CN108597676A - A kind of preparation method and application containing organobentonite low-temperature solidified silver paste - Google Patents
A kind of preparation method and application containing organobentonite low-temperature solidified silver paste Download PDFInfo
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- CN108597676A CN108597676A CN201711202232.5A CN201711202232A CN108597676A CN 108597676 A CN108597676 A CN 108597676A CN 201711202232 A CN201711202232 A CN 201711202232A CN 108597676 A CN108597676 A CN 108597676A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Abstract
The invention discloses a kind of preparation method and applications containing organobentonite low-temperature solidified silver paste.The preparation for serving high-performance low-temperature solidified electric slurry uses.The slurry is made of the following each raw material of mass percentage：1~5wt%'s utilizes surfactant-modified obtained organobentonite, the silver powder of 35~65wt% and the organic carrier of 34~60wt%.The surfactant-modified obtained organobentonite is suitable for low-temperature setting electric slurry formula, including organic carrier systems such as epoxy, chlorine vinegar, polyester, polyurethane, acrylic acid, while being suitable for piece powder, ball powder and its silver powder system.The Effective Regulation for not only realizing slurry viscosity is added in bentonite in the present invention, obtain good rheological behavior, meet high-resolution silk-screen printing requirement, effectively solve the decentralized stable problem of low viscosity resin carrier and silver powder particles, realize that efficient conductive path, conductive film layer have good electric property.
Description
Technical field
The invention belongs to photoelectricity information material preparing technical fields, containing modified organic swelling more particularly, to one kind
The preparation method and application of native low-temperature solidified silver paste.
Background technology
When the viscosity of electric slurry reduces, series of malpractice is often will produce, low viscosity system first is not easy to store,
During storage, sedimentation, layering easily occurs.In printing, poor rheological property, extremely low thixotropy so that after printing
Flared end occurs for film layer, influences the electric property of film layer.However be the good electric conductivity of acquisition, the addition of auxiliary agent should be avoided, this
It is as small as possible to require that added auxiliary agent influences the electrical property of silver paste.
For slurry system, it is hydrophilic without oleophylic that the organobentonite prepared by the present invention overcomes traditional Na base bentonites
Property defect, it can be dispersed in organic phase, in the case of unused organic functions auxiliary agent, realize to superfines
Dispersion and architecture stabilization, bentonite addition enhance system powder inside electrical charges between particles repulsion and sky
Between steric stabilization so that slurry has good stably dispersing performance, and precipitation, layering are not susceptible in storing process；It starches simultaneously
Material obtains good rheology printing characteristic, and it is full that printing prepares pattern densification, bubble-free, stomata.Modification produced by the present invention has
Machine bentonite is suitable for most low-temperature setting slurry system, in terms of the electric property on, the advantages of compared to other thickening aids,
It does not influence the electric conductivity of slurry, while promoting effective overlap joint between powder granule, is obtained after slurry low-temperature setting good
Electric conductivity.Formula system has the advantages that low silver content is low-resistance, significantly reduces the production cost of slurry.
Invention content
The present invention using it is a kind of by surfactant-modified obtained organobentonite as the thickening aids of low viscous silver paste,
While improving dispersion, the rheology printing performance of slurry, good electric property can also be obtained.After solidification drying, Ke Yishi
Existing conductive film layer current-carrying capability is strong, the strong attachment to material substrate, and the product yield prepared is high.
To achieve the goals above, according to one aspect of the present invention, a kind of preparation side of organic modified bentonite is provided
Method, it is preferred that such surfactant-modified obtained organobentonite is made as follows：
(1) reaction bulb is taken, 8~10 parts of two or more surfactants are added to 10~15 times of deionized waters
In, mixed surfactants solutions are made.Take another reaction bulb, by 5~8 parts of Na base bentonites be added to 10~15 times go from
In sub- water, bentonite suspension is made in 50~60 DEG C of high speed dispersions of constant temperature.Be warming up to 60~70 DEG C under stirring conditions slowly
Prepared surfactant solution is added, 2~3h of high speed dispersion, makes it fully react under high speed dispersor, reuses super
Sound wave disperses 3~6h, is put into centrifugation in centrifuge.
(2) it with deionized water by the organobentonite ultrasonic washing 4~5 times of synthesis, finally filters separation and is dried at 70 DEG C
Decompression drying in case ground 100 mesh ultrasound filtrations sieve, the organobentonite containing surfactant is made.
