CN104439278A - Method for preparing nanometer spherical nickel powder - Google Patents
Method for preparing nanometer spherical nickel powder Download PDFInfo
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- CN104439278A CN104439278A CN201410712512.0A CN201410712512A CN104439278A CN 104439278 A CN104439278 A CN 104439278A CN 201410712512 A CN201410712512 A CN 201410712512A CN 104439278 A CN104439278 A CN 104439278A
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Abstract
The invention relates to a method for preparing nanometer spherical nickel powder. The method includes the following steps that a solution including Ni2+ and a reducibility solution are mixed and reacted to prepare a solution including the nickel powder; a solution including M2+ and a solution including R2- are added to the solution including the nickel powder to be sufficiently reacted to obtain the nickel powder cladded by a cladding agent, wherein M2+ is selected from at least one of Mg2+, Ca2+ and Zn2+, and R2- is selected from at least one of C2O42- and CO32-; the nickel powder cladded by the cladding agent is baked in a vacuum mode for 1-5 hours under the temperature of 600-1100 DEG C; acid pickling is conducted on the nickel powder cladded by the cladding agent, drying is conducted, and the nanometer spherical nickel powder is obtained. By means of the method for preparing the nanometer spherical nickel powder, operation is simple, the requirement for equipment is low, and the method is suitable for industrial production. A surfactant does not need to be added for controlling the appearance, a nucleating agent and a stabilizer do not need to be added for controlling a reaction, and it is tested that the obtained nanometer spherical nickel powder is high in crystallinity, even in granularity, and good in sphericity degree and dispersibility.
Description
Technical field
The present invention relates to a kind of preparation method of nanometer spherical nickel powder.
Background technology
Nano-nickel powder has that surface energy is high, specific area is large, electric conductivity, thermal conductivity are good, the physicochemical properties of a series of uniquenesses such as oxidation resistance is strong, many exceptional functions are demonstrated in magnetic, thermal resistance, interior pressure, light absorption, chemism etc., therefore having broad application prospects in fields such as electrocondution slurry, effective catalyst, additive and light absorbing materials, is the application focus of domestic and international functional material.
The main production method of current nano-nickel powder has spray pyrolysis, plasma method, chemical vapour deposition technique, electrochemical process, liquid phase reduction etc.Liquid phase reduction prepares the most frequently used method of extra-fine nickel powder, and liquid phase reduction utilizes reducing agent in the liquid phase nickel to be restored to be gathered into extra-fine nickel powder.The nickel powder degree of crystallinity prepared of existing liquid phase reduction is low and granularity is uneven.
Summary of the invention
Based on this, be necessary to provide a kind of degree of crystallinity high and the preparation method of even-grained nanometer spherical nickel powder.
A preparation method for nanometer spherical nickel powder, comprises the following steps:
Will containing Ni
2+solution mix with reducing solution after react to prepare and contains the solution of nickel powder;
Will containing M
2+solution and containing R
2-solution be added to and described be fully obtained by reacting the nickel powder being coated with covering, wherein said M containing in the solution of nickel powder
2+be selected from Mg
2+, Ca
2+and Zn
2+in at least one, described R
2-be selected from C
2o
4 2-and CO
3 2-in at least one;
By the described nickel powder being coated with covering vacuum bakeout 1 hour ~ 5 hours at 600 DEG C ~ 1100 DEG C; And
Carry out pickling to the described nickel powder being coated with covering to remove described covering post-drying and obtain nanometer spherical nickel powder.。
Wherein in an embodiment, described containing Ni
2+solution in also containing dispersant, described dispersant is selected from least one in ethanol, polyvinylpyrrolidone and polyethylene glycol, described dispersant and described Ni
2+mol ratio be 10:1 ~ 50:1.
Wherein in an embodiment, containing BH in described reducing solution
4 -and dispersant, described dispersant is selected from least one in ethanol, polyvinylpyrrolidone and polyethylene glycol, described dispersant and described BH
4 -mol ratio be 10:1 ~ 50:1.
Wherein in an embodiment, described Ni
2+with NH
4 -mol ratio be 1:2 ~ 1:5.
Wherein in an embodiment, will containing Ni
2+solution mix with reducing solution after react prepare contain nickel powder solution step in, reacting in pH value is 8-10, at 30 DEG C ~ 80 DEG C reaction 1 hour ~ 2 hours.
