CN105834450B - The preparation method of silver powder - Google Patents
The preparation method of silver powder Download PDFInfo
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- CN105834450B CN105834450B CN201610315653.8A CN201610315653A CN105834450B CN 105834450 B CN105834450 B CN 105834450B CN 201610315653 A CN201610315653 A CN 201610315653A CN 105834450 B CN105834450 B CN 105834450B
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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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- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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Abstract
Present invention discloses a kind of preparation methods of silver powder.The preparation method of silver powder of the invention includes: water reaction system A, reducing agent solution B, the dispersant solution C that silver ion is respectively configured；A, B and C are injected in continuous conduit formula reactor, hybrid reaction, to deposit Argent grain；With the drying Argent grain, crush and screen to obtain.
Description
Technical field
The present invention relates to a kind of preparation methods of silver powder, more particularly it relates to a kind of silver for electronic component
The preparation method of powder.
Background technique
Metallic silver has excellent conductive, thermally conductive and inoxidizability, suffers from electrician and electronics industry and widely answers
With.The silver-colored adaptable electronic component of material, printed circuit, the solar battery of interior electrode, circuit board including multi-layer capacitor
Electrode, Plasmia indicating panel (PDP) substrate electrode conventional electrocondution slurry, usually by organic carrier mix silver powder,
Glass powder and inorganic assistant etc., agitated grinding roll, and wherein mass fraction highest shared by silver powder, the quality of silver powder are very big
Ground affects the performance of final slurry.With the reduction of these component sizes, the silver powder for electrocondution slurry is needed to have
Rationally small partial size and rationally narrow particle size range, to form the printed circuit with high density and fine line.It is especially current
Research and extensively, the huge solar cell size of dosage because sintering time is short need enough sintering activities, appropriate
Diffusion is dissolved, studies have shown that better electricity, mechanics can be obtained by narrow, the of uniform size silver powder of collocation distribution of particles
Performance.
Existing there are many ways to preparing ultra tiny silver powder, liquid phase method, solid phase method and vapor phase method have for studying, but most
Common, most economical large scale production method is still liquid-phase precipitation method.But it is most of in liquid-phase precipitation method to be prepared for batch process
Silver powder particles.Such as the patent of patent No. CN200480020987.8 provides a kind of manufacturing method of particle silver powder, makes silver nitrate
Aqueous solution and ammonium hydroxide hybrid reaction obtain silver ammonia complex aqueous solution, are restored by adding in the silver ammonia complex aqueous solution
Agent, reduction are precipitated silver particles, are filtered, wash, being dried to obtain particle silver powder, which is characterized in that making above-mentioned silver ammonia complex
Aqueous solution contacts mixing with organic reducing agent, also, in solution upon mixing, and silver concentration maintains 1g/l~6g/l, organic
Reductant concentration maintains 1g/l~3g/l to restore precipitation silver particles.
Such as the patent of patent No. CN200480020988.2 provides a kind of manufacturing method of particle silver powder, makes silver nitrate water
Solution and ammonium hydroxide hybrid reaction obtain silver ammonia complex aqueous solution, by adding reducing agent also in the silver ammonia complex aqueous solution
Silver particles are precipitated in original, are filtered, wash, being dried to obtain particle silver powder, which is characterized in that making above-mentioned silver ammonia complex aqueous solution
Mixing is contacted with organic reducing agent, and to maintain 1g/l~6g/l, organic reducing agent dense for silver concentration in solution upon mixing
Degree maintains 1g/l~3g/l to restore precipitation silver particles, which is filtered, is washed, is washed with excessive amount of ethanol solution
It washs.
In short, in the prior art, generally preparing silver powder using batch process, products obtained therefrom is able to satisfy the need of general conductive silver paste
It wants, but there is also many problems, such as single batch of limits throughput, the deficiencies of unstable quality when high-volume expanding production, production process is various.This
It is the concentration of material, stirring, ion diffusion, the formation of nucleus because batch process produces in the entire production process of silver powder
It is all continually changing with growth.Therefore, when prepared by laboratory, since mixing effect is very good, stirring is easily uniform, and
Amount is few, and the reaction time is short, is typically easy to prepare the silver powder sample haveing excellent performance, but in contrast, industrialization product it is equal
Even property, dispersibility are with regard to deviation.
