CN106334802B - Metal powder with spongy microstructure and preparation method thereof, conductive material - Google Patents
Metal powder with spongy microstructure and preparation method thereof, conductive material Download PDFInfo
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- CN106334802B CN106334802B CN201610865032.7A CN201610865032A CN106334802B CN 106334802 B CN106334802 B CN 106334802B CN 201610865032 A CN201610865032 A CN 201610865032A CN 106334802 B CN106334802 B CN 106334802B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Abstract
The invention discloses a kind of metal powders with spongy microstructure and preparation method thereof, conductive material.The preparation method of metal powder is the following steps are included: S1, prepares metal salt solution, reducing agent solution and surfactant solution, the ratio between metal salt solution, molar concentration of reducing agent solution and surfactant solution are 1:0.1~10:0.05~50 respectively；S2, reducing agent solution is added in reaction vessel, it is stirred with the mixing speed of 10~1000rpm, then metal salt solution is added at the uniform velocity with second speed, -10 DEG C~80 DEG C at a temperature of sufficiently react after, surfactant solution is added at the uniform velocity with third speed, adjusts range of the pH value in 7.5≤pH≤12 of mixed solution, sufficiently after reaction, precipitating is generated；Second speed and third speed are in the range of 0.1~1L/min；Precipitating is filtered, carrying out washing treatment and vacuum drying by S3, and metal powder is made.Particle in metal powder produced by the present invention is in nanoscale, and monodispersity is preferable, and surface has fining structure abundant.
Description
[technical field]
The present invention relates to the preparation methods of metal powder, more particularly to a kind of metal powder with spongy microstructure
The preparation method at end.
[background technique]
Since proposing from nanotechnology, metal nano material is always the research heat being concerned in research in nanotechnology field
Point, the metal nano material of different structure size is because of its significant physical and chemical performance and in optics, electricity, the side such as magnetics
Potentially application etc. is valued by people in face.And metal nano sponge is penetrated due to its high-specific surface area, low-density, high gas
Rate, high-termal conductivity have huge application value in terms of catalyst, membrane material, energy battery, sensor, electrode material.
It includes template, selective dissolution alloy that preparation at present, which has the method for the metal powder of spongy microstructure,
Method, pH regulation method of glucose reduction, reaction limitation aggregation method, lotion synthetic method and biological reducing method.But made from these methods
Metal powder monodispersity is not good enough, and the size of powder is different, and generally in millimeter, centimetre rank, it is difficult to nanometer be made
The metal powder of rank.In addition, be also individually present in these methods reaction step complexity, low yield, production equipment require it is high,
The problems such as product specific surface area is small, metal material type is limited etc..
[summary of the invention]
The technical problems to be solved by the present invention are: making up above-mentioned the deficiencies in the prior art, propose a kind of with spongy
Metal powder of microstructure and preparation method thereof, the particle in metal powder obtained is in nanoscale, and monodispersity is preferable,
And surface has fining structure abundant.
Technical problem of the invention is resolved by technical solution below:
A kind of preparation method of the metal powder with spongy microstructure, comprising the following steps: S1 prepares gold respectively
Belong to salting liquid, reducing agent solution and surfactant solution, the metal salt solution, reducing agent solution and surfactant solution
The ratio between molar concentration be 1:0.1~10:0.05~50；The reducing agent solution is added in reaction vessel by S2, with 10~
The mixing speed of 1000rpm is stirred, and the metal salt solution is at the uniform velocity then added with second speed (V2), -10 DEG C~
After sufficiently being reacted at a temperature of 80 DEG C, the surfactant solution is added at the uniform velocity with third speed (V3), adjusts mixed solution
PH value 7.5≤pH≤12 range, sufficiently reaction after, in the reaction vessel generate precipitating；Wherein, the second speed
(V2) and third speed (V3) is in the range of 0.1~1L/min；The precipitating is filtered, carrying out washing treatment and true by S3
Sky is dry, and the metal powder with spongy microstructure is made.
A kind of basis preparation method as described above metal powder obtained with spongy microstructure.
A kind of conductive material, including base material and the metal powder being dispersed in base material, the metal powder is
Metal powder as described above.
