CN108359393A - A kind of sandwich for photovoltaic adulterates conductive silver glue and preparation method - Google Patents
A kind of sandwich for photovoltaic adulterates conductive silver glue and preparation method Download PDFInfo
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- CN108359393A CN108359393A CN201810154944.2A CN201810154944A CN108359393A CN 108359393 A CN108359393 A CN 108359393A CN 201810154944 A CN201810154944 A CN 201810154944A CN 108359393 A CN108359393 A CN 108359393A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/08—Metals
- C08K2003/0806—Silver
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention proposes that a kind of sandwich for photovoltaic adulterates conductive silver glue and preparation method, first nano silver wire is dispersed in mensuration dissolubility silicic saline solution, prefabricated solubility calcium saline solution is slowly added dropwise again, and control the addition of calcium saline solution, persistently stirring to get load has the nano lamellar calcium silicates of nano silver wire, go out flake silver powder in nano lamellar calcium silicates surface reduction again, it obtains that there are the double passage of heat doping laminal filters of the nanoscale of sandwich, is then mixed and made into high conductivity elargol with other elargol raw materials such as epoxy resin.The present invention provides the above method and solves the problems, such as that nano silver wire is easily reunited, and in-situ reducing generates silver powder after fixed nano silver wire, form the double passage of heat of nanoscale of sandwich, ensure that adulterate filler is in close contact with silver powder, the significant increase electric conductivity of conductive silver glue, the dosage for reducing silver powder simultaneously, reduces manufacturing cost.
Description
Technical field
The present invention relates to conducting resinl technical field of material, and in particular to a kind of sandwich for photovoltaic
Adulterate conductive silver glue and preparation method.
Background technology
It uses lead/tin (Pb/Sn) alloy as each built-up circuit of solder connection in traditional industrial production, makes each section
Part can be obtained the sufficient of electric power and support, can steadily transmit signal.However, lead/tin solder gradually exposes in recent years
Many disadvantages.Therefore, the use of conducting resinl, which becomes, solves micro-nano connectivity problem effective ways in electronics industry industry.
Conducting resinl is a kind of adhesive being provided simultaneously with electric conductivity and adhesive property, it can connect a variety of conductive materials
It is connected together, makes to be connected storeroom formation conductive path.It is by the way that metal packing is filled in organic polymer matrix,
To make it have and electric conductivity similar in metal.Unlike common conductive polymer, conducting resinl requires system storing up
There is mobility under the conditions of depositing, can be cured by heating or other modes, to form the connection with some strength.
Solar energy is constantly subjected to people's favor as inexhaustible, nexhaustible reproducible green energy resource, wherein
Solar cell converts solar energy into electric energy, is one of research topic most popular in the world today.Solar cell and light
The group of volt component is construed as be unableing to do without the use of conducting resinl, wherein conductive silver glue is people frequent used one in conducting resinl
Kind, the electrode of the front and back of solar cell is may be used as, the extraction electrode and solar cell of battery are can be used for
Repairing on silicon chip has good turn-on effect and adhesive force, is widely applied in area of solar cell, conductive silver glue
Performance and cost impact the electricity conversion and price of solar cell, therefore, the development of conductive silver glue R＆D work
It is promoted to meet the needs of photovoltaic field.
The mechanical property and adhesive property of conductive silver glue mainly determine by polymeric matrix, the resistivity such as gold, silver, copper, nickel
Lower metal powder determines the electric property of conducting resinl as conductive filler.Filler silver is more in traditional silver conductive adhesive
Brilliant micro-silver powder particle to form conductive channel conduction by contacting with each other between silver particles, but due between silver powder particles
Contact area it is small, the node between particle and particle is more, and electric conductivity can not be promoted；And silver contains in conventional conductive elargol
Amount is very high, and weight percentage is generally 70-80%, and in the case where silver powder doping is smaller, conductive rubber has been unable to get
Conductive effect, also can not just reduce the cost of conducting resinl, and industrial application value also receives certain limitation.