Hence it is highly desirable to which the improvement by formula and production technology more efficiently prepares dispersibility by continuity method
Silver powder high, uniformity is good.
Summary of the invention
To solve the above-mentioned problems, one aspect of the present invention provides a kind of preparation method of silver powder, comprising:
Water reaction system A, reducing agent solution B, the dispersant solution C of silver ion is respectively configured；
A, B and C are injected in continuous conduit formula reactor, hybrid reaction, to deposit Argent grain；With the drying silver
Particle crushes and screens to obtain.
In a kind of embodiment of the method for the present invention, the water reaction system A of the silver ion include silver-containing material and
Pure water.
At least one of in a kind of embodiment of the method for the present invention, the silver-containing material is selected from the group: silver chlorate,
Silver nitrate, silver acetate, silver carbonate and silver sulfate.
In a kind of embodiment of the method for the present invention, the reducing agent solution B includes reducing agent and pure water.
At least one of in a kind of embodiment of the method for the present invention, the reducing agent is selected from the group: formaldehyde, first
Acid, vitamin C, hydrazine hydrate, hydroxyl sulfate, glucose, sodium borohydride, alkanolamine and quinhydrones.
In a kind of embodiment of the method for the present invention, the dispersant solution C includes:
Dispersing agent；
With at least one of pure water or ethyl alcohol.
At least one of in a kind of embodiment of the method for the present invention, the dispersing agent is selected from the group: fatty acid, rouge
Fat hydrochlorate, surfactant, organic metal, chelating agent, hydroxy polymer, ethoxy based polyalcohol and protecting colloid.
In a kind of embodiment of the method for the present invention, the injection by A, B and C injection continuous conduit formula reactor
Mode one of is selected from the group:
C is mixed with A, A/C mixed liquor and B are then injected separately into continuous conduit formula reactor；
C is mixed with B, B/C mixed liquor and A are then injected separately into continuous conduit formula reactor；
A, B, C are injected separately into continuous conduit formula reactor；
A and B are injected separately into continuous conduit formula reactor, and behind the contact point of A and B, inject C.
In a kind of embodiment of the method for the present invention, the internal diameter of the continuous conduit formula reactor is 10mm-200mm,
Length is 10cm-10m.
In a kind of embodiment of the method for the present invention, the inside of the continuous conduit formula reactor is filled equipped with mechanical stirring
Set and ultrasound wave vibrating bar in it is one or two kinds of.
The present invention by adjusting the good variable grain size of the available uniformity of PH of reaction solution silver powder, by adjusting
The additive amount and injection mode of dispersing agent, the built-in stirring of binding reactor and ultrasonic wave distributing device, can be very good adjustment powder
Dispersibility, the uniformity of particle diameter distribution of body.Particle described herein can uniformly observe from scanning electron microscope, particle
Size can be adjusted from tens nanometers to several microns.Silver powder is particularly suitable for solar energy face electrode slurry, PDP slurry is burnt
Junction type etc..
The above-mentioned of the application and other features, aspects and advantages are more readily understood with reference to following detailed description.
Specific embodiment
The detailed description for preferred implementation method of the invention below of participating in the election of and including embodiment this hair can be more easily to understand
Bright content.Unless otherwise defined, all technologies used herein and scientific term have common with fields of the present invention
The normally understood identical meaning of technical staff.When there is a conflict, the definition in this specification shall prevail.
As used herein term " by ... preparation " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover non-exclusionism includes.For example, the combination comprising listed elements
Object, step, method, product or device are not necessarily limited to those elements, but may include not expressly listed other elements or
Such composition, step, method, product or the intrinsic element of device.
Conjunction " Consists of " excludes any element that do not point out, step or component.If in claim, this
Phrase will make claim closed, so that it is not included the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following after theme in the clause that phrase " Consists of " appears in claim main body,
It is only limited to element described in the clause；Other elements are not excluded except the claim as a whole.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range is intended to include its end
Value and all integers and score in the range.