The beneficial effect of the present invention compared with the prior art is:
The preparation method of metal powder with spongy microstructure of the invention, by using strong reductant and metal
Presoma stirs under the speed of 10~1000rpm to be reacted, and metal salt is oxidized to the metallic of Nano grade, simultaneously
Surfactant is introduced, so that metallic crystal, during growing into particle, certain orientation preferentially growths, certain directions are pressed down
System growth, final multiple particle aggregations grow into the metal powder with spongy microscopic appearance.Pass through the concentration of solution, stirring
The regulation of speed etc. ground, the effect of matching surface activating agent, so as in high volume controllably prepare 300~1000 nanometers of rulers
The metallic particles of narrow ditribution is spent, and surface of metal particles has the fine structure of 10~100 nanometer feature sizes abundant.This hair
Bright preparation method is easy, reaction condition is mild, and the size of multiple metallic particles in metal powder is closer to, monodispersity compared with
It is good.By adjusting reaction raw materials and additive types and ratio, charging and mixing speed, reaction temperature and pH value, reaction time
Design synthesizes the biscuit nanometer powder of different size and shape structures, is easy to carry out expanding production, realizes industrialization.
[Detailed description of the invention]
Fig. 1 is that a kind of scanning electron of silver powder obtained under multiple is aobvious in the embodiment 1 of the specific embodiment of the invention
Micro mirror photo；
Fig. 2 is the scanning electron of silver powder obtained under another multiple in the embodiment 1 of the specific embodiment of the invention
Microscope photo；
Fig. 3 is in the embodiment 1 of the specific embodiment of the invention in silver powder obtained under single Argent grain dispersity
Transmission electron microscope photo；
Fig. 4 is the electron scanning micrograph of silver powder obtained in the embodiment 2 of the specific embodiment of the invention；
Fig. 5 is the electron scanning micrograph of silver powder obtained in the embodiment 3 of the specific embodiment of the invention；
Fig. 6 is the electron scanning micrograph of silver powder obtained in the embodiment 4 of the specific embodiment of the invention；
Fig. 7 is the electron scanning micrograph of silver powder obtained in the embodiment 5 of the specific embodiment of the invention；
Fig. 8 is the electron scanning micrograph of silver powder obtained in the embodiment 6 of the specific embodiment of the invention；
Fig. 9 is the electron scanning micrograph of silver powder obtained in the embodiment 7 of the specific embodiment of the invention；
Figure 10 is the electron scanning micrograph of bronze obtained in the embodiment 8 of the specific embodiment of the invention.
[specific embodiment]
With reference to embodiment and compares attached drawing the present invention is described in further details.
Present embodiment provides a kind of preparation method of metal powder with spongy microstructure, including following
Step:
S1 prepares metal salt solution, reducing agent solution and surfactant solution, the metal salt solution, reduction respectively
The ratio between molar concentration of agent solution and surfactant solution is 1:0.1~10:0.05~50.
In the step, the type of metal salt and reducing agent can be selected according to oxidation-reduction quality, and meeting reducing agent can be effective
Metal salt is reduced into metal simple-substance by ground.The oxidisability of different metal salt is different, and reducing agent used guarantees will be right
The metal cation answered is reduced into metallic atom.Specifically, the metal salt solution is gold salt solution, and the reducing agent is 2- ammonia
One of base -3- mercaptopropionic acid, sodium borohydride or a variety of mixing.The metal salt solution is copper salt solution, the reduction
Agent is hydroxylamine hydrochloride or the one or more mixing of sodium borohydride.Preferably, metal salt solution is silver salt solution, the reduction
Agent is one of formaldehyde, acetaldehyde, citric acid, ascorbic acid, sodium borohydride, azanol, hydrazine or a variety of mixing.According to experiment
As a result, by selection silver salt solution and correspondingly strong reductant, especially sodium borohydride, azanol, hydrazine, Vitamin C
Acid, the pattern of silver powder obtained, dimensional homogeneity are preferable.
The reducing agent solution is added in reaction vessel by S2, is stirred with the mixing speed of 10~1000rpm,
Then the metal salt solution is added at the uniform velocity with speed V2, -10 DEG C~80 DEG C at a temperature of sufficiently react after, it is even with speed V3
The surfactant solution is added in speed, adjusts range of the pH value in 7.5≤pH≤12 of mixed solution, sufficiently after reaction, institute
It states and generates precipitating in reaction vessel；Wherein, the second speed V2 and third speed V3 is in the range of 0.1~1L/min.
In above-mentioned steps, after metal salt and reducing agent is added in reaction vessel, metal ion is reduced into metal by reducing agent
Atom obtains metal nanoparticle, which is to form nanosponges knot by forming core gradually and growth course
The basis of structure.The reaction process in the stage is for 5 seconds~and 10 minutes, the main size and shape for influencing primary granule, thus shadow
Ring the aggregation and intergranular alloying process of subsequent particle.
