CN107393626A - A kind of hot method powdery electric slurry and preparation method thereof - Google Patents
A kind of hot method powdery electric slurry and preparation method thereof Download PDFInfo
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- CN107393626A CN107393626A CN201710498447.XA CN201710498447A CN107393626A CN 107393626 A CN107393626 A CN 107393626A CN 201710498447 A CN201710498447 A CN 201710498447A CN 107393626 A CN107393626 A CN 107393626A
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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
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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
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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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
Abstract
It is composed of the following components according to mass percent the invention discloses a kind of hot method powdery electric slurry：Conductive phase is 85.5%~97.5%, conduction enhancing phase 0.5%~5%, binding agent 0.5%~8.0%, catalyst 0.1~0.8%, lubricant 0.1~0.5%, adds up to 100%.The invention also discloses the preparation method of this kind of hot method powdery electric slurry.The hot method powdery electric slurry of the present invention, cost is more cheap, preparation technology is simple, laser sintered straight forming is utilized during 3D printing, avoid in method for printing screen and change the rheological equationm of state of slurry and viscosity using organic carrier, and then method on a ceramic substrate is printed, reduce influence of the organic carrier to size performance.
Description
Technical field
The invention belongs to electric slurry field, is related to a kind of hot method powdery electric slurry, the invention further relates to this kind of hot method
The preparation method of powdery electric slurry.
Background technology
Electric slurry is to integrate metallurgy, material, chemical industry, the electronic functional material of electronic technology, with electronics industry
It is integrated developed rapidly with digitlization, Information And Communication industry, electric slurry is conductive compared to traditional circuit equipment
Good, high efficiency, advanced technology, it is applied widely the features such as, be widely used in various fields.
Electric slurry is made up of conductive phase, binding agent, organic carrier and other additives, its performance largely by
Conductive phase determines, but can also be influenceed simultaneously by binding agent, organic carrier, sintering process etc. are many.Organic carrier is dissolving
In the polymer solution of organic solvent, its function is that metal dust and binding agent and the mixing of other solid powders are dispersed into cream
Shape slurry, the rheological behavior of slurry is can control, the viscosity of slurry is adjusted, to be printed on ceramics with method for printing screen
On substrate.With organic carrier, some existing defects limit the application of electric slurry to electric slurry in use, directly affect
Electric conductivity, mobility, volatility and bonding strength performance of slurry etc..
China Electronics Components Industry industry to the demand of electric slurry kind quality and quantity considerably long in the period of in rely on
External a large amount of imports, therefore development of practical is strong, the electric slurry of high-performance, low cost, accelerates China's electric slurry development step
Cut down, turn into a technical problem for being badly in need of solving.
The content of the invention
It is an object of the invention to provide a kind of hot method powdery electric slurry, solve prior art electric slurry and employed
The problem of airborne body, organic carrier are bigger to electric slurry performance impact.
It is a further object of the present invention to provide the preparation method of this kind of hot method powdery electric slurry, solve prior art and exist
The problem of organic carrier is big to electric slurry performance impact in preparation process.
The technical scheme is that a kind of hot method powdery electric slurry, composed of the following components according to mass percent：
Conductive phase 85.5%~97.5%, conduction enhancing phase 0.5%~5%, binding agent 0.5%~8.0%, catalyst 0.1~
0.8%, lubricant 0.1~0.5%, add up to 100%.
Another technical scheme that the present invention uses is a kind of preparation method of hot method powdery electric slurry, according to following step
It is rapid to implement：
Preliminary step：Following components is weighed according to mass percent：Conductive phase 85.5%~97.5%, conduction enhancing phase
0.5%~5%, binding agent 0.5%~8.0%, catalyst 0.1~0.8%, lubricant 0.1~0.5%, add up to 100%；
Step 1, conductive phase metal dust is surface-treated, removes sull, obtain the clean proof gold in surface
Belong to powder；
Step 2, decentralized processing is mutually carried out to conduction enhancing, then obtain finely dispersed powder after drying；
The conductive enhancing that step 3, the conductive phase that step 1 is obtained and step 2 obtain is mixed and stirred, and is heated to certain
After temperature, binding agent is added, obtains hybrid conductive phase；
After step 4, to be bonded dose of complete cladding hybrid conductive phase, temperature is reduced, is eventually adding catalyst and lubricant, and
Make it well mixed, obtain hot method powdery electric slurry.
