CN110157363A - A kind of preparation method of electromagnetic shielding conductive glue conductive powder - Google Patents
A kind of preparation method of electromagnetic shielding conductive glue conductive powder Download PDFInfo
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- CN110157363A CN110157363A CN201910502077.1A CN201910502077A CN110157363A CN 110157363 A CN110157363 A CN 110157363A CN 201910502077 A CN201910502077 A CN 201910502077A CN 110157363 A CN110157363 A CN 110157363A
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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
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
- C09J133/12—Homopolymers or copolymers of methyl methacrylate
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/28—Metal sheet
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0862—Nickel
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/314—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive layer and/or the carrier being conductive
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- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The present invention provides a kind of preparation method of electromagnetic shielding conductive glue conductive powder, belongs to electromagnetic shielding conductive glue technical field.The preparation method of the electromagnetic shielding conductive glue conductive powder, which includes metallic conduction powder, be stirred by ultrasonic under 85-98 DEG C of constant temperature by complex reducing agent system and mixes 0.5-1h, metallic conduction powder surface self-catalysis plating has the nickel particles sponge coating of chain spherical morphology, it is at least cleaned 3 times with deionized water and dehydrated alcohol, 80-90 DEG C of vacuum drying, which saves, obtains the spongy nickel gold filled category conductive powder of in-stiu coating generation.The present invention utilizes surface self-catalysis technology, prepares the nickel-nickel composite powder conductive filler with sponge surface；The low Ni-coated nano-Al_2O_3 filler of resistivity is prepared by diffusion into the surface activating technology using liquid phase reduction；Liquid phase reduction therein directly generates the spongy nickel particles clad uniformly coated, simple process, economy without carrying out matrix powder surface active sensitization.
Description
Technical field
The present invention relates to electromagnetic shielding conductive glue technical fields, more particularly, to a kind of electromagnetic shielding conductive glue conducting powder
The preparation method at end.
Background technique
Silver powder or silver-plated powder are widely used as conductive powder in conducting resinl field, especially need conduction some
Glue has the field of excellent conductive performance even more so, these fields generally use silver powder as the conductive powder in conducting resinl.
But sliver-powder conducting glue is easy to that ELECTROMIGRATION PHENOMENON occurs in wet environment, this seriously reduces the practical of conducting resinl
Property；Moreover the silver powder higher cost of sliver-powder conducting glue, sedimentation stability are poor.
The volume resistivity of copper is 1.72x10-6Ω * cm, silver-colored volume resistivity are 1.59x10-6Ω * cm, and the valence of copper
Lattice are the 1/20 of silver, therefore copper powder is the ideal conducting filler for preparing electromagnetic shielding conductive glue.Compared with silver powder, copper powder not only has
There is preferable electric conductivity, and is also significantly less than silver powder in cost.But the copper powder chemical property in copper system conducting resinl is active,
Surface is oxidizable, to form nonconducting Cu oxide, causes the electric conductivity of copper system conducting resinl unstable, or even cannot be formed
Complete conductive path.Although copper system conducting resinl is after decades of development, significant progress is achieved, unstability is still
The problem of being so long-term existence, such as limited impact resistance, long-term mechanicalness and conductive stable etc., so that copper system is conductive
Conducting resinl is still difficult to widely be received glue instead of welding in the electronics industry.
Compared with traditional silver system and copper system conducting resinl, nickel is tied up to while guarantee that electric conductivity is preferable, than silver system conducting resinl
Cost substantially reduce, significantly improved than copper system conducting resinl oxidation resistance, and have excellent magnetic property, in some spies
The occasions such as different occasion such as coating for EMI shielding, anti-counterfeit package, anti-counterfeit printing are with a wide range of applications, and are a kind of novel more
Function, inexpensive conducting resinl.
Conductive filler is mainly electrolytic nickel powder and conductive copper powder at present, since nickel powder electric conductivity is poor, nickel coated copper powder cladding
Effect is poor, causes current conductive filler product cost not high, because when chemical nickel plating, metal with catalytic activity itself is
Limited, only N, Pd, Co, Pt etc. need to be deposited with catalytic activity on surface for the material of those catalytically inactive itself
Metal core, acquisition, such as Fe, Al, Be, Ti can be reacted by the way that displacement occurs with the nickel ion in solution by being catalyzed being formed for core.Also
There are some metals, such as Cu, Ag, Au, metal catalytic core can be obtained by contacting with some metals more active than nickel.For
Plastics etc. are nonmetallic, then obtain catalytic activity point by the sensitization such as tin tetrachloride, palladium chloride, activation.Inactive surface is (such as
Adsorptivity very strong corrosion inhibiter is accidentally added when steel plating piece acidic derusting) it can not plating.