In order to improve the electric conductivity of elargol, Chinese invention patent application number 201310702004.X discloses a kind of conduction
Elargol, the conductive silver glue are made of hundred parts of ratios of following weight：Epoxy resin 12-25, curing agent 0.08-1.0, graphene 1-1.5,
Conductive filler 75-90, the epoxy resin are bisphenol A epoxide resin, and curing agent is dicyandiamide, and conductive filler is micron level
Piece silver and ball silver mixture.Chinese invention patent application number 200610154638.6 discloses a kind of high-performance for preparing and leads
The method of electric glue is prepared for the mixing of nano silver wire and Nano silver grain using the method for reduction of ethylene glycol silver nitrate in large quantity
The mixed powder of nano silver wire and Nano silver grain is filled epoxy resin as conductive filler or is prepared by phenolic resin by powder
A kind of novel isotropic conductive adhesive.It is conductive that Chinese invention patent application number 201510645681.1 discloses a kind of low cost
Elargol, composition include：Nano silver wire, 0-2%；Flake silver powder, 10-20%；Metal oxide, 30-40%；Cellulose, 10-
42.3%；Bisphenol A epoxide resin, 10-20%；Curing agent, 3-5%；Accelerating agent, 0.5-1%；Diluent, 2-6%；K-570 or K-
550,1-3%；Terephthalic acid (TPA), 0.5-1%；Nano silicon dioxide, 0.5-1%；Antifoaming agent, 0.1-0.5%；ICAM8401 or
8402,0.1-0.5%.
Said program is by adulterating the filler material of the nanoscale of the combinations such as some Nano silver pieces, nano silver wire, nanosphere
Material is modified silver conductive adhesive, but existing scheme often has following point：First due to nano-sized materials surface energy
Height is easy to happen reunion, and dispersion is uneven in the carrier, influences conducting resinl uniformity, is second unable to ensure doping filler and silver powder is tight
It is close to be connected, it is unstable to be easy to cause electric conductivity.It is therefore prevented that Nano filling is reunited, it is ensured that Nano filling is tight with silver powder
Close connected method is to promote the electric conductivity of conductive silver glue, and reducing silver powder dosage reduces the important link of cost.
Invention content
For current photovoltaic module conductive silver glue, and silver powder dosage height bad there are electric conductivity leads to lacking for cost increase etc.
It falls into, the present invention proposes that a kind of sandwich for photovoltaic adulterates conductive silver glue and preparation method, by nano lamellar
The generation of calcium silicates drives the nano silver wire dispersion of attachment, solves the problems, such as that nano silver wire is easily reunited, and significant increase is led
The electric conductivity of electric elargol, while reducing the dosage of silver powder, reduce manufacturing cost.
To solve the above problems, the present invention uses following technical scheme：A kind of sandwich for photovoltaic is mixed
Miscellaneous conductive silver glue, the conductive silver glue are that conductive filler is filled in organic polymer matrix composition, and the conductive filler is：With silver
Nano wire has interlayer as conducting matrix grain material, outer layer covers laminar silicic acid calcium/flake silver powder composite conducting material, composition
The double passage of heat flaky materials of the nanoscale of structure, the organic polymer matrix are organic resin, the uniform filling filling
It is constituted in the organic polymer and adulterates conductive silver glue for the sandwich of photovoltaic.
Preferably, a diameter of 20-80nm of the nano silver wire, length are 100-600 μm, and the organic resin is epoxy
The combination of one or more of resin, acrylic resin and polyurethane resin.
A kind of preparation method of the sandwich doping conductive silver glue for photovoltaic, specific preparation method are provided
For：
（1）Weighed respectively by mass fraction 15-30 parts of soluble silicate, 20-36 parts of soluble calcium salt, 2-8 parts of nano silver wire,
8-13 parts of silver nitrate solution, 0.1-0.5 parts of dispersant, 0.3-0.8 parts of protective agent, 28-36 parts of organic resin, 10-15 parts of solvent,
2-4 parts of reducing agent, 2-3 parts of curing agent, 1.5-2 parts of additive, appropriate amount of deionized water is spare；
（2）The soluble silicate is dissolved in deionized water, the mensuration dissolubility silicic saline solution of 1mol/L is configured to, by institute
It states nano silver wire to be scattered in the mensuration dissolubility silicic saline solution, after ultrasound is evenly dispersed, obtains the Yin Na of silicate cladding
Rice noodles dispersion liquid；
（3）Soluble calcium salt is dissolved in deionized water, the solubility calcium salting liquid of 1mol/L is configured to, by the solubility calcium
Saline solution is slowly added dropwise into step（2）In be prepared silicate cladding nano silver wire dispersion liquid in, obtain load have
The nano silver wire dispersion liquid of nano lamellar calcium silicates；
（4）Dispersant, protective agent are dissolved in silver nitrate solution, then the nano silver wire dispersion liquid that nano lamellar calcium silicates will be loaded
It mixes with silver nitrate solution, after high-speed stirred, reducing agent is slowly dropped into, the interlayer nano grade pair for obtaining flake silver powder package is led
The passage of heat adulterates conductive filler；
（5）The double passage of heat doping conductive fillers of interlayer nano grade that the flake silver powder is wrapped up and organic resin, curing agent,
Additive mixes, and in vacuum suction de-bubble, obtains highly conductive elargol.
