CN101698496B - Preparation method of electronic grade high-purity copper oxide superfine powder - Google Patents
Preparation method of electronic grade high-purity copper oxide superfine powder Download PDFInfo
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- CN101698496B CN101698496B CN2009101934046A CN200910193404A CN101698496B CN 101698496 B CN101698496 B CN 101698496B CN 2009101934046 A CN2009101934046 A CN 2009101934046A CN 200910193404 A CN200910193404 A CN 200910193404A CN 101698496 B CN101698496 B CN 101698496B
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Abstract
The invention discloses a preparation method of electronic grade high-purity copper oxide superfine powder, comprising the following steps: copper nitrate is dissolved in dilute nitric acid to prepare copper nitrate solution, and the mole ratio of the copper nitrate and the dilute nitric acid is 1:1-1:4; the copper nitrate solution is placed in a vessel, ammonia water solution is dropwise added under the stirring condition, the pH value is controlled to be 9-11, so as to obtain precursor sediment; the precursor sediment is washed and filtered by deionized water and absolute alcohol; ultrasonic oscillating dispersion is carried out for 15-20min, and then filtration and vacuum drying are carried out; calcination is carried out for 2.5 hours at 235 DEG C, so as to obtain the electronic grade high-purity copper oxide superfine powder. In the method, potassium hydroxide solution or sodium hydroxide solution is replaced by ammonia water without leading in other impurities in solution, so as to ensure high purity of copper oxide powder, and the purity of the copper oxide powder can reach more than 99.9 percent; by adopting the ultrasound dispersion technology, superfine copper oxide powder with small mean grain size and narrow particle size distribution range can be obtained.
Description
Technical field
The invention belongs to chemical production field, particularly a kind of preparation method of electronic grade high-purity copper oxide superfine powder.
Background technology
The ultrafine copper oxide powder has basic physical influence such as peculiar surface effects, volume effect, quantum size effect, macro quanta tunnel effect, and this makes it have character such as special electricity, optics, catalysis.The ultrafine copper oxide powder has been applied to fields such as catalytic material, sensing material, and demonstrates good application prospects.
The preparation method of ultrafine copper oxide powder can be divided into two big classes by character: physics method and chemical method.The physics method mainly is to use external force such as mechanical force, makes conventional bulk or powder material be ground into ultra-fine nano-powder.Conventional machinery comminuting method in the physics method is difficult to obtain the ultrafine powder of particle diameter less than 100nm, and crushing process is also easily sneaked into impurity, and particle shape be difficult to control, difficulty reaches industrial application requirements.Chemical method can be divided into solid phase method, liquid phase method and vapor phase process again.The powder that solid phase method makes often has the shortcomings such as the easy reunion of particle that globule size differs, chemical constitution is inhomogeneous, generate.Liquid phase method can make that particle is thin, narrow particle size distribution, particulate that purity is high, but the energy consumption height, the time is long, environmental pollution is serious.Vapor phase process has the Technology complexity, cost height, the shortcoming that one-time investment is big.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, the object of the present invention is to provide a kind of preparation method of electronic grade high-purity copper oxide superfine powder.Technology of the present invention is simple, and is with low cost, and can to prepare particle diameter be 1.3～1.6 microns.
Purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of electronic grade high-purity copper oxide superfine powder is characterized in that comprising following operation steps:
(1) preparation of copper nitrate solution: cupric nitrate is dissolved in rare nitric acid is made into copper nitrate solution; The mass ratio of described cupric nitrate and rare nitric acid is 1: 1～1: 4;
(2) the sedimentary preparation of presoma: step (1) gained copper nitrate solution is placed container, dropping ammonia solution under agitation condition, control pH value is 9～11, prepares the presoma throw out;
(3) preparation of copper oxide superfine powder: step (2) gained precursor sediment with deionized water and absolute ethanol washing, is filtered; Ultrasonic oscillation disperses 15～20min, filters, and vacuum-drying is 1～2 hour under 80～90 ℃ of conditions; Calcined 2.5 hours down at 230～240 ℃ then, obtain electronic grade high-purity copper oxide superfine powder.
The mass percent concentration of the described rare nitric acid of step (1) is 5%.
The stir speed (S.S.) of the described stirring of step (2) is 1000～2000r/min; The volumetric molar concentration of described ammonia soln is 5～10mol/L; Described dropping ammonia is that the speed of ammoniacal liquor with 2～10mL/min is dripped.
It is to adopt 50KHz～10MHz ultrasonic frequency to carry out vibrating dispersion that the described ultra-sonic oscillation of step (3) are disperseed.