Summary of the invention
The present invention provides a kind of preparation methods of electromagnetic shielding conductive glue conductive powder, solve prior art electromagnetism
Screen conducting adhesive with conductive powder prepare present in " conductive filler mainly uses liquid phase reduction at present, and the Ni-based of generation is led
Electric powder resistivity is higher, while Copper Powder Surface needs to be sensitized activation in advance, cost is too high without autocatalytic activity " the problems such as.
The present invention provides a kind of preparation method of electromagnetic shielding conductive glue conductive powder, and the electromagnetic shielding conductive glue is used
The preparation method of conductive powder, which includes metallic conduction powder, be stirred by ultrasonic under 85-98 DEG C of constant temperature by complex reducing agent system and mixes
0.5-1h is closed, metallic conduction powder surface self-catalysis plating has the nickel particles sponge coating of chain spherical morphology, uses deionized water
It is at least cleaned 3 times with dehydrated alcohol, 80-90 DEG C of vacuum drying, which saves, obtains the spongy nickel packet metallic conduction of in-stiu coating generation
Powder；
The complex reducing agent system includes the nickel chloride that concentration is 20-30g/L, the reducing agent boron hydrogen of 0.65-0.9g/L
Change sodium, the pH adjusting agent sodium hydroxide of 40-50g/L makes the pH value of solution of complex reducing agent system be maintained at 12-14 highly basic state,
The complexing agent ethylenediamine of 60-90g/L, the stabilizer lead chloride of 0.01-2g/L, the strong reductant hydrazine hydrate of 1-10ml.
Preferably, the metallic conduction powder is nickel conductive powder or nickel copper-clad composite conductive powder.
Preferably, the nickel conductive powder is any one of spherical shape, dendroid, irregular shape and sheet, granularity model
Enclose is 10-75 μm.
Preferably, the preparation method of the nickel copper-clad composite conductive powder includes that nano-nickel powder and copper powder are dissolved in ethylene glycol
Alcoholic solution is mixed in wall-breaking machine and obtains slurry, and vacuum dried and prealloy diffusion activation is crushed spare.
Preferably, the nano-nickel powder particle size range is 100nm-1 μm, and copper powder pattern is spherical shape, dendriform, irregular shape
Any one of shape and sheet, particle size range are 15-75 μm, and the mass ratio of nano-nickel powder and copper powder is 1:20, ethylene glycol and wine
The volume ratio of essence is 1:80, and the wall-breaking machine working speed can be controlled in 10000-35000 revs/min, after gained slurry filtration,
It is dried in vacuo at 80-90 DEG C, nano-nickel powder is evenly coated at Copper Powder Surface；Then, under hydrogen shield atmosphere, flow control is in 8-
12ml/min, 870-950 DEG C of diffusion-alloying in tube furnace, is crushed spare.
A kind of electromagnetic shielding conductive glue conductive powder is for double methods for leading the preparation of aluminum foil and adhesive tape finished product, according to release paper
Thickness, aluminum foil thickness and rubberization thickness determine that the partial size of conductive powder, conductive powder partial size will be slightly larger than the thickness of applied dry glue,
Acrylic glue is weighed, according to the ratio weighing conductive powder for accounting for acrylic glue weight percent 2.5, uses blender after mixing
It is sufficiently stirred, pours into coating groove, first by release paper gluing, heating, then release paper is run into aluminium foil and meets end position, carry out aluminium foil
Paper and the release paper after gluing are compound, and after rubber rollers sufficiently squeeze, by spool, i.e., formation is double leads aluminum foil and adhesive tape finished product.
Preferably, double to lead the New Nickel system filler conducting resinl having a size of 2.5cm*15cm obtained by aluminum foil and adhesive tape finished product, sample
Resistance < 50m Ω.
Preferably, the release paper is with a thickness of 100-110 μm, and for aluminium-foil paper with a thickness of 55-62 μm, rubberization thickness is 60-65 μ
m。
Preferably, the method is shown in specific step is as follows:
S1, the acrylic glue for weighing 18 liters；
S2, conductive powder of weighing according to the ratio for accounting for acrylic glue weight percent 2.5；
S3, it load weighted conductive powder is poured slowly into acrylic glue mixes, while with the revolving speed of adjustment blender
At least 5 minutes realization conductive powder being uniformly distributed in acrylic glue；
After S4, conductive powder being uniformly distributed in acrylic glue, it is directly poured into coating groove；
S5, starting device carry out release paper gluing, and the release paper after gluing is warming up to 80-110 DEG C in temperature control device,
Heating-up time is 1-2 minutes；
S7, after the completion of heating, when release paper run to aluminium foil meet end position, aluminium-foil paper and the release paper after gluing are answered
It closes；
S8, shaft clearance set to zero gap will be rolled in recombination process, by spool, formation is double to lead aluminum foil and adhesive tape finished product.
The advantageous effects of the above technical solutions of the present invention are as follows:
The present invention utilizes surface self-catalysis technology, prepares the nickel-nickel composite powder conductive filler with sponge surface；Using
Liquid phase reduction prepares the low Ni-coated nano-Al_2O_3 filler of resistivity by diffusion into the surface activating technology；Liquid phase therein is also
Former method directly generates the spongy nickel particles clad uniformly coated, technique letter without carrying out matrix powder surface active sensitization
It is single, economical.