Preferably, the soluble silicate be one or both of sodium metasilicate, potassium silicate, alumina silicate and lithium metasilicate with
On combination, the soluble calcium salt be calcium nitrate, calcium bicarbonate, calcium bisulfate, calcium bisulfite, calcium dihydrogen phosphate, secondary chlorine
The combination of one or more of sour calcium, calcium chlorate, calcium bromide, calcium iodide, Calcium perchlorate and acerdol.
Preferably, the dispersant is triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative
The combination of one or more of object, polyacrylamide, fatty acid polyethylene glycol ester；The protective agent be PVP, PEG,
A combination of one or more in PVA, P123, tween and DPAS；The reducing agent is glucose, sodium hypophosphite, tannic acid, second
The combination of one or more of glycol, DMF and hydrazine hydrate；The solvent is from ethylene glycol, acetone, benzyl alcohol, benzene second
The combination of one or more of alkene and cyclohexanone；The curing agent is benzene sulfone, dicyandiamide, organic acid hydrazides and three ethyl alcohol
The combination of one or more of amine；The additive includes one or both of antifoaming agent, levelling agent and coupling agent
Above combination.
Preferably, step（3）Described in solubility calcium saline solution instill speed be 10-30 drops/sec.
Preferably, step（4）Described in high-speed stirred rotating speed be 800-1200rpm.
Preferably, a concentration of 0.5-1.8mol/L of the silver nitrate solution.
Preferably, the vacuum degassing is evacuated to 10-150Pa using vacuum pump, is made after standing 2-10 hours.
For current photovoltaic module conductive silver glue, and silver powder dosage height bad there are electric conductivity leads to lacking for cost increase etc.
It falls into, existing scheme, which is modified often silver conductive adhesive by the filler of nanoscale, to be had filler surface energy height and be easy to happen group
Poly-, dispersion is uneven in the carrier, and is unable to ensure doping filler and silver powder is closely coupled, to be easy to cause electric conductivity not
Stablize.In consideration of it, the present invention proposes that a kind of sandwich for photovoltaic adulterates conductive silver glue and preparation method, first will
Nano silver wire is dispersed in mensuration dissolubility silicic saline solution, then prefabricated solubility calcium saline solution is slowly added dropwise, and is controlled
The addition of calcium saline solution processed, persistently stirring to get load has the nano lamellar calcium silicates of nano silver wire, then adds containing dispersion
Reducing agent is slowly dropped into after agent and protectant silver-colored solution, goes out flake silver powder in nano lamellar calcium silicates surface reduction, obtains
The double passage of heat of nanoscale with sandwich adulterate laminal filter, are then mixed with other elargol raw materials such as epoxy resin,
Deaeration is stirred in the case of vacuum suction to various material mixings uniformly up to high conductivity elargol.The present invention is by nanometer layer
The generation of shape calcium silicates drives the nano silver wire dispersion of attachment, solves the problems, such as that nano silver wire is easily reunited, and fixed silver nanoparticle
In-situ reducing generates silver powder after line, forms the double passage of heat of nanoscale of sandwich, it is ensured that doping filler closely connects with silver powder
It touches, the significant increase electric conductivity of conductive silver glue, while reducing the dosage of silver powder, reduce manufacturing cost.
Sandwich doping conductive silver glue prepared by the present invention is led with commercially available common conductive elargol, silver nano material doping
Electric elargol carries out test comparison, and the present invention has a clear superiority as shown in table 1.
Table 1：
The present invention provides a kind of sandwich doping conductive silver glue and preparation method for photovoltaic, with prior art phase
Than the feature and excellent effect protruded is：
1, the present invention drives the nano silver wire of attachment to disperse by the generation of nano lamellar calcium silicates, solves nano silver wire and easily rolls into a ball
Poly- problem, and in-situ reducing generates silver powder after fixed nano silver wire, forms the double passage of heat of nanoscale of sandwich, it is ensured that
It adulterates filler and silver powder to be in close contact, the significant increase electric conductivity of conductive silver glue.
