CN103537708B - A kind of solar cell conductive silver slurry ultrapure argentum powder and preparation method thereof - Google Patents
A kind of solar cell conductive silver slurry ultrapure argentum powder and preparation method thereof Download PDFInfo
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- CN103537708B CN103537708B CN201310408019.5A CN201310408019A CN103537708B CN 103537708 B CN103537708 B CN 103537708B CN 201310408019 A CN201310408019 A CN 201310408019A CN 103537708 B CN103537708 B CN 103537708B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000000843 powder Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 30
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 15
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 15
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 15
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 13
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000013019 agitation Methods 0.000 claims abstract description 7
- 238000006722 reduction reaction Methods 0.000 claims abstract description 7
- 230000005611 electricity Effects 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 42
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 24
- 229910021529 ammonia Inorganic materials 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000004568 cement Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- 230000006641 stabilisation Effects 0.000 claims description 6
- 238000011105 stabilization Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920000136 polysorbate Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 13
- 239000006185 dispersion Substances 0.000 abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 230000033228 biological regulation Effects 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- -1 pattern Substances 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
The present invention relates to a kind of solar cell conductive silver slurry ultrapure argentum powder and preparation method thereof, the step of preparation method is: configuration silver nitrate and the mixed reaction solution A and ascorbic acid mixing reducing solution B of dispersant；Thermostat water bath preheated solution A and B, under magnetic agitation, mixing carries out reduction reaction；Obtain post-treated for gained argentum powder and plasma process meeting the ultrapure argentum powder that solar cell conductive silver slurry requires.The application of plasma technology of the present invention makes the argentum powder purity prepared higher, reaches >=99.99%, is more beneficial for argentum powder and the Ohmic contact of silicon chip, formation dense film during silver slurry sintering；On the premise of improving purity, do not change the characteristic of argentum powder so that it is 0.1 5 μm, narrow particle size distribution, good dispersion, tap density >=4.5g/cm that the argentum powder of preparation has mean diameter3, be conducive to improving the electricity conversion of solaode；Plasma post process is easy, beneficially large-scale production.
Description
Technical field
The present invention relates to a kind of ultrapure argentum powder and preparation method thereof, particularly relate to a kind of solar cell conductive
Silver slurry, with ultrapure argentum powder and preparation method thereof, belongs to technical field of electronic materials.
Background technology
Along with exhaustion and the deterioration of environment of global resources, following solar energy power technology and industry have very
Strong competitiveness.Under the promotion of international photovoltaic market great potential, the solaode manufacturing industry of various countries
Falling over each other to put into huge fund, expanding production, to strive one seat, China has become the maximum of silicon solar cell
Produce and exported country.
Argentum powder has become the important material of Electrical and Electronic industry due to excellent electric conductivity and application performance
Material, is most widely used a kind of noble metal powder in electronics industry, for thick film, resistance, pottery, Jie
The basic function material of the electric slurries such as matter.And the conducting function that argentum powder is starched as solar cell conductive silver
Phase, pattern, particle diameter, dispersibility, tap density and purity all determine the electrical property of slurry, and affect
The machinery of sintered membrane and physical property, and then affect the electricity conversion of solaode.
The preparation method of argentum powder is varied, through the exploration discovery to prior art, current preparation side
Method mainly based on chemical liquid phase reducing process, it be the most frequently used be also most important method, because of technique stream
Journey is simple and feasible, cost is relatively low, production scale is big, has obtained commonly used in electronics industry.But
It is as the reduction of Argent grain size, electrostatic attraction between granule, Van der Waals force, capillary force etc.