Detailed description of the invention
Below in conjunction with the attached drawing in this patent embodiment, the technical solution in this patent embodiment is carried out furtherly
It is bright.
Fig. 1 is the structural schematic diagram of electromagnetic shielding conductive glue conductive powder of the present invention；
Fig. 2 is electromagnetic shielding conductive plastic structure schematic diagram of the invention.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
The technical problem to be solved by the present invention is to overcome prior art electromagnetic shielding conductive glue with conductive powder prepare in deposit
" conductive filler mainly uses liquid phase reduction at present, and the nickel based conductive powder resistivity of generation is higher, at the same Copper Powder Surface without
Autocatalytic activity needs to be sensitized activation in advance, and cost is too high " the problems such as.
In order to solve the above technical problems, the present invention provides a kind of preparation method of electromagnetic shielding conductive glue conductive powder,
The preparation method of the electromagnetic shielding conductive glue conductive powder includes that metallic conduction powder passes through complex reducing agent system in 85-
Ultrasonic agitation mixing 0.5-1h, metallic conduction powder surface self-catalysis plating have the nickel particles of chain spherical morphology under 98 DEG C of constant temperature
Sponge coating is at least cleaned 3 times with deionized water and dehydrated alcohol, and 80-90 DEG C of vacuum drying preservation obtains in-stiu coating generation
Spongy nickel gold filled category conductive powder, spongy nickel coated structure is as shown in Figure 1；
The complex reducing agent system includes the nickel chloride that concentration is 20-30g/L, the reducing agent boron hydrogen of 0.65-0.9g/L
Change sodium, the pH adjusting agent sodium hydroxide of 40-50g/L makes the pH value of solution of complex reducing agent system be maintained at 12-14 highly basic state,
The complexing agent ethylenediamine of 60-90g/L, the stabilizer lead chloride of 0.01-2g/L, the strong reductant hydrazine hydrate of 1-10ml.
Above-mentioned electromagnetic shielding conductive glue conductive powder is for double methods for leading the preparation of aluminum foil and adhesive tape finished product, according to release paper
Thickness, aluminum foil thickness and rubberization thickness determine that the partial size of conductive powder, conductive powder partial size will be slightly larger than the thickness of applied dry glue,
Acrylic glue is weighed, according to the ratio weighing conductive powder for accounting for acrylic glue weight percent 2.5, uses blender after mixing
Be sufficiently stirred, pour into coating groove, the conducting resinl pattern in the coating groove as shown in Fig. 2, first by release paper gluing, heating, then
Release paper is run into aluminium foil and meets end position, aluminium-foil paper is carried out and the release paper after gluing is compound, after rubber rollers sufficiently squeeze,
By spool, i.e., formation is double leads aluminum foil and adhesive tape finished product.
Specific electromagnetic shielding conductive glue conductive powder preparation method and corresponding conducting resinl preparation method combine following
Embodiment is illustrated:
Embodiment 1
A kind of preparation method of electromagnetic shielding conductive glue conductive powder, the electromagnetic shielding conductive glue conductive powder
Preparation method, which includes metallic conduction powder, be stirred by ultrasonic under 85 DEG C of constant temperature by complex reducing agent system and mixes 0.5h, and metal is led
Self-catalysis plating in electro-powder surface has the nickel particles sponge coating of chain spherical morphology, at least clear with deionized water and dehydrated alcohol
It washes 3 times, 80 DEG C of vacuum drying, which save, obtains the spongy nickel gold filled category conductive powder of in-stiu coating generation；
The complex reducing agent system include concentration be 20g/L nickel chloride, the reducing agent sodium borohydride of 0.65g/L,
The pH adjusting agent sodium hydroxide of 40g/L makes the pH value of solution of complex reducing agent system be maintained at 12 highly basic states, the complexing of 60g/L
Agent ethylenediamine, the stabilizer lead chloride of 0.01g/L, the strong reductant hydrazine hydrate of 1ml.
The metallic conduction powder is nickel conductive powder.
The nickel conductive powder is spherical shape, and granularity is 10 μm.
Above-mentioned electromagnetic shielding conductive glue conductive powder is used for double methods for leading the preparation of aluminum foil and adhesive tape finished product, the method
Shown in specific step is as follows:
S1, the acrylic glue for weighing 18 liters；
S2, conductive powder of weighing according to the ratio for accounting for acrylic glue weight percent 2.5；
S3, it load weighted conductive powder is poured slowly into acrylic glue mixes, while with the revolving speed of adjustment blender
At least 5 minutes realization conductive powder being uniformly distributed in acrylic glue；
After S4, conductive powder being uniformly distributed in acrylic glue, it is directly poured into coating groove；
S5, starting device carry out release paper gluing, and the release paper after gluing is warming up to 80-110 DEG C in temperature control device,
Heating-up time is 1-2 minutes；
S7, after the completion of heating, when release paper run to aluminium foil meet end position, aluminium-foil paper and the release paper after gluing are answered
It closes；
S8, shaft clearance set to zero gap will be rolled in recombination process, by spool, formation is double to lead aluminum foil and adhesive tape finished product.