2, the sandwich doping conductive silver glue electric conductivity for photovoltaic that prepared by the present invention is excellent, so as to
The shortcomings that enough avoiding the too high levels of conductive filler in conventional conductive glue reduces application amount, is effectively reduced production cost.
3, not only electric conductivity is excellent for the sandwich doping conductive silver glue for photovoltaic prepared by the present invention, folder
The double passage of heat of nanoscale of layer structure assign electric elargol and lead excellent thermal conductivity, suitable for electronics such as all kinds of solar cells
Device assembly.
4, the present invention uses simple for process easily-controllable, and raw materials for production and production process are safe and non-toxic, environmentally protective, is suitble to work
Industry is promoted the use of.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
（1）Weigh 15 parts of sodium metasilicate, 36 parts of calcium nitrate, a diameter of 20nm, the silver nanoparticle that length is 300 μm respectively by mass fraction
8 parts of line, 9 parts of the silver nitrate solution of a concentration of 1mol/L, 0.4 part of triethyl group hexyl phosphoric acid, 0.6 part of PVP, 36 parts of epoxy resin,
2 parts of 10 parts of ethylene glycol, 2 parts of benzene sulfone, XWC-295B types antifoaming agent, dc-57 types levelling agent and silane coupling agent, appropriate deionization
Water；
（2）Sodium metasilicate is dissolved in deionized water, the mensuration dissolubility silicic saline solution of 1mol/L is configured to, by the nano silver wire
It is scattered in the mensuration dissolubility silicic saline solution, after ultrasound is evenly dispersed, obtains the nano silver wire dispersion liquid of silicate cladding；
（3）Calcium nitrate is dissolved in deionized water, the solubility calcium salting liquid of 1mol/L is configured to, by the solubility calcium brine
Solution is slowly added dropwise for 10 drops/sec into step according to speed is instilled（2）In the nano silver wire point of silicate cladding that is prepared
In dispersion liquid, obtaining load has the nano silver wire dispersion liquid of nano lamellar calcium silicates；
（4）Triethyl group hexyl phosphoric acid, PVP are dissolved in silver nitrate solution, then the nano silver wire that nano lamellar calcium silicates will be loaded
Dispersion liquid is mixed with the silver nitrate solution of a concentration of 0.5mol/L, after high-speed stirred, is slowly dropped into glucose solution, is obtained sheet
The double passage of heat of interlayer nano grade of silver powder package adulterate conductive filler；
（5）By the flake silver powder wraps up double passage of heat doping conductive fillers of interlayer nano grade and epoxy resin, benzene sulfone, disappear
Infusion, levelling agent and coupling agent mixing are evacuated to 130Pa using vacuum pump, and use is made after standing 3 hours in vacuum suction de-bubble
Conductive silver glue is adulterated in the sandwich of photovoltaic.
Conductive silver glue in embodiment 1 is subjected to room temperature condition and in 150 DEG C of temperature, pressure 15Kg/cm2 ,Hot pressing time 20
Second, adhesive property and conducting performance test are as shown in table 2, and the conductive silver glue prepared in the present embodiment is used to prepare the film sun
The back electrode of energy battery carries out photoelectric conversion efficiency test to solar cell, and the results are shown in Table 2.
Embodiment 2
（1）Weigh 19 parts of soluble silicate lithium metasilicate, 22 parts of calcium bisulfate, a diameter of 40nm, length respectively by mass fraction
For 120 μm of 8 parts of nano silver wire, 8 parts of the silver nitrate solution of a concentration of 1.5mol/L, 0.4 part of lauryl sodium sulfate, tween
0.5 part, 33 parts of acrylic resin, 12 parts of acetone, 2.5 parts of dicyandiamide, WC-295B types antifoaming agent, dc-57 types levelling agent and coupling
1.5 parts of agent, appropriate amount of deionized water；
（2）Lithium metasilicate is dissolved in deionized water, the mensuration dissolubility silicic saline solution of 1mol/L is configured to, by the nano silver wire
It is scattered in lithium silicate aqueous solution, after ultrasound is evenly dispersed, obtains the nano silver wire dispersion liquid of silicate cladding；
（3）Calcium bisulfate is dissolved in deionized water, the solubility calcium salting liquid of 1mol/L is configured to, calcium bisulfate solution is pressed
It is slowly added dropwise into step for 16 drops/sec according to speed is instilled（2）In be prepared silicate cladding nano silver wire dispersion liquid in,
Obtaining load has the nano silver wire dispersion liquid of nano lamellar calcium silicates；
（4）Dispersant, protective agent are dissolved in silver nitrate solution, then the nano silver wire dispersion liquid that nano lamellar calcium silicates will be loaded
It is mixed with the silver nitrate solution of a concentration of 1.35mol/L, after high-speed stirred, is slowly dropped into sodium hypophosphite, obtain flake silver powder packet
The double passage of heat doping conductive fillers of interlayer nano grade wrapped up in；
（5）The double passage of heat doping conductive fillers of interlayer nano grade and acrylic resin, the double cyanogen that the flake silver powder is wrapped up
Amine, antifoaming agent, levelling agent and coupling agent mixing are evacuated to 45Pa using vacuum pump, and vacuum suction de-bubble is made after standing 2 hours
Conductive silver glue is adulterated to the sandwich for photovoltaic.
