CN110202164A - A kind of nano-silver powder and preparation method thereof for electric source material - Google Patents
A kind of nano-silver powder and preparation method thereof for electric source material Download PDFInfo
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- CN110202164A CN110202164A CN201910493627.8A CN201910493627A CN110202164A CN 110202164 A CN110202164 A CN 110202164A CN 201910493627 A CN201910493627 A CN 201910493627A CN 110202164 A CN110202164 A CN 110202164A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- 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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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The nano-silver powder and preparation method thereof that the invention discloses a kind of for electric source material, this method includes: step 1, selecting and weighs each raw material;Step 2, gum arabic powder and sodium ascorbate are added to the water, stirring and dissolving, adjust pH value;Step 3, silver nitrate is added to the water, stirring and dissolving, adjusts pH value;Step 4, sodium ascorbate and oleic acid are added to the water, stirring and dissolving;Step 5, silver nitrate solution is added in reducing solution, while compounding agent solution is added, reacted, stir and keep the temperature;Step 6, cooling after the formation of nano-silver powder particle, centrifugation is separated by solid-liquid separation, then is cleaned with pure water, is then cleaned with ethyl alcohol, is finally filtered, is dried, re-dry.Present invention provides the nano-silver powders of this method preparation.The present invention is used to prepare the nano-silver powder that partial size is less than or equal to 50 rans, and crystallinity is high, good dispersion, and pattern uniform particle diameter is high, and preparation method is simple, low in cost, and yield is high.
Description
Technical field
The present invention relates to silver powder of a kind of Material Field and preparation method thereof, and in particular, to one kind is used for electric light source material
Nano-silver powder of material and preparation method thereof.
Background technique
With the development of science and technology with the application of electronic product, the quality of electricity generating layer, electrode etc. determines electricity in electronic instrument
The service life of sub- instrument.Yin Yin has good natural high conductivity, sterilising, thermal conductivity and oxidation resistance wide by force
It is general to be used for the numerous areas such as electronics industry, sewage treatment, construction material.Using silver powder mainly by by silver powder in electronics industry
Manufactured silver paste agent is coated or printed on various substrates, is then heating and curing or is heated roasting, forms conductive film, thus
Form access.Conductive silver powder be production electric slurry, conductive silver paste, LED epoxy conducting, electromagnetic screen coating, conductive coating,
The primary raw material of electrically conductive ink, conductive rubber, conductive plastics, conductivity ceramics etc..Therefore, the consumption of silver powder is huge, Er Qieru
The quality requirement of fruit silver powder is not up to standard, the product being made into will performance be not sufficiently stable and easy to fall off, so needing to silver powder
It can be carried out improvement.
It is needed to select different silver powder products according to use condition, super fine silver powder is mainly used for medium and high temperature conductor paste and electricity
Pole slurry, silver conductive paste are then widely used in capacitor, resistor, potentiometer, thick film mixing concentration circuit, sensing element
With the electronics industry every field such as surface installation technique.
Nano-silver powder in super fine silver powder includes Nanometer silver flakes and 2 kinds of Nanometer spherical silver powders.In the electronics industry, it uses
The micro-silver powder that uses currently on the market of nano-silver powder substitution has the advantage that in the electric slurry that (1) is produced with nano-silver powder
The granularity of metal particle is smaller, in the silk screen for carrying out the bigger mesh number of silk-screen printing Shi Keyong, so that it is better to obtain compactness extent
Surface covering, and work efficiency is high for silk screen operation.(2) silver-colored dosage can be reduced, production cost is reduced.According to Bremen, Germany
The research achievement of Applied Physics research institute, with nano-silver powder replace micro-silver powder made of conducting resinl, can be with welding metal and pottery
Porcelain, coating are not required to too thick, and coating surface is smooth, can save 50% silver medal dosage.(3) since the fusing point of nano-silver powder is usual
Lower than coarse grain object, therefore the electrocondution slurry made of nano-silver powder, sintering temperature are generally below common slurry, this is just reduced
Requirement to substrate material high temperature resistance, it might even be possible to use plastics etc. as substrate material.Therefore the preparation of nano-silver powder
It is just particularly important with research.