More weak interaction force increasingly highlights.In liquid phase reduction preparation process, the silver particles restored
Easily produce reunion, form bulky grain.At present, almost all of liquid phase reduction when preparing argentum powder,
Enough dispersants will be added to prevent the reunion between Argent grain, used for solar batteries to reach to prepare
The requirement of the particle diameter of argentum powder, pattern and dispersibility.Dispersant is divided into three processes to the dispersion of argentum powder: silver
Reassembling of the moistening of powder, the dispersion of silver particles group and prevention argentum powder.Finally, dispersant adsorption is at silver
Powder surface, prevents reassembling of argentum powder, and the dispersant added reduces the boundary of solid-liquid interface
Surface tension, therefore adds the thermodynamic stability of dispersion, and argentum powder is not susceptible to reunite.But this
Also the purification for argentum powder has buried hidden danger, and the amount of dispersant is crossed and is not enough to be coated with completely argentum powder at least, rises not
To scattered effect, cross and bring difficulty to washing at most.The argentum powder higher in order to obtain purity, major part
Way is argentum powder to carry out a large amount of washing the most repeatedly and alcohol is washed, and not only causes waste, and can not get purity
Higher argentum powder；Prepared by chemical reduction method disclosed in the Chinese patent of Application No. 200910218356.1
In the method for spherical super fine silver powder, the argentum powder higher in order to obtain purity, use 350 DEG C of heat preservation hot to process
Method remove impurity, although obtained purer argentum powder, but argentum powder be easily in high-temperature calcination process
Reunite, it can be seen that, the removal of dispersant is to prepare in polymolecularity and highly purified argentum powder preparation process
The technical problem faced.Solar energy disclosed in the Chinese patent of Application No. 200610027065.0
In battery electrode printing slurry in the preparation method of argentum powder, the protective agent added during preparing due to this method
Too much, the covering causing argentum powder surface is more, affect the conductive effect of electrode, and prepares by this method
Argentum powder can pollute silicon chip, and when the silver of configuration starches high temperature sintering, shrinkage factor is big, it is impossible to real with semiconductor substrate
Now preferable Ohmic contact, reduces the electricity conversion of solaode.
Summary of the invention
The technical problem to be solved is to provide a kind of preparation process simplicity, epigranular, high score
Dissipate property, the preparation method of the ultrapure argentum powder of highly purified applicable silver paste of solar cells and the silver prepared thereof
Powder, overcomes above-mentioned the deficiencies in the prior art, is simultaneously adapted to large-scale production.
The technical scheme is that a kind of solar cell conductive silver slurry is used
The preparation method of ultrapure argentum powder, comprises the following steps:
(1) configuration of mixed reaction solution A: be dissolved in pure water by silver nitrate, makes the dense of silver nitrate
Degree is 0.2～1.2mol/L, and the pH value adding ammonia or nitric acid adjustment solution is 4～10, adds simultaneously
Enter dispersant, obtain mixed reaction solution A；
(2) configuration of reducing solution B is mixed: by dissolution of ascorbic acid in pure water, make ascorbic acid
Concentration 0.8～4.8mol/L, adds ammonia or the pH value of nitric acid adjustment solution and mixed reaction solution A
Identical, obtain mixing reducing solution B；
(3) with thermostat water bath preheating described mixed reaction solution A and described mixing reducing solution B extremely
20～80 DEG C；
(4) by mixing reducing solution B described in thermostat water bath magnetic agitation, the rotating speed of stirring be 500～
2000r/min, after stabilization of speed, adds described mixed reaction solution A with the rate of addition of 1-8ml/s
Carry out reduction reaction；
(5), after dropping, continue stirring 10～60min, obtain the mixed solution containing argentum powder, then
Carry out sucking filtration, washing, alcohol are washed, are dried, are sieved and after Cement Composite Treated by Plasma, obtain solaode and lead
Ultrapure argentum powder used by electricity silver slurry.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in described step (1), silver nitrate used by preparation solution is analytical reagent, prepares molten
Pure electrical conductivity of water used by liquid is 0.05～5 μ S/cm.
Further, in described step (1) dispersant be polyvinyl alcohol, gelatin, tween, Polyethylene Glycol,
The mixing of one or more in polyvinylpyrrolidone, mentioned reagent is analytical reagent, described dispersion
Amount is silver nitrate quality 4%～the 12% of agent addition.
Further, in described step (2), ascorbic acid used by preparation solution is analytical reagent, preparation
Pure electrical conductivity of water used by solution is 0.05～5 μ S/cm.
Further, in described step (3), mixed reaction solution A and mixing reducing solution B is preheated to same
One temperature.
Further, the mixed reaction solution A added in described step (4) mixes reducing solution B with described
Volume ratio be 1:1.