Wherein in an embodiment, use at least one adjust ph in sodium carbonate, NaOH and ammoniacal liquor.
Wherein in an embodiment, described containing M
2+solution in M
2+with described containing Ni
2+solution in Ni
2+mol ratio be 1.2:1 ~ 2:1.
Wherein in an embodiment, the operation of described pickling is specially: first with hydrochloric acid or sulfuric acid scrubbing 2 minutes ~ 10 minutes, then wash 30 minutes ~ 60 minutes with citric acid, be washed with water to neutrality afterwards, then filter with alcohol.
Wherein in an embodiment, the mass concentration of described hydrochloric acid or described sulfuric acid is 1% ~ 20%, and the mass concentration of described citric acid is 0.5% ~ 10%.
Wherein in an embodiment, the temperature of described oven dry is 60 DEG C ~ 100 DEG C, and time dry, low vacuum is in 10Pa.
The preparation method of above-mentioned nanometer spherical nickel powder, simple to operate, low for equipment requirements, be applicable to suitability for industrialized production; Control pattern without the need to adding surfactant and control reaction without the need to adding nucleating agent and stabilizing agent; After tested, the nanometer spherical nickel powder degree of crystallinity obtained is high, epigranular, good sphericity and good dispersion.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the nanometer spherical nickel powder that embodiment 1 obtains;
Fig. 2 is the SEM figure of the nanometer spherical nickel powder that embodiment 1 obtains.
Detailed description of the invention
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with embodiment.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
The preparation method of the nanometer spherical nickel powder of one embodiment, comprises the following steps:
Step S110, will containing Ni
2+solution mix with reducing solution after react to prepare and contains the solution of nickel powder.
Preferably, containing Ni
2+solution in also containing dispersant.Dispersant is selected from least one in ethanol, polyvinylpyrrolidone (PVP) and polyethylene glycol (PEG).Dispersant and Ni
2+mol ratio be 10:1 ~ 50:1.
Preferably, containing Ni
2+solution in Ni
2+concentration be 0.5mol/L ~ 1mol/L.
Preferably, containing Ni
2+solution be at least one in nickel sulfate solution and nickel chloride solution.
Preferably, BH is contained in reducing solution
4 -and dispersant, dispersant is selected from least one in ethanol, polyvinylpyrrolidone and polyethylene glycol, dispersant and described BH
4 -mol ratio be 10:1 ~ 50:1.
Preferably, reducing solution is for containing BH
4-solution.Further, containing Ni
2+solution in Ni
2+with the BH in reducing solution
4 -mol ratio be 1:2 ~ 1:5.Further, containing BH
4 -solution in BH
4 -concentration be 0.05mol/L ~ 0.1mol/L.
Preferably, reducing solution is selected from NaBH
4or KBH
4at least one in solution.
Preferably, reacting in pH value is 8-10, reacts 1 hour ~ 2 hours at 30 DEG C ~ 80 DEG C.Further, at least one adjust ph in sodium carbonate, NaOH and ammoniacal liquor is used.
Step S120, will containing M
2+solution and containing R
2-solution be added to containing nickel powder solution in be fully obtained by reacting the nickel powder being coated with covering, wherein M
2+be selected from M
g 2+, Ca
2+and Zn
2+in at least one, R
2-be selected from C
2o
4 2-and CO
3 2-in at least one.
Preferably, containing M
2+solution in M
2+with described containing Ni
2+solution in Ni
2+mol ratio be 1.2:1 ~ 2:1.
Preferably, containing M
2+solution be MCl
2solution.
Preferably, containing M
2+solution in M
2+concentration be 1mol/L ~ 10mol/L.
Preferably, containing R
2-solution be (NH
4)
2r solution.Further, R
2-concentration be 1mol/L ~ 10mol/L.
Preferably, the reaction time is 20 minutes ~ 60 minutes.
Preferably, will containing M
2+solution and containing R
2-solution be added in the solution containing nickel powder simultaneously.
Preferably, reaction terminates the nickel powder that rear filtration drying obtains being coated with covering.Further, dry temperature is 200 DEG C ~ 280 DEG C.