The invention has the advantages that including following aspect：
1) conductive phase in the present invention is using one of micron-size spherical metal dust copper, silver, gold, aluminium, nickel, nano-level conducting
Enhancing mutually mutually has big ratio surface from one of graphene, CNT, onion carbon, nano-silver thread, nano-level conducting enhancing
Long-pending and excellent electric conductivity, both can be very good to contact, and improve the uniformity of slurry, make the electric conductivity of slurry more
It is good.
2) preparation method of the present invention, raw material sources are extensive, and cost is cheap, and preparation technology is relatively simple.
3) the hot method powdery electric slurry for being prepared the present invention using 3D printing technique carries out laser sintering and moulding, avoids
Electric slurry performance is had an impact using organic carrier, and saves raw material, is advantageous to environmental protection.
Embodiment
With reference to embodiment, the present invention is described in detail.
The hot method powdery electric slurry of the present invention, it is composed of the following components according to mass percent：Conductive phase 85.5%~
97.5%, conduction enhancing phase 0.5%~5%, binding agent 0.5%~8.0%, catalyst 0.1~0.8%, lubricant 0.1~
0.5%, add up to 100%；Wherein, conductive phase is from one of micro-sized metal powder copper, silver, gold, aluminium, nickel, conduction enhancing phase
From one of graphene, CNT, onion carbon, nano-silver thread, from epoxy resin, (the main trade mark is bisphenol A-type to binding agent
One of epoxy E-44, E-51, E-55), catalyst selects Latence catalyst aromatic polyamine, acid anhydrides, dicyandiamide and hydrazides
One of, lubricant selects one or both of calcium stearate or zinc stearate mixture.
The preparation method of the hot method powdery electric slurry of the present invention, implements according to following steps：
Preliminary step：Following components is weighed according to mass percent：Conductive phase 85.5%~97.5%, conduction enhancing phase
0.5%~5%, binding agent 0.5%~8.0%, catalyst 0.1~0.8%, lubricant 0.1~0.5%, add up to 100%；
Step 1, conductive phase metal dust is surface-treated, removes sull, obtain the clean proof gold in surface
Belong to powder,
Concretely comprise the following steps：The micro-sized metal powder that particle diameter is 1~15 μm is inserted sour in 5%~13% dilute hydrochloric acid solution
To wash, supersonic oscillations make both be uniformly dispersed, and remove the sull on surface, and surface solution is removed after standing 8~10min,
Repeat the process 3~5 times, then repeatedly washed with deionized water after metal dust is filtered until there is no hydrochloric acid smell.
Step 2, decentralized processing is mutually carried out to conduction enhancing, then obtains finely dispersed powder after drying,
Concretely comprise the following steps：Appropriate absolute ethyl alcohol is added in nano-level conducting strengthens phase, then ultrasonic wave shakes at normal temperatures
After swinging 50~70min, dispersion liquid is placed in drying box and dried, temperature control is at 50 ± 2 DEG C.
The conductive enhancing that step 3, the conductive phase that step 1 is obtained and step 2 obtain is mixed and stirred, and is heated to certain
After temperature, binding agent is added, obtains hybrid conductive phase.
Concretely comprise the following steps：The conductive phase obtained after processing and conduction enhancing are mixed, and pass through efficient batch type
Blender stirs 5~30min, until obtaining well mixed hybrid conductive phase；Under nitrogen atmosphere protection, by hybrid conductive phase
80~180 DEG C are heated to, adds epoxy resin of binder, compressed air is passed through and stirs 10~30min, make epoxy resin equal
It is even to be coated on hybrid conductive phase surface.