Preferably, the surfactant is quaternary cationics, main carbochain C atom numbers 10~
In 20 ranges, molecular characterization is [(CH3)3NR]+X-Or [(CH3)2NR2]+X-Or SiX3R, wherein R represent alkyl, and X is represented
Halogens.Such as tetradecyl trimethyl ammonium chloride, tetradecyltrimethylammonium bromide, cetyl trimethylammonium bromide,
Octadecyltrimethylammonium chloride, octadecyl trichlorosilane alkane etc..
Preferably, 2.4~4.0g/cm of range tap density of the flake silver powder3, 4.5~6.7um of average grain diameter, burning
Damage ＜ 1%, 1.5~2.5m of specific surface area2/g.4.1~5.0g/cm of range tap density of spherical silver powder3, average grain diameter 0.5~
1.4um, scaling loss ＜ 0.5%, 0.8~1.0m of specific surface area2/g。
It is another aspect of this invention to provide that a kind of preparation method containing organobentonite low-temperature solidified silver paste, feature
It is, the preparation of organic carrier includes the following steps：
Resin is dissolved in solvent, 70 DEG C of stirring in water bath of constant temperature, it is to be dissolved completely after be down to room temperature, add curing agent, it is high
Disperse 40min under rotating speed and organic carrier is made.
Preferably, the resin includes in epoxy resin, vinyl chloride-vinyl acetate resin, polyester resin, polyurethane, acrylic resin
One or more composition.
Preferably, the organic solvent is isophorone, DBE, dimethylformamide, butyl acetate, penta
One or more kinds of mixed solvents of acid dimethyl, hexanedioic acid dimethyl ester, t-butyl methyl ether.
Preferably, the curing agent is blocked isocyanate either dicyandiamide or imidazoles, wherein enclosed type isocyanide
It is 110~135 DEG C that acid esters, which unseals temperature,.
It is another aspect of this invention to provide that a kind of preparation method containing organobentonite low-temperature solidified silver paste, feature
It is, silver paste preparation includes the following steps：
Organic carrier and organic modified bentonite are slurried using double planetary mixer premixing, leaching is stirred in dispersion machine
Moisten 2~5h, then by silver powder and premix centrotheca disperseed using three-roll grinder, until slurry fineness be less than 6 μm, finally depressurize
Deaeration obtains high-performance low-temperature solidified silver paste made from a kind of organic modified bentonite.
Through the invention it is contemplated above technical scheme is compared with the prior art, have the advantages that：
1. realize slurry viscosity Effective Regulation, obtain good rheological behavior, meet height put into several classes rate silk-screen printing use
It is required that.
2. the decentralized stable problem of low viscosity resin carrier and silver powder particles is effectively solved, with traditional printing electric slurry phase
Than organobentonite enhances system powder inside electrical charges between particles repulsion and space stability ultimate load so that superfine powder somaplasm
Material has good stably dispersing performance, and caking, precipitation and layering are not susceptible in storing process.
3. printing process pattern densification is full, bubble-free, stomata.After electric slurry solidification, organobentonite helps to lead
Electric powder interface overlap joint realizes that efficient conductive path, conductive film layer have good electric property.
4. this silver paste effectively promotes the stability of slurry, film-forming silk-screen line width is stable, resistivity is low, yields
Height significantly reduces the production cost of slurry.
Description of the drawings：
Fig. 1 is the SEM figures of organic modified bentonite made from the embodiment of the present invention 1；Mag20000×
Fig. 2 is silver paste line width pattern made from the embodiment of the present invention 1；
Fig. 3 is the SEM figures of organic modified bentonite made from the embodiment of the present invention 2；Mag20000×
Fig. 4 is silver paste line width pattern made from the embodiment of the present invention 2；
Fig. 5 is the SEM figures of organic modified bentonite made from the embodiment of the present invention 3；Mag20000×
Fig. 6 is silver paste line width pattern made from the embodiment of the present invention 3.
Specific implementation mode
The electrocondution slurry of the embodiment of the present invention is made of the following each raw material of mass percentage：1~5wt%'s utilizes table
The organobentonite that face activating agent is modified, the silver powder of 35~65wt% and the organic carrier of 34~60wt%.