Step S130, nickel powder vacuum bakeout 1 hour ~ 5 hours at 600 DEG C ~ 1100 DEG C that will covering be coated with.
Preferably, the vacuum of vacuum bakeout is less than 10Pa.
Preferably, 600 DEG C ~ 1000 DEG C are heated to the heating rate of 3 DEG C/min ~ 10 DEG C/min.
Step S140, the nickel powder being coated with covering carried out to pickling removing covering post-drying and obtain nanometer spherical nickel powder.
Preferably, the operation of pickling is specially: first with hydrochloric acid or sulfuric acid scrubbing 2 minutes ~ 10 minutes, then wash 30 minutes ~ 60 minutes with citric acid, be washed with water to neutrality afterwards, then filter with alcohol.Further, the mass concentration of hydrochloric acid or sulfuric acid is 1% ~ 20%, and the mass concentration of citric acid is 0.5% ~ 10%.
Preferably, the hydrochloric acid of pickling use or the amount of sulfuric acid are theoretical amount 110% ~ 150%, theoretical amount refers to the amount required for covering dissolving making nickel powder surface in theory.
Preferably, the temperature of oven dry is 60 DEG C ~ 100 DEG C, and time dry, low vacuum is in 10Pa.
The preparation method of above-mentioned nanometer spherical nickel powder, simple to operate, low for equipment requirements, be applicable to suitability for industrialized production; Control pattern without the need to adding surfactant and control reaction without the need to adding nucleating agent and stabilizing agent; After tested, the nanometer spherical nickel powder degree of crystallinity obtained is high, epigranular, good sphericity and good dispersion.
Below in conjunction with specific embodiment, the preparation method to nanometer spherical nickel powder is described in further details.
Embodiment 1
60 DEG C of mixed aqueous solution 100ml containing 0.5mol/L nickel chloride, 120g/L ethanol are at the uniform velocity added 60 DEG C containing 0.05mol/L NaBH
4, 120g/LPVP mixed aqueous solution 2000ml in, in stirring reactor (speed of agitator is 150rpm), adopt saturated aqueous sodium carbonate to regulate pH value to be 10, react after 60 minutes, obtain containing the solution of nickel powder.
Then, at the uniform velocity will add in stirring-type reaction vessel by the mol ratio 1:1 of magnesium and oxalate with the magnesium chloride brine of 5mol/L of nickel metering mole 1.5 times and the ammonium oxalate aqueous solution of 1.0mol/L, add rear reaction 30min, then use pure water cyclic washing 3 times, after 250 DEG C of oven dry in electric dry oven, obtain the nickel being enclosed with magnesium oxalate.
Then, the nickel being enclosed with magnesium oxalate is warmed up to 800 DEG C of insulation 5h with the heating rate of 10 DEG C/min under vacuum (vacuum < 6Pa) condition, be cooled to room temperature to come out of the stove, with the chlorohydric acid pickling 10 minutes that mass concentration is 1%, acid amount is 150% of theoretical amount, after pickling, acid solution is outwelled, then mass concentration is adopted to be that 1% citric acid solution washs 60 minutes, outwell acid solution, with pure water lotion to PH=7, filter, by the nickel powder after lotion through 80 DEG C with alcohol subsequently, after 8Pa vacuum drying, obtain subglobose nanometer spherical nickel powder.
Refer to Fig. 1, Fig. 1 is the XRD figure of the nanometer spherical nickel powder that embodiment 1 obtains, as can be seen from Figure 1, and nickel powder better crystallinity degree, crystal size 42.3nm.
Refer to Fig. 2, Fig. 2 is the SEM figure of the nanometer spherical nickel powder that embodiment 1 obtains, as can be seen from Figure 2, and soap-free emulsion polymeization between nickel powder particle, good dispersion.Adopting absorption method to record nickel powder particle diameter is 80nm.
Embodiment 2
By 80 DEG C of mixed aqueous solution 200ml containing 1mol/L nickelous sulfate, 50g/L PEG, at the uniform velocity add 5000ml, 80 DEG C containing 0.1mol/L KBH
4, 80g/L alcohol mixed aqueous solution stirring reactor in (speed of agitator is 200rpm), adopt NaOH regulate PH to 9, react after 1.5 hours, obtain nickel powder.