Summary of the invention
The object of the present invention is to provide a kind of silver powder and preparation method thereof, are used to prepare partial size less than or equal to 50 nanometers of left sides
Right nano-silver powder, the silver powder crystallinity is high, and good dispersion, pattern uniform particle diameter is high, and performance is stablized, good quality, and makes
Preparation Method is simple, low in cost, and yield is high.
In order to achieve the above object, the present invention provides a kind of preparation method of nano-silver powder for electric source material,
Wherein, the method includes: step 1, selecting and weighs each raw material;Step 2, reducing solution is prepared: in water bath with thermostatic control condition
Under, gum arabic powder and sodium ascorbate are added to the water, stirring and dissolving, and adjust solution ph;Step 3, nitric acid is prepared
Silver-colored solution: silver nitrate is added to the water, stirring and dissolving, and adjusts solution ph;Step 4, prepare auxiliary agent: by sodium ascorbate and
Oleic acid is added to the water, spare after stirring and dissolving;Step 5, the resulting reduction of step 2 is added in the resulting silver nitrate solution of step 3
In solution, while entering the resulting compounding agent solution of step 4, is reacted, stir and keep the temperature in reaction process;Step 6, in nano silver
After powder particles are formed, is cooled down, be then centrifuged for being separated by solid-liquid separation, then cleaned with pure water, then be cleaned with ethyl alcohol, finally
Moisture is leached out, carries out drying and processing, then be dried.
The preparation method of the above-mentioned nano-silver powder for electric source material, wherein in the step 2, by weight
Number meter is placed in 800~1200 parts of addition beakers of pure water in the constant water bath box with circulating-heating function, set temperature 25
DEG C, after temperature reaches setting value, 60~65 parts of gum arabic powder and 30~50 parts of ascorbic acid are added into beaker
Sodium adjusts pH value after stirring and dissolving again.
The preparation method of the above-mentioned nano-silver powder for electric source material, wherein in the step 2, by 1000ml
Pure water is added in the beaker of 5L, is placed in the constant water bath box with circulating-heating function, 25 DEG C of set temperature, reaches to temperature
After setting value, gum arabic powder 62.5g and sodium ascorbate 40g is added into beaker and is stirred, dissolves it sufficiently, then
Adjusting pH value is 3.5~4, spare.
The preparation method of the above-mentioned nano-silver powder for electric source material, wherein in the step 3, by weight
Number meter adds in 800~1200 parts of addition beakers of pure water 250~350 parts of silver nitrate, is stirred dissolution, then adjust pH
Value.
The preparation method of the above-mentioned nano-silver powder for electric source material, wherein in the step 3, by 1000ml
Pure water is added in the beaker of 5L, adds silver nitrate 300g and is stirred dissolution, and then adjusting pH value is 3.5~4, spare.
The preparation method of the above-mentioned nano-silver powder for electric source material, wherein in the step 4, by weight
200~300 parts of pure water are added in beaker number meter, add 15~25 parts of sodium ascorbate, 3~6 parts of oleic acid, are stirred molten
It is spare after solution.
The preparation method of the above-mentioned nano-silver powder for electric source material, wherein in the step 4,250ml is pure
Water is added in 2L beaker, adds sodium ascorbate 20g, oleic acid 5g, is stirred spare after dissolving.
The preparation method of the above-mentioned nano-silver powder for electric source material, wherein in the step 5, use peristaltic pump
Silver nitrate solution is added in reducing solution with the speed of 30ml/min, while compounding agent solution is added with the speed of 5ml/min, into
Row reaction, adition process are 50~60min, and being kept stirring in this process and keeping temperature is 25 DEG C.
The preparation method of the above-mentioned nano-silver powder for electric source material, wherein in the step 6, in nano silver
It is cooling after powder particles are formed, it is then separated by solid-liquid separation with centrifuge, and cleaned 3 times or more with pure water, until conductivity is small
It is cleaned until being equal to 50, then with ethyl alcohol, removes extra moisture, be put into after suction filtration in baking pan and carry out drying and processing, drying temperature
Degree is 45 DEG C, then is dried with low-temperature vacuum drying case, until moisture content is less than or equal to 0.2%.