Wherein, modified alta-mud is made by surfactant-modified, and wherein surfactant is existed by main carbochain C atom numbers
In 10~20 ranges, molecular characterization is [(CH3)3NR]+X-、[(CH3)2NR2]+X-Or SiX3R, wherein R represent alkyl, X generations
Table halogens, mixing composition.Such as tetradecyl trimethyl ammonium chloride, tetradecyltrimethylammonium bromide, cetyl three
The mixed system of the compositions such as methyl bromide ammonium, octadecyltrimethylammonium chloride, octadecyl trichlorosilane alkane.It is thus obtained to have
The bentonitic colloidity of machine is 7.8~9.7%, 12.1~18.2m of specific surface area2/ g, 65~75ml/100g of oil factor-1, whiteness
76.61~78.63%.2.4~4.0g/cm of range tap density of flake silver powder3, 4.5~6.7um of average grain diameter, scaling loss ＜
1%, 1.5~2.5m of specific surface area2/g.4.1~5.0g/cm of range tap density of spherical silver powder3, average grain diameter 0.5~
1.4um, scaling loss ＜ 0.5%, 0.8~1.0m of specific surface area2/g.The type of resin includes epoxy resin, vinyl chloride-vinyl acetate resin, polyester tree
One or more of fat, polyurethane, acrylic resin form.Organic solvent is isophorone, DBE, dimethylformamide, two
2-Butoxyethyl acetate, dimethyl glutarate, hexanedioic acid dimethyl ester, the one or more mixing of t-butyl methyl ether are molten
Agent.Curing agent is blocked isocyanate either dicyandiamide or imidazoles, wherein blocked isocyanate deblocking temperature be 110~
135℃。
One kind prepared by the embodiment of the present invention contains organobentonite low-temperature solidified silver paste-making method, includes the following steps：
(1) preparation of organic modified bentonite.Specifically, reaction bulb is taken, by 8~10 parts of two or more surfaces
Activating agent is added in 10~15 times of deionized waters, and mixed surfactants solutions are made.Another reaction bulb is taken, by 5~8 parts of Na
Base bentonite is added in 10~15 times of deionized water, 50~60 DEG C of high speed dispersions of constant temperature, and bentonite suspension is made.Heating
It is slowly added to prepared surfactant solution under stirring conditions to 60~70 DEG C, the high speed dispersion under high speed dispersor
2~3h makes it fully react, and reuses ultrasonic wave and disperses 3~6h, is put into centrifugation in centrifuge.With deionized water by synthesis
Organobentonite ultrasonic washing 4~5 times finally filters separation decompression drying in 70 DEG C of baking ovens, it is super to grind 100 mesh
The organobentonite containing surfactant is made in sound sieves.
(2) preparation of organic carrier.Specifically, by the epoxy resin of content 25~45%, vinyl chloride-vinyl acetate resin, polyester resin,
One or more of polyurethane, acrylic resin resin is dissolved in 53~73% isophorones, DBE, dimethylformamide, diethyl
One or more kinds of mixed solvents of glycol monobutyl ether acetate, dimethyl glutarate, hexanedioic acid dimethyl ester, t-butyl methyl ether
In, 70 DEG C of stirring in water bath of constant temperature, it is to be dissolved completely after be down to room temperature, the blocked isocyanate or dicyandiamide of addition 2~5%
Or imidazoles, organic carrier is made in dispersion 40min under high rotating speed.
(3) preparation of slurry.Specifically, silver powder with organic carrier and organobentonite is mixed to dispersion and conductive paste is made
Material.Specifically, raw material is weighed by following mass percent：1~5wt%'s utilizes surfactant-modified obtained organic swelling
Soil, the silver powder of 35~65wt% and the organic carrier of 34~60wt%.Organic carrier and organic modified bentonite are used double
Planetary mixer premixing is slurried, 2~5h of stirring infiltration in dispersion machine, then silver powder and premix centrotheca are used three-roll grinder
Dispersion, until slurry fineness is less than 6 μm, last vacuum deaerator obtains high-performance made from a kind of organic modified bentonite
Low-temperature solidified silver paste.