The particle size range of the described copper oxide superfine powder of step (3) is 1.3～1.6 microns.
A kind of electronic grade high-purity copper oxide superfine powder according to method for preparing.
Above-mentioned electronic grade high-purity copper oxide superfine powder is applied to prepare catalytic material or sensing material.
The present invention compared with prior art, have following advantage and beneficial effect: among (1) preparation method of the present invention, replace potassium hydroxide solution or sodium hydroxide solution with ammoniacal liquor, can not introduce other impurity in the solution, guaranteed the high purity of cupric oxide powder, the purity of gained cupric oxide powder is that the content of metallic impurity Fe, Pb, Zn, Ni, Co, Cd, Mn is all below 2ppm more than 99.9% by percentage to the quality; (2) the present invention adopts the ultra-sonic dispersion technology, can obtain the ultrafine copper oxide powder that median size is little, particle size distribution is narrow.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) preparation of copper nitrate solution: it is to be made into copper nitrate solution in 5% rare nitric acid that cupric nitrate is dissolved in mass percent concentration; The mass ratio of described cupric nitrate and rare nitric acid is 1: 1;
(2) the sedimentary preparation of presoma: step (1) gained copper nitrate solution is placed reactor, under 1000r/min speed agitation condition, with the speed dropping ammonia solution (volumetric molar concentration is 5mol/L) of 2mL/min, control pH value is 9, prepares the presoma throw out;
(3) preparation of copper oxide superfine powder: step (2) gained precursor sediment with deionized water and absolute ethanol washing, is filtered; Use the ultrasonic oscillation of 50KHz to disperse 15min, filter, vacuum-drying is 1 hour under 80 ℃ of conditions; Calcined 2.5 hours down at 240 ℃ then, obtain electronic grade high-purity copper oxide superfine powder; After testing, the purity of this copper oxide superfine powder is 99.95% by percentage to the quality, the content of metallic impurity Fe, Pb, Zn, Ni, Co, Cd, Mn all≤2ppm; From 8000 times of electron microscope photo scannings as seen, morphology microstructure is complete, and particle diameter is 1.3 ± 0.4 microns, and good dispersity does not have agglomeration.
Embodiment 2
(1) preparation of copper nitrate solution: cupric nitrate is dissolved in mass percent counts in rare nitric acid of 5% and be made into copper nitrate solution; The mass ratio of described cupric nitrate and rare nitric acid is 1: 4;
(2) the sedimentary preparation of presoma: step (1) gained copper nitrate solution is placed reactor, under 2000r/min speed agitation condition, with the speed dropping ammonia solution (volumetric molar concentration is 10mol/L) of 2mL/min, control pH value is 11, prepares the presoma throw out;
(3) preparation of copper oxide superfine powder: step (2) gained precursor sediment with deionized water and absolute ethanol washing, is filtered; Use the ultrasonic oscillation of 1MHz to disperse 20min, filter, vacuum-drying is 2 hours under 80 ℃ of conditions; Calcined 2.5 hours down at 235 ℃ then, obtain electronic grade high-purity copper oxide superfine powder; After testing, the purity of this copper oxide superfine powder is 99.93% by percentage to the quality, the content of metallic impurity Fe, Pb, Zn, Ni, Co, Cd, Mn all≤2ppm; From 8000 times of electron microscope photo scannings as seen, morphology microstructure is complete, and particle diameter is 1.6 ± 0.4 microns, and good dispersity does not have agglomeration.
Embodiment 3
(1) preparation of copper nitrate solution: it is to be made into copper nitrate solution in rare nitric acid of 5% that cupric nitrate is dissolved in mass percent concentration; The mass ratio of described cupric nitrate and rare nitric acid is 1: 3;
(2) the sedimentary preparation of presoma: step (1) gained copper nitrate solution is placed reactor, under 1500r/min speed agitation condition, with the speed dropping ammonia solution (volumetric molar concentration is 5mol/L) of 5mL/min, control pH value is 9, prepares the presoma throw out;
(3) preparation of copper oxide superfine powder: step (2) gained precursor sediment with deionized water and absolute ethanol washing, is filtered; Use the ultrasonic oscillation of 5MHz to disperse 18min, filter, vacuum-drying is 1 hour under 90 ℃ of conditions; Calcined 2.5 hours down at 230 ℃ then, obtain electronic grade high-purity copper oxide superfine powder; After testing, the purity of this copper oxide superfine powder is 99.97% by percentage to the quality, the content of metallic impurity Fe, Pb, Zn, Ni, Co, Cd, Mn all≤2ppm; From 8000 times of electron microscope photo scannings as seen, morphology microstructure is complete, and particle diameter is 1.5 ± 0.4 microns, and good dispersity does not have agglomeration.