The present invention also provides a kind of nano-silver powders of above-mentioned method preparation, wherein the nano-silver powder is for electricity
The preparation of source material.
It is had the advantage that provided by the present invention for the nano-silver powder and preparation method thereof of electric source material
The present invention is used to prepare the nano-silver powder that partial size is less than or equal to 50 rans.Exist in gum arabic powder
Under, with hydrogen peroxide and ascorbic acid sodium reduction AgNO3, nano-silver powder is made.The Component Source for preparing silver powder is extensive, reduces life
Cost is produced, gained silver powder crystallinity is high, and pattern uniform particle diameter is high, good dispersion smaller than existing silver powder, and performance is stablized, quality
It is excellent, and preparation method is simple, low in cost, yield is high.
Detailed description of the invention
Fig. 1 is 80000 times of scanning transmission electron microscope (STEM) figures of present invention gained silver powder.
Fig. 2 is 160000 times of scanning transmission electron microscope (STEM) figures of present invention gained silver powder.
Specific embodiment
A specific embodiment of the invention is further described below in conjunction with attached drawing.
Provided by the present invention for the preparation method of the nano-silver powder of electric source material, it includes: step 1, selects and claim
Take each raw material;Step 2, it prepares reducing solution: under the conditions of water bath with thermostatic control, water is added in gum arabic powder and sodium ascorbate
In, stirring and dissolving, and adjust solution ph;Step 3, it prepares silver nitrate solution: silver nitrate is added to the water, stirring and dissolving, and
Adjust solution ph;Step 4, it prepares auxiliary agent: sodium ascorbate and oleic acid is added to the water, it is spare after stirring and dissolving;Step 5,
The resulting silver nitrate solution of step 3 is added in the resulting reducing solution of step 2, while entering the resulting compounding agent solution of step 4, into
Row reacts, and stirs and keeps the temperature in reaction process;Step 6, nano-silver powder particle formation after, cooled down, be then centrifuged for into
Row is separated by solid-liquid separation, then is cleaned with pure water, is then cleaned with ethyl alcohol, and moisture is finally leached out, and carries out drying and processing, then done
It is dry.
In step 2, according to parts by weight by 800~1200 parts of addition beakers of pure water, it is placed in circulating-heating function
Constant water bath box in, 25 DEG C of set temperature, after temperature reaches setting value, 60~65 parts of Arabic tree is added into beaker
Rubber powder and 30~50 parts of sodium ascorbate adjust pH value after stirring and dissolving again.
Gum arabic powder (Arabic gum) is a kind of chemicals, is in fine particle, sheet or powdered, can be dissolved in
Water, colorless and odorless, aqueous solution toughness, micro- muddiness do not dissolve in alcohol under room temperature.It can be used as preventing protecting colloid, the biochemistry of precipitating
Reagent, colloid stabilizer, emulsifier, adhesive etc..EINECS (the European Inventory of of gum arabic powder
Existing commercial Chemical Substances, the existing commercial chemicals catalogue in Europe) number: 232-519-5.
Sodium ascorbate (L-Ascorbic Acid Sodium Salt, alias: vitamine C sodium) is white to micro- yellowish-white
Color crystalline powder or particle, odorless, taste is slightly salty.It is 218 DEG C of decomposition temperature, more stable under drying regime, light then color burn is met,
After the moisture absorption and in aqueous solution slow oxygenolysis, it is more soluble easily in water than ascorbic acid.
Preferably, 1000ml pure water is added in the beaker of 5L, is placed in the constant water bath box with circulating-heating function,
25 DEG C of set temperature, after temperature reaches setting value, gum arabic powder 62.5g and sodium ascorbate 40g is added into beaker
It is stirred, dissolves it sufficiently, then adjusting pH value is 3.5~4, it is spare.Solution ph is adjusted using nitric acid.