It is double to lead the New Nickel system filler conducting resinl having a size of 2.5cm*15cm obtained by aluminum foil and adhesive tape finished product, sample resistance <
50mΩ。
The release paper is with a thickness of 100 μm, and for aluminium-foil paper with a thickness of 55 μm, rubberization thickness is 60 μm.
Embodiment 2
A kind of preparation method of electromagnetic shielding conductive glue conductive powder, the electromagnetic shielding conductive glue conductive powder
Preparation method, which includes metallic conduction powder, be stirred by ultrasonic under 98 DEG C of constant temperature by complex reducing agent system and mixes 1h, metallic conduction
Self-catalysis plating in powder surface has the nickel particles sponge coating of chain spherical morphology, is at least cleaned with deionized water and dehydrated alcohol
4 times, 90 DEG C of vacuum drying, which save, obtains the spongy nickel gold filled category conductive powder of in-stiu coating generation；
The complex reducing agent system includes the nickel chloride that concentration is 30g/L, the reducing agent sodium borohydride of 0.9g/L, 50g/
The pH adjusting agent sodium hydroxide of L makes the pH value of solution of complex reducing agent system be maintained at 14 highly basic states, the complexing agent second of 90g/L
Diamines, the stabilizer lead chloride of 2g/L, the strong reductant hydrazine hydrate of 10ml.
The metallic conduction powder is nickel conductive powder.
The nickel conductive powder is dendroid, and granularity is 75 μm.
Above-mentioned electromagnetic shielding conductive glue conductive powder is used for double methods for leading the preparation of aluminum foil and adhesive tape finished product, the method
Shown in specific step is as follows:
S1, the acrylic glue for weighing 18 liters；
S2, conductive powder of weighing according to the ratio for accounting for acrylic glue weight percent 2.5；
S3, it load weighted conductive powder is poured slowly into acrylic glue mixes, while with the revolving speed of adjustment blender
At least 5 minutes realization conductive powder being uniformly distributed in acrylic glue；
After S4, conductive powder being uniformly distributed in acrylic glue, it is directly poured into coating groove；
S5, starting device carry out release paper gluing, and the release paper after gluing is warming up to 80-110 DEG C in temperature control device,
Heating-up time is 1-2 minutes；
S7, after the completion of heating, when release paper run to aluminium foil meet end position, aluminium-foil paper and the release paper after gluing are answered
It closes；
S8, shaft clearance set to zero gap will be rolled in recombination process, by spool, formation is double to lead aluminum foil and adhesive tape finished product.
It is double to lead the New Nickel system filler conducting resinl having a size of 2.5cm*15cm obtained by aluminum foil and adhesive tape finished product, sample resistance <
50mΩ。
The release paper is with a thickness of 110 μm, and for aluminium-foil paper with a thickness of 62 μm, rubberization thickness is 65 μm.
Embodiment 3
A kind of preparation method of electromagnetic shielding conductive glue conductive powder, the electromagnetic shielding conductive glue conductive powder
Preparation method, which includes metallic conduction powder, be stirred by ultrasonic under 85 DEG C of constant temperature by complex reducing agent system and mixes 0.5h, and metal is led
Self-catalysis plating in electro-powder surface has the nickel particles sponge coating of chain spherical morphology, at least clear with deionized water and dehydrated alcohol
It washes 3 times, 80 DEG C of vacuum drying, which save, obtains the spongy nickel gold filled category conductive powder of in-stiu coating generation；
The complex reducing agent system include concentration be 20g/L nickel chloride, the reducing agent sodium borohydride of 0.65g/L,
The pH adjusting agent sodium hydroxide of 40g/L makes the pH value of solution of complex reducing agent system be maintained at 12 highly basic states, the complexing of 60g/L
Agent ethylenediamine, the stabilizer lead chloride of 0.01g/L, the strong reductant hydrazine hydrate of 1ml.
The metallic conduction powder is nickel copper-clad composite conductive powder.
The preparation method of the nickel copper-clad composite conductive powder includes that nano-nickel powder is dissolved in ethylene glycol alcohol with copper powder is molten
Liquid is mixed in wall-breaking machine and obtains slurry, and vacuum dried and prealloy diffusion activation is crushed spare.