Conductive silver glue in embodiment 2 is subjected to room temperature condition and in 150 DEG C of temperature, pressure 15Kg/cm2 ,Hot pressing time 20
Second, adhesive property and conducting performance test are as shown in table 2, and the conductive silver glue prepared in the present embodiment is used to prepare the film sun
The back electrode of energy battery carries out photoelectric conversion efficiency test to solar cell, and preparation is same as Example 1 with test condition,
The results are shown in Table 2.
Embodiment 3
（1）Weigh 22 parts of soluble silicate alumina silicate, calcium bicarbonate, calcium bisulfate, calcium bisulfite respectively by mass fraction
28 parts of mixture, a diameter of 65nm, length be 550 μm 15 parts of nano silver wire, a concentration of 0.8mol/L silver nitrate solution
13 parts, 0.65 part of combination, epoxy resin, acrylic resin and the polyurethane of 0.45 part of fatty acid polyethylene glycol ester, tween and DPA
32 parts of combination, ethylene glycol and 13 parts of the combination of benzyl alcohol of resin, 2.6 parts of organic acid hydrazides, WC-295B types antifoaming agent, dc-57
2 parts of type levelling agent and coupling agent, appropriate amount of deionized water；
（2）Alumina silicate is dissolved in deionized water, the mensuration dissolubility silicic saline solution of 1mol/L is configured to, by the nano silver wire
It is scattered in the mensuration dissolubility silicic saline solution, after ultrasound is evenly dispersed, obtains the nano silver wire dispersion liquid of silicate cladding；
（3）The mixture of calcium bicarbonate, calcium bisulfate, calcium bisulfite is dissolved in deionized water, be configured to 1mol/L can
The solubility calcium saline solution is slowly added dropwise for 25 drops/sec into step dissolubility calcium salt soln according to speed is instilled（2）Middle system
In the nano silver wire dispersion liquid of standby obtained silicate cladding, obtaining load has the nano silver wire of nano lamellar calcium silicates to disperse
Liquid；
（4）Dispersant, protective agent are dissolved in silver nitrate solution, then the nano silver wire dispersion liquid that nano lamellar calcium silicates will be loaded
It is mixed with the silver nitrate solution of a concentration of 0.8mol/L, after high-speed stirred, is slowly dropped into tannic acid and hydrazine hydrate mixture, obtains piece
The double passage of heat of interlayer nano grade of shape silver powder package adulterate conductive filler；
（5）The double passage of heat doping conductive fillers of interlayer nano grade and epoxy resin, the acrylic acid that the flake silver powder is wrapped up
Combination, organic acid hydrazides, antifoaming agent, levelling agent and the coupling agent mixing of resin and polyurethane resin, are evacuated to using vacuum pump
50Pa, vacuum suction de-bubble are made after standing 6.5 hours and adulterate conductive silver glue for the sandwich of photovoltaic.
Conductive silver glue in embodiment 3 is subjected to room temperature condition and in 150 DEG C of temperature, pressure 15Kg/cm2 ,Hot pressing time 20
Second, adhesive property and conducting performance test are as shown in table 2, and the conductive silver glue prepared in the present embodiment is used to prepare the film sun
The back electrode of energy battery carries out photoelectric conversion efficiency test to solar cell, and preparation is same as Example 1 with test condition,
The results are shown in Table 2.