After step 4, to be bonded dose of complete cladding hybrid conductive phase, temperature is reduced, is eventually adding catalyst and lubricant, and
Make it well mixed, obtain hot method powdery electric slurry,
Concretely comprise the following steps：After epoxy resin evenly and completely coats hybrid conductive phase, cool 20~60 DEG C, add latent
Property catalyst, continues 5~20min of stirring；Cool again 15~50 DEG C, add the mixing of one or both of calcium stearate or zinc stearate
Thing after being passed through compressed air and stirring 3~15min, is cooled to room temperature, obtains hot method powdery electric slurry as lubricant.
The hot method powdery electric slurry of the present invention is used for 3D printing, process is as follows：
Before 3D printing, 3D models are first established, and slicing delamination is carried out to model, are exported as STL formatted files, print command
Printer head running is guided, the hot method powdery electric slurry obtained to step 4 is laser sintered, and solidification process makes resin scattered
Conductive phase bond on a ceramic substrate, electroconductive stuffing be conductive phase mutually in chain connect, it is conductive.Its whole work
Skill process includes model foundation and data processing, powdering, sintering and subsequent treatment.
During 3D printing, powder feeding piston rises, and powder-laying roller uniformly spreads the thick powder of 0.01~0.08mm on working piston
Layer, computer control the scanning track of laser beam according to STL formatted files, and sintered powder material is to form a layer.After the completion of,
Working piston declines 0.01~0.08mm thickness, powdering system work, and laser beam scans the new layer of sintering, so moved in circles again,
Until complete.It should be noted that before sintering, whole workbench need to be heated, forming process can be significantly reduced
In thermal deformation.
Embodiment 1
Preliminary step：Following components is weighed according to mass percent：Conductive phase copper 95%, conduction enhancing phase graphene
2.5%, binding agent bisphenol type epoxy E-44 are 1.5%, catalyst Latence catalyst aromatic polyamine 0.5%, lubricant
0.5%, add up to 100%；
Step 1：Copper powders as conductive phase are surface-treated, remove sull, it is clean to obtain surface
Fine copper powder.
The Micron-Sized Copper Powders Coated end that particle diameter is 1 μm is put into pickling in 5% dilute hydrochloric acid solution, supersonic oscillations make both scattered
Uniformly, remove the sull on surface, remove surface solution after standing 10min, repeat the process 3 times, then by copper powders mistake
Filter, is repeatedly washed with deionized water, until without hydrochloric acid smell.
Step 2：Decentralized processing is carried out to nano-level conducting enhancing phase graphene, then obtains finely dispersed powder after drying
End.
Appropriate absolute ethyl alcohol is added in nano-level conducting strengthens phase, then at normal temperatures after supersonic oscillations 60min, will
Dispersion liquid is placed in drying box and dried, and control temperature is at 50 DEG C.
Step 3：The conductive enhancing that the conductive phase and step 2 that step 1 is obtained obtain is mixed and stirred, and is heated to certain
After temperature, binding agent is added, obtains hybrid conductive phase.
The conductive phase obtained after processing and conduction enhancing are mixed, and stirred by efficient batch type blender
20min, until well mixed.Under nitrogen atmosphere protection, by hybrid conductive heat phase to 100 DEG C, binding agent epoxy is added
Resin, it is passed through compressed air and stirs 25min, epoxy resin is evenly coated at hybrid conductive phase surface.
Step 4：After to be bonded dose coats hybrid conductive phase completely, temperature is reduced, adds catalyst and lubricant, and make
It is well mixed, obtains hot method powdery electric slurry.