Embodiment 1
Reaction bulb is taken, by 8 parts of cetyl trimethylammonium bromides and octadecyltrimethylammonium chloride (W:W=1:1) add
Enter into 10 times of deionized waters and mixed surfactant is made.Another reaction bulb is taken, 5 parts of Na base bentonites are added to 10 times
In deionized water, bentonite suspension is made in 50 DEG C of high speed dispersions of constant temperature.60 DEG C are warming up to, is slowly added under stirring conditions
Enter prepared surfactant solution, high speed dispersion 3h, makes it fully react under high speed dispersor, reuses ultrasonic wavelength-division
6h is dissipated, centrifugation in centrifuge is put into.With deionized water by the organobentonite ultrasonic washing 4 times of synthesis, separation is finally filtered,
The decompression drying in 70 DEG C of baking ovens ground 100 mesh ultrasound filtrations sieve, surfactant-modified organic swelling is made
Soil.
By 35wt% vinyl chloride-vinyl acetate resins and polyurethane according to (W:W=2:1) 63wt% dimethyl glutarates, two are added to
Dimethyl phthalate in the mixed solvent (V:V=1:1), 70 DEG C of stirring in water bath of constant temperature, it is to be dissolved completely after be down to room temperature, add 2wt%
Blocked isocyanate, organic carrier is made in dispersion 40min under high rotating speed.
Raw material is weighed by following mass percent：35wt% pieces powder (tap density 2.4g/cm3, average grain diameter 6.7um, burning
Damage ＜ 1wt%, specific surface area 1.5m2/ g), the organic carrier of 60wt%, the organic modified bentonite of 5wt%；By organic carrier,
Organic modified bentonite is slurried using double planetary mixer premixing in mass ratio, the stirring infiltration 2h in dispersion machine, then will be silver-colored
Powder and premix centrotheca are disperseed using three-roll grinder, and until slurry fineness is less than 6 μm, last vacuum deaerator obtains one kind
High-performance low-temperature solidified silver paste made from organic modified bentonite.
Embodiment 2
Reaction bulb is taken, by 9 parts of tetradecyltrimethylammonium bromide and eicosyl trimethyl ammonium chloride (W:W=2:1) add
Enter into 12 times of deionized waters and mixed surfactant is made.Another reaction bulb is taken, 6 parts of Na base bentonites are added to 15 times
In deionized water, bentonite suspension is made in 55 DEG C of high speed dispersions of constant temperature.65 DEG C are warming up to, is slowly added under stirring conditions
Enter prepared surfactant solution, high speed dispersion 2.5h, makes it fully react under high speed dispersor, reuses ultrasonic wave
Disperse 4h, is put into centrifugation in centrifuge.With deionized water by the organobentonite ultrasonic washing 4 times of synthesis, finally filter point
From the decompression drying in 70 DEG C of baking ovens ground 100 mesh ultrasound filtrations sieve, surfactant-modified organic bentonite is made
Profit soil.
By 40wt% polyester resin and epoxy resin according to (W:W=1:2) it is added to 57wt% butyl acetic acid
Ester, dimethyl glutarate, isophorone in the mixed solvent (V:V:V=2:2:1), 70 DEG C of stirring in water bath of constant temperature, it is to be dissolved complete
After be down to room temperature, add 3wt% blocked isocyanates, organic carrier is made in dispersion 40min under high rotating speed.
Raw material is weighed by following mass percent：Mixed-powder (the W of 50wt% pieces powder, ball powder:W=9:1, flake silver powder
Tap density 4.0g/cm3, average grain diameter 4.5um, scaling loss ＜ 1wt%, specific surface area 2.5m2/g；Spherical silver powder tap density
5.0g/cm3, average grain diameter 0.5um, scaling loss ＜ 0.5wt%, specific surface area 1.0m2/ g), the organic carrier of 48wt%, 2wt% changes
Property machine bentonite；Organic carrier, organic modified bentonite are slurried using double planetary mixer premixing in mass ratio, disperseed
In machine stirring infiltration 3h, then by silver powder and premix centrotheca disperseed using three-roll grinder, until slurry fineness be less than 6 μm,
Last vacuum deaerator obtains high-performance low-temperature solidified silver paste made from a kind of organic modified bentonite.
