Graphene-based electrocondution slurry and preparation method thereofTechnical field
The present invention relates to electrocondution slurry technical field, specially a kind of graphene-based electrocondution slurry and preparation method thereof.
Background technique
Electrocondution slurry is also known as conducting resinl, is the mixture of precious metal powder and base metal powder, glass powder and synthetic resin, whereinIt is can be made into after addition solvent except material or graphite-like object, the partial size of metal powder are about 1-2um, it is being developed to there is partial size to receive for tensThe slurry of the Ultramicro-powder of rice, these slurries are coated on position required for substrate with silk-screen printing or other methods, thenTemperature be 400-1000 DEG C at be burnt into electric conductor, be mainly used for the electrodes such as wiring and the ceramic capacitor of thick film integrated circuit withAnd the lead of hydrid integrated circuit, it is core and NMP as solvent that graphene-based electrocondution slurry, which is using graphene, adds a certain amount of carbonThe graphene composite conductive slurry of black class material, using the excellent electric conductivity of graphene, thermal conductivity and flexible flake structure, with heightThe carbon black of structure mixes according to a certain percentage, and efficient 3 D stereo conductive network can be formed on entire material system, canThe internal resistance of cell is reduced, its charge-discharge magnification and cycle performance are improved.
Traditional graphene-based electrocondution slurry preparation method complex circuit, for preparing the more demanding of environment in operation,Some need high temperature and high pressure environment, some need uses inert gas shielding, and whole preparation process is all relatively complicated, so that systemStandby cost greatly improves, thus is difficult to promote, and user is rather worried to this, so propose a kind of graphene-based electrocondution slurryAnd preparation method thereof.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides graphene-based electrocondution slurries, have the advantages that preparation cost is cheap, solutionIt has determined traditional graphene-based electrocondution slurry preparation method complex circuit, for preparing the more demanding of environment in operation, has hadHigh temperature and high pressure environment is needed, some need uses inert gas shielding, and whole preparation process is all relatively complicated, so that preparationCost greatly improves, thus is difficult to promote, user's problem rather worried to this.
(2) technical solution
To realize the cheap purpose of above-mentioned preparation cost, the invention provides the following technical scheme: graphene-based electrocondution slurry, includingThe raw material of following number: 40-60 parts of graphene, single 15-25 parts of Tryfac 5573,20-30 parts of resin, 80-100 parts of solvent,10-20 parts of dispersing agent, 5-7 parts of carbon nanotube, 50-60 parts of ammonium hydroxide and 30-40 parts of filler.
Preferably, described resin 20-30 parts are epoxy resin, polyurethane resin, carbamide resin, acrylic resin, alkydThe combination of one or more of moon purport, silicone resin, chlorinated resin, furane resins and polyester resin is set, described resin 20-30 parts areParticle of the diameter less than one centimetre.
Preferably, ammonium hydroxide 50-60 parts of the concentration is 30 percent, and solvent 80-100 parts of the concentration is percentage40.
The preparation method of graphene-based electrocondution slurry, comprising the following steps:
1) 80-100 parts of solvent are put into container with 50-60 parts of ammonium hydroxide and are mixed, stir 20 with 80 rpms of frequencyMinute, single 15-25 parts of Tryfac 5573 is added after stirring, 80 degrees Celsius is heated to, with 60 rpms of frequencyRate stirs 15 minutes, and mixed liquor 1 is made；
2) water grinding will be added in 40-60 parts of investment disperse mills of graphene, graphene suspension is obtained, in graphene suspensionIt 10-20 parts and carbon nanotube 5-7 parts of middle addition dispersing agent, is shaken one hour using ultrasonic oscillation device, mixed liquor 2 is made, it willMixed liquor 2 dries, and 50 degrees Celsius of dryings are arranged using drying machine, obtain stock 1；
3) filler 30-40 parts, 5-7 parts of carbon nanotube and 20-30 parts of resin will be added in mixed liquor 1, with 100 rpmsFrequency stirs 30 minutes, and mixed liquor 1 and stock 1 is added, and is shaken ten minutes using ultrasonic oscillation device, dense using thickenerContracting, setting thickening temperature take out after being 60 degrees Celsius, two hours to get required graphene-based electrocondution slurry.