Silver nitrate 250~350 is added by 800~1200 parts of addition beakers of pure water according to parts by weight in step 3
Part, it is stirred dissolution, then adjust pH value.
Preferably, in step 3 will 1000ml pure water be added 5L beaker in, add silver nitrate 300g be stirred it is molten
Solution, then adjusting pH value is 3.5~4, spare.Solution ph is adjusted using nitric acid.
200~300 parts of pure water are added in beaker according to parts by weight in step 4, add sodium ascorbate 15~25
Part, 3~6 parts of oleic acid are stirred spare after dissolving.
Preferably, 250ml pure water is added in 2L beaker in step 4, adds sodium ascorbate 20g, oleic acid 5g, carried out
It is spare after stirring and dissolving.
Silver nitrate solution is added in reducing solution with the speed of 30ml/min with peristaltic pump in step 5, while with 5ml/
Compounding agent solution is added in the speed of min, is reacted, and adition process is 50~60min, is kept stirring in this process and keeps temperature
Degree is 25 DEG C.
In step 6 after the formation of nano-silver powder particle, cooling reaction is carried out at room temperature, is then consolidated with centrifuge
Liquid separation, and cleaned 3 times or more with pure water, it is cleaned until conductivity is less than or equal to 50, then with ethyl alcohol, removes extra water
Point, it is put into after suction filtration in baking pan and carries out drying and processing, drying temperature is 45 DEG C, then is dried with low-temperature vacuum drying case, directly
Until moisture content is less than or equal to 0.2%.
The present invention also provides the nano-silver powder of this method preparation, which is used for the preparation of electric source material.
The nano-silver powder and preparation method thereof provided by the present invention for electric source material is done more below with reference to embodiment
It further describes.
Embodiment 1
A kind of preparation method of the nano-silver powder for electric source material, it includes:
Step 1, it selects and weighs each raw material.
Step 2, it prepares reducing solution: 1000ml pure water being added in the beaker of 5L, be placed in circulating-heating function
In constant water bath box, 25 DEG C of set temperature, after temperature reach setting value after, into beaker be added gum arabic powder 62.5g and
Sodium ascorbate 40g is stirred, and dissolves it sufficiently, then nitric acid is used to adjust solution ph as 3.5~4, spare.
Step 3, it prepares silver nitrate solution: 1000ml pure water being added in the beaker of 5L, add silver nitrate 300g progress
Then stirring and dissolving uses nitric acid to adjust solution ph as 3.5~4, spare.
Step 4, it prepares auxiliary agent: 250ml pure water being added in 2L beaker, sodium ascorbate 20g, oleic acid 5g are added, into
It is spare after row stirring and dissolving.
Step 5, with the speed of 30ml/min that the resulting silver nitrate solution addition step 2 of step 3 is resulting with peristaltic pump
In reducing solution, while compounding agent solution is added with the speed of 5ml/min, is reacted, adition process is 50~60min, at this
Being kept stirring in the process and keeping temperature is 25 DEG C.
Step 6, after the formation of nano-silver powder particle, cooling reaction is carried out at room temperature, is then consolidated with centrifuge
Liquid separation, and cleaned 3 times or more with pure water, it is cleaned until conductivity is less than or equal to 50, then with ethyl alcohol, removes extra water
Point, it is put into after suction filtration in baking pan and carries out drying and processing, drying temperature is 45 DEG C, then is dried with low-temperature vacuum drying case, directly
Until moisture content is less than or equal to 0.2%.
The present embodiment also provides the nano-silver powder of this method preparation, which is used for the preparation of electric source material.
Embodiment 2
A kind of preparation method of the nano-silver powder for electric source material, it includes:
Step 1, it selects and weighs each raw material.
Step 2, it prepares reducing solution: 800ml pure water being added in the beaker of 5L, be placed in the perseverance with circulating-heating function
In warm water bath cabinet, 25 DEG C of set temperature, after temperature reaches setting value, gum arabic powder 60g and anti-bad is added into beaker
Hematic acid sodium 30g is stirred, and dissolves it sufficiently, then nitric acid is used to adjust solution ph as 3.5~4, spare.
