CN106583751A - Preparation method of flat silver powder - Google Patents
Preparation method of flat silver powder Download PDFInfo
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- CN106583751A CN106583751A CN201611241747.1A CN201611241747A CN106583751A CN 106583751 A CN106583751 A CN 106583751A CN 201611241747 A CN201611241747 A CN 201611241747A CN 106583751 A CN106583751 A CN 106583751A
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- preparation
- argentum powder
- silver nitrate
- flattening
- powder
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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
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
Abstract
The invention discloses a preparation method of flat silver powder. The preparation method comprises the following steps: firstly, weighing a silver nitrate solid, adding water for dissolving; then adding water for diluting, and uniformly stirring to obtain a silver nitrate system; secondly, weighing ascorbic acid, adding water for dissolving, adding a pH regulator for carrying out pH value regulation, adding an inductive agent and adding a dispersing agent; finally, adding water for diluting, and uniformly stirring to obtain a reduction system; thirdly, adjusting the two systems to be 40 to 80DEG C, using the reduction system as a parent body, and adding the silver nitrate system into the reduction system for reacting under the set stirring speed; and fourthly, after the reaction is finished, cleaning silver powder until the electric conductivity is smaller than or equal to 20mu s/cm, filtering and pumping the silver powder, and carrying out drying. According to the preparation method disclosed by the invention, the flat silver powder is reduced from the solution at a time by a chemical reduction method; a flat structure of the prepared silver powder better facilitates laminated stacking and has great advantage in conducting property; and in a production process of the method, complicated working procedures such as preparation of a precursor and physical ball milling are not needed, and a process flow of the production is simple.
Description
Technical field
The present invention relates to metal powder material technical field, and in particular to a kind of preparation method of flattening argentum powder.
Background technology
With developing rapidly for electronics and information industry, the development of electronic silver paste and argentum powder industry has been driven.The electric conductivity of silver
The indispensable material of electronics industry is become with heat conductivity, argentum powder product is most widely used and is used in being even more electronics industry
A kind of maximum noble metal powder of amount, is the basic and key function material for producing various electronic component products.
The preparation method of argentum powder has a lot, can be divided into Physical, the such as side such as comminuting method, mechanical ball milling, vacuum evaporation condensation
Method；The method such as bioanalysises, such as microorganism, plant tissue reduction；Chemical method, such as liquid phase chemical reduction, sonochemistry method, microemulsion etc.
Method；Chemical reduction method is that current argentum powder prepares most common method, the method be in dicyandiamide solution or aqueous solution, by metal from
Son is reduced into argent simple substance with reducing agent under the parcel of surfactant.The method has that simple to operate, equipment cost is low, grain
Many advantages, such as footpath Relative distribution compares concentration.
The fast development of electron trade in recent years, model change are fast, the raw material to upstream it is also proposed that different requirement,
The argentum powder of traditional specification has been difficult the use requirement for meeting downstream client.Constantly development ＆ production New raxa argentum powder, improves argentum powder
Applicable performance become the needs of argentum powder industry development.
The conventional argentum powder species for being prepared by chemical reduction method at present has super fine silver powder, ball shape silver powder, micro silver powder；If desired for
The performance such as electric conductivity is improved, then on the basis of super fine silver powder, ball shape silver powder or micro silver powder these front axle shells, by physics ball milling
Etc. method, flattening argentum powder, Bright Silver Powder or the flake silver powder of different technologies index are prepared.
In application number CN201610321789.X patent applications, a kind of system of the ball shape silver powder of high-tap density is disclosed
Preparation Method, argentum powder tap density obtained by which are 3.5-6.0g/cm3, particle size dispersion narrow range, its granule sphericity it is high, surface
Smooth, specific surface area is little and is easy to large-scale production, is widely used in the positive silver of automobile de-fog, solaode, thick film collection
Into fields such as circuits；In application number CN201610316321.1 patent applications, disclose one kind and be accurately controlled specific surface area
Micro silver powder preparation method, its pass through control argentum powder reduction reaction in dispersant and protectant different ratio, realization can essence
The preparation method of the micro silver powder of specific surface area is controlled really, the granularity of its micro silver powder for preparing is 0.1-8.0 μm, and specific surface area is
1.0-8.0m2/ g, is widely used in medium and high temperature sintering electric slurry；In application number CN201510758839.6 patent applications
In, a kind of preparation method of the flake silver powder of the high narrow diameter distribution of lamellar rate is disclosed, precursor spherical argentum powder is selected first, so
High speed ball milling, obtains lamellar rate height, the flake silver powder of narrow diameter distribution afterwards, and the argentum powder of preparation can contain in the silver in reducing elargol
The requirement on electric performance of elargol is met on the premise of amount.