Preferably, the revolving speed of disperse mill described in step 2 is 21000rmp, after the graphene 40-60 parts of grindingsDiameter is less than 0. 3 millimeters.
Preferably, described in step 2 in graphene 40-60 parts plus water, water is distilled water, and the ratio of graphene and water is 1.2:2.5。
(3) beneficial effect
Compared with prior art, the present invention provides graphene-based electrocondution slurry and preparation method thereof, have it is following the utility model has the advantages that
1, graphene-based electrocondution slurry and preparation method thereof, by being put into container with ammonium hydroxide 50-60 parts for 80-100 parts of solventInterior mixing is stirred 20 minutes with 80 rpms of frequency, and single 15-25 parts of Tryfac 5573 is added after stirring,80 degrees Celsius are heated to, is stirred 15 minutes with 60 rpms of frequency, mixed liquor 1 is made and by graphene 40-60In part investment disperse mill plus water is ground, and obtains graphene suspension, dispersing agent 10-20 parts is added in graphene suspensionWith 5-7 parts of carbon nanotube, using ultrasonic oscillation device shake one hour, be made mixed liquor 2, mixed liquor 2 is dried, drying is used50 degrees Celsius of dryings are arranged in machine, obtain stock 1, and user prepares institute when preparing graphene-based electrocondution slurry using this methodThe equipment used is simple and easy to get, and material price is cheap, this allows for preparation cost and substantially reduces, and is conducive to promote, eliminating makesThe worry of user, the use for the person of being convenient to use.
2, graphene-based electrocondution slurry and preparation method thereof, by that filler 30-40 parts of addition, carbon will be received in mixed liquor 1It 5-7 parts and resin 20-30 parts of mitron, is stirred 30 minutes with 100 rpms of frequency, mixed liquor 1 and stock 1 is added, makesIt is shaken ten minutes with ultrasonic oscillation device, is concentrated using thickener, setting thickening temperature takes after being 60 degrees Celsius, two hoursOut to get required graphene-based electrocondution slurry, thickener concentration removes the moisture in slurry, graphene-based electrocondution slurry obtainedConductive effect is good, and using effect is preferable, has further facilitated the use of user.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouchedIt states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present inventionIn embodiment, every other implementation obtained by those of ordinary skill in the art without making creative effortsExample, shall fall within the protection scope of the present invention.
Embodiment one: graphene-based electrocondution slurry, the raw material including following number: 50 parts of graphene, single lauryl phosphoric acid20 parts of ester, 25 parts of resin, 80 parts of solvent, 15 parts of dispersing agent, 6 parts of carbon nanotube, 55 parts of ammonium hydroxide and 35 parts of filler.
25 parts of resin for epoxy resin, polyurethane resin, carbamide resin, acrylic resin, alkyd tree moon purport, silicone resin,The combination of one or more of chlorinated resin, furane resins and polyester resin, 25 parts of resin are particle of the diameter less than one centimetre.
The concentration that 55 parts of ammonium hydroxide is 30 percent, and the concentration that 80 parts of solvent is 40 percent.
The preparation method of graphene-based electrocondution slurry, comprising the following steps:
1) 80 parts of solvent are put into container with 55 parts of ammonium hydroxide and are mixed, stirred 20 minutes, stirred with 80 rpms of frequencySingle 20 parts of Tryfac 5573 is added after mixing, is heated to 80 degrees Celsius, stirs 15 with 60 rpms of frequencyMinute, mixed liquor 1 is made；
2) water grinding will be added in 50 parts of investment disperse mills of graphene, graphene suspension is obtained, in graphene suspension15 parts and 6 parts of carbon nanotube of dispersing agent are added, is shaken one hour using ultrasonic oscillation device, mixed liquor 2 is made, by mixed liquor 2Drying is arranged 50 degrees Celsius of dryings using drying machine, obtains stock 1；
3) 35 parts of filler, 6 parts of carbon nanotube and 25 parts of resin will be added in mixed liquor 1, stirred with 100 rpms of frequency30 minutes, mixed liquor 1 and stock 1 is added, is shaken ten minutes using ultrasonic oscillation device, is concentrated using thickener, is arranged denseContracting temperature is taken out after being 60 degrees Celsius, two hours to get required graphene-based electrocondution slurry.
