2016-06-22 烟台大学 A kind of method of preparing nano-bronze powder using electric deposition
CN102978667A (en) * 2012-10-25 2013-03-20 烟台大学 Preparation method for nanometer copper powder through electro-deposition
CN103276412A (en) * 2013-05-29 2013-09-04 辽宁科技大学 Method for preparing copper or nickel powder and electrolysis device based on same
CN103276412B (en) * 2013-05-29 2015-10-21 辽宁科技大学 A kind of method and electrolyzer thereof preparing copper powder or nickel powder
CN103639420B (en) * 2013-11-27 2016-03-30 昆明理工大学 A kind of low melt type ionic liquid electrodeposition altogether prepares the method for copper nanoparticle
CN103639420A (en) * 2013-11-27 2014-03-19 昆明理工大学 Method for utilizing low co-fusion type ionic liquid electro-deposition to manufacture nanometer copper powder
CN105097297B (en) * 2014-05-08 2018-04-03 同济大学 The method for preparing high activity electrode material for super capacitor nano cupric oxide
CN105097297A (en) * 2014-05-08 2015-11-25 同济大学 Method for preparing high-activity nano-copper oxide serving as super-capacitor electrode material
CN105063664A (en) * 2015-07-24 2015-11-18 山东金宝电子股份有限公司 Additive for producing electrolytic copper powder of uniform particle diameter
CN107022772A (en) * 2017-06-20 2017-08-08 广东工业大学 A kind of nano copper slurry and preparation method thereof
CN108315771A (en) * 2018-02-11 2018-07-24 中国工程物理研究院材料研究所 A kind of electrochemical preparation method of sub-nanometer size copper particle elctro-catalyst
CN108517541A (en) * 2018-04-16 2018-09-11 沈阳建筑大学 A kind of electrochemical preparation method of Nanometer Copper powder
CN108677219A (en) * 2018-06-26 2018-10-19 中南大学 A method of superfine cupper powder is prepared using microemulsion
CN108468069A (en) * 2018-06-26 2018-08-31 中南大学 A method of copper powder is prepared using green surfactant
CN108677220A (en) * 2018-06-26 2018-10-19 中南大学 A kind of electrolyte being used to prepare Nano metal powder
CN108728871A (en) * 2018-06-26 2018-11-02 中南大学 A method of copper nanoparticle is prepared using fluorocarbon surfactant
CN108728871B (en) * 2018-06-26 2019-11-08 中南大学 A method of copper nanoparticle is prepared using fluorocarbon surfactant
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CN108914164A (en) * 2018-08-09 2018-11-30 金陵科技学院 A method of Anti-Oxidation Copper Nanopowders are prepared from contained waste liquid recycling
CN110760892A (en) * 2019-11-15 2020-02-07 清华大学 Method for preparing metal particles by continuous electrochemical deposition

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