Embodiment 4
（1）Weigh soluble silicate sodium metasilicate, alumina silicate and 25 parts of lithium metasilicate composition, Calcium perchlorate respectively by mass fraction
With 20 parts of composition, a diameter of 30nm of acerdol, 13 parts of nano silver wire that length is 240 μm, a concentration of 1.45mol/L
0.8 part of 9.5 parts of silver nitrate solution, 0.3 part of methyl anyl alcohol, PVP and DPAS combinations, the combination of acrylic resin and polyurethane resin
28 parts, benzyl alcohol and 15 parts of the combination of styrene, 2.5 parts of organic acid hydrazides, WC-295B types antifoaming agent, dc-57 types levelling agent and
1.7 parts of coupling agent, appropriate amount of deionized water；
（2）The combination of sodium metasilicate and lithium metasilicate is dissolved in deionized water, the sodium metasilicate of 1mol/L and the group of lithium metasilicate are configured to
The nano silver wire is scattered in the mensuration dissolubility silicic saline solution by Heshui solution, after ultrasound is evenly dispersed, obtains silicic acid
The nano silver wire dispersion liquid of root cladding；
（3）The composition of Calcium perchlorate and acerdol is dissolved in deionized water, the soluble calcium salt for being configured to 1mol/L is molten
The composition solution of Calcium perchlorate and acerdol is slowly added dropwise for 17 drops/sec into step liquid according to speed is instilled（2）In
In the nano silver wire dispersion liquid for the silicate cladding being prepared, obtaining load has the nano silver wire of nano lamellar calcium silicates to disperse
Liquid；
（4）Dispersant, protective agent are dissolved in silver nitrate solution, then the nano silver wire dispersion liquid that nano lamellar calcium silicates will be loaded
It is mixed with the silver nitrate solution of a concentration of 1.2mol/L, after high-speed stirred, is slowly dropped into hydrazine hydrate, obtain flake silver powder package
The double passage of heat of interlayer nano grade adulterate conductive filler；
（5）The double passage of heat doping conductive fillers of interlayer nano grade and acrylic resin and the poly- ammonia that the flake silver powder is wrapped up
Combination, organic acid hydrazides, antifoaming agent, levelling agent and the coupling agent mixing of ester resin, are evacuated to 120Pa, vacuum is taken out using vacuum pump
Gas de-bubble is made after standing 2 hours and adulterates conductive silver glue for the sandwich of photovoltaic.
Conductive silver glue in embodiment 4 is subjected to room temperature condition and in 150 DEG C of temperature, pressure 15Kg/cm2 ,Hot pressing time 20
Second, adhesive property and conducting performance test are as shown in table 2, and the conductive silver glue prepared in the present embodiment is used to prepare the film sun
The back electrode of energy battery carries out photoelectric conversion efficiency test to solar cell, and preparation is same as Example 1 with test condition,
The results are shown in Table 2.
Embodiment 5
（1）Weigh 30 parts of soluble silicate alumina silicate, 28 parts of calcium hypochlorite, a diameter of 80nm, length respectively by mass fraction
For 600 μm of 13 parts of nano silver wires, 0.35 part of 10.5 parts of silver nitrate solution, the methyl anyl alcohol of a concentration of 1.4mol/L, P123 and
0.6 part of tween combination, epoxy resin, acrylic resin and 33 parts of polyurethane resin combination, ethylene glycol and 15 parts of acetone, dicyandiamide
With 1.8 parts of 2.5 parts of organic acid hydrazides, WC-295B types antifoaming agent, dc-57 types levelling agent and silane coupling agent, appropriate deionization
Water；
（2）Alumina silicate is dissolved in deionized water, the silicic acid aluminum water solution of 1mol/L is configured to, the nano silver wire is scattered in
In the mensuration dissolubility silicic saline solution, after ultrasound is evenly dispersed, the nano silver wire dispersion liquid of silicate cladding is obtained；
（3）Calcium hypochlorite is dissolved in deionized water, the calcium hypochlorite solution of 1mol/L is configured to, by the calcium hypochlorite solution
It is slowly added dropwise into step for 30 drops/sec according to speed is instilled（2）In be prepared silicate cladding nano silver wire dispersion liquid
In, obtaining load has the nano silver wire dispersion liquid of nano lamellar calcium silicates；
（4）Methyl anyl alcohol, P123 and tween composition are dissolved in silver nitrate solution, then the silver that nano lamellar calcium silicates will be loaded
Nanowire dispersion is mixed with the silver nitrate solution of a concentration of 0.9mol/L, after high-speed stirred, is slowly dropped into ethylene glycol and DMF groups
It closes, obtains the double passage of heat doping conductive fillers of interlayer nano grade of flake silver powder package；
（5）The double passage of heat doping conductive fillers of interlayer nano grade and epoxy resin, the acrylic acid that the flake silver powder is wrapped up
Resin and polyurethane resin combination, dicyandiamide and organic acid hydrazides, antifoaming agent, levelling agent and coupling agent mixing, using vacuum pump
It is evacuated to 120Pa, vacuum suction de-bubble is made after standing 6.5 hours and adulterates conductive silver for the sandwich of photovoltaic
Glue, filer content 20%.