Embodiment 3
Reaction bulb is taken, by 10 parts of tetradecyl trimethyl ammonium chlorides, octadecyltrimethylammonium chloride, octadecyl trichlorine
Silane (W:W:W=1:1:2) it is added in 15 times of deionized waters and mixed surfactant is made.Another reaction bulb is taken, by 8 parts of Na
Base bentonite is added in 12 times of deionized water, 60 DEG C of high speed dispersions of constant temperature, and bentonite suspension is made.70 DEG C are warming up to,
It is slowly added to prepared surfactant solution under stirring conditions, high speed dispersion 2h, makes it fill under high speed dispersor
Divide reaction, reuses ultrasonic wave dispersion 3h, be put into centrifugation in centrifuge.With deionized water by the organobentonite ultrasonic wave of synthesis
Washing 4 times, finally filters separation, and the decompression drying in 70 DEG C of baking ovens ground 100 mesh ultrasound filtrations sieve, surface is made
The organobentonite that activating agent is modified.
By 45wt% epoxy resin and acrylic resin according to (W:W=2:1) 51wt% dimethyl glutarates, are added to
Acid dimethyl in the mixed solvent (V:V:V=1:1:1), 70 DEG C of stirring in water bath of constant temperature, it is to be dissolved completely after be down to room temperature, add
4wt% dicyandiamides, organic carrier is made in dispersion 40min under high rotating speed.
Raw material is weighed by following mass percent：65wt% balls powder (spherical silver powder tap density 4.1g/cm3, average grain diameter
1.4um, scaling loss ＜ 0.5wt%, specific surface area 0.8m2/ g), the organic carrier of 34wt%, 1wt% organic modified bentonites；It will
Organic carrier, organic modified bentonite are slurried using double planetary mixer premixing in mass ratio, and infiltration is stirred in dispersion machine
3h, then by silver powder and premix centrotheca disperseed using three-roll grinder, until slurry fineness be less than 6 μm, last vacuum deaerator
Obtain high-performance low-temperature solidified silver paste made from a kind of organic modified bentonite.
Electrocondution slurry prepared by above-described embodiment is tested for the property, the specific test method is as follows.
(1) line width pattern is printed
By 350 mesh web plates, electrocondution slurry is printed on PET film layer, prints snakelike 0.6mm × 1m conductive lines, 135
DEG C × 30min solidification after take out.It is cooled to room temperature whether straight, line width width of observing conductive line edge in contourgraph,
Calculating judges whether that flared end (flared end rate≤5%) occurs.
(2) electrical performance testing
The resistance of serpentine, uses Fluke17B after test solidification+Multimeter, film thickness gauge to the silver wire of line width 0.6mm into
The test of row resistance, film thickness obtains the resistivity of slurry by resistivity calculation formula.
(3) anti-settling is tested
Prepared 300g silver pastes are put into 500ml graduated cylinders, are placed 6 months at room temperature, whether observation slurry occurs
Sedimentation, layering.
(4) modified alta-mud scanning electron microscope
The modified alta-mud that will be prepared carries out microscopic appearance observation with field emission scanning electron microscope.
The results are shown in Table 1 for the partial test of electrocondution slurry prepared by above-described embodiment.
The performance indicator of electrocondution slurry prepared by 1 Examples 1 to 3 of table
| Performance indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Hardening time (min) | 30 | 30 | 30 |
| Solidification temperature (DEG C) | 135 | 135 | 200 |
| Resistance (Ω) | 103 | 76 | 58 |
| Film thickness (um) | 5.96 | 7.74 | 8.84 |
| Resistivity (Ω cm) | 3.68×10-5 | 3.53×10-5 | 3.07×10-5 |
| (6 months) are tested in anti-settling | Without sedimentation, layering | Without sedimentation, layering | Without sedimentation, layering |
As can be seen from Table 1, the present invention can be after low-temperature setting, and silver paste possesses lower resistance, ensure that charge
Effectively transmission, volume resistivity is low, while with good stability.Silk-screen printing test result show silk-screen line width it is stable,
Printed resolution is high, figure is smooth sees figure.