Singular includes that plural number discusses object, unless the context clearly dictates otherwise." optional " or it is " any
It is a kind of " refer to that the item described thereafter or event may or may not occur, and the description include situation that event occurs and
The situation that event does not occur.
Approximate term in specification and claims is used to modify quantity, and it is specific to indicate that the present invention is not limited to this
Quantity further includes the acceptable modified part without will lead to the change of dependency basis this function close with the quantity.Phase
It answers, modifies a numerical value with " about ", " about " etc., mean that the present invention is not limited to the exact numericals.In some examples, approximate
Term likely corresponds to the precision of the instrument of measurement numerical value.In present specification and claims, range limits can be with
Combination and/or exchange, these ranges if not stated otherwise include all subranges contained therebetween.
In addition, indefinite article "an" before element of the present invention or component and "one" quantitative requirement to element or component
(i.e. frequency of occurrence) unrestriction.Therefore "one" or "an" should be read as including one or at least one, and odd number
The element or component of form also include plural form, unless the obvious purport of the quantity refers to singular.
One aspect of the present invention provides a kind of preparation method of silver powder, comprising:
Water reaction system A, reducing agent solution B, the dispersant solution C of silver ion is respectively configured；
A, B and C are injected in continuous conduit formula reactor, hybrid reaction, to deposit Argent grain；With the drying silver
Particle crushes and screens to obtain.
The water reaction system A of silver ion
As the water reaction system of silver ion, can be used containing the water-soluble of silver nitrate, silver salt complex compound or silver-colored intermediate
Liquid or slurry.Silver salt complex compound can be formed by the way that ammonium hydroxide, ammonium salt, chelate compound etc. is added.Silver-colored intermediate can be by adding
Enter sodium hydroxide, sodium chloride, sodium carbonate etc. to prepare.In water reaction system of the invention, the concentration of silver ion is preferably 10-
250g/L, more preferably 100-200g/L, most preferably 150g/L.
It in one embodiment, include silver-containing material and pure water for the water reaction system of silver ion of the invention.
Silver-containing material for the application at least one of is selected from the group: silver chlorate, silver nitrate, silver acetate, silver carbonate
And silver sulfate；Preferably, the silver-containing material is silver nitrate.
In one embodiment, for the water reaction system of silver ion of the invention, ammonium hydroxide and PH are further included
Regulator.
In one embodiment, the PH regulator is sodium hydroxide.
The addition of PH regulator can effectively adjust the pH value of the water reaction system of silver ion, keep it in 7.5~
Between 13.5, it is preferable that the pH value of the water reaction system is 8~12, it is highly preferred that the pH value of the water reaction system is
12。
Reducing agent solution B
In a kind of embodiment of the method for the present invention, the reducing agent solution B includes reducing agent and pure water.
At least one of in a kind of embodiment of the method for the present invention, the reducing agent is selected from the group: formaldehyde, first
Acid, vitamin C, hydrazine hydrate, hydroxyl sulfate, glucose, sodium borohydride, alkanolamine and quinhydrones；Preferably, the reducing agent
For vitamin C.
In a kind of embodiment of the method for the present invention, the reducing agent solution B further includes PH regulator.
In one embodiment, the PH regulator is sodium hydroxide.
The addition of PH regulator can effectively adjust the pH value of reducing agent solution B, it is preferable that the PH of the reducing agent solution B
Value is 8.
Dispersant solution C
In a kind of embodiment of the method for the present invention, the dispersant solution C includes:
Dispersing agent；
At least one of pure water or ethyl alcohol.
At least one of in a kind of embodiment of the method for the present invention, the dispersing agent is selected from the group: fatty acid, rouge
Fat hydrochlorate, surfactant, organic metal, chelating agent, hydroxy polymer, ethoxy based polyalcohol and protecting colloid；For example, typical
Dispersing agent oleic acid or PVA can be used.