After surfactant is added, surfactant can prevent further assembling between primary granule and grow up, and energy
Regulation influences the direction of growth of crystal, so that certain crystal plane direction preferred growths, certain crystal plane directions are suppressed growth, to have
Effect controls the size and microscopic appearance of finally obtained metal powder.Duration is reacted probably at 5~30 minutes.In the step, table
Face activating agent can be polyvinylpyrrolidone, polyethenoxy ether class surfactant, sorbitan ester, non-ion fluorin carbon surface
One of activating agent or a variety of mixing.
In whole process, redox reaction first occurs between reducing agent and metal salt, metal salt is oxidized to clipped wire
Son, but what is most initially formed is nanoscale metallic, and is grown along certain crystal growth direction.It is living when surface is added
Property agent after, certain directions of crystal growth can preferred growth or certain directions can be suppressed growth, thus multiple crystal accumulations
The metal powder of spongy pattern can be grown into afterwards.Entire reaction process carries out under the mixing speed of 10~1000rpm, this is stirred
Mix that speed is very fast relative to general hunting speed, the collision probability between metallic particles is relatively large, be easily formed size compared with
Big particle.But the mixing speed when speed is relative to the usual metal powder for preparing spherical microscopic appearance wants lower, from
And it is unlikely to so that multiple metallic particles excessively assemble formation spherical shape.Preferably, model of the setting mixing speed in 100~800rpm
It encloses, the sponge pattern that crystal is formed after generating is preferable.
The precipitating is filtered, carrying out washing treatment and vacuum drying, the metal with spongy microstructure is made by S3
Powder.
In present embodiment, by the effect of surfactant, and cooperates and reacted under above-mentioned mixing speed, simultaneously
Control response hierarchy, condition, charging rate etc., can Effective Regulation nano particle coherent condition, so that obtaining has specific ruler
Very little nanosponges structure.Each nanoparticle size narrowly distributing, is distributed in the size of 300~1000nm in metal powder obtained
In range, and surface has structure of the characteristic size within the scope of 10~100nm.Preparation process is simple, and reaction condition is mild, and
Obtained product structure and size is controllable, reproducible.
Each metallic particles is in 300~1000nm size range in metal powder made from present embodiment, size
Controllably.Size distribution, can be dispersed in various substrates (such as resin) and prepare high-performance composite materials, and and kinds of processes
(as printed, inkjet printing etc.) is compatible, has broad application prospects.Currently on the market or this structure size of academia and
All there is not been reported for the metal powder of pattern.Surface of metal particles has the fine structure of 10~100nm characteristic size abundant,
Has the characteristics that this metallic particles, due to its surface nanometer feature sizes fine structure abundant, in optics, electricity, magnetics
Etc. all there is potential application, the composite material to be formed can be made to have the excellent performances such as conductive, thermally conductive.For example, its 10~
The fine structure of 100 nanometer feature sizes is prone to low-temperature sintering and forms Ohmic contact, it can be effectively reduced and fills out as conduction
The conductive seepage flow value of material can be used as excellent conductive filler dispersion and form conductive material in the substrate.The preparation of this concrete mode
Each metallic particles in metal powder made from method, size uniformityization is good, and monodispersity is good, is suitable for industrial production in large quantity
Using.
Following setting specific embodiment verifies the microscopic appearance and single gold of metal powder made from present embodiment
The size and structure feature of metal particles.
Embodiment 1:
The polysorbate60 for preparing 0.1mol/L silver nitrate solution, 0.05mol/L hydrazine hydrate solution and 0.05mol/L respectively (loses
Water sorbierite esters surface active agent) each 1L of solution, i.e. metal salt solution, the reducing agent solution and the table
The ratio between molar concentration of face activator solution is 1:0.5:0.5).First 1L hydrazine hydrate solution is added in reaction vessel, and with
The speed of 200rpm carries out magnetic agitation；After velocity-stabilization to be mixed, it is molten that 1L silver nitrate is at the uniform velocity added with the speed of 100mL/min
Liquid；After 25 DEG C of reaction 1min, the polysorbate60 solution of 1L is added with the speed of 100mL/min.Controlling pH value of solution is 7.5, reaction
Temperature is 25 DEG C, continues to be stirred to react 10min, gained precipitating is filtered, deionized water cleaning 2-3 times, is then carried out true
Sky is dry, and silver powder is made.