After epoxy resin evenly and completely coats hybrid conductive phase, cool 30 DEG C, add Latence catalyst, continue to stir
After mixing 10min, then cool 15 DEG C, add calcium stearate as lubricant, after being passed through compressed air and stirring 8min, be cooled to room
Temperature, obtain hot method powdery electric slurry.
The hot method powdery electric slurry of the present invention is used for 3D printing, establishes 3D models, and slicing delamination is carried out to model,
Export as STL formatted files, guiding printer head running.During work, powder feeding piston rises, and powder-laying roller is equal on working piston
Even to spread 0.01mm, computer controls the scanning track of laser beam according to STL formatted files, and sintered powder material is to form one
Layer.After the completion of, working piston declines a thickness 0.01mm, powdering system work, and laser beam scans the new layer of sintering, so followed again
Ring is reciprocal, until completing.
Embodiment 2
Preliminary step：Following components is weighed according to mass percent：Conductive phase silver 92%, conduction enhancing phase CNT
3.5%, binding agent bisphenol type epoxy E-51 are 3.5%, catalyst aromatic polyamine 0.8%, lubricant 0.2%, are added up to
100%；
Step 1：Silver powder as conductive phase is surface-treated, removes sull, it is clean to obtain surface
Fine silver powder.
The micro nanometer silver powder that particle diameter is 5 μm is put into pickling in 8% dilute hydrochloric acid solution, supersonic oscillations make both scattered
Uniformly, the sull on surface is removed, surface solution is removed after standing 9min, repeats the process 4 times, then silver powder is filtered
Repeatedly washed with deionized water afterwards until without hydrochloric acid smell.
Step 2：Decentralized processing is mutually carried out to nano-level conducting enhancing, then obtains finely dispersed powder after drying.
Appropriate absolute ethyl alcohol is added in nano-level conducting strengthens phase, then at normal temperatures after supersonic oscillations 60min, will
Dispersion liquid is placed in drying box and dried, and control temperature is at 52 DEG C.
Step 3：The conductive enhancing that the conductive phase and step 2 that step 1 is obtained obtain is mixed and stirred, and is heated to certain
After temperature, binding agent is added, obtains hybrid conductive phase.
The conductive phase obtained after processing and conduction enhancing are mixed, and stirred by efficient batch type blender
15min, until well mixed.Under nitrogen atmosphere protection, by hybrid conductive heat phase to 80 DEG C, binding agent asphalt mixtures modified by epoxy resin is added
Fat, it is passed through compressed air and stirs 20min, epoxy resin is evenly coated at hybrid conductive phase surface.
Step 4：After to be bonded dose coats hybrid conductive phase completely, temperature is reduced, adds catalyst and lubricant, and make
It is well mixed, obtains hot method powdery electric slurry.
After epoxy resin evenly and completely coats hybrid conductive phase, cool 40 DEG C, add Latence catalyst, continue to stir
Mix 15min, cool 20 DEG C, add zinc stearate as lubricant, after being passed through compressed air and stirring 10min, be cooled to room temperature,
Obtain hot method powdery electric slurry.
The hot method powdery electric slurry of the present invention is used for 3D printing, establishes 3D models, and slicing delamination is carried out to model,
Export as STL formatted files, print command guiding printer head running.During work, powder feeding piston rises, and powder-laying roller is working
Uniformly spread 0.05mm on piston, computer controls the scanning track of laser beam according to STL formatted files, sintered powder material with
Form a layer.After the completion of, working piston declines a thickness 0.05mm, and powdering system work, it is new that laser beam scans sintering again
Layer, so moves in circles, until completing.
Embodiment 3
Preliminary step：Following components is weighed according to mass percent：Conductive phase gold 90%, conduction enhancing phase onion carbon
3.5%, binding agent bisphenol type epoxy E-55 are 5.5%, catalyst acid anhydrides 0.6%, lubricant 0.4%, add up to 100%；
Step 1：Bronze end as conductive phase is surface-treated, removes sull, it is clean to obtain surface
Proof gold powder.