Injection mode
In the present invention, the mode of A, B and C injection continuous conduit formula reactor is not particularly limited, can be infused respectively
Enter, it can also any mixed injection, it is preferable that the injection mode by A, B and C injection continuous conduit formula reactor is selected from
One of the following group:
C is mixed with A, A/C mixed liquor and B are then injected separately into continuous conduit formula reactor；
C is mixed with B, B/C mixed liquor and A are then injected separately into continuous conduit formula reactor；
A, B, C are injected separately into continuous conduit formula reactor；
A and B are injected separately into continuous conduit formula reactor, and behind the contact point of A and B, inject C；
It is highly preferred that the injection mode by A, B and C injection continuous conduit formula reactor is to be injected separately into A and B
Continuous conduit formula reactor, and behind the contact point of A and B, inject C.
Preferably, when A and B are injected separately into continuous conduit formula reactor by selection, and behind the contact point of A and B, C is injected
When, A, B inject continuous conduit formula reactor with the flow of 5L/Min, and behind the contact point of A and B at 2 meters, with 1L/Min's
Flow injects C, and implant angle is to flow to 90 ° of angle > with solution A, B mixed liquor.
Continuous conduit formula reactor
Continuous conduit formula reactor be it is a kind of in a tubular form, the very big continuous manipulation reactor of draw ratio.This reactor can
With very long, if the reactor pipe range of propylene dimerization is in terms of kilometer.It has the advantages that back-mixing is small, volumetric efficiency is high.
It is not particularly limited for continuous conduit formula reactor of the invention, it is preferred that the continuous conduit formula is reacted
The internal diameter of device is 10mm-200mm, length 10cm-10m；It is highly preferred that the internal diameter of the continuous conduit formula reactor is
50mm-180mm, length 3m-8m；Most preferably, the internal diameter of the continuous conduit formula reactor is 100mm, length 6m.
In order to further increase the efficiency of continuous conduit formula reactor, in one embodiment, the continuous conduit formula
The inside of reactor is equipped with one or two kinds of in mechanical stirring device and ultrasound wave vibrating bar；Preferably, the continuous conduit
The inside of formula reactor is equipped with mechanical stirring device and ultrasound wave vibrating bar simultaneously, and the built-in machines agitating device is electricity
The multi-layer oar blade formula agitating paddle that machine drives, mixing speed are in 1-10000RPM, the ultrasonic power of the ultrasound wave vibrating bar
0.1-5KW。
The present invention includes following implementation:
A kind of preparation method of the silver powder of embodiment 1., comprising:
Water reaction system A, reducing agent solution B, the dispersant solution C of silver ion is respectively configured；
A, B and C are injected in continuous conduit formula reactor, hybrid reaction, to deposit Argent grain；With
The dry Argent grain, crushes and screens to obtain.
The method of 2. embodiment 1 of embodiment, wherein the water reaction system A of the silver ion include silver-containing material and
Pure water.
The method of 3. embodiment 2 of embodiment, wherein the silver-containing material at least one of is selected from the group: chlorination
Silver, silver nitrate, silver acetate, silver carbonate and silver sulfate.
The method of any one of 4. embodiment 2-3 of embodiment, wherein the water reaction system A of the silver ion, into
One step includes ammonium hydroxide and PH regulator.
The method of any one of 5. embodiment 1-4 of embodiment, wherein in the water reaction system A, silver ion it is dense
Degree is 10-250g/L.
The method of any one of 6. embodiment 1-5 of embodiment, wherein in the water reaction system A, silver ion it is dense
Degree is 150g/L.
The method of any one of 7. embodiment 1-6 of embodiment, wherein the pH value of the water reaction system A be 7.5~
13.5。
The method of any one of 8. embodiment 1-7 of embodiment, wherein the pH value of the water reaction system A is 12.
The method of any one of 9. embodiment 1-8 of embodiment, wherein the reducing agent solution B include reducing agent and
Pure water.
Method described in 10. embodiment 9 of embodiment, wherein the reducing agent at least one of is selected from the group: first
Aldehyde, formic acid, vitamin C, hydrazine hydrate, hydroxyl sulfate, glucose, sodium borohydride, alkanolamine and quinhydrones.
The method of any one of 11. embodiment 9-10 of embodiment, wherein the reducing agent solution B further includes PH tune
Save agent.
The method of any one of 12. embodiment 1-11 of embodiment, wherein the dispersant solution C includes:
Dispersing agent；With
At least one of pure water or ethyl alcohol.