Then, to add in stirring-type reaction vessel by calcium and oxalate mol ratio 1:1 than at the uniform velocity with the calcium chloride water of 2mol/l of nickel metering mole 2 times and the ammonium oxalate aqueous solution of 1.0mol/l, add rear reaction 50min, then use pure water cyclic washing 2 times, then 250 DEG C of oven dry in electric dry oven, obtain the nickel powder being enclosed with calcium oxalate.
Then, being warmed up to 1100 DEG C of insulation 1h by being enclosed with the nickel of calcium oxalate (vacuum < 6Pa) in vacuum atmosphere with the heating rate of 3 DEG C/min, being cooled room temperature subsequently and coming out of the stove.With the sulfuric acid washing 3 minutes that mass concentration is 10%, acid amount is 120% of theoretical amount, after pickling, acid solution is outwelled, then adopting mass concentration for being 10% citric acid solution washing 30 minutes, outwelling acid solution, with pure water lotion to PH=7, filter with alcohol subsequently, be in 6Pa vacuum drying oven in vacuum, 90 DEG C of oven dry, obtain spherical nanometer spherical nickel powder.
The average grain diameter of the nanometer spherical nickel powder adopting adsorption method testing example 2 to prepare is 63nm.
The crystal size 43.1nm of the nanometer spherical nickel powder adopting XRD method testing example 2 to prepare.
Embodiment 3
By 30 DEG C containing 1mol/L nickel chloride, 180g/L ethanol mixed aqueous solution 200ml at the uniform velocity add 4000ml, 30 DEG C containing 0.1mol/L NaBH4,180g/LPEG mixed aqueous solutions stirring reactor in (speed of agitator is 200rpm), ammonia spirit is adopted to regulate pH value to be 8, react after 30 minutes, obtain the solution containing nickel powder.
Then, at the uniform velocity will add in stirring-type reaction vessel by the mol ratio 1:1 of magnesium and carbonate with the calcium chloride water of 5mol/L of nickel metering mole 1.2 times and the ammonium carbonate solution of 1.0mol/L, add rear reaction 40min, then use pure water cyclic washing 3 times, after 200 DEG C of oven dry in electric dry oven, obtain the nickel being enclosed with calcium carbonate.
Then, the nickel being enclosed with magnesium oxalate is warmed up to 800 DEG C of insulation 3h with the heating rate of 5 DEG C/min under vacuum (vacuum < 6Pa) condition, be cooled to room temperature to come out of the stove, with the chlorohydric acid pickling 5 minutes that mass concentration is 5%, acid amount is 130% of theoretical amount, after pickling, acid solution is outwelled, then adopt mass concentration for washing 40 minutes for 0.7% citric acid solution, outwell acid solution, with pure water lotion to PH=7, filter, by the nickel powder after lotion through 70 DEG C with alcohol subsequently, after 5Pa vacuum drying, obtain subglobose nanometer spherical nickel powder.
The average grain diameter of the nanometer spherical nickel powder adopting adsorption method testing example 3 to prepare is 70nm.
The crystal size 43.7nm of the nanometer spherical nickel powder adopting XRD method testing example 3 to prepare.
Embodiment 4
60 DEG C of mixed aqueous solution 100ml containing 0.5mol/L nickel chloride, 120g/L ethanol are at the uniform velocity added 2000ml, 60 DEG C containing 0.05mol/L NaBH
4, 120g/L PVP mixed aqueous solution stirring reactor in (speed of agitator is 150rpm), adopt saturated aqueous sodium carbonate to regulate pH value to be 10, react after 60 minutes, obtain containing the solution of nickel powder.
Then, magnesium chloride and the calcium chloride mixed aqueous solution of mole 1.5 times will be measured with nickel, magnesium calcium mol ratio is 1:1, at the uniform velocity add in stirring-type reaction vessel with the ammonium oxalate aqueous solution of 1.0mol/L by the mol ratio 1:1 of magnesium and calcium total amount and oxalate, add rear reaction 30min, then use pure water cyclic washing 3 times, after 250 DEG C of oven dry in electric dry oven, obtain the nickel being enclosed with magnesium oxalate and calcium oxalate.