It is micro- that common process prepares the ball shape silver powder or silver for predominantly disposably preparing a point-contact by chemical reduction reaction
Powder, or the flake silver powder of surface-to-surface contact is prepared through secondary operations, physics ball milling etc..It is difficult to disposable by electronation
Preparation possesses the high jolt ramming of ball shape silver powder, piles up closely knit feature, takes into account the satisfactory electrical conductivity feature of flake silver powder surface-to-surface contact again
Argentum powder.
The content of the invention
Present invention aim to address the deficiencies in the prior art, there is provided a kind of preparation method of flattening argentum powder, using height
Molecular orientation derivant, disposably restores flattening argentum powder from solution by chemical reduction method.The conventional ball for preparing of contrast
Shape argentum powder or micro silver powder, the compressed structure of argentum powder prepared by the method are more conducive to lamination and pile up, and have very big on electric conductivity
Advantage；The conventional Bright Silver Powder for preparing of contrast or flake silver powder, the method production are not required to carry out the preparation of presoma, physics ball
The complicated procedures of forming such as mill, the technological process of production are simple, energy efficient, more suitable for industrial large-scale production.Prepared by the present invention
Argentum powder can meet seriation requirement, and silver powder particles size tunable is adjustable, can prepare 1-10 μm of different-grain diameter argentum powder, can meet difference
Technological requirement.
The present invention is achieved by the following technical solutions：
A kind of preparation method of flattening argentum powder, it is characterised in that step is as follows：
(1) weigh silver nitrate solid to be dissolved in water, then dilute, stir and be made into silver nitrate system；
(2) weigh ascorbic acid to be dissolved in water, add pH adjusting agent, add derivant, add dispersant, finally add water dilute
Release, stir and be made into reduction system；
(3) two systems are adjusted to 40～80 DEG C, with reduction system as parent, under the mixing speed of setting, by nitric acid
Silver-colored system is reacted in being added to reduction system；
(4) argentum powder is cleaned after completion of the reaction, and to cleaning mixture electrical conductivity≤20 μ s/cm, filtration is drained argentum powder and dried.
Further, in step (1) the silver nitrate system, silver nitrate concentration is 100～300g/L, it is preferable that silver nitrate
Concentration is 150～250g/L.
Further, in the step (1), the volume of silver nitrate system and the volume ratio of reduction system in step (2) are 1 ︰
2～1 ︰ 6, it is preferable that volume ratio is 1 ︰ 4.
Further, step (2) the ascorbic acid addition for silver nitrate weight 55%～65%.
Further, in the step (2) pH adjusting agent be ammonia, sodium hydroxide, one or more in sodium carbonate.
Further, step (2) the derivant addition for silver nitrate weight 0.01%～0.50%.
Further, in the step (2), derivant is sodium methylene bis-naphthalene sulfonate, diisobutyl sodium naphthalene sulfonate, methylene
One or more in the double methyl naphthalene sulfonic acid sodium of base, sodium lignin sulfonate.
Further, dispersant addition for silver nitrate weight 0.10%～2.00% in the step (2)..
Further, in the step (2), dispersant is polyethylene glycol oxide, aminated polyethylene glycol oxide, carboxylated polyoxy
Change one or more in ethylene, ammonium polyacrylate salt, modified polypropene hydrochlorate.
Further, in the step (3), mixing speed is 40～100r/min.
Compared with prior art, the invention has the advantages that：
1st, directional induction agent is present invention employs, Argent grain can be induced during the course of the reaction spatially laterally to be given birth to
It is long, flattening argentum powder is disposably restored from solution by chemical reduction method.Contrast traditional handicraft first prepares ball shape silver powder, silver
The presomas such as micropowder, then the complicated technology for preparing flattening argentum powder is polished by material ball milling, the technological process of production of the present invention is more
Simply, more energy efficient.