The method of 13. embodiment 12 of embodiment, wherein the dispersing agent at least one of is selected from the group: fat
Acid, fatty acid salt, surfactant, organic metal, chelating agent, hydroxy polymer, ethoxy based polyalcohol and protecting colloid.
The method of any one of 14. embodiment 1-13 of embodiment, wherein described inject continuous conduit for A, B and C
The injection mode of formula reactor is to mix C with A, and A/C mixed liquor and B are then injected separately into continuous conduit formula reactor.
The method of any one of 15. embodiment 1-13 of embodiment, wherein described inject continuous conduit for A, B and C
The injection mode of formula reactor is to mix C with B, and B/C mixed liquor and A are then injected separately into continuous conduit formula reactor.
The method of any one of 16. embodiment 1-13 of embodiment, wherein described inject continuous conduit for A, B and C
The injection mode of formula reactor is that A, B, C are injected separately into continuous conduit formula reactor.
The method of any one of 17. embodiment 1-13 of embodiment, wherein described inject continuous conduit for A, B and C
The injection mode of formula reactor is A and B to be injected separately into continuous conduit formula reactor, and behind the contact point of A and B, inject C.
The method of 18. embodiment 17 of embodiment, wherein A, B are with the flow injection continuous conduit formula reaction of 5L/Min
Device, and behind the contact point of A and B at 2 meters, C is injected with the flow of 1L/Min, implant angle is to flow to solution A, B mixed liquor
90 ° of angle >.
The method of any one of 19. embodiment 1-18 of embodiment, wherein the internal diameter of the continuous conduit formula reactor
For 10mm-200mm, length 10cm-10m.
The method of any one of 20. embodiment 1-19 of embodiment, wherein the internal diameter of the continuous conduit formula reactor
For 100mm, length 6m.
The method of any one of 21. embodiment 1-20 of embodiment, wherein the inside of the continuous conduit formula reactor
Equipped with one or two kinds of in mechanical stirring device and ultrasound wave vibrating bar.
The method of any one of 22. embodiment 1-21 of embodiment, wherein the inside of the continuous conduit formula reactor
Mechanical stirring device and ultrasound wave vibrating bar are housed simultaneously, and the built-in machines agitating device is motor-driven multilayer paddle
Leaf formula agitating paddle, mixing speed are 0.1-5KW in 1-10000RPM, the ultrasonic power of the ultrasound wave vibrating bar.
Embodiments of the present invention further define in the following example.
Embodiment 1
10.2L ammonium hydroxide (wt%=28%) is added in 200L container, adds pure water and 1.7Kg silver nitrate, stirring and dissolving adds
It is 12 that adding sodium hydroxide, which adjusts solution pH value, is configured to the solution A of concentration of silver ions 10g/L, and temperature is kept for 40 DEG C；Add 10g
Oleic acid to 20g ethyl alcohol, stirring and dissolving obtains solution C；Solution C is added to solution A, stirring and maintaining temperature is 40 DEG C.It will
The commercially available CP grades of formalin (wt%=37%) of 8.5L is dissolved in 80L pure water and obtains solution B, and constant temperature is in 40 DEG C；Solution A, C it is mixed
It closes liquid and solution B is pumped into pipeline reactor respectively with the flow of 20L/Min, mixed liquor is filtered after reaction, filtered silver
Powder is cleaned to conductivity with deionized water less than 100 μ S/cm, washed once with dehydrated alcohol, filter cake dry, pulverize sieve in 50 DEG C
Get silver powder；
The internal diameter of the continuous conduit formula reactor is 100mm, length 6m；The inside of the continuous conduit formula reactor
Mechanical stirring device and ultrasonic echography wave vibrating head are housed simultaneously, and the built-in machines agitating device is motor-driven
Multi-layer oar blade formula agitating paddle, mixing speed are 0.1-5KW in 1-10000RPM, the ultrasonic power of the ultrasound wave vibrating bar.