The nano-nickel powder particle size range is 100nm, and copper powder pattern is spherical shape, and granularity is 15 μm, nano-nickel powder and copper powder
Mass ratio be 1:20, the volume ratio of ethylene glycol and alcohol is 1:80, the wall-breaking machine working speed can be controlled in 10000 turns/
Minute, it after gained slurry filtration, is dried in vacuo at 80 DEG C, nano-nickel powder is evenly coated at Copper Powder Surface；Then, hydrogen shield gas
Under atmosphere, flow control 870 DEG C of diffusion-alloyings in 8ml/min, tube furnace are crushed spare.
Above-mentioned electromagnetic shielding conductive glue conductive powder is used for double methods for leading the preparation of aluminum foil and adhesive tape finished product, the method
Shown in specific step is as follows:
S1, the acrylic glue for weighing 18 liters；
S2, conductive powder of weighing according to the ratio for accounting for acrylic glue weight percent 2.5；
S3, it load weighted conductive powder is poured slowly into acrylic glue mixes, while with the revolving speed of adjustment blender
At least 5 minutes realization conductive powder being uniformly distributed in acrylic glue；
After S4, conductive powder being uniformly distributed in acrylic glue, it is directly poured into coating groove；
S5, starting device carry out release paper gluing, and the release paper after gluing is warming up to 80-110 DEG C in temperature control device,
Heating-up time is 1-2 minutes；
S7, after the completion of heating, when release paper run to aluminium foil meet end position, aluminium-foil paper and the release paper after gluing are answered
It closes；
S8, shaft clearance set to zero gap will be rolled in recombination process, by spool, formation is double to lead aluminum foil and adhesive tape finished product.
It is double to lead the New Nickel system filler conducting resinl having a size of 2.5cm*15cm obtained by aluminum foil and adhesive tape finished product, sample resistance <
50mΩ。
The release paper is with a thickness of 100 μm, and for aluminium-foil paper with a thickness of 55 μm, rubberization thickness is 60 μm.
Embodiment 4
A kind of preparation method of electromagnetic shielding conductive glue conductive powder, the electromagnetic shielding conductive glue conductive powder
Preparation method, which includes metallic conduction powder, be stirred by ultrasonic under 98 DEG C of constant temperature by complex reducing agent system and mixes 0.5-1h, metal
Self-catalysis plating in conductive powder surface has the nickel particles sponge coating of chain spherical morphology, at least with deionized water and dehydrated alcohol
Cleaning 4 times, 90 DEG C of vacuum drying, which save, obtains the spongy nickel gold filled category conductive powder of in-stiu coating generation；
The complex reducing agent system includes the nickel chloride that concentration is 30g/L, the reducing agent sodium borohydride of 0.9g/L, 50g/
The pH adjusting agent sodium hydroxide of L makes the pH value of solution of complex reducing agent system be maintained at 14 highly basic states, the complexing agent second of 90g/L
Diamines, the stabilizer lead chloride of 2g/L, the strong reductant hydrazine hydrate of 10ml.
The metallic conduction powder is nickel copper-clad composite conductive powder.
The preparation method of the nickel copper-clad composite conductive powder includes that nano-nickel powder is dissolved in ethylene glycol alcohol with copper powder is molten
Liquid is mixed in wall-breaking machine and obtains slurry, and vacuum dried and prealloy diffusion activation is crushed spare.
The nano-nickel powder particle size range is 1 μm, and copper powder pattern is dendriform, and granularity is 75 μm, nano-nickel powder and copper powder
Mass ratio be 1:20, the volume ratio of ethylene glycol and alcohol is 1:80, the wall-breaking machine working speed can be controlled in 35000 turns/
Minute, it after gained slurry filtration, is dried in vacuo at 90 DEG C, nano-nickel powder is evenly coated at Copper Powder Surface；Then, hydrogen shield gas
Under atmosphere, flow control 950 DEG C of diffusion-alloyings in 12ml/min, tube furnace are crushed spare.
Above-mentioned electromagnetic shielding conductive glue conductive powder is used for double methods for leading the preparation of aluminum foil and adhesive tape finished product, the method
Shown in specific step is as follows:
S1, the acrylic glue for weighing 18 liters；
S2, conductive powder of weighing according to the ratio for accounting for acrylic glue weight percent 2.5；
S3, it load weighted conductive powder is poured slowly into acrylic glue mixes, while with the revolving speed of adjustment blender
At least 5 minutes realization conductive powder being uniformly distributed in acrylic glue；
After S4, conductive powder being uniformly distributed in acrylic glue, it is directly poured into coating groove；
S5, starting device carry out release paper gluing, and the release paper after gluing is warming up to 80-110 DEG C in temperature control device,
Heating-up time is 1-2 minutes；
S7, after the completion of heating, when release paper run to aluminium foil meet end position, aluminium-foil paper and the release paper after gluing are answered
It closes；
S8, shaft clearance set to zero gap will be rolled in recombination process, by spool, formation is double to lead aluminum foil and adhesive tape finished product.