The revolving speed of step 2 disperse mill is 21000rmp, and the diameter after 50 parts of graphene grindings is less than 0. 3 millimeters.
In 50 parts of step 2 graphene plus water, water is distilled water, and the ratio of graphene and water is 1.2:2.5.
Revolving speed is that the disperse mill of 21000rmp can smash graphene, and grinding effect is preferable.
Embodiment two: graphene-based electrocondution slurry, the raw material including following number: 40 parts of graphene, single lauryl phosphoric acid15 parts of ester, 20 parts of resin, 80 parts of solvent, 10 parts of dispersing agent, 5 parts of carbon nanotube, 50 parts of ammonium hydroxide and 30 parts of filler.
20 parts of resin for epoxy resin, polyurethane resin, carbamide resin, acrylic resin, alkyd tree moon purport, silicone resin,The combination of one or more of chlorinated resin, furane resins and polyester resin, 20 parts of resin are particle of the diameter less than one centimetre.
The concentration that 50 parts of ammonium hydroxide is 30 percent, and the concentration that 80 parts of solvent is 40 percent.
The preparation method of graphene-based electrocondution slurry, comprising the following steps:
1) 80 parts of solvent are put into container with 50 parts of ammonium hydroxide and are mixed, stirred 20 minutes, stirred with 80 rpms of frequencySingle 15 parts of Tryfac 5573 is added after mixing, is heated to 80 degrees Celsius, stirs 15 with 60 rpms of frequencyMinute, mixed liquor 1 is made；
2) water grinding will be added in 40 parts of investment disperse mills of graphene, graphene suspension is obtained, in graphene suspension10 parts and 5 parts of carbon nanotube of dispersing agent are added, is shaken one hour using ultrasonic oscillation device, mixed liquor 2 is made, by mixed liquor 2Drying is arranged 50 degrees Celsius of dryings using drying machine, obtains stock 1；
3) 30 parts of filler, 5 parts of carbon nanotube and 20 parts of resin will be added in mixed liquor 1, stirred with 100 rpms of frequency30 minutes, mixed liquor 1 and stock 1 is added, is shaken ten minutes using ultrasonic oscillation device, is concentrated using thickener, is arranged denseContracting temperature is taken out after being 60 degrees Celsius, two hours to get required graphene-based electrocondution slurry.
The revolving speed of step 2 disperse mill is 21000rmp, and the diameter after 40 parts of graphene grindings is less than 0. 3 millimeters.
In 40 parts of step 2 graphene plus water, water is distilled water, and the ratio of graphene and water is 1.2:2.5.
Distilled water itself is free of or few impurity, and impurity will not be generated in late phase reaction, influences normal reaction, reduces waveTake.
Embodiment three: graphene-based electrocondution slurry, the raw material including following number: 60 parts of graphene, single lauryl phosphoric acid25 parts of ester, 30 parts of resin, 100 parts of solvent, 20 parts of dispersing agent, 7 parts of carbon nanotube, 60 parts of ammonium hydroxide and 40 parts of filler.
30 parts of resin for epoxy resin, polyurethane resin, carbamide resin, acrylic resin, alkyd tree moon purport, silicone resin,The combination of one or more of chlorinated resin, furane resins and polyester resin, 30 parts of resin are particle of the diameter less than one centimetre.
The concentration that 60 parts of ammonium hydroxide is 30 percent, and the concentration that 100 parts of solvent is 40 percent.