2nd, the present invention prepares flattening argentum powder in traditional chemical reduction method, and compressed structure is more conducive to lamination and piles up,
There is very big advantage on electric conductivity, exist better than in the performance of ball shape silver powder and flake silver powder.
3rd, the present invention can be poor by the use to pH adjusting agent, the different adjustment reaction potentials using system pH, prepares not
With particle diameter and the argentum powder of flatness.So as to prepare different in width, the flattening argentum powder of different-thickness, preparing 1-10 μm of particle diameter can
Control argentum powder, argentum powder centralized particle diameter can prepare multiple specification argentum powder.
4th, flattening argentum powder prepared by the present invention has the high jolt ramming of ball shape silver powder, high filling line；It is provided simultaneously with lamellar silver
The features such as high conductivity of powder plane-plane contact, energy effectively solving argentum powder bulk density in electric slurry, are low, and poorly conductive etc. is asked
Topic.
5th, charging reaction mode of the present invention is simple, preparation flow is simple, technique is easily-controllable, the argentum powder good stability of preparation, easily
In industrial amplification.
Description of the drawings
Fig. 1 is the flattening argentum powder scanning electron microscope (SEM) photograph of embodiments of the invention 1；
Fig. 2 is the flattening argentum powder scanning electron microscope (SEM) photograph of embodiments of the invention 2；
Fig. 3 is the flattening argentum powder scanning electron microscope (SEM) photograph of embodiments of the invention 3；
Fig. 4 is the flattening argentum powder scanning electron microscope (SEM) photograph of embodiments of the invention 4.
Specific embodiment
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that preferred reality described herein
Apply example and be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Embodiment 1：
The preparation method of the flattening argentum powder of the present embodiment, step are as follows：
(1) weigh silver nitrate solid 1kg and be placed in mixer, add pure water 4L to be dissolved；Finally plus pure water is dilute by system
Release to 5L, be made into the silver nitrate system of silver nitrate content about 200g/L；
(2) weigh ascorbic acid 0.6kg and add pure water 18L dissolvings, add sodium hydroxide 50g dissolvings；Add and dissolve in advance
Good sodium methylene bis-naphthalene sulfonate 0.5g；Carboxylated polyethylene glycol oxide 10g；Stir and add pure water that system is diluted to 20L,
Stir and be made into reduction system；
(3) silver nitrate system and reduction system are heated to into 50 DEG C, with reduction system as parent, in the stirring of 80r/min
Under speed, reacted adding in silver nitrate system 1-2min into reduction system；
(4), after reaction is finished and is aged 5min, argentum powder moves to filter tank and carries out cleaning filtration, cleans to filter liquor electrical conductivity
Till≤20 μ s/cm；Gained argentum powder is moved to into 70 DEG C of drying in baking oven.
The present embodiment is obtained the Lycoperdon polymorphum Vitt argentum powder of about 0.63kg, and argentum powder electronic microscope photos granule is uniform, height flattening is (see figure
1), between 0.5～1.0 μm, powder tapping density is 3.0-3.5g/ml to particle diameter distribution.
Embodiment 2：
The preparation method of the flattening argentum powder of the present embodiment, step are as follows：
(1) weigh silver nitrate solid 1kg and be placed in mixer, add pure water 4L to be dissolved；Finally plus pure water is dilute by system
Release to 5L, be made into the silver nitrate system of silver nitrate content about 200g/L；
(2) weigh ascorbic acid 0.6kg and add pure water 18L dissolvings, add sodium hydroxide 5g dissolvings；Addition is dissolved in advance
Sodium methylene bis-naphthalene sulfonate 0.5g；Carboxylated polyethylene glycol oxide 5g；Stir and add pure water that system is diluted to 20L, stir
Mix；
(3) silver nitrate system and reduction system are heated to into 50 DEG C, with reduction system as parent, in the stirring of 80r/min
Under speed, reacted adding in silver nitrate system 1-2min into reduction system；
(4), after reaction is finished and is aged 5min, argentum powder moves to filter tank and carries out cleaning filtration, cleans to filter liquor electrical conductivity
Till≤20 μ s/cm；Gained argentum powder is moved to into 70 DEG C of drying in baking oven.
