CN1966187A - Method for preparing nano nickel powder in emulsion system - Google Patents
Method for preparing nano nickel powder in emulsion system Download PDFInfo
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- CN1966187A CN1966187A CN 200610070831 CN200610070831A CN1966187A CN 1966187 A CN1966187 A CN 1966187A CN 200610070831 CN200610070831 CN 200610070831 CN 200610070831 A CN200610070831 A CN 200610070831A CN 1966187 A CN1966187 A CN 1966187A
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Abstract
The invention relates to a method for preparing nanometer metal nickel powder, wherein the invention is characterized in that: it uses the W/O emulsion system formed by nickel sulfate solution/ sodium dodecylbenzene sulfonate/amyl alcohol/heptane as micro reactor; and it uses sodium borohydride to reduce nickel sulfate to prepare nanometer nickel particles; it can adjust time, to prepare the nanometer nickel powder at 20-50nm. The invention uses the instable property of emulsion, control stable time, to prepare the nanometer nickel powder with difference diameters, at normal temperature and pressure.
Description
Technical field
The present invention relates to the preparation method of nano metal nickel powder, belong to field of nanometer technology.Be applicable to the suitability for industrialized production of nanoscale nickel powder.
Background technology
Nickel is a kind of argenteous metal, has magnetic, electric conductivity and better chemical stability, high-temperature stability, mechanical stability.Nano-nickel powder has unique physics, chemical property as a kind of nanoscale metal material, is used widely in many fields such as battery material, catalyst, magnetic material, nano-coating material and carbide alloy bonding agents.Owing to have magnetic property, can be used as magnetic fluid; Because the huge and high activity of specific surface can be used as effective catalyst; Nano-nickel powder is added to the combustion heat, the efficiency of combustion that can increase substantially fuel in the solid fuel propellant of rocket, improve the stability of burning, can be used as high active combustion agent; Have good electrical conductivity, can be applicable to electrocondution slurry, multilayer ceramic capacitor and nickel-cadmium cell; Add suitable technology with nano-nickel powder is auxilliary, can produce electrode, can increase substantially discharging efficiency, can be used for high performance electrode material with huge surface area; Nanometer powder so have high energy state, just has strong caking power because surface area and surface atom proportion are all very big at a lower temperature, is a kind of effective activated sintering additive.
China has than the nickel resources of horn of plenty and strong exploitation, smelting ability.In recent years, because the fast development of automobile, electronics, machinery, information industry, constantly rose to the demand of nano-nickel powder in market.Can predict, the improvement of Preparation Method of Nanometer nickel Ultrafine will promote it and bring into play more importantly effect in national economy.At present, the preparation method of nano-nickel powder mainly contains multiple novel methods such as using vaporization condensation process, discharge-induced explosion silk method, sol-gel processing, hydro-thermal method, microemulsion method.
According to the literature survey result, the method for utilizing time control particle diameter to prepare nano-nickel powder in emulsion has not yet to see report.Compare with traditional preparation method, this legal system is equipped with nano-nickel powder, and to have an experimental provision simple, and processing ease can be controlled advantages such as granular size, good dispersion artificially.Applicability in operational simplification and the application provides a simple and easy preparation approach for the preparation of nanoparticle, particle size was controlled by the time, production output is compared with the output of microemulsion method preparation and is improved many times, makes it have very big development potentiality.
Summary of the invention
A kind of method that adopts emulsion to prepare nano-nickel powder provided by the invention is characterized in that it comprises the steps:
(1) preparation of nickelous sulfate emulsion
Add n-amyl alcohol, normal heptane in SDBS (neopelex), the stirred in water bath in uniform temperature mixes, and adds nickel sulfate solution, stirs, and gets nickelous sulfate clear (light green color) emulsion.
(2) preparation of nano-nickel powder
Nickelous sulfate emulsion preparation finish and stable certain hour after, in water bath with thermostatic control, nickelous sulfate emulsion is joined rapidly in the sodium borohydride of weighing, under agitation react a period of time, finish reaction.