The micron order bronze end that particle diameter is 10 μm is put into pickling in 10% dilute hydrochloric acid solution, supersonic oscillations divide both
The sull for uniformly, removing surface is dissipated, surface solution is removed after standing 10min, repeats the process 5 times, then bronze is last
Repeatedly washed until without hydrochloric acid smell with deionized water after filtering.
Step 2：Decentralized processing is mutually carried out to nano-level conducting enhancing, then obtains finely dispersed powder after drying.
Appropriate absolute ethyl alcohol is added in nano-level conducting strengthens phase, then at normal temperatures after supersonic oscillations 70min, will
Dispersion liquid is placed in drying box and dried, and control temperature is at 49 DEG C.
Step 3：The conductive enhancing that the conductive phase and step 2 that step 1 is obtained obtain is mixed and stirred, and is heated to certain
After temperature, binding agent is added, obtains hybrid conductive phase.
The conductive phase obtained after processing and conduction enhancing are mixed, and stirred by efficient batch type blender
30min, until well mixed.Under nitrogen atmosphere protection, by hybrid conductive heat phase to 120 DEG C, binding agent epoxy is added
Resin, it is passed through compressed air and stirs 30min, epoxy resin is evenly coated at hybrid conductive phase surface.
Step 4：After to be bonded dose coats hybrid conductive phase completely, temperature is reduced, adds catalyst and lubricant, and make
It is well mixed, obtains hot method powdery electric slurry.
After epoxy resin evenly and completely coats hybrid conductive phase, cool 35 DEG C, add Latence catalyst, continue to stir
Mix 15min, cool 25 DEG C, add zinc stearate as lubricant, after being passed through compressed air and stirring 15min, be cooled to room temperature,
Obtain hot method powdery electric slurry.
The hot method powdery electric slurry of the present invention is used for 3D printing, establishes 3D models, and slicing delamination is carried out to model,
Export as STL formatted files, print command guiding printer head running.During work, powder feeding piston rises, and powder-laying roller is working
Uniformly spread 0.08mm on piston, computer controls the scanning track of laser beam according to STL formatted files, sintered powder material with
Form a layer.After the completion of, working piston declines a thickness 0.08mm, and powdering system work, it is new that laser beam scans sintering again
Layer, so moves in circles, until completing.
Embodiment 4
Preliminary step：Following components is weighed according to mass percent：Conductive phase aluminium 88%, conduction enhancing phase nano-silver thread
4.5%, binding agent bisphenol type epoxy E-44 are 6.5%, catalyst dicyandiamide 0.7%, lubricant 0.3%, add up to 100%；
Step 1：Aluminium powder as conductive phase is surface-treated, removes sull, it is clean to obtain surface
Pure aluminium powder.
The micron order aluminium powder that particle diameter is 15 μm is put into pickling in 10% dilute hydrochloric acid solution, supersonic oscillations divide both
Dissipate uniform, remove the sull on surface, remove surface solution after standing 10min, repeat the process 4 times, then by aluminium powder
Repeatedly washed until without hydrochloric acid smell with deionized water after filtering.
Step 2：Decentralized processing is mutually carried out to nano-level conducting enhancing, then obtains finely dispersed powder after drying.
Appropriate absolute ethyl alcohol is added in nano-level conducting strengthens phase, then at normal temperatures after supersonic oscillations 70min, will
Dispersion liquid is placed in drying box and dried, and control temperature is at 50 DEG C.
Step 3：The conductive enhancing that the conductive phase and step 2 that step 1 is obtained obtain is mixed and stirred, and is heated to certain
After temperature, binding agent is added, obtains hybrid conductive phase.
The conductive phase obtained after processing and conduction enhancing are mixed, and stirred by efficient batch type blender
30min, until well mixed.Under nitrogen atmosphere protection, by hybrid conductive heat phase to 120 DEG C, binding agent epoxy is added
Resin, it is passed through compressed air and stirs 30min, epoxy resin is evenly coated at hybrid conductive phase surface.