The present embodiment is obtained the khaki argentum powder of about 0.63kg, and argentum powder electronic microscope photos obtain the larger flattening granule of particle diameter
(see Fig. 2), between 2.0～4.0 μm, powder tapping density is 4.0-4.5g/ml to particle diameter distribution.
Embodiment 3：
The preparation method of the flattening argentum powder of the present embodiment, step are as follows：
(1) weigh silver nitrate solid 1kg and be placed in mixer, add pure water 3L to be dissolved；Finally plus pure water is dilute by system
Release to 4L, be made into the silver nitrate system of silver nitrate content about 250g/L；
(2) weigh ascorbic acid 0.6kg and add pure water 12L dissolvings, add sodium hydroxide 5g dissolvings；Addition is dissolved in advance
Diisobutyl sodium naphthalene sulfonate 0.3g；Aminated polyethylene glycol oxide 8g；Stir and add pure water that system is diluted to 16L, stir
Mix；
(3) silver nitrate system and reduction system are heated to into 50 DEG C, with reduction system as parent, in the stirring of 80r/min
Under speed, reacted adding in silver nitrate system 1-2min into reduction system；
(4), after reaction is finished and is aged 5min, argentum powder moves to filter tank and carries out cleaning filtration, cleans to filter liquor electrical conductivity
Till≤20 μ s/cm；Gained argentum powder is moved to into 70 DEG C of drying in baking oven.
The present embodiment obtains the silver gray argentum powder of about 0.63kg, and argentum powder electronic microscope photos obtain that particle diameter is larger, thickness is larger
Flattening granule (see Fig. 3), between 3.0～5.0 μm, powder tapping density is 4.0-5.0g/ml to particle diameter distribution.
Embodiment 4：
The preparation method of the flattening argentum powder of the present embodiment, step are as follows：
(1) weigh silver nitrate solid 1kg and be placed in mixer, add pure water 4L to be dissolved；Finally plus pure water is dilute by system
Release to 5L, be made into the silver nitrate system of silver nitrate content about 200g/L；
(2) weigh ascorbic acid 0.6kg and add pure water 18L dissolvings, add ammonia 200ml dissolvings；Addition is dissolved in advance
Diisobutyl sodium naphthalene sulfonate 0.2g；Carboxylated polyethylene glycol oxide 5g；Stir and add pure water that system is diluted to 20L, stir
Mix；
(3) silver nitrate system and reduction system are heated to into 50 DEG C, with reduction system as parent, in the stirring of 80r/min
Under speed, reacted adding in silver nitrate system 1-2min into reduction system；
(4), after reaction is finished and is aged 5min, argentum powder moves to filter tank and carries out cleaning filtration, cleans to filter liquor electrical conductivity
Till≤20 μ s/cm；Gained argentum powder is moved to into 70 DEG C of drying in baking oven.
The present embodiment obtains the canescence argentum powder of about 0.63KG, and it is not high that electronic microscope photos obtain granule spheroid, flattening
Argentum powder (see Fig. 4), between 2.0～4.0 μm, powder tapping density is 5.0-5.5g/ml to particle diameter distribution.
Embodiment 5：
The preparation method of the flattening argentum powder of the present embodiment, step are as follows：
(1) weigh silver nitrate solid 500g to be dissolved in water, be then diluted with water to 5L, stir and be made into silver nitrate content
For the silver nitrate system of 100g/L；
(2) weigh ascorbic acid 275g to be dissolved in water, add sodium hydroxide 100ml, add two isobutyls for having dissolved in advance
Base sodium naphthalene sulfonate 0.05g, adds polyethylene glycol oxide 0.5g, is finally diluted with water to 10L, stirs and be made into reduction system；
(3) two systems are adjusted to 40 DEG C, with reduction system as parent, under the mixing speed of 40r/min, by silver nitrate
System is reacted in being added to reduction system；
(4) argentum powder is cleaned after completion of the reaction, and to cleaning mixture electrical conductivity≤20 μ s/cm, filtration is drained argentum powder and dried.