(3) breakdown of emulsion separates
Wash breakdown of emulsion with acetone, the high speed centrifugation separated product after the washing several times, disperses with ultrasonic wave in absolute ethyl alcohol the back with the washing of 50% ethanol more several times, obtains nano-nickel powder.
The aforesaid operations process is all carried out under normal pressure, and step (1), (2) described water bath with thermostatic control temperature are 18-30 ℃.The described borane reducing agent sodium hydride of step (2) particle can prepare the nano-nickel powder of different-grain diameter in different time sections (promptly in different emulsion stabilization time), and this time period scope is 15-60 minute, mixing time 20-40 minute.
The present invention adopts W/O (Water-In-Oil) the type emulsion system of nickel sulfate solution/neopelex/n-amyl alcohol/normal heptane formation to prepare the nanoscale nickel particle as microreactor with the sodium borohydride reduction nickelous sulfate.
The electromicroscopic photograph that transmission electron microscope from figure is taken as can be seen.In this emulsion system, because crystallization is aqueous phase formation in the emulsion (W/O) in the confined space, so the particulate of preparation has high evenness and fine-grained characteristics, has improved surface-active, specific area greatly, has great skin effect and bulk effect.The pattern of prepared particulate is spherical.Not only particle size distribution is even to adopt the nano-nickel powder of emulsion preparation, and can regulate emulsion stabilization time as required, and to obtain the nano-nickel powder of different-grain diameter, particle diameter is 20-50nm.
Description of drawings
Fig. 1: the nanometer nickel transmission electron microscope photo of preparation method's example 4 of the present invention.
The specific embodiment
The present invention is described further with following embodiment:
Example 1: take by weighing 13.135gNiSO
46H
2O is dissolved in the suitable quantity of water, constant volume in the 50ml volumetric flask, the NiSO of preparation 1.0M
4The aqueous solution.Take by weighing 4.075g SDBS in triangular flask, add 10.0ml n-amyl alcohol, 26.0ml normal heptane, the stirred in water bath 25 ℃ of temperature mixes, and drips the above-mentioned NiSO of 2.0ml
4The aqueous solution is used DF-101S heat collecting type heated at constant temperature magnetic stirrer 2min (30r/min) simultaneously, and system forms nickelous sulfate clear (light green color) emulsion gradually.Take by weighing 0.114gNaBH
4(sodium borohydride) particle when treating that emulsion is stablized 15min, is poured into NaBH is housed in another triangular flask
4Triangular flask in, magnetic agitation (30r/min) 30min reacts completely Ni in 25 ℃ of waters bath with thermostatic control
2+Be reduced into nano nickle granules.In above-mentioned mixed liquor, add small amount of acetone, separate mother liquor and nickel powder sediment, clean repeatedly 2 times with acetone again, clean 2 times with 50% ethanol then with (3000rpm) LD5-2A centrifuge.Obtain the nano-nickel powder that particle diameter is 20nm.
Example 2: take by weighing 13.135gNiSO
46H
2O is dissolved in the suitable quantity of water, constant volume in the 50ml volumetric flask, the NiSO of preparation 1.0M
4The aqueous solution.Take by weighing 4.075g SDBS in triangular flask, add 10.0ml n-amyl alcohol, 26.0ml normal heptane, the stirred in water bath 25 ℃ of temperature mixes, and drips the above-mentioned NiSO of 2.0ml
4The aqueous solution is used DF-101S heat collecting type heated at constant temperature magnetic stirrer 2min (30r/min) simultaneously, and system forms nickelous sulfate clear (light green color) emulsion gradually.Take by weighing 0.114gNaBH
4(sodium borohydride) particle when treating that emulsion is stablized 30min, is poured into NaBH is housed in another triangular flask
4Triangular flask in, magnetic agitation (30r/min) 30min reacts completely Ni in 25 ℃ of waters bath with thermostatic control
2+Be reduced into nano nickle granules.In above-mentioned mixed liquor, add small amount of acetone, separate mother liquor and nickel powder sediment, clean repeatedly 2 times with acetone again, clean 2 times with 50% ethanol then with (3000rpm) LD5-2A centrifuge.Obtain the nano-nickel powder that particle diameter is 30nm.