Step 3, it prepares silver nitrate solution: 800ml pure water being added in the beaker of 5L, add silver nitrate 250g and stirred
Dissolution is mixed, nitric acid is then used to adjust solution ph as 3.5~4, it is spare.
Step 4, it prepares auxiliary agent: 200ml pure water being added in 2L beaker, sodium ascorbate 15g, oleic acid 3g are added, into
It is spare after row stirring and dissolving.
Step 5, with the speed of 30ml/min that the resulting silver nitrate solution addition step 2 of step 3 is resulting with peristaltic pump
In reducing solution, while compounding agent solution is added with the speed of 5ml/min, is reacted, adition process is 50~60min, at this
Being kept stirring in the process and keeping temperature is 25 DEG C.
Step 6, after the formation of nano-silver powder particle, cooling reaction is carried out at room temperature, is then consolidated with centrifuge
Liquid separation, and cleaned 3 times or more with pure water, it is cleaned until conductivity is less than or equal to 50, then with ethyl alcohol, removes extra water
Point, it is put into after suction filtration in baking pan and carries out drying and processing, drying temperature is 45 DEG C, then is dried with low-temperature vacuum drying case, directly
Until moisture content is less than or equal to 0.2%.
The present embodiment also provides the nano-silver powder of this method preparation, which is used for the preparation of electric source material.
Embodiment 3
A kind of preparation method of the nano-silver powder for electric source material, it includes:
Step 1, it selects and weighs each raw material.
Step 2, it prepares reducing solution: 1200ml pure water being added in the beaker of 5L, be placed in circulating-heating function
In constant water bath box, 25 DEG C of set temperature, after temperature reaches setting value, gum arabic powder 65g is added into beaker and resists
Bad hematic acid sodium 50g is stirred, and dissolves it sufficiently, then nitric acid is used to adjust solution ph as 3.5~4, spare.
Step 3, it prepares silver nitrate solution: 1200ml pure water being added in the beaker of 5L, add silver nitrate 350g progress
Then stirring and dissolving uses nitric acid to adjust solution ph as 3.5~4, spare.
Step 4, it prepares auxiliary agent: 300ml pure water being added in 2L beaker, sodium ascorbate 25g, oleic acid 6g are added, into
It is spare after row stirring and dissolving.
Step 5, with the speed of 30ml/min that the resulting silver nitrate solution addition step 2 of step 3 is resulting with peristaltic pump
In reducing solution, while compounding agent solution is added with the speed of 5ml/min, is reacted, adition process is 50~60min, at this
Being kept stirring in the process and keeping temperature is 25 DEG C.
Step 6, after the formation of nano-silver powder particle, cooling reaction is carried out at room temperature, is then consolidated with centrifuge
Liquid separation, and cleaned 3 times or more with pure water, it is cleaned until conductivity is less than or equal to 50, then with ethyl alcohol, removes extra water
Point, it is put into after suction filtration in baking pan and carries out drying and processing, drying temperature is 45 DEG C, then is dried with low-temperature vacuum drying case, directly
Until moisture content is less than or equal to 0.2%.
The present embodiment also provides the nano-silver powder of this method preparation, which is used for the preparation of electric source material.
The nano-silver powder of preparation of the embodiment of the present invention is referring to figure 1 and figure 2.
Provided by the present invention for the nano-silver powder and preparation method thereof of electric source material, be synthesis reduction process in,
In the presence of gum arabic powder, with hydrogen peroxide and ascorbic acid sodium reduction AgNO3, nano-silver powder is made.The silver powder of preparation
Component Source is extensive, reduces the cost produced, and gained silver powder crystallinity is high, and pattern uniform particle diameter is high, than existing silver
The small good dispersion of powder, performance is stablized, and preparation method is simple, low in cost, and yield is high.