Then, the nickel being enclosed with magnesium oxalate and calcium oxalate is warmed up to 600 DEG C of insulation 5h with the heating rate of 10 DEG C/min under vacuum (vacuum < 6Pa) condition, be cooled to room temperature to come out of the stove, with the chlorohydric acid pickling 8 minutes of quality 1%, acid amount is 110% of theoretical amount, after pickling, acid solution is outwelled, then concentration is adopted to be that mass concentration 10% citric acid solution washs 30 minutes, outwell acid solution, with pure water lotion to PH=7, filter with alcohol subsequently, by the nickel powder after lotion through 80 DEG C, after 8Pa vacuum drying, obtain subglobose nanometer spherical nickel powder.
The average grain diameter of the nanometer spherical nickel powder adopting adsorption method testing example 3 to prepare is 90nm.
The degree of crystallinity of the nanometer spherical nickel powder adopting XRD method testing example 3 to prepare is crystal size is 42.5nm.
Each technical characteristic of the above embodiment can combine arbitrarily, for making description succinct, the all possible combination of each technical characteristic in above-described embodiment is not all described, but, as long as the combination of these technical characteristics does not exist contradiction, be all considered to be the scope that this description is recorded.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for nanometer spherical nickel powder, is characterized in that, comprises the following steps:
Will containing Ni
2+solution mix with reducing solution after react to prepare and contains the solution of nickel powder;
Will containing M
2+solution and containing R
2-solution be added to and described be fully obtained by reacting the nickel powder being coated with covering, wherein said M containing in the solution of nickel powder
2+be selected from Mg
2+, Ca
2+and Zn
2+in at least one, described R
2-be selected from C
2o
4 2-and CO
3 2-in at least one;
By the described nickel powder being coated with covering vacuum bakeout 1 hour ~ 5 hours at 600 DEG C ~ 1100 DEG C; And
Carry out pickling to the described nickel powder being coated with covering to remove described covering post-drying and obtain nanometer spherical nickel powder.
2. the preparation method of nanometer spherical nickel powder according to claim 1, is characterized in that, described containing Ni
2+solution in also containing dispersant, described dispersant is selected from least one in ethanol, polyvinylpyrrolidone and polyethylene glycol, described dispersant and described Ni
2+mol ratio be 10:1 ~ 50:1.
3. the preparation method of nanometer spherical nickel powder according to claim 1, is characterized in that, containing BH in described reducing solution
4 -and dispersant, described dispersant is selected from least one in ethanol, polyvinylpyrrolidone and polyethylene glycol, described dispersant and described BH
4 -mol ratio be 10:1 ~ 50:1.
4. the preparation method of nanometer spherical nickel powder according to claim 3, is characterized in that, described Ni
2+with NH
4 -mol ratio be 1:2 ~ 1:5.
5. the preparation method of nanometer spherical nickel powder according to claim 1, is characterized in that, will containing Ni
2+solution mix with reducing solution after react prepare contain nickel powder solution step in, reacting in pH value is 8-10, at 30 DEG C ~ 80 DEG C reaction 1 hour ~ 2 hours.
6. the preparation method of nanometer spherical nickel powder according to claim 5, is characterized in that, uses at least one adjust ph in sodium carbonate, NaOH and ammoniacal liquor.
7. the preparation method of nanometer spherical nickel powder according to claim 1, is characterized in that, described containing M
2+solution in M
2+with described containing Ni
2+solution in Ni
2+mol ratio be 1.2:1 ~ 2:1.
8. the preparation method of nanometer spherical nickel powder according to claim 1, it is characterized in that, the operation of described pickling is specially: first with hydrochloric acid or sulfuric acid scrubbing 2 minutes ~ 10 minutes, then wash 30 minutes ~ 60 minutes with citric acid, be washed with water to neutrality afterwards, then filter with alcohol.
9. the preparation method of nanometer spherical nickel powder according to claim 8, is characterized in that, the mass concentration of described hydrochloric acid or described sulfuric acid is 1% ~ 20%, and the mass concentration of described citric acid is 0.5% ~ 10%.
10. the preparation method of nanometer spherical nickel powder according to claim 1, is characterized in that, the temperature of described oven dry is 60 DEG C ~ 100 DEG C, and time dry, low vacuum is in 10Pa.
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Cited By (1)
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