As Fig. 1~2 show made from silver powder the electron scanning micrograph under two kinds of different multiples, Fig. 3 is
Transmission electron microscope photo in silver powder under individual particle monodisperse status.Available from Fig. 1~2, silver powder is spongy shape
Looks.Available from Fig. 3 and its scale, individual particle size is in the range of 300~1000nm, and individual particle surface is distributed with
Branch shape fine structure, size is within the scope of the fining of 10~100nm.
Embodiment 2
Polysorbas20 (the dehydration of 0.01mol/L silver nitrate solution, 0.1mol/L hydrazine hydrate solution and 0.5mol/L is prepared respectively
Sorbierite esters surface active agent) each 1L of solution, i.e. metal salt solution, the reducing agent solution and the surface
The ratio between activating agent molar concentration a is 1:10:50.First 1L hydrazine hydrate solution is added in reaction vessel, and with the speed of 500rpm
Carry out magnetic agitation；After velocity-stabilization to be mixed, 1L silver nitrate solution is added at the uniform velocity with the speed of 1L/min；It is reacted at 25 DEG C
After 1min, the polysorbas20 solution of 1L is added with the speed of 1L/min.Controlling pH value of solution is 12.0, and reaction temperature is 25 DEG C, is continued
It is stirred to react 10min, gained precipitating is filtered, deionized water is cleaned 2-3 times, is then dried in vacuo, obtained silver powder.
Fig. 4 is the electron scanning micrograph of silver powder obtained, and silver powder is spongy pattern as we know from the figure.In silver powder
The transmission electron microscope photo of individual particle is similar with Fig. 3, is not repeated to provide herein.
Embodiment 3
The present embodiment preparation method is similar to Example 1, is a difference in that and changes each reactive component concentration ratio and reducing agent
Type.The ratio between metal salt solution, reducing agent solution and surfactant molar concentration a are 1:0.5:0.5, reduction in embodiment 1
Agent is hydrazine hydrate solution；A is 1:2:5 in embodiment 3, and reducing agent is hydroxylamine solution.
(the dehydration mountain of Span 60 of 0.1mol/L silver nitrate solution, 0.2mol/L hydroxylamine solution and 0.5mol/L is prepared respectively
Pears alkoxide surfactant) each 1L of solution, i.e. the metal salt solution, the reducing agent solution and the surface is lived
Property the ratio between agent molar concentration a be 1:2:5.First 1L hydroxylamine solution is added in reaction vessel, and magnetic is carried out with the speed of 200rpm
Power stirring；After velocity-stabilization to be mixed, 1L silver nitrate solution is added at the uniform velocity with the speed of 100mL/min；In 25 DEG C of reaction 1min
Afterwards, 60 solution of Span of 1L is added with the speed of 100mL/min.Controlling pH value of solution is 7.5, and reaction temperature is 25 DEG C, continues to stir
Reaction 10min is mixed, gained precipitating is filtered, deionized water is cleaned 2-3 times, is then dried in vacuo, obtained silver powder.
Fig. 5 is the electron scanning micrograph of silver powder obtained, and silver powder is spongy pattern as we know from the figure.In silver powder
The transmission electron microscope photo of individual particle is similar with Fig. 3, is not repeated to provide herein.
Embodiment 4
The present embodiment preparation method is similar to Example 2, is a difference in that and changes reaction temperature and pH value.In embodiment 2
Reaction temperature is 25 DEG C, pH value 12.0；Reaction temperature is 60 DEG C in embodiment 4, pH value 8.0
Polysorbas20 (the dehydration of 0.01mol/L silver nitrate solution, 0.1mol/L hydrazine hydrate solution and 0.5mol/L is prepared respectively
Sorbierite esters surface active agent) each 1L of solution.First 1L hydrazine hydrate solution is added in reaction vessel, and with the speed of 500rpm
Carry out magnetic agitation；After velocity-stabilization to be mixed, 1L silver nitrate solution is added at the uniform velocity with the speed of 1L/min；It is reacted at 60 DEG C
After 1min, the polysorbas20 solution of 1L is added with the speed of 1L/min.Controlling pH value of solution is 8.0, and reaction temperature is 25 DEG C, continues to stir
Reaction 10min is mixed, gained precipitating is filtered, deionized water is cleaned 2-3 times, is then dried in vacuo, obtained silver powder.
Fig. 6 is the electron scanning micrograph of silver powder obtained, and silver powder is spongy pattern as we know from the figure.In silver powder
The transmission electron microscope photo of individual particle is similar with Fig. 3, is not repeated to provide herein.