It is double to lead the New Nickel system filler conducting resinl having a size of 2.5cm*15cm obtained by aluminum foil and adhesive tape finished product, sample resistance <
50mΩ。
The release paper is with a thickness of 110 μm, and for aluminium-foil paper with a thickness of 62 μm, rubberization thickness is 65 μm.
Embodiment 5
A kind of preparation method of electromagnetic shielding conductive glue conductive powder, the electromagnetic shielding conductive glue conductive powder
Preparation method, which includes metallic conduction powder, be stirred by ultrasonic under 90 DEG C of constant temperature by complex reducing agent system and mixes 1.5h, and metal is led
Self-catalysis plating in electro-powder surface has the nickel particles sponge coating of chain spherical morphology, at least clear with deionized water and dehydrated alcohol
It washes 3 times, 85 DEG C of vacuum drying, which save, obtains the spongy nickel gold filled category conductive powder of in-stiu coating generation；
The complex reducing agent system include concentration be 25g/L nickel chloride, the reducing agent sodium borohydride of 0.75g/L,
The pH adjusting agent sodium hydroxide of 45g/L makes the pH value of solution of complex reducing agent system be maintained at 13 highly basic states, the complexing of 75g/L
Agent ethylenediamine, the stabilizer lead chloride of 1g/L, the strong reductant hydrazine hydrate of 5ml.
The metallic conduction powder is nickel conductive powder.
The nickel conductive powder is sheet, and granularity is 45 μm.
Above-mentioned electromagnetic shielding conductive glue conductive powder is used for double methods for leading the preparation of aluminum foil and adhesive tape finished product, the method
Shown in specific step is as follows:
S1, the acrylic glue for weighing 18 liters；
S2, conductive powder of weighing according to the ratio for accounting for acrylic glue weight percent 2.5；
S3, it load weighted conductive powder is poured slowly into acrylic glue mixes, while with the revolving speed of adjustment blender
At least 5 minutes realization conductive powder being uniformly distributed in acrylic glue；
After S4, conductive powder being uniformly distributed in acrylic glue, it is directly poured into coating groove；
S5, starting device carry out release paper gluing, and the release paper after gluing is warming up to 80-110 DEG C in temperature control device,
Heating-up time is 1-2 minutes；
S7, after the completion of heating, when release paper run to aluminium foil meet end position, aluminium-foil paper and the release paper after gluing are answered
It closes；
S8, shaft clearance set to zero gap will be rolled in recombination process, by spool, formation is double to lead aluminum foil and adhesive tape finished product.
It is double to lead the New Nickel system filler conducting resinl having a size of 2.5cm*15cm obtained by aluminum foil and adhesive tape finished product, sample resistance <
50mΩ。
The release paper is with a thickness of 105 μm, and for aluminium-foil paper with a thickness of 58 μm, rubberization thickness is 63 μm.
Embodiment 6
A kind of preparation method of electromagnetic shielding conductive glue conductive powder, the electromagnetic shielding conductive glue conductive powder
Preparation method, which includes metallic conduction powder, be stirred by ultrasonic under 90 DEG C of constant temperature by complex reducing agent system and mixes 1.2h, and metal is led
Self-catalysis plating in electro-powder surface has the nickel particles sponge coating of chain spherical morphology, at least clear with deionized water and dehydrated alcohol
It washes 4 times, 88 DEG C of vacuum drying, which save, obtains the spongy nickel gold filled category conductive powder of in-stiu coating generation；
The complex reducing agent system include concentration be 22g/L nickel chloride, the reducing agent sodium borohydride of 0.85g/L,
The pH adjusting agent sodium hydroxide of 47g/L makes the pH value of solution of complex reducing agent system be maintained at 12 highly basic states, the complexing of 75g/L
Agent ethylenediamine, the stabilizer lead chloride of 0.56g/L, the strong reductant hydrazine hydrate of 3ml.
The metallic conduction powder is nickel copper-clad composite conductive powder.
The preparation method of the nickel copper-clad composite conductive powder includes that nano-nickel powder is dissolved in ethylene glycol alcohol with copper powder is molten
Liquid is mixed in wall-breaking machine and obtains slurry, and vacuum dried and prealloy diffusion activation is crushed spare.
The nano-nickel powder particle size range is 600nm, and copper powder pattern is sheet, and granularity is 60 μm, nano-nickel powder and copper powder
Mass ratio be 1:20, the volume ratio of ethylene glycol and alcohol is 1:80, the wall-breaking machine working speed can be controlled in 28000 turns/
Minute, it after gained slurry filtration, is dried in vacuo at 90 DEG C, nano-nickel powder is evenly coated at Copper Powder Surface；Then, hydrogen shield gas
Under atmosphere, flow control 890 DEG C of diffusion-alloyings in 10ml/min, tube furnace are crushed spare.