Further, sucking filtration in described step (5), wash, be dried, sieve and Cement Composite Treated by Plasma
Detailed process is: argentum powder is after sucking filtration, and first pure water twice, then washing with alcohol twice, in 60～100 DEG C
Vacuum drying oven is dried 3～12h, after crossing 250 mesh sieves, locates under plasma room temperature 80～150W
Reason 30～60min.
Further, described Cement Composite Treated by Plasma atmosphere is that one or more in hydrogen, argon, helium are mixed
Close.
Another technical scheme that the present invention solves above-mentioned technical problem is as follows: a kind of method system prepared as above
For the solar cell conductive silver ultrapure argentum powder of slurry gone out, ultrapure silver used by described solar cell conductive silver slurry
The specification of powder is: high dispersive, uniform particle diameter, mean diameter 0.1-5 μm, narrow particle size distribution, vibration density
Degree is >=4.5g/cm3, purity >=99.99%.
Compared with prior art, advantage is the present invention:
1. the application of plasma technique makes the argentum powder purity of preparation higher, reaches >=99.99%, more
When being conducive to silver slurry to sinter, argentum powder and the Ohmic contact of silicon chip, form dense film；
2. plasma post process is easy, reduces the use of a large amount of pure water and ethanol, is conducive to big
Large-scale production；
3., on the premise of improving purity, do not change the characteristic of argentum powder so that the argentum powder of preparation has flat
All particle diameters are 0.1-5 μm, narrow particle size distribution, good dispersion, tap density >=4.5g/cm3, be conducive to
Improve the electricity conversion of solaode.
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, and
Non-for limiting the scope of the present invention.
Embodiment 1
1. weighing 102g silver nitrate to be dissolved in 300ml pure water, ammonia regulation pH is 10, weighs 4.08g and gathers
Vinyl alcohol is dissolved in 500ml pure water, and after mix homogeneously, constant volume becomes the mixed reaction solution A of 1000ml；
2. weighing 250g dissolution of ascorbic acid in 300ml pure water, ammonia regulation pH is 10, and constant volume becomes
The ascorbic acid of 1000ml-ammonia mixing reducing solution B；
3. with thermostat water bath heating mixed reaction solution A and mixing reducing solution B to design temperature 50 DEG C；
4. stirring mixing reducing solution B under thermostat water bath magnetic agitation, the rotating speed of stirring is
1000r/min, after stabilization of speed, adds mixed reaction solution A with the rate of addition of 5ml/s；
5. after dropping, continue stirring 10min, gained argentum powder sucking filtration, washing twice, ethanol are washed
Twice, 80 DEG C are dried 3 hours, cross 250 mesh sieves, and hydrogen gas plasma 80W room temperature processes 30min,
Mean diameter be 1.3 μm, particle size range be 0.5～2.5 μm, tap density be 4.5g/cm3, pure
The dispersing ball argentum powder of degree >=99.99%.
Embodiment 2
1. weighing 51g silver nitrate to be dissolved in 300ml pure water, ammonia regulation pH is 7, weighs the poly-second of 4.08g
Enol is dissolved in 500ml pure water, and after mix homogeneously, constant volume becomes the mixed solution A of 1000ml；
2. weighing 211g dissolution of ascorbic acid in 300ml pure water, ammonia regulation pH is 7, and constant volume becomes
The ascorbic acid of 1000ml-ammonia mixed solution B；
3. mixed solution A and B are heated to design temperature 50 DEG C with thermostat water bath；
4. stirring mixed solution B under thermostat water bath magnetic agitation, the rotating speed of stirring is 2000r/min, treats
After stabilization of speed, add mixed liquor A with the rate of addition of 5ml/s；
5. after dropping, continue stirring 30min, gained argentum powder sucking filtration, washing twice, ethanol are washed
Twice, 60 DEG C are dried 3 hours, cross 250 mesh sieves, and helium gas plasma 100W room temperature processes 30min,
Mean diameter be 1.0 μm, particle size range be 0.6～1.2 μm, tap density be 5.5g/cm3, pure
The high dispersive ball shape silver powder of degree >=99.99%.