The preparation method of graphene-based electrocondution slurry, comprising the following steps:
1) 100 parts of solvent are put into container with 60 parts of ammonium hydroxide and are mixed, stirred 20 minutes, stirred with 80 rpms of frequencySingle 25 parts of Tryfac 5573 is added after mixing, is heated to 80 degrees Celsius, stirs 15 with 60 rpms of frequencyMinute, mixed liquor 1 is made；
2) water grinding will be added in 60 parts of investment disperse mills of graphene, graphene suspension is obtained, in graphene suspension20 parts and 7 parts of carbon nanotube of dispersing agent are added, is shaken one hour using ultrasonic oscillation device, mixed liquor 2 is made, by mixed liquor 2Drying is arranged 50 degrees Celsius of dryings using drying machine, obtains stock 1；
3) 40 parts of filler, 7 parts of carbon nanotube and 30 parts of resin will be added in mixed liquor 1, stirred with 100 rpms of frequency30 minutes, mixed liquor 1 and stock 1 is added, is shaken ten minutes using ultrasonic oscillation device, is concentrated using thickener, is arranged denseContracting temperature is taken out after being 60 degrees Celsius, two hours to get required graphene-based electrocondution slurry.
The revolving speed of step 2 disperse mill is 21000rmp, and the diameter after 60 parts of graphene grindings is less than 0. 3 millimeters.
In 60 parts of step 2 graphene plus water, water is distilled water, and the ratio of graphene and water is 1.2:2.5.
100 parts of solvent are put into container with 60 parts of ammonium hydroxide and is mixed, is stirred 20 minutes with 80 rpms of frequency,Single 25 parts of Tryfac 5573 is added after stirring, is heated to 80 degrees Celsius, stirs ten with 60 rpms of frequencyIt five minutes, is uniformly mixed between raw material, clear route.
The beneficial effects of the present invention are: the graphene-based electrocondution slurry and preparation method thereof, by by 80-100 parts of solventIt is put into container and mixes with 50-60 parts of ammonium hydroxide, stirred 20 minutes with 80 rpms of frequency, added after stirring single15-25 parts of Tryfac 5573,80 degrees Celsius are heated to, is stirred 15 minutes with 60 rpms of frequency, is made mixedIt closes liquid 1 and water grinding will be added in 40-60 parts of investment disperse mills of graphene, obtain graphene suspension, it is suspended in grapheneDispersing agent 10-20 parts and carbon nanotube 5-7 parts is added in liquid, is shaken one hour using ultrasonic oscillation device, mixed liquor 2 is made,Mixed liquor 2 is dried, 50 degrees Celsius of dryings are set using drying machine, obtain stock 1, user is preparing graphite using this methodWhen alkenyl electrocondution slurry, equipment used in preparation is simple and easy to get, and material price is cheap, this allows for preparation cost and drops significantlyIt is low, being conducive to promote, eliminating the worry of user, the use for the person of being convenient to use, by filler will be added in mixed liquor 130-40 parts, 5-7 parts of carbon nanotube and 20-30 parts of resin, are stirred 30 minutes with 100 rpms of frequency, and mixing is addedLiquid 1 and stock 1, are shaken ten minutes using ultrasonic oscillation device, are concentrated using thickener, and setting thickening temperature is 60 CelsiusDegree is taken out after two hours to get required graphene-based electrocondution slurry, and thickener concentration removes the moisture in slurry, stone obtainedMertenyl electrocondution slurry conductive effect is good, and using effect is preferable, has further facilitated the use of user, solves traditional stoneMertenyl electrocondution slurry preparation method complex circuit, for preparing the more demanding of environment, some need high temperature and pressure in operationEnvironment, some need uses inert gas shielding, and whole preparation process is all relatively complicated, so that the cost of preparation mentions significantlyHeight, thus be difficult to promote, user's problem rather worried to this.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be withA variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understandingAnd modification, the scope of the present invention is defined by the appended.