Embodiment 6：
The preparation method of the flattening argentum powder of the present embodiment, step are as follows：
(1) weigh silver nitrate solid 1.2kg to be dissolved in water, be then diluted with water to 4L, stirring is made into silver nitrate and contains
Measure the silver nitrate system for 300g/L；
(2) weigh ascorbic acid 780g to be dissolved in water, add sodium carbonate 200ml, add the di-2-ethylhexylphosphine oxide for having dissolved in advance
Sodium naphthalene sulfonate 6g, adds aminated polyethylene glycol oxide 24g, is finally diluted with water to 24L, stirs and be made into reduction system；
(3) two systems are adjusted to 80 DEG C, with reduction system as parent, under the mixing speed of 100r/min, by nitric acid
Silver-colored system is reacted in being added to reduction system；
(4) argentum powder is cleaned after completion of the reaction, and to cleaning mixture electrical conductivity≤20 μ s/cm, filtration is drained argentum powder and dried.
Above-mentioned embodiment is the invention is not limited in, if the various changes to the present invention or deformation are without departing from the present invention
Spirit and scope, if these change and deformation belong to the present invention claim and equivalent technologies within the scope of, then this
It is bright to be also intended to comprising these changes and deform.
Claims (10)
1. a kind of preparation method of flattening argentum powder, it is characterised in that step is as follows：
(1) weigh silver nitrate solid to be dissolved in water, then dilute, stir and be made into silver nitrate system；
(2) weigh ascorbic acid to be dissolved in water, addition pH adjusting agent, addition derivant, addition dispersant, last dilute,
Stir and be made into reduction system；
(3) two systems are adjusted to 40～80 DEG C, with reduction system as parent, under the mixing speed of setting, by silver nitrate body
System is reacted in being added to reduction system；
(4) argentum powder is cleaned after completion of the reaction, and to cleaning mixture electrical conductivity≤20 μ s/cm, filtration is drained argentum powder and dried.
2. the preparation method of flattening argentum powder according to claim 1, it is characterised in that step (1) the silver nitrate body
In system, silver nitrate concentration is 100～300g/L.
3. the preparation method of flattening argentum powder according to claim 1, it is characterised in that silver nitrate in the step (1)
The volume of system is 1 ︰, 2～1 ︰ 6 with the volume ratio of reduction system in step (2).
4. the preparation method of flattening argentum powder according to claim 1, it is characterised in that step (2) ascorbic acid
Addition for silver nitrate weight 55%～65%.
5. the preparation method of flattening argentum powder according to claim 1, it is characterised in that pH regulator in the step (2)
Agent is ammonia, sodium hydroxide, one or more in sodium carbonate.
6. the preparation method of flattening argentum powder according to claim 1, it is characterised in that step (2) derivant adds
Enter amount for the 0.01%～0.50% of silver nitrate weight.
7. the preparation method of flattening argentum powder according to claim 1, it is characterised in that derivant in the step (2)
It is sodium methylene bis-naphthalene sulfonate, diisobutyl sodium naphthalene sulfonate, dispersing agent MF, the one kind in sodium lignin sulfonate
Or it is several.
8. the preparation method of flattening argentum powder according to claim 1, it is characterised in that dispersant in the step (2)
Addition for silver nitrate weight 0.10%～2.00%.
9. the preparation method of flattening argentum powder according to claim 1, it is characterised in that dispersant in the step (2)
Be polyethylene glycol oxide, aminated polyethylene glycol oxide, carboxylated polyethylene glycol oxide, ammonium polyacrylate salt, in modified polypropene hydrochlorate
One or more.
10. the preparation method of flattening argentum powder according to claim 1, it is characterised in that stirring speed in the step (3)
Spend for 40～100r/min.
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| CN201611241747.1A CN106583751A (en) | 2016-12-29 | 2016-12-29 | Preparation method of flat silver powder |
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| CN201611241747.1A CN106583751A (en) | 2016-12-29 | 2016-12-29 | Preparation method of flat silver powder |
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Cited By (1)
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| CN110355380A (en) * | 2019-08-13 | 2019-10-22 | 山东建邦胶体材料有限公司 | A kind of preparation method of hexagonal flake micron crystalline substance silver powder |
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