Embodiment 3
1. weighing 51g silver nitrate to be dissolved in 300ml pure water, ammonia regulation pH is 5, weighs 8.16g gelatin
Being dissolved in 500ml pure water, after mix homogeneously, constant volume becomes the mixed solution A of 1000ml；
2. weighing 300g dissolution of ascorbic acid in 300ml pure water, ammonia regulation pH is 5, and constant volume becomes
The ascorbic acid of 1000ml-ammonia mixed solution B；
3. mixed solution A and B are heated to design temperature 30 DEG C with thermostat water bath；
4. stirring mixed solution B under thermostat water bath magnetic agitation, the rotating speed of stirring is 1500r/min, treats
After stabilization of speed, add mixed liquor A with the rate of addition of 1ml/s；
5. after dropping, continue stirring 30min, gained argentum powder sucking filtration, washing twice, ethanol are washed
Twice, 60 DEG C are dried 3 hours, cross 250 mesh sieves, and argon plasma 150W room temperature processes 30min,
Mean diameter be 1.0 μm, particle size range be 0.3～3 μm, tap density be 4.8g/cm3, purity >=
The high dispersive ball shape silver powder of 99.99%.
Embodiment 4
1. weighing 51g silver nitrate to be dissolved in 300ml pure water, ammonia regulation pH is 7, weighs the poly-second of 4.08g
Alkene pyrrolidone is dissolved in 500ml pure water, and after mix homogeneously, constant volume becomes the mixed solution A of 1000ml；
2. weighing 211g dissolution of ascorbic acid in 300ml pure water, ammonia regulation pH is 7, and constant volume becomes
The ascorbic acid of 1000ml-ammonia mixed solution B；
3. mixed solution A and B are heated to design temperature 70 DEG C with thermostat water bath；
4. stirring mixed solution B under thermostat water bath magnetic agitation, the rotating speed of stirring is 500r/min, treats
After stabilization of speed, add mixed liquor A with the rate of addition of 5ml/s；
5. after dropping, continue stirring 10min, gained argentum powder sucking filtration, washing twice, ethanol are washed
Twice, 60 DEG C are dried 3 hours, cross 250 mesh sieves, and helium gas plasma 100W room temperature processes 30min,
Mean diameter be 1.1 μm, particle size range be 0.5～3 μm, tap density be 5.0g/cm3, purity
The high dispersive ball shape silver powder of >=99.99%.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in the present invention
Spirit and principle within, any modification, equivalent substitution and improvement etc. made, should be included in this
Within bright protection domain.
Claims (8)
1. the solar cell conductive silver slurry preparation method of ultrapure argentum powder, it is characterised in that bag
Include following steps:
(1) configuration of mixed reaction solution A: be dissolved in pure water by silver nitrate, makes the dense of silver nitrate
Degree is 0.2～1.2mol/L, and the pH value adding ammonia or nitric acid adjustment solution is 4～10, adds simultaneously
Enter dispersant, obtain mixed reaction solution A；
(2) configuration of reducing solution B is mixed: by dissolution of ascorbic acid in pure water, make ascorbic acid
Concentration 0.8～4.8mol/L, adds ammonia or the pH value of nitric acid adjustment solution and mixed reaction solution A
Identical, obtain mixing reducing solution B；
(3) with thermostat water bath preheating described mixed reaction solution A and described mixing reducing solution B extremely
20～80 DEG C；
(4) by mixing reducing solution B described in thermostat water bath magnetic agitation, the rotating speed of stirring is
500～2000r/min, after stabilization of speed, add described hybrid reaction with the rate of addition of 1-8ml/s
Solution A carries out reduction reaction, the mixed reaction solution A of addition and the described volume mixing reducing solution B
Ratio is 1:1；
(5), after dropping, continue stirring 10～60min, obtain the mixed solution containing argentum powder,
Carry out sucking filtration again, washing, alcohol are washed, are dried, are sieved and after Cement Composite Treated by Plasma, obtain solaode
The ultrapure argentum powder of conductive silver paste.
The solar cell conductive silver slurry preparation method of ultrapure argentum powder the most according to claim 1,
It is characterized in that, in described step (1), silver nitrate used by preparation solution is analytical reagent, prepares molten
Pure electrical conductivity of water used by liquid is 0.05～5 μ S/cm.