Step 4：After to be bonded dose coats hybrid conductive phase completely, temperature is reduced, adds catalyst and lubricant, and make
It is well mixed, obtains hot method powdery electric slurry.
After epoxy resin evenly and completely coats hybrid conductive phase, cool 35 DEG C, add Latence catalyst dicyandiamide,
Continue to stir 15min, cool 25 DEG C, add calcium stearate with both zinc stearates mixture (according to 1:2 mass ratio mixing)
As lubricant, after being passed through compressed air and stirring 15min, room temperature is cooled to, obtains hot method powdery electric slurry.
The hot method powdery electric slurry of the present invention is used for 3D printing, establishes 3D models, and slicing delamination is carried out to model,
Export as STL formatted files, print command guiding printer head running.During work, powder feeding piston rises, and powder-laying roller is working
Uniformly spread 0.07mm on piston, computer controls the scanning track of laser beam according to STL formatted files, sintered powder material with
Form a layer.After the completion of, working piston declines a thickness 0.07mm, and powdering system work, it is new that laser beam scans sintering again
Layer, so moves in circles, until completing.
Embodiment 5
Preliminary step：Following components is weighed according to mass percent：Conductive phase nickel 86%, conduction enhancing phase graphene 5%,
Epoxy resin of binder bisphenol type epoxy E-51 is 8%, catalyst hydrazides 0.6%, lubricant 0.4%, adds up to 100%；
Step 1：Nickel by powder as conductive phase is surface-treated, removes sull, it is clean to obtain surface
Pure nickel powder.
The micrometer nickel powder that particle diameter is 12 μm is put into pickling in 10% dilute hydrochloric acid solution, supersonic oscillations divide both
Dissipate uniform, remove the sull on surface, remove surface solution after standing 10min, repeat the process 4 times, then by nickel by powder
Repeatedly washed until without hydrochloric acid smell with deionized water after filtering.
Step 2：Decentralized processing is mutually carried out to nano-level conducting enhancing, then obtains finely dispersed powder after drying.
Appropriate absolute ethyl alcohol is added in nano-level conducting strengthens phase, then at normal temperatures after supersonic oscillations 70min, will
Dispersion liquid is placed in drying box and dried, and control temperature is at 49 DEG C.
Step 3：The conductive enhancing that the conductive phase and step 2 that step 1 is obtained obtain is mixed and stirred, and is heated to certain
After temperature, binding agent is added, obtains hybrid conductive phase.
The conductive phase obtained after processing and conduction enhancing are mixed, and stirred by efficient batch type blender
30min, until well mixed.Under nitrogen atmosphere protection, by hybrid conductive heat phase to 120 DEG C, binding agent epoxy is added
Resin, it is passed through compressed air and stirs 30min, epoxy resin is evenly coated at hybrid conductive phase surface.
Step 4：After to be bonded dose coats hybrid conductive phase completely, temperature is reduced, adds catalyst and lubricant, and make
It is well mixed, obtains hot method powdery electric slurry.
After epoxy resin evenly and completely coats hybrid conductive phase, cool 35 DEG C, add Latence catalyst hydrazides, after
Continuous stirring 15min, cools 25 DEG C, adds calcium stearate with both zinc stearates mixture (according to 1:1 mass ratio mixing) make
For lubricant, after being passed through compressed air and stirring 15min, room temperature is cooled to, obtains hot method powdery electric slurry.
The hot method powdery electric slurry of the present invention is used for 3D printing, establishes 3D models, and slicing delamination is carried out to model,
Export as STL formatted files, print command guiding printer head running.During work, powder feeding piston rises, and powder-laying roller is working
Uniformly spread 0.04mm on piston, computer controls the scanning track of laser beam according to STL formatted files, sintered powder material with
Form a layer.After the completion of, working piston declines a thickness 0.04mm, and powdering system work, it is new that laser beam scans sintering again
Layer, so moves in circles, until completing.