Organic modified bentonite produced by the present invention meets the requirement of high-performance low-temperature solidified electric slurry, not only
The Effective Regulation for realizing slurry viscosity, obtains good rheological behavior, meets high-resolution silk-screen printing requirement, Er Qieyou
The bentonitic addition of machine effectively solves the decentralized stable problem of low viscosity resin carrier and silver powder particles, is starched with traditional printing electronics
Material is compared, and organobentonite enhances system powder inside electrical charges between particles repulsion and space stability ultimate load so that superfine powder
Somaplasm material has good stably dispersing performance, and caking, sedimentation and layering are not susceptible in storing process, and printing process pattern causes
It is close full, bubble-free, stomata.After electric slurry solidification, organobentonite contributes to conductive powder body interface to overlap, and realizes efficient
Conductive path, conductive film layer have good electric property.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of by surfactant-modified obtained method for preparing organobentonite, it is characterised in that walked containing following technique
Suddenly：
(1) reaction bulb is taken, 8~10 parts of two or more surfactants are added in 10~15 times of deionized waters,
Mixed surfactants solutions are made, takes another reaction bulb, 5~8 parts of Na base bentonites is added to 10~15 times of deionization
In water, bentonite suspension is made in 50~60 DEG C of high speed dispersions of constant temperature, is warming up to 60~70 DEG C and slowly adds under stirring conditions
Enter prepared surfactant solution, 2~3h of high speed dispersion, makes it fully react under high speed dispersor, reuses ultrasound
Wavelength-division dissipates 3~6h, is put into centrifugation in centrifuge；
(2) the organobentonite ultrasonic washing 4~5 times of synthesis is finally filtered into separation, in 70 DEG C of baking ovens with deionized water
Decompression drying ground 100 mesh ultrasound filtrations sieve, the organobentonite containing surfactant is made.
2. a kind of surfactant-modified obtained organobentonite according to claim 1, which is characterized in that the surface
Activating agent is quaternary cationics, and in 10~20 ranges, molecular characterization is main carbochain C atom numbers
[(CH3)3NR]+X-Or [(CH3)2NR2]+X-Or SiX3R, wherein R represent alkyl, and X represents halogens, such as tetradecyl trimethyl
Ammonium chloride, tetradecyltrimethylammonium bromide, cetyl trimethylammonium bromide, octadecyltrimethylammonium chloride or 18
Alkyltrichlorosilanes.
3. a kind of preparation method containing organobentonite low-temperature solidified silver paste, it is characterised in that：Silver paste is by mass percentage
Following each raw material composition：1~5wt%'s utilizes surfactant-modified obtained organobentonite, the silver of 35~65wt%
The organic carrier of powder and 34~60wt%, the silver powder is by one or both of sheet, spherical silver powder, the model of flake silver powder
Enclose 2.4~4.0g/cm of tap density3, 4.5~6.7um of average grain diameter, scaling loss ＜ 1%, 1.5~2.5m of specific surface area2/ g, it is spherical
4.1~5.0g/cm of range tap density of silver powder3, 0.5~1.4um of average grain diameter, scaling loss ＜ 0.5%, specific surface area 0.8~
1.0m2/ g,
Organic carrier and organic modified bentonite are slurried using double planetary mixer premixing, the stirring infiltration 2 in dispersion machine
~5h, then silver powder and premix centrotheca are disperseed using three-roll grinder, until slurry fineness is less than 6 μm, finally decompression is de-
Bubble obtains a kind of high-performance low-temperature solidified silver paste made from organic modified bentonite.
4. a kind of preparation method containing organobentonite low-temperature solidified silver paste according to claim 3, which is characterized in that
The surfactant-modified obtained method for preparing organobentonite contains following processing step：
(1) reaction bulb is taken, 8~10 parts of two or more surfactants are added in 10~15 times of deionized waters,
Mixed surfactants solutions are made, takes another reaction bulb, 5~8 parts of Na base bentonites is added to 10~15 times of deionization
In water, bentonite suspension is made in 50~60 DEG C of high speed dispersions of constant temperature, is warming up to 60~70 DEG C and slowly adds under stirring conditions
Enter prepared surfactant solution, 2~3h of high speed dispersion, makes it fully react under high speed dispersor, reuses ultrasound
Wavelength-division dissipates 3~6h, is put into centrifugation in centrifuge；
(2) the organobentonite ultrasonic washing 4~5 times of synthesis is finally filtered into separation, in 70 DEG C of baking ovens with deionized water
Decompression drying ground 100 mesh ultrasound filtrations sieve, the organobentonite containing surfactant is made.
5. a kind of surfactant-modified obtained organobentonite according to claim 4, which is characterized in that the surface
Activating agent is quaternary cationics, and in 10~20 ranges, molecular characterization is main carbochain C atom numbers
[(CH3)3NR]+X-Or [(CH3)2NR2]+X-Or SiX3R, wherein R represent alkyl, and X represents halogens, such as tetradecyl trimethyl
Ammonium chloride, tetradecyltrimethylammonium bromide, cetyl trimethylammonium bromide, octadecyltrimethylammonium chloride or 18
Alkyltrichlorosilanes.