The solar cell conductive silver slurry preparation method of ultrapure argentum powder the most according to claim 1,
It is characterized in that, in described step (1) dispersant be polyvinyl alcohol, gelatin, tween, Polyethylene Glycol,
The mixing of one or more in polyvinylpyrrolidone, above-mentioned dispersant is analytical reagent, described point
Amount is silver nitrate quality 4%～the 12% of powder addition.
The solar cell conductive silver slurry preparation method of ultrapure argentum powder the most according to claim 1,
It is characterized in that, in described step (2), ascorbic acid used by preparation solution is analytical reagent, preparation
Pure electrical conductivity of water used by solution is 0.05～5 μ S/cm.
The solar cell conductive silver slurry preparation method of ultrapure argentum powder the most according to claim 1,
It is characterized in that, in described step (3), mixed reaction solution A and mixing reducing solution B is preheated to same
One temperature.
The solar cell conductive silver slurry preparation method of ultrapure argentum powder the most according to claim 1,
It is characterized in that, sucking filtration in described step (5), wash, be dried, sieve and Cement Composite Treated by Plasma
Detailed process is: argentum powder is after sucking filtration, and first pure water twice, then washing with alcohol twice, in 60～100 DEG C
Vacuum drying oven is dried 3～12h, after crossing 250 mesh sieves, locates under plasma room temperature 80～150W
Reason 30～60min.
The solar cell conductive silver slurry preparation method of ultrapure argentum powder the most according to claim 6,
It is characterized in that, described Cement Composite Treated by Plasma atmosphere is that one or more in hydrogen, argon, helium are mixed
Close.
8. the solaode that a preparation method as described in any one of claim 1 to 7 is prepared is led
Ultrapure argentum powder used by electricity silver slurry, it is characterised in that described solar cell conductive silver is starched with the rule of ultrapure argentum powder
Lattice are: mean diameter 0.1～5 μm, tap density are >=4.5g/cm3, purity >=99.99%.
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| CN104084599B (en) * | 2014-08-02 | 2016-03-30 | 天津市职业大学 | A kind of production method of conductive silver paste superfine spherical silver powder |
| CN104162682B (en) * | 2014-08-15 | 2016-04-13 | 华中科技大学 | The preparation method of a kind of silicon solar cell front silver electrode silver powder |
| CN104289726B (en) * | 2014-09-25 | 2017-02-15 | 中国船舶重工集团公司第七一二研究所 | Method for preparing high-specific-surface-area cotton-shaped super-fine silver powder and silver powder prepared with method |
| CN104575676A (en) * | 2014-12-23 | 2015-04-29 | 合肥中南光电有限公司 | Low-temperature electric conduction silver paste |
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| CN105127445A (en) * | 2015-09-15 | 2015-12-09 | 无锡英特派金属制品有限公司 | Preparing method for superfine silver powder used for solar energy front face silver paste |
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| CN106825544A (en) * | 2017-02-17 | 2017-06-13 | 江苏欧耐尔新型材料股份有限公司 | Improve the high-specific surface area silver powder and preparation method of electrode of solar battery electric conductivity |
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| CN112536445A (en) * | 2020-12-10 | 2021-03-23 | 长沙新材料产业研究院有限公司 | Micro-nano dendritic silver powder and preparation method and application thereof |
| CN116618675A (en) * | 2023-05-30 | 2023-08-22 | 上海银波生物科技有限公司 | Preparation method of low-temperature sintering silver powder for heterojunction solar cell |
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| CN102921944A (en) * | 2012-11-05 | 2013-02-13 | 昆明理工大学 | Silver powder for printing size for solar cell electrodes and preparation process thereof |
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| CN101834004A (en) * | 2010-05-28 | 2010-09-15 | 中国乐凯胶片集团公司 | Silver powder for conductive silver paste of solar battery electrode and preparation method thereof |
| CN102921944A (en) * | 2012-11-05 | 2013-02-13 | 昆明理工大学 | Silver powder for printing size for solar cell electrodes and preparation process thereof |
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