Above-mentioned electromagnetic shielding conductive glue conductive powder is used for double methods for leading the preparation of aluminum foil and adhesive tape finished product, the method
Shown in specific step is as follows:
S1, the acrylic glue for weighing 18 liters；
S2, conductive powder of weighing according to the ratio for accounting for acrylic glue weight percent 2.5；
S3, it load weighted conductive powder is poured slowly into acrylic glue mixes, while with the revolving speed of adjustment blender
At least 5 minutes realization conductive powder being uniformly distributed in acrylic glue；
After S4, conductive powder being uniformly distributed in acrylic glue, it is directly poured into coating groove；
S5, starting device carry out release paper gluing, and the release paper after gluing is warming up to 80-110 DEG C in temperature control device,
Heating-up time is 1-2 minutes；
S7, after the completion of heating, when release paper run to aluminium foil meet end position, aluminium-foil paper and the release paper after gluing are answered
It closes；
S8, shaft clearance set to zero gap will be rolled in recombination process, by spool, formation is double to lead aluminum foil and adhesive tape finished product.
It is double to lead the New Nickel system filler conducting resinl having a size of 2.5cm*15cm obtained by aluminum foil and adhesive tape finished product, sample resistance <
50mΩ。
The release paper is with a thickness of 100 μm, and for aluminium-foil paper with a thickness of 55 μm, rubberization thickness is 62 μm.
Embodiment 7
A kind of preparation method of electromagnetic shielding conductive glue conductive powder, the electromagnetic shielding conductive glue conductive powder
Preparation method, which includes metallic conduction powder, be stirred by ultrasonic under 98 DEG C of constant temperature by complex reducing agent system and mixes 1h, metallic conduction
Self-catalysis plating in powder surface has the nickel particles sponge coating of chain spherical morphology, is at least cleaned with deionized water and dehydrated alcohol
3 times, 90 DEG C of vacuum drying, which save, obtains the spongy nickel gold filled category conductive powder of in-stiu coating generation；
The complex reducing agent system include concentration be 23g/L nickel chloride, the reducing agent sodium borohydride of 0.72g/L,
The pH adjusting agent sodium hydroxide of 48g/L makes the pH value of solution of complex reducing agent system be maintained at 12 highly basic states, the complexing of 69g/L
Agent ethylenediamine, the stabilizer lead chloride of 1.23g/L, the strong reductant hydrazine hydrate of 8ml.
The metallic conduction powder is nickel copper-clad composite conductive powder.
The preparation method of the nickel copper-clad composite conductive powder includes that nano-nickel powder is dissolved in ethylene glycol alcohol with copper powder is molten
Liquid is mixed in wall-breaking machine and obtains slurry, and vacuum dried and prealloy diffusion activation is crushed spare.
The nano-nickel powder particle size range be 400nm, copper powder pattern be spherical shape, particle size range be 70 μm, nano-nickel powder and
The mass ratio of copper powder is 1:20, and the volume ratio of ethylene glycol and alcohol is 1:80, and the wall-breaking machine working speed can be controlled in 30000
Rev/min, it after gained slurry filtration, is dried in vacuo at 90 DEG C, nano-nickel powder is evenly coated at Copper Powder Surface；Then, hydrogen is protected
It protects under atmosphere, flow control 920 DEG C of diffusion-alloyings in 12ml/min, tube furnace are crushed spare.
Above-mentioned electromagnetic shielding conductive glue conductive powder is used for double methods for leading the preparation of aluminum foil and adhesive tape finished product, the method
Shown in specific step is as follows:
S1, the acrylic glue for weighing 18 liters；
S2, conductive powder of weighing according to the ratio for accounting for acrylic glue weight percent 2.5；
S3, it load weighted conductive powder is poured slowly into acrylic glue mixes, while with the revolving speed of adjustment blender
At least 5 minutes realization conductive powder being uniformly distributed in acrylic glue；
After S4, conductive powder being uniformly distributed in acrylic glue, it is directly poured into coating groove；
S5, starting device carry out release paper gluing, and the release paper after gluing is warming up to 80-110 DEG C in temperature control device,
Heating-up time is 1-2 minutes；
S7, after the completion of heating, when release paper run to aluminium foil meet end position, aluminium-foil paper and the release paper after gluing are answered
It closes；
S8, shaft clearance set to zero gap will be rolled in recombination process, by spool, formation is double to lead aluminum foil and adhesive tape finished product.
It is double to lead the New Nickel system filler conducting resinl having a size of 2.5cm*15cm obtained by aluminum foil and adhesive tape finished product, sample resistance <
50mΩ。
The release paper is with a thickness of 110 μm, and for aluminium-foil paper with a thickness of 60 μm, rubberization thickness is 63 μm.