It is discussed in detail although the contents of the present invention have passed through above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. a kind of preparation method of the nano-silver powder for electric source material, which is characterized in that the method includes:
Step 1, it selects and weighs each raw material;
Step 2, it prepares reducing solution: under the conditions of water bath with thermostatic control, gum arabic powder and sodium ascorbate being added to the water, stirred
Dissolution is mixed, and adjusts solution ph;
Step 3, it prepares silver nitrate solution: silver nitrate is added to the water, stirring and dissolving, and adjust solution ph;
Step 4, it prepares auxiliary agent: sodium ascorbate and oleic acid is added to the water, it is spare after stirring and dissolving;
Step 5, the resulting silver nitrate solution of step 3 is added in the resulting reducing solution of step 2, while it is resulting to enter step 4
Compounding agent solution is reacted, and is stirred and is kept the temperature in reaction process;
Step 6, it after the formation of nano-silver powder particle, is cooled down, is then centrifuged for being separated by solid-liquid separation, then cleaned with pure water,
Then it is cleaned with ethyl alcohol, finally leaches out moisture, carry out drying and processing, then be dried.
2. the preparation method for the nano-silver powder of electric source material as described in claim 1, which is characterized in that the step
In rapid 2, according to parts by weight by 800~1200 parts of addition beakers of pure water, it is placed in the water bath with thermostatic control with circulating-heating function
In case, 25 DEG C of set temperature, after temperature reach setting value after, into beaker be added 60~65 parts gum arabic powder and 30~
50 parts of sodium ascorbate adjusts pH value after stirring and dissolving again.
3. the preparation method for the nano-silver powder of electric source material as claimed in claim 2, which is characterized in that the step
In rapid 2,1000ml pure water is added in the beaker of 5L, is placed in the constant water bath box with circulating-heating function, set temperature
25 DEG C, after temperature reaches setting value, gum arabic powder 62.5g and sodium ascorbate 40g is added into beaker and is stirred,
Dissolve it sufficiently, then adjusting pH value is 3.5~4, it is spare.
4. the preparation method for the nano-silver powder of electric source material as described in claim 1, which is characterized in that the step
In rapid 3, according to parts by weight by 800~1200 parts of addition beakers of pure water, 250~350 parts of silver nitrate is added, is stirred
Dissolution, then adjust pH value.
5. the preparation method for the nano-silver powder of electric source material as claimed in claim 4, which is characterized in that the step
In rapid 3,1000ml pure water is added in the beaker of 5L, adds silver nitrate 300g and be stirred dissolution, then adjusting pH value is
3.5~4, it is spare.
6. the preparation method for the nano-silver powder of electric source material as described in claim 1, which is characterized in that the step
In rapid 4,200~300 parts of pure water are added in beakers according to parts by weight, add 15~25 parts of sodium ascorbate, oleic acid 3~
It 6 parts, is stirred spare after dissolving.
7. the preparation method for the nano-silver powder of electric source material as claimed in claim 6, which is characterized in that the step
In rapid 4,250ml pure water is added in 2L beaker, sodium ascorbate 20g, oleic acid 5g are added, is stirred spare after dissolving.
8. the preparation method for the nano-silver powder of electric source material as described in claim 1, which is characterized in that the step
In rapid 5, silver nitrate solution is added in reducing solution with the speed of 30ml/min with peristaltic pump, while with the speed of 5ml/min
Compounding agent solution is added, is reacted, adition process is 50~60min, and being kept stirring in this process and keeping temperature is 25 DEG C.
9. the preparation method for the nano-silver powder of electric source material as described in claim 1, which is characterized in that the step
It is cooling after the formation of nano-silver powder particle in rapid 6, be then separated by solid-liquid separation with centrifuge, and with pure water clean 3 times with
On, it is cleaned until conductivity is less than or equal to 50, then with ethyl alcohol, removes extra moisture, be put into baking pan and carry out after suction filtration
Drying and processing, drying temperature is 45 DEG C, then is dried with low-temperature vacuum drying case, until moisture content is less than or equal to 0.2%
Until.
10. a kind of nano-silver powder of the method preparation as described in any one of claim 1~9, which is characterized in that described
Nano-silver powder is used for the preparation of electric source material.
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