Embodiment 2
10.2L ammonium hydroxide (wt%=28%) is added in 50L container, adds pure water and 1.7Kg silver nitrate, stirring and dissolving adds
It is 13 that adding sodium hydroxide, which adjusts solution pH value, is configured to the solution A of concentration of silver ions 100g/L, and temperature is kept for 40 DEG C.By 0.5L
Commercially available CP grades of hydrazine hydrate solution (wt%=80%) is dissolved in 5L pure water and obtains solution B, and constant temperature is in 40 DEG C；15gPVA is stirred
It is dissolved in 5.5L pure water and obtains solution C.Solution A, B, C are pumped into pipeline reactor respectively with the flow of 2L/Min, 1L/min, reaction
Mixed liquor is filtered afterwards, and filtered silver powder is cleaned to conductivity with deionized water less than 100 μ S/cm, is washed with dehydrated alcohol
It washs once, filter cake dry, pulverize in 50 DEG C and sieve to obtain silver powder；
The internal diameter of the continuous conduit formula reactor is 25mm, length 6m；The inside of the continuous conduit formula reactor
Mechanical stirring device and ultrasound wave vibrating bar are housed simultaneously, and the built-in machines agitating device is motor-driven multilayer paddle
Leaf formula agitating paddle, mixing speed are 0.1-5KW in 1-10000RPM, the ultrasonic power of the ultrasound wave vibrating bar.
Embodiment 3
1.7Kg silver nitrate is dissolved in pure water, stirring and dissolving is configured to the silver nitrate solution A of concentration of silver ions 150g/L,
Temperature is kept for 40 DEG C.Addition sodium hydroxide, 2000g vitamin C are dissolved in 8L pure water, are configured to the aqueous solution B that pH value is 8, temperature
Degree is kept for 40 DEG C.Solution A, B are pumped into pipeline reactor with the flow of 5L/Min, behind the contact point reactor solution A, B at 2 meters
The PVA aqueous solution C of 15g/L is injected, flow 1L/Min is injected, implant angle is to flow to 90 ° of angle > with solution A, B mixed liquor.
Mixed silver powder is filtered, and filtered silver powder is cleaned to conductivity with deionized water less than 100 μ S/cm, with anhydrous second
Alcohol washed once, and filter cake dry, pulverize in 50 DEG C and sieve to obtain silver powder；
The internal diameter of the continuous conduit formula reactor is 40mm, length 6m；The inside of the continuous conduit formula reactor
Mechanical stirring device and ultrasound wave vibrating bar are housed simultaneously, and the built-in machines agitating device is motor-driven multilayer paddle
Leaf formula agitating paddle, mixing speed are 0.1-5KW in 1-10000RPM, the ultrasonic power of the ultrasound wave vibrating bar.
Comparative example 1
10.2L ammonium hydroxide (wt%=28%) is added in 50L container, adds pure water and 1.7Kg silver nitrate, stirring and dissolving adds
It is 13 that adding sodium hydroxide, which adjusts solution pH value, is configured to the solution A of concentration of silver ions 50g/L, and temperature is kept for 40 DEG C.By the city 0.5L
It sells CP grades of hydrazine hydrate solution (wt%=80%) and is dissolved in 21L pure water and obtain solution B, constant temperature is in 40 DEG C.Solution A, B with
The flow of 2L/Min is pumped into pipeline reactor, and mixed silver powder is filtered, and filtered silver powder is cleaned with deionized water
It to conductivity less than 100 μ S/cm, washed once with dehydrated alcohol, filter cake dry, pulverize in 50 DEG C and sieve to obtain silver powder；
The internal diameter of the continuous conduit formula reactor is 100cm, length 6m；The inside of the continuous conduit formula reactor
Mechanical stirring device and ultrasound wave vibrating bar are housed simultaneously, and the built-in machines agitating device is motor-driven multilayer paddle
Leaf formula agitating paddle, mixing speed are 0.1-5KW in 1-10000RPM, the ultrasonic power of the ultrasound wave vibrating bar.
Comparative example 2
10.2L ammonium hydroxide (wt%=28%) is added in 200L container, adds pure water and 1.7Kg silver nitrate, stirring and dissolving adds
It is 12 that adding sodium hydroxide, which adjusts solution pH value, adds 2g oleic acid stirring and dissolving, is configured to the solution A of concentration of silver ions 10g/L, temperature
Degree is kept for 40 DEG C.The commercially available CP grades of formalin (wt%=37%) of 8.5L is dissolved in 80L pure water and obtains solution B, constant temperature is in 40
℃；Solution B is pumped into solution A with the flow of 10L/Min under stirring, mixed liquor is filtered after reaction, and filtered silver powder is used
Deionized water is cleaned to conductivity less than 100 μ S/cm, washed once with dehydrated alcohol, and filter cake dry, pulverize in 50 DEG C and sieve
Silver powder.