Conductive silver glue in embodiment 5 is subjected to room temperature condition and in 150 DEG C of temperature, pressure 15Kg/cm2 ,Hot pressing time 20
Second, adhesive property and conducting performance test are as shown in table 2, and the conductive silver glue prepared in the present embodiment is used to prepare the film sun
The back electrode of energy battery carries out photoelectric conversion efficiency test to solar cell, and preparation is same as Example 1 with test condition,
The results are shown in Table 2.
Comparative example 1
Certain commercially available brand conductive silver glue, filer content 78%.
Comparative example 2
Nano silver wire 16%, micro-silver powder 30%, bisphenol A epoxide resin 44%, adipic dihydrazide and dicyandiamide 5%, ethylene glycol, neighbour
Rutgers 19.13%, accelerating agent 0.87%, diluent 4.5%, K-57 3%, terephthalic acid (TPA) 0.5%, antifoaming agent
0.2%, ICAM8401 0.3%.
Comparative example 3
（1）Take a diameter of 40nm, 8 parts of the silver nitrate solution of 8 parts of nano silver wire, a concentration of 1.5mol/L that length is 120 μm, ten
0.4 part of sodium dialkyl sulfate, 0.5 part of tween, 33 parts of acrylic resin, 12 parts of acetone, 2.5 parts of dicyandiamide, the defoaming of WC-295B types
1.5 parts of agent, dc-57 types levelling agent and coupling agent, appropriate amount of deionized water；
（2）Nano silver wire is scattered in lithium silicate aqueous solution, after ultrasound is evenly dispersed, obtains nano silver wire dispersion liquid；
（3）Lauryl sodium sulfate, tween are dissolved in silver nitrate solution, then the nano silver wire that nano lamellar calcium silicates will be loaded
Dispersion liquid is mixed with the silver nitrate solution of a concentration of 1.35mol/L, after high-speed stirred, is slowly dropped into sodium hypophosphite, is obtained sheet
Silver powder conductive filler；
（4）The nano silver wire conductive filler that the flake silver powder is wrapped up is defoamed with acrylic resin, dicyandiamide, WC-295B types
Agent, dc-57 types levelling agent and silane coupling agent mixing are evacuated to 45Pa, vacuum suction de-bubble, after standing 2 hours using vacuum pump
The conductive silver glue that the nano silver wire of obtained content 28% is filled out altogether with flake silver powder.
Prepared by the back electrode that conducting resinl prepared by comparative example 1,2 and 3 is used to prepare to solar cell, condition and embodiment
1 is identical, tests solar cell transformation efficiency, carries out room temperature condition to conductive silver glue before preparing and in 150 DEG C of temperature,
Pressure 15Kg/cm2, properties test is as shown in table 2 under the conditions of hot pressing time 20 seconds.
Table 2
Claims (9)
1. a kind of sandwich for photovoltaic adulterates conductive silver glue, the conductive silver glue is that conductive filler has been filled in
Organic polymer matrix is constituted, which is characterized in that the conductive filler is：Using nano silver wire as conducting matrix grain material, outer layer packet
Covering layer shape calcium silicates/flake silver powder composite conducting material, the double passage of heat sheet materials of the nanoscale with sandwich of composition
Material, the organic polymer matrix are organic resin, and the uniform filling is filled in the organic polymer and constitutes for too
The sandwich of positive energy photovoltaic adulterates conductive silver glue.
2. a kind of sandwich for photovoltaic according to claim 1 adulterates conductive silver glue, which is characterized in that
A diameter of 20-80nm of the nano silver wire, length are 100-600 μm, and the organic resin is epoxy resin, acrylic resin
With the combination of one or more of polyurethane resin.