Example 3: take by weighing 19.703gNiSO
46H
2O is dissolved in the suitable quantity of water, constant volume in the 50ml volumetric flask, the NiSO of preparation 1.5M
4The aqueous solution.Take by weighing 4.075g SDBS in triangular flask, add 10.0ml n-amyl alcohol, 26.0ml normal heptane, the stirred in water bath 25 ℃ of temperature mixes, and drips the above-mentioned NiSO of 2.0ml
4The aqueous solution is used DF-101S heat collecting type heated at constant temperature magnetic stirrer 2min (30r/min) simultaneously, and system forms nickelous sulfate clear (light green color) emulsion gradually.Take by weighing 0.114gNaBH
4(sodium borohydride) particle in another triangular flask, treat that emulsion is stablized 15min after, be poured into NaBH be housed
4Triangular flask in, magnetic agitation (30r/min) 30min reacts completely Ni in 25 ℃ of waters bath with thermostatic control
2+Be reduced into nano nickle granules.In above-mentioned mixed liquor, add small amount of acetone, separate mother liquor and nickel powder sediment, clean repeatedly 2 times with acetone again, clean 2 times with 50% ethanol then with (3000rpm) LD5-2A centrifuge.Obtain the nano-nickel powder that particle diameter is 33nm.
Example 4: take by weighing 13.135gNiSO
46H
2O is dissolved in the suitable quantity of water, constant volume in the 50ml volumetric flask, the NiSO of preparation 1.0M
4The aqueous solution.Take by weighing 4.075g SDBS in triangular flask, add 10.0ml n-amyl alcohol, 26.0ml normal heptane, the stirred in water bath 25 ℃ of temperature mixes, and drips the above-mentioned NiSO of 2.4ml
4The aqueous solution is used DF-101S heat collecting type heated at constant temperature magnetic stirrer 2min (30r/min) simultaneously, and system forms nickelous sulfate clear (light green color) emulsion gradually.Take by weighing 0.114gNaBH
4(sodium borohydride) particle when treating that emulsion is stablized 15min, is poured into NaBH is housed in another triangular flask
4Triangular flask in, magnetic agitation (30r/min) 30min reacts completely Ni in 25 ℃ of waters bath with thermostatic control
2+Be reduced into nano nickle granules.In above-mentioned mixed liquor, add small amount of acetone, separate mother liquor and nickel powder sediment, clean repeatedly 2 times with acetone again, clean 2 times with 50% ethanol then with (3000rpm) LD5-2A centrifuge.Obtain the nano-nickel powder that particle diameter is 40nm.
Claims (4)
1, a kind of method for preparing nano-nickel powder in emulsion system is characterized in that it may further comprise the steps:
(1) preparation of nickelous sulfate emulsion
Add n-amyl alcohol, normal heptane in SDBS (neopelex), the stirred in water bath in uniform temperature mixes, and adds nickel sulfate solution, stirs, and gets nickelous sulfate clear (light green color) emulsion.
(2) preparation of nano-nickel powder
Nickelous sulfate emulsion preparation finish and stable certain hour after, in water bath with thermostatic control, nickelous sulfate emulsion is joined rapidly in the sodium borohydride of weighing, under agitation react a period of time, finish reaction.
(3) breakdown of emulsion separates
Wash breakdown of emulsion with acetone, the high speed centrifugation separated product, wash 2-6 time after, with 50% ethanol washing 3-6 time, in absolute ethyl alcohol, disperse at last again with ultrasonic wave.Obtain nano-nickel powder.