Embodiment 4
(1) preparation of copper nitrate solution: it is to be made into copper nitrate solution in rare nitric acid of 5% that cupric nitrate is dissolved in mass percent concentration; The mass ratio of described cupric nitrate and rare nitric acid is 1: 2.5;
(2) the sedimentary preparation of presoma: step (1) gained copper nitrate solution is placed reactor, under 1200r/min speed agitation condition, with the speed dropping ammonia solution (volumetric molar concentration is 7mol/L) of 7mL/min, control pH value is 10, prepares the presoma throw out;
(3) preparation of copper oxide superfine powder: step (2) gained precursor sediment with deionized water and absolute ethanol washing, is filtered; Use the ultrasonic oscillation of 10MHz to disperse 20min, filter, vacuum-drying is 1.5 hours under 80 ℃ of conditions; Calcined 2.5 hours down at 240 ℃ then, obtain electronic grade high-purity copper oxide superfine powder; After testing, the purity of this copper oxide superfine powder is 99.96% by percentage to the quality, the content of metallic impurity Fe, Pb, Zn, Ni, Co, Cd, Mn all≤2ppm; From 8000 times of electron microscope photo scannings as seen, morphology microstructure is complete, and particle diameter is 1.4 ± 0.4 microns, and good dispersity does not have agglomeration.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (4)
1. the preparation method of an electronic grade high-purity copper oxide superfine powder is characterized in that comprising following operation steps:
(1) preparation of copper nitrate solution: cupric nitrate is dissolved in rare nitric acid is made into copper nitrate solution; The mass ratio of described cupric nitrate and rare nitric acid is 1: 1～1: 4; The mass percent concentration of described rare nitric acid is 5%;
(2) the sedimentary preparation of presoma: step (1) gained copper nitrate solution is placed container, dropping ammonia solution under agitation condition, control pH value is 9～11, prepares the presoma throw out;
(3) preparation of copper oxide superfine powder: step (2) gained precursor sediment with deionized water and absolute ethanol washing, is filtered; Ultrasonic oscillation disperses 15～20min, filters, and vacuum-drying is 1～2 hour under 80～90 ℃ of conditions; Calcined 2.5 hours down at 230～240 ℃ then, obtain electronic grade high-purity copper oxide superfine powder.
2. the preparation method of a kind of electronic grade high-purity copper oxide superfine powder according to claim 1, it is characterized in that: the stir speed (S.S.) of the described stirring of step (2) is 1000～2000r/min; The volumetric molar concentration of described ammonia soln is 5～10mol/L; Described dropping ammonia is that the speed of ammoniacal liquor with 2～10mL/min is dripped.
3. the preparation method of a kind of electronic grade high-purity copper oxide superfine powder according to claim 1 is characterized in that: it is to adopt 50KHz～10MHz ultrasonic frequency to carry out vibrating dispersion that the described ultra-sonic oscillation of step (3) are disperseed.
4. the preparation method of a kind of electronic grade high-purity copper oxide superfine powder according to claim 1, it is characterized in that: the particle size range of the described copper oxide superfine powder of step (3) is 1.3～1.6 microns.
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| CN102320644A (en) * | 2011-08-17 | 2012-01-18 | 金川集团有限公司 | Method for preparing copper-oxide powder |
| CN102602976A (en) * | 2012-03-09 | 2012-07-25 | 天津理工大学 | Method for preparing CuO nano-film |
| CN102941351B (en) * | 2012-11-27 | 2015-08-26 | 中国船舶重工集团公司第七一二研究所 | A kind of preparation method of superfine cupper powder |
| CN103071498B (en) * | 2013-01-14 | 2015-04-22 | 杜亚丽 | Preparation method of Cu2O compound photocatalyst |
| CN104985175B (en) * | 2015-07-02 | 2017-03-08 | 广东光华科技股份有限公司 | A kind of method for removing nano metal powder surface anion |
| CN110642284A (en) * | 2019-09-16 | 2020-01-03 | 浙江天能能源科技股份有限公司 | Preparation method of flower-shaped CuO negative electrode material |
| CN111269543B (en) * | 2020-03-31 | 2023-01-10 | 佛山市富臣新材料科技有限公司 | Preparation method of magnesium-doped flower-shaped copper oxide polylactic acid composite material |
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