Above-mentioned test result is shown in Table 1.
Table 1
Above data can be seen that the type of reducing agent, the type of dispersing agent and adding manner, feed way, system PH
The factors such as value and the additional amount of dispersing agent can produce a very large impact the quality of gained silver powder.By the adjustment of above-mentioned factor,
The silver powder specific surface area that the application obtains is less than 1.55m2/ g, and there is excellent dispersibility and uniformity, thus provide this
The advantageous effects of invention.
Example above-mentioned is merely illustrative, some features of the feature for explaining the disclosure.The attached claims
It is intended to the range as wide as possible for requiring to be contemplated that, and embodiments as presented herein is only according to all possible embodiment
Combined selection embodiment explanation.Therefore, the purpose of applicant is that the attached claims are not illustrated the present invention
Feature exemplary selectional restriction.And the progress in science and technology will be formed language express it is inaccurate due to and not
The possible equivalent being presently considered or son replacement, and these variations should also be interpreted in the conceived case by appended
Claim covering.
Claims (1)
1. a kind of preparation method of silver powder, comprising:
10.2L ammonium hydroxide is added in 50L container, adds pure water and 1.7Kg silver nitrate, stirring and dissolving, and addition sodium hydroxide adjusts molten
Liquid pH value is 13, is configured to the solution A of concentration of silver ions 100g/L, and temperature is kept for 40 DEG C；By the commercially available CP grades of hydrazine hydrate of 0.5L
Solution is dissolved in 5L pure water and obtains solution B, and constant temperature is in 40 DEG C；15gPVA stirring and dissolving is obtained into solution C in 5.5L pure water；It will be molten
Liquid A and B injects continuous conduit formula reactor respectively with the flow of 2L/Min, and behind the contact point of A and B at 2 meters, with 1L/Min
Flow inject C, mixed liquor is filtered after reaction, and filtered silver powder is cleaned to conductivity with deionized water less than 100 μ S/
Cm washed once with dehydrated alcohol, and filter cake dry, pulverize in 50 DEG C and sieve to obtain silver powder；
The concentration of the ammonium hydroxide is 28wt%；The concentration of the hydrazine hydrate solution is 80wt%；
The internal diameter of the continuous conduit formula reactor is 25mm, length 6m；The inside of the continuous conduit formula reactor is simultaneously
Equipped with mechanical stirring device and ultrasound wave vibrating bar, and the built-in machines agitating device is motor-driven multi-layer oar blade formula
Agitating paddle, mixing speed are 0.1-5KW in 1-10000RPM, the ultrasonic power of the ultrasound wave vibrating bar.
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| CN106334802B (en) * | 2016-09-29 | 2018-12-28 | 清华大学深圳研究生院 | Metal powder with spongy microstructure and preparation method thereof, conductive material |
| CN106493390B (en) * | 2016-11-29 | 2018-06-08 | 金川集团股份有限公司 | A kind of liquid phase slit interference synthesis device |
| CN108213455A (en) * | 2016-12-22 | 2018-06-29 | 富士康(昆山)电脑接插件有限公司 | The preparation method of nano metal colloidal sol |
| CN107457411B (en) * | 2017-06-15 | 2019-02-05 | 昆明理工大学 | A method of preparing super fine silver powder |
| CN108941599B (en) * | 2018-07-03 | 2021-06-08 | 珠海市彩龙科技有限公司 | Continuous preparation method of nano-copper |
| CN110102778B (en) * | 2019-06-14 | 2021-11-02 | 珠海银波科技发展有限公司 | Preparation method of low-temperature sintered high-crystallinity silver powder |
| CN116372181B (en) * | 2023-06-07 | 2023-09-05 | 长春黄金研究院有限公司 | Rod-shaped silver powder and preparation method thereof |
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