Embodiment 5
The present embodiment preparation method is similar to Example 3, is a difference in that change charging rate.Silver nitrate in embodiment 3
It is respectively 100mL/min and 100mL/min, silver nitrate solution and Span in embodiment 5 that speed, which is added, in solution and 60 solution of Span
It is respectively 500mL/min and 500mL/min that speed, which is added, in 60 solution.
Tween 80 (the dehydration mountain of 0.1mol/L silver nitrate solution, 0.2mol/L hydroxylamine solution and 0.5mol/L is prepared respectively
Pears alkoxide surfactant) each 1L of solution.First 1L hydroxylamine solution is added in reaction vessel, and with the progress of the speed of 200rpm
Magnetic agitation；After velocity-stabilization to be mixed, 1L silver nitrate solution is added at the uniform velocity with the speed of 500mL/min；It is reacted at 25 DEG C
After 1min, the Tween 80 solution of 1L is added with the speed of 500mL/min.Controlling pH value of solution is 7.5, and reaction temperature is 25 DEG C, after
It is continuous to be stirred to react 10min, gained precipitating is filtered, deionized water is cleaned 2-3 times, is then dried in vacuo, obtained silver
Powder.
Fig. 7 is the electron scanning micrograph of silver powder obtained, and silver powder is spongy pattern as we know from the figure.In silver powder
The transmission electron microscope photo of individual particle is similar with Fig. 3, is not repeated to provide herein.
Embodiment 6
The present embodiment preparation method is similar to Example 3, is a difference in that change mixing speed.Speed is stirred in embodiment 3
Degree is 200rpm, and mixing speed is 10rpm. in embodiment 6
(the dehydration mountain of Span 60 of 0.1mol/L silver nitrate solution, 0.2mol/L hydroxylamine solution and 0.5mol/L is prepared respectively
Pears alkoxide surfactant) each 1L of solution.First 1L hydroxylamine solution is added in reaction vessel, and with the progress of the speed of 10rpm
Magnetic agitation；After velocity-stabilization to be mixed, 1L silver nitrate solution is added at the uniform velocity with the speed of 500mL/min；It is reacted at 25 DEG C
After 1min, 60 solution of Span of 1L is added with the speed of 500mL/min.Controlling pH value of solution is 7.5, and reaction temperature is 25 DEG C, after
It is continuous to be stirred to react 10min, gained precipitating is filtered, deionized water is cleaned 2-3 times, is then dried in vacuo, obtained silver
Powder.
Fig. 8 is the electron scanning micrograph of silver powder obtained, and silver powder is spongy pattern as we know from the figure.In silver powder
The transmission electron microscope photo of individual particle is similar with Fig. 3, is not repeated to provide herein.
After comparing Fig. 5 (embodiment 3) and Fig. 8 (embodiment 6) it is found that reducing mixing speed, the microcosmic knot of silver powder obtained
In structure, the fining structure on surface is relatively abundant, has more branch shape structures.The possible reason is reducing mixing speed
Afterwards, collision probability is smaller between Argent grain, to assemble less, the branch structure of particle surface then retains more.
Embodiment 7
The present embodiment preparation method is similar to Example 3, is a difference in that and changes the reaction time.When being reacted in embodiment 3
Between T1 be 1min, T2 10min, reaction time T1 is 5s, T2 5min in embodiment 7.
(the dehydration mountain of Span 60 of 0.1mol/L silver nitrate solution, 0.2mol/L hydroxylamine solution and 0.5mol/L is prepared respectively
Pears alkoxide surfactant) each 1L of solution.First 1L hydroxylamine solution is added in reaction vessel, and with the progress of the speed of 10rpm
Magnetic agitation；After velocity-stabilization to be mixed, 1L silver nitrate solution is added at the uniform velocity with the speed of 500mL/min；In 25 DEG C of reaction 5s
Afterwards, 60 solution of Span of 1L is added with the speed of 500mL/min.Controlling pH value of solution is 7.5, and reaction temperature is 25 DEG C, continues to stir
Reaction 5min is mixed, gained precipitating is filtered, deionized water is cleaned 2-3 times, is then dried in vacuo, obtained silver powder.
Fig. 9 is the electron scanning micrograph of silver powder obtained, and silver powder is spongy pattern as we know from the figure.In silver powder
The transmission electron microscope photo of individual particle is similar with Fig. 3, is not repeated to provide herein.
Embodiment 8
The present embodiment is to prepare bronze.