To sum up, the present invention utilizes surface self-catalysis technology, and it is conductive to prepare the nickel-nickel composite powder with sponge surface
Filler；The low Ni-coated nano-Al_2O_3 filler of resistivity is prepared by diffusion into the surface activating technology using liquid phase reduction；Its
In liquid phase reduction without carrying out matrix powder surface active sensitization, directly generate the spongy nickel particles cladding uniformly coated
Layer, simple process, economy.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of electromagnetic shielding conductive glue conductive powder, which is characterized in that the electromagnetic shielding conductive glue is used
The preparation method of conductive powder, which includes metallic conduction powder, be stirred by ultrasonic under 85-98 DEG C of constant temperature by complex reducing agent system and mixes
0.5-1h is closed, metallic conduction powder surface self-catalysis plating has the nickel particles sponge coating of chain spherical morphology, uses deionized water
It is at least cleaned 3 times with dehydrated alcohol, 80-90 DEG C of vacuum drying, which saves, obtains the spongy nickel packet metallic conduction of in-stiu coating generation
Powder；
The complex reducing agent system include concentration be 20-30g/L nickel chloride, the reducing agent sodium borohydride of 0.65-0.9g/L,
The pH adjusting agent sodium hydroxide of 40-50g/L makes the pH value of solution of complex reducing agent system be maintained at 12-14 highly basic state, 60-
The complexing agent ethylenediamine of 90g/L, the stabilizer lead chloride of 0.01-2g/L, the strong reductant hydrazine hydrate of 1-10ml.
2. the preparation method of electromagnetic shielding conductive glue conductive powder according to claim 1, which is characterized in that the metal
Conductive powder is nickel conductive powder or nickel copper-clad composite conductive powder.
3. the preparation method of electromagnetic shielding conductive glue conductive powder according to claim 2, which is characterized in that the nickel is led
Electro-powder is any one of spherical shape, dendroid, irregular shape and sheet, and particle size range is 10-75 μm.
4. the preparation method of electromagnetic shielding conductive glue conductive powder according to claim 2, which is characterized in that the nickel packet
The preparation method of copper composite conductive powder includes that nano-nickel powder and copper powder are dissolved in ethylene glycol alcoholic solution, is mixed in wall-breaking machine
Slurry is stirred to get, vacuum dried and prealloy diffusion activation is crushed spare.
5. the preparation method of electromagnetic shielding conductive glue conductive powder according to claim 4, which is characterized in that the nanometer
Nickel powder particle size range is 100nm-1 μm, and copper powder pattern is any one of spherical shape, dendriform, irregular shape and sheet, granularity
Range is 15-75 μm, and the mass ratio of nano-nickel powder and copper powder is 1:20, and the volume ratio of ethylene glycol and alcohol is 1:80, described broken
Wall machine working speed can be controlled in 10000-35000 revs/min, after gained slurry filtration, is dried in vacuo at 80-90 DEG C, nanometer
Nickel powder is evenly coated at Copper Powder Surface；Then, under hydrogen shield atmosphere, flow control 870- in 8-12ml/min, tube furnace
950 DEG C of diffusion-alloyings, are crushed spare.
6. any electromagnetic shielding conductive glue of claim 1-5 is used to double to lead aluminum foil and adhesive tape finished product preparation with conductive powder
Method, which is characterized in that the partial size of conductive powder, conductive powder are determined according to release paper thickness, aluminum foil thickness and rubberization thickness
Partial size will be slightly larger than the thickness of applied dry glue, acrylic glue be weighed, according to the ratio for accounting for acrylic glue weight percent 2.5
It weighs conductive powder, is sufficiently stirred after mixing with blender, pours into coating groove, first by release paper gluing, heating, then by release paper
It runs to aluminium foil and meets end position, carry out aluminium-foil paper and the release paper after gluing is compound, after rubber rollers sufficiently squeeze, pass through volume
Axis, i.e. formation are double to lead aluminum foil and adhesive tape finished product.
7. method according to claim 6, which is characterized in that double to lead obtained by aluminum foil and adhesive tape finished product having a size of 2.5cm*15cm's
New Nickel system filler conducting resinl, sample resistance < 50m Ω.
8. method according to claim 6, which is characterized in that the release paper with a thickness of 100-110 μm, aluminium-foil paper with a thickness of
55-62 μm, rubberization thickness is 60-65 μm.
9. method according to claim 6, which is characterized in that the method is shown in specific step is as follows:
S1, the acrylic glue for weighing 18 liters；
S2, conductive powder of weighing according to the ratio for accounting for acrylic glue weight percent 2.5；
S3, it load weighted conductive powder is poured slowly into acrylic glue mixes, while with the revolving speed at least 5 of adjustment blender
Minute realizes conductive powder being uniformly distributed in acrylic glue；
After S4, conductive powder being uniformly distributed in acrylic glue, it is directly poured into coating groove；
S5, starting device carry out release paper gluing, the release paper after gluing are warming up to 80-110 DEG C in temperature control device, heating
Time is 1-2 minutes；
S7, after the completion of heating, when release paper run to aluminium foil meet end position, aluminium-foil paper and the release paper after gluing is compound；
S8, shaft clearance set to zero gap will be rolled in recombination process, by spool, formation is double to lead aluminum foil and adhesive tape finished product.
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