Embodiment 6
Preliminary step：Following components is weighed according to mass percent：Conductive phase copper 86%, conduction enhancing phase CNT
5%, epoxy resin of binder bisphenol type epoxy E-55 are 8%, catalyst hydrazides 0.6%, lubricant 0.4%, are added up to
100%；
Step 1：Copper powders as conductive phase are surface-treated, remove sull, it is clean to obtain surface
Pure nickel powder.
The Micron-Sized Copper Powders Coated end that particle diameter is 8 μm is put into pickling in 10% dilute hydrochloric acid solution, supersonic oscillations divide both
Dissipate uniform, remove the sull on surface, remove surface solution after standing 10min, repeat the process 4 times, then by copper powders
Repeatedly washed until without hydrochloric acid smell with deionized water after filtering.
Step 2：Decentralized processing is mutually carried out to nano-level conducting enhancing, then obtains finely dispersed powder after drying.
Appropriate absolute ethyl alcohol is added in nano-level conducting strengthens phase, then at normal temperatures after supersonic oscillations 70min, will
Dispersion liquid is placed in drying box and dried, and control temperature is at 49 DEG C.
Step 3：The conductive enhancing that the conductive phase and step 2 that step 1 is obtained obtain is mixed and stirred, and is heated to certain
After temperature, binding agent is added, obtains hybrid conductive phase.
The conductive phase obtained after processing and conduction enhancing are mixed, and stirred by efficient batch type blender
30min, until well mixed.Under nitrogen atmosphere protection, by hybrid conductive heat phase to 120 DEG C, binding agent epoxy is added
Resin, it is passed through compressed air and stirs 30min, epoxy resin is evenly coated at hybrid conductive phase surface.
Step 4：After to be bonded dose coats hybrid conductive phase completely, temperature is reduced, adds catalyst and lubricant, and make
It is well mixed, obtains hot method powdery electric slurry.
After epoxy resin evenly and completely coats hybrid conductive phase, cool 35 DEG C, add Latence catalyst hydrazides, after
Continuous stirring 15min, cools 25 DEG C, adds calcium stearate with both zinc stearates mixture (according to 1:2 mass ratio mixing) make
For lubricant, after being passed through compressed air and stirring 15min, room temperature is cooled to, obtains hot method powdery electric slurry.
The hot method powdery electric slurry of the present invention is used for 3D printing, establishes 3D models, and slicing delamination is carried out to model,
Export as STL formatted files, print command guiding printer head running.During work, powder feeding piston rises, and powder-laying roller is working
Uniformly spread 0.06mm on piston, computer controls the scanning track of laser beam according to STL formatted files, sintered powder material with
Form a layer.After the completion of, working piston declines a thickness 0.06mm, and powdering system work, it is new that laser beam scans sintering again
Layer, so moves in circles, until completing.
The slurry prepared to six above-mentioned embodiments detects, and resistivity is reduced to 5-15m Ω cm, relative to
Existing copper slurry resistivity 50-60m Ω cm, the present invention is hot, and method powdery electric slurry electric conductivity is greatly improved.
Claims (8)
1. a kind of hot method powdery electric slurry, it is characterised in that composed of the following components according to mass percent：Conductive phase
85.5%~97.5%, conduction enhancing phase 0.5%~5%, binding agent 0.5%~8.0%, catalyst 0.1~0.8%, lubrication
Agent 0.1~0.5%, add up to 100%.
2. hot method powdery electric slurry according to claim 1, it is characterised in that described conductive phase is from micron order gold
Belong to one of powder copper, silver, gold, aluminium, nickel；Conduction enhancing is mutually from one of graphene, CNT, onion carbon, nano-silver thread；It is viscous
It is more from Latence catalyst aromatic series from one of epoxy resin bisphenol type epoxy E-44, E-51, E-55, catalyst to tie agent
One of amine, acid anhydrides, dicyandiamide and hydrazides, lubricant select one or both of calcium stearate or zinc stearate mixture.