The Qu Datong X-100 for preparing 0.1mol/L chlorauric acid solution, 0.2mol/L hydroxylamine solution and 0.2mol/L respectively is (poly-
Ethylene oxide ether surfactant) each 1L of solution.First 1L hydroxylamine solution is added in reaction vessel, and with the progress of the speed of 5rpm
Magnetic agitation；After velocity-stabilization to be mixed, 1L silver nitrate solution is added at the uniform velocity with the speed of 200mL/min；It is reacted at 25 DEG C
After 1min, the Qu Datong X-100 solution of 1L is added with the speed of 200mL/min.Controlling pH value of solution is 7.5, reaction temperature 25
DEG C, continue to be stirred to react 5min, gained precipitating is filtered, deionized water cleaning 2-3 times, is then dried in vacuo, is made
Obtain bronze.
Figure 10 is the electron scanning micrograph of bronze obtained, and bronze is spongy pattern as we know from the figure.Bronze
The transmission electron microscope photo of middle individual particle is similar with Fig. 3, is not repeated to provide herein.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Several alternative or obvious variations are made under the premise of not departing from present inventive concept, and performance or use is identical, all should be considered as
It belongs to the scope of protection of the present invention.
Claims (8)
1. a kind of preparation method of the metal powder with spongy microstructure, it is characterised in that: the following steps are included: S1,
Metal salt solution, reducing agent solution and surfactant solution, the metal salt solution, reducing agent solution and surface are prepared respectively
The ratio between molar concentration of activator solution is 1:0.1~10:0.05~50, the metal salt solution, reducing agent solution and surface
The volume ratio of activator solution is 1:1:1；The reducing agent solution is added in reaction vessel, with 10~1000rpm's by S2
Mixing speed is stirred, and the metal salt solution is at the uniform velocity then added with second speed (V2), in 25 DEG C~80 DEG C of temperature
After lower sufficiently reaction 5 seconds~1 minute, the surfactant solution is added at the uniform velocity with third speed (V3), adjusts mixed solution
PH value 7.5≤pH≤12 range, sufficiently react 5~after ten minutes, in the reaction vessel generate precipitating；Wherein, institute
Second speed (V2) and third speed (V3) are stated in the range of 0.1~1L/min；The precipitating is filtered, washes by S3
Processing and vacuum drying are washed, the metal powder with spongy microstructure is made.
2. the preparation method of the metal powder according to claim 1 with spongy microstructure, it is characterised in that: step
In rapid S2, the mixing speed is in the range of 100~800rpm.
3. the preparation method of the metal powder according to claim 1 with spongy microstructure, it is characterised in that: step
In rapid S1, silver nitrate solution, hydrazine hydrate solution and arlacels surfactant solution are prepared respectively.
4. the preparation method of the metal powder according to claim 1 with spongy microstructure, it is characterised in that: step
In rapid S1, the metal salt solution is silver salt solution, and the reducing agent in the reducing agent solution is formaldehyde, acetaldehyde, citric acid, resists
One of bad hematic acid, sodium borohydride, azanol, hydrazine or a variety of mixing.
5. the preparation method of the metal powder according to claim 1 with spongy microstructure, it is characterised in that: step
In rapid S1, the metal salt solution is gold salt solution, the reducing agent in the reducing agent solution be 2- amino-3-mercaptopropionic acid,
One of sodium borohydride or a variety of mixing；Alternatively, the metal salt solution is copper salt solution, in the reducing agent solution
Reducing agent is one of hydroxylamine hydrochloride, sodium borohydride or a variety of mixing.
6. the preparation method of the metal powder according to claim 1 with spongy microstructure, it is characterised in that: step
In rapid S1, the surfactant in the surfactant solution is polyvinylpyrrolidone, polyethenoxy ether class surface-active
One of agent, sorbitan ester, non-ion fluorin carbon surface active agent or a variety of mixing.
7. a kind of preparation method according to claims 1 to 6 metal powder obtained with spongy microstructure.
8. a kind of conductive material, it is characterised in that: including base material and the metal powder being dispersed in base material, the gold
Category powder is metal powder as claimed in claim 7.
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| JP4487067B2 (en) * | 2004-07-30 | 2010-06-23 | 国立大学法人 宮崎大学 | Platinum nanoparticles and method for producing the same |
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| CN103537708A (en) * | 2013-09-09 | 2014-01-29 | 烟台同立高科新材料股份有限公司 | Hyperpure silver powder for solar cell conductive silver paste and preparing method of hyperpure silver powder |
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