3. a kind of sandwich for photovoltaic as described in any claims of claim 1-2 adulterates the system of conductive silver glue
Preparation Method, which is characterized in that specifically preparation method is：
（1）Weigh 15-30 parts of soluble silicate, 20-36 parts of soluble calcium salt, nano silver wire 8-18 respectively by mass fraction
Part, 8-13 parts of silver nitrate solution, 0.1-0.5 parts of dispersant, 0.3-0.8 parts of protective agent, 28-36 parts of organic resin, solvent 10-15
Part, 2-4 parts of reducing agent, 2-3 parts of curing agent, 1.5-2 parts of additive, appropriate amount of deionized water is spare；
（2）The soluble silicate is dissolved in deionized water, the mensuration dissolubility silicic saline solution of 1mol/L is configured to, by institute
It states nano silver wire to be scattered in the mensuration dissolubility silicic saline solution, after ultrasound is evenly dispersed, obtains the Yin Na of silicate cladding
Rice noodles dispersion liquid；
（3）Soluble calcium salt is dissolved in deionized water, the solubility calcium salting liquid of 1mol/L is configured to, by the solubility calcium
Saline solution is slowly added dropwise into step（2）In be prepared silicate cladding nano silver wire dispersion liquid in, obtain load have
The nano silver wire dispersion liquid of nano lamellar calcium silicates；
（4）Dispersant, protective agent are dissolved in silver nitrate solution, then the nano silver wire dispersion liquid that nano lamellar calcium silicates will be loaded
It mixes with silver nitrate solution, after high-speed stirred, reducing agent is slowly dropped into, the interlayer nano grade pair for obtaining flake silver powder package is led
The passage of heat adulterates conductive filler；
（5）The double passage of heat doping conductive fillers of interlayer nano grade that the flake silver powder is wrapped up and organic resin, curing agent,
Additive mixes, and in vacuum suction de-bubble, obtains highly conductive elargol.
4. a kind of sandwich for photovoltaic according to claim 3 adulterates the preparation method of conductive silver glue,
It is characterized in that, the soluble silicate is one or more of sodium metasilicate, potassium silicate, alumina silicate and lithium metasilicate
Combination, the soluble calcium salt be calcium nitrate, calcium bicarbonate, calcium bisulfate, calcium bisulfite, calcium dihydrogen phosphate, calcium hypochlorite,
The combination of one or more of calcium chlorate, calcium bromide, calcium iodide, Calcium perchlorate and acerdol.
5. a kind of sandwich for photovoltaic according to claim 3 adulterates the preparation method of conductive silver glue,
It is characterized in that, the dispersant is triethyl group hexyl phosphoric acid, lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, gathers
The combination of one or more of acrylamide, fatty acid polyethylene glycol ester；The protective agent be PVP, PEG, PVA,
A combination of one or more in P123, tween and DPAS；The reducing agent is glucose, sodium hypophosphite, tannic acid, second two
The combination of one or more of alcohol, DMF and hydrazine hydrate；The solvent is from ethylene glycol, acetone, benzyl alcohol, styrene
With the combination of one or more of cyclohexanone；The curing agent is benzene sulfone, dicyandiamide, organic acid hydrazides and triethanolamine
One or more of combination；The additive include one or both of antifoaming agent, levelling agent and coupling agent with
On combination.
6. a kind of sandwich for photovoltaic according to claim 3 adulterates the preparation method of conductive silver glue,
It is characterized in that, step（3）Described in solubility calcium saline solution instill speed be 10-30 drops/sec.
7. a kind of sandwich for photovoltaic according to claim 3 adulterates the preparation method of conductive silver glue,
It is characterized in that, step（4）Described in high-speed stirred rotating speed be 800-1200rpm.
8. a kind of sandwich for photovoltaic according to claim 3 adulterates the preparation method of conductive silver glue,
It is characterized in that, a concentration of 0.5-1.8mol/L of the silver nitrate solution.
9. a kind of sandwich for photovoltaic according to claim 3 adulterates the preparation method of conductive silver glue,
It is characterized in that, the vacuum degassing is evacuated to 10-150Pa using vacuum pump, it is made after standing 2-10 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116525175A (en) * | 2023-05-17 | 2023-08-01 | 浙江光达电子科技有限公司 | Electrode slurry, preparation method, electrode plate and photovoltaic cell |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116525175A (en) * | 2023-05-17 | 2023-08-01 | 浙江光达电子科技有限公司 | Electrode slurry, preparation method, electrode plate and photovoltaic cell |
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