3. a kind of preparation method of hot method powdery electric slurry, it is characterised in that implement according to following steps：
Preliminary step：Following components is weighed according to mass percent：Conductive phase 85.5%~97.5%, conduction enhancing phase 0.5%
~5%, binding agent 0.5%~8.0%, catalyst 0.1~0.8%, lubricant 0.1~0.5%, add up to 100%；
Step 1, conductive phase metal dust is surface-treated, removes sull, obtain the clean simple metal powder in surface
End；
Step 2, decentralized processing is mutually carried out to conduction enhancing, then obtain finely dispersed powder after drying；
The conductive enhancing that step 3, the conductive phase that step 1 is obtained and step 2 obtain is mixed and stirred, and is heated to certain temperature
Afterwards, binding agent is added, obtains hybrid conductive phase；
After step 4, to be bonded dose of complete cladding hybrid conductive phase, temperature is reduced, is eventually adding catalyst and lubricant, mixing is equal
It is even, obtain hot method powdery electric slurry.
4. the preparation method of hot method powdery electric slurry according to claim 3, it is characterised in that in preliminary step, institute
The conductive phase stated is from one of micro-sized metal powder copper, silver, gold, aluminium, nickel；Conduction enhancing mutually from graphene, CNT,
One of onion carbon, nano-silver thread；Binding agent is from one of epoxy resin bisphenol type epoxy E-44, E-51, E-55, catalyst choosing
With one of Latence catalyst aromatic polyamine, acid anhydrides, dicyandiamide and hydrazides, lubricant selects calcium stearate or zinc stearate
One or both of mixture.
5. the preparation method of hot method powdery electric slurry according to claim 4, it is characterised in that in step 1, specific step
Suddenly it is：
The micro-sized metal powder that particle diameter is 1~15 μm is inserted into pickling in 5%~13% dilute hydrochloric acid solution, supersonic oscillations make
Both are uniformly dispersed, and remove the sull on surface, remove surface solution after standing 8~10min, repeat the process 3~5
It is secondary, then repeatedly washed with deionized water after metal dust is filtered until there is no hydrochloric acid smell.
6. the preparation method of hot method powdery electric slurry according to claim 4, it is characterised in that in step 2, specific step
Suddenly it is：
Appropriate absolute ethyl alcohol is added in nano-level conducting strengthens phase, then at normal temperatures after 50~70min of supersonic oscillations, will
Dispersion liquid is placed in drying box and dried, and temperature control is at 50 ± 2 DEG C.
7. the preparation method of hot method powdery electric slurry according to claim 4, it is characterised in that in step 3, specific step
Suddenly it is：
The conductive phase obtained after processing and conductive enhancing are mixed, and by efficient batch type blender stirring 5~
30min, until obtaining well mixed hybrid conductive phase；Under nitrogen atmosphere protection, by hybrid conductive heat phase to 80~180
DEG C, epoxy resin of binder is added, compressed air is passed through and stirs 10~30min, epoxy resin is evenly coated at mixing
Conductive phase surface.
8. the preparation method of hot method powdery electric slurry according to claim 4, it is characterised in that in step 4, specific step
Suddenly it is：
After epoxy resin evenly and completely coats hybrid conductive phase, cool 20~60 DEG C, add Latence catalyst, continue to stir
After mixing 5~20min, then cool 15~50 DEG C；One or both of calcium stearate or zinc stearate mixture are added as lubricant,
After being passed through compressed air and stirring 3~15min, room temperature is cooled to, obtains hot method powdery electric slurry.
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| CN107978384A (en) * | 2017-11-27 | 2018-05-01 | 西安工程大学 | A kind of electrocondution slurry aerosol and preparation method thereof |
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