2, the method that in emulsion system, prepares nano-nickel powder according to claim 1, it is characterized in that: this method is carried out under normal pressure, and wherein the mass ratio of water/SDBS/ n-amyl alcohol/normal heptane is 0.8-1.2: 2: 4: 8.
3, Preparation Method of Nanometer nickel Ultrafine according to claim 1 is characterized in that: step (1), (2) described water bath with thermostatic control temperature are 18-30 ℃.
4, Preparation Method of Nanometer nickel Ultrafine according to claim 1, it is characterized in that: the described borane reducing agent sodium hydride of step (2) particle adds in different time sections (promptly in different emulsion stabilization time), the nano-nickel powder that can prepare different-grain diameter, this time period scope is 15-60 minute, and mixing time is 20-40 minute.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100708311A CN100450676C (en) | 2006-03-09 | 2006-03-09 | Method for preparing nano nickel powder in emulsion system |
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| CNB2006100708311A CN100450676C (en) | 2006-03-09 | 2006-03-09 | Method for preparing nano nickel powder in emulsion system |
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| CN1966187A true CN1966187A (en) | 2007-05-23 |
| CN100450676C CN100450676C (en) | 2009-01-14 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102327806A (en) * | 2011-06-20 | 2012-01-25 | 宁波广博纳米新材料股份有限公司 | Method taking organic solvent as medium for grading nano-nickel powder for MLCC (multilayer ceramic capacitor) |
| CN102989576A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Method for grading silver powder for solar battery |
| CN103737018A (en) * | 2014-01-17 | 2014-04-23 | 昆明理工大学 | Method for continuous and rapid preparation of nano nickel by microfluidics technology |
| CN105081347A (en) * | 2015-09-07 | 2015-11-25 | 赣州市华新金属材料有限公司 | Normal-pressure production method for low-apparent-density high-purity spherical ultrafine nickel powder |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004211191A (en) * | 2003-01-08 | 2004-07-29 | Mitsubishi Gas Chem Co Inc | Chemical for producing nickel fine powder |
| JP2004323866A (en) * | 2003-04-21 | 2004-11-18 | Murata Mfg Co Ltd | Method for manufacturing nickel powder, and nickel powder |
| JP2005023395A (en) * | 2003-07-04 | 2005-01-27 | Murata Mfg Co Ltd | Production method of nickel powder |
| CN1225336C (en) * | 2003-12-19 | 2005-11-02 | 北京科技大学 | Preparation of nano nickle powder by micro-wave activated aqueous solution reduction process |
| JP2005240164A (en) * | 2004-02-27 | 2005-09-08 | Sumitomo Metal Mining Co Ltd | Nickel powder and manufacturing method therefor |
| CN1273251C (en) * | 2004-08-06 | 2006-09-06 | 中山大学 | Nano structure nickel powde and its preparing method |
-
2006
- 2006-03-09 CN CNB2006100708311A patent/CN100450676C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102327806A (en) * | 2011-06-20 | 2012-01-25 | 宁波广博纳米新材料股份有限公司 | Method taking organic solvent as medium for grading nano-nickel powder for MLCC (multilayer ceramic capacitor) |
| CN102327806B (en) * | 2011-06-20 | 2014-03-26 | 宁波广博纳米新材料股份有限公司 | Method taking organic solvent as medium for grading nano-nickel powder for MLCC (multilayer ceramic capacitor) |
| CN102989576A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Method for grading silver powder for solar battery |
| CN102989576B (en) * | 2012-11-07 | 2015-04-08 | 宁波广博纳米新材料股份有限公司 | Method for grading silver powder for solar battery |
| CN103737018A (en) * | 2014-01-17 | 2014-04-23 | 昆明理工大学 | Method for continuous and rapid preparation of nano nickel by microfluidics technology |
| CN105081347A (en) * | 2015-09-07 | 2015-11-25 | 赣州市华新金属材料有限公司 | Normal-pressure production method for low-apparent-density high-purity spherical ultrafine nickel powder |
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| CN100450676C (en) | 2009-01-14 |
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