6. a kind of preparation method containing organobentonite low-temperature solidified silver paste according to claim 3, which is characterized in that
The preparation of the organic carrier includes the following steps：
Resin is dissolved in organic solvent, 70 DEG C of stirring in water bath of constant temperature, it is to be dissolved completely after be down to room temperature, add curing agent, it is high
Disperse 40min under rotating speed and organic carrier is made.
7. a kind of preparation method and application containing organobentonite low-temperature solidified silver paste according to claim 3, special
Sign is.
8. a kind of preparation method containing organobentonite low-temperature solidified silver paste according to claim 3, which is characterized in that institute
The resin stated includes one or more of epoxy resin, vinyl chloride-vinyl acetate resin, polyester resin, polyurethane, acrylic resin composition.
9. a kind of preparation method containing organobentonite low-temperature solidified silver paste according to claim 3, which is characterized in that institute
It is isophorone, DBE, dimethylformamide, butyl acetate, dimethyl glutarate, hexanedioic acid to state organic solvent
One or more kinds of mixed solvents of dimethyl ester, t-butyl methyl ether.
10. a kind of preparation method containing organobentonite low-temperature solidified silver paste according to claim 3, feature exist
In the curing agent is blocked isocyanate either dicyandiamide or imidazoles, and wherein blocked isocyanate unseals temperature
It is 110~135 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109645986A (en) * | 2018-11-30 | 2019-04-19 | 昆明贵金属研究所 | A kind of flexible biological electrode low-temperature solidified silver/chlorination silver paste and preparation method thereof |
| CN110136863A (en) * | 2019-04-29 | 2019-08-16 | 南通天盛新能源股份有限公司 | A kind of low-temperature conductive silver paste and preparation method thereof for HIT solar battery |
| CN112735629A (en) * | 2020-12-01 | 2021-04-30 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Low-temperature polymer conductive silver paste with low silver content and preparation method thereof |
| CN112735628A (en) * | 2020-12-01 | 2021-04-30 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Low-temperature polymer conductive silver paste and preparation method thereof |
| CN113903497A (en) * | 2021-12-09 | 2022-01-07 | 西安宏星电子浆料科技股份有限公司 | Isolation medium slurry and preparation method thereof |
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| CN105632588A (en) * | 2016-02-22 | 2016-06-01 | 昆山海斯电子有限公司 | High-conductivity silver paste and preparation method thereof |
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| JP2004039379A (en) * | 2002-07-02 | 2004-02-05 | Sumitomo Electric Ind Ltd | Conductive paste, conductive membrane, and manufacturing method of conductive membrane |
| CN102295295A (en) * | 2011-06-13 | 2011-12-28 | 中国石油化工股份有限公司 | Method for preparing organoclay by using composite organic modifier |
| CN104332214A (en) * | 2014-10-28 | 2015-02-04 | 深圳市思迈科新材料有限公司 | Low-temperature curing conductive silver paste and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109645986A (en) * | 2018-11-30 | 2019-04-19 | 昆明贵金属研究所 | A kind of flexible biological electrode low-temperature solidified silver/chlorination silver paste and preparation method thereof |
| CN110136863A (en) * | 2019-04-29 | 2019-08-16 | 南通天盛新能源股份有限公司 | A kind of low-temperature conductive silver paste and preparation method thereof for HIT solar battery |
| CN110136863B (en) * | 2019-04-29 | 2020-09-15 | 南通天盛新能源股份有限公司 | Low-temperature conductive silver paste for HIT solar cell and preparation method thereof |
| CN112735629A (en) * | 2020-12-01 | 2021-04-30 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Low-temperature polymer conductive silver paste with low silver content and preparation method thereof |
| CN112735628A (en) * | 2020-12-01 | 2021-04-30 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Low-temperature polymer conductive silver paste and preparation method thereof |
| CN113903497A (en) * | 2021-12-09 | 2022-01-07 | 西安宏星电子浆料科技股份有限公司 | Isolation medium slurry and preparation method thereof |
| CN113903497B (en) * | 2021-12-09 | 2022-03-08 | 西安宏星电子浆料科技股份有限公司 | Isolation medium slurry and preparation method thereof |
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