CN106366409B - A kind of ultra-high molecular weight polyethylene/graphite alkene/nickel composite material and preparation method - Google Patents
A kind of ultra-high molecular weight polyethylene/graphite alkene/nickel composite material and preparation method Download PDFInfo
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- CN106366409B CN106366409B CN201610763277.9A CN201610763277A CN106366409B CN 106366409 B CN106366409 B CN 106366409B CN 201610763277 A CN201610763277 A CN 201610763277A CN 106366409 B CN106366409 B CN 106366409B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
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- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/0083—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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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
Abstract
The present invention relates to functional composite material field, specifically a kind of ultra-high molecular weight polyethylene/graphite alkene/nickel composite material and preparation method with high capability of electromagnetic shielding.The compound particle for preparing composite material is to coat ultra-high molecular weight polyethylene particle using metallic nickel as shell structurre, graphene coated ultra-high molecular weight polyethylene for the Ni-coated graphite alkene of core, wherein the content of graphene coated ultra-high molecular weight polyethylene particle is 97.42 vol% ~ 98.91vol%, the content of metallic nickel is the vol% of 1.09vol% ~ 2.58, and the wherein content of graphene in the composite is at least 0.028 vol%.The present invention can significantly improve the conductivity and capability of electromagnetic shielding of composite material by composite material of the preparation with isolation structure in the case of metallic nickel and extremely low graphene content, realize the target of highly conductive, the high capability of electromagnetic shielding of composite material.
Description
Technical field
The present invention relates to functional composite material field, specifically a kind of super high molecular weight with high capability of electromagnetic shielding is poly-
Ethylene/graphene/nickel composite material and preparation method.
Background technology
With the high speed development of modern electronics industry, electronic apparatus and radio communication are generally used, electromagnetic radiation
Oneself becomes the another big public hazards after noise pollution, atmosphere pollution, water pollution, solid waste pollution.Electromagnetic wave not only interferes
The normal operation for various electronic equipments threatens the information security of communication equipment, and will produce pole to the health of the mankind
Big harm.The method for eliminating electromagnetic wave harm at present mainly shields it using electromagnetic shielding material.Therefore, it explores high
Imitating electromagnetic shielding material becomes problem in the urgent need to address.Compared with conventional metals shielding material, conducting polymer composite wood
Material (CPCs) has become most application prospect since it has many advantages, such as that at low cost, conductivity is controllable, has wide range of applications
Electromagnetic shielding material [Yan et al.Nanotechnology, 2014,25,145705；Mohammed H et al.,
Carbon,2013,60,146-156]。
Currently, the research of CPCs is mostly concentrated on be with carbon system (carbon black, carbon fiber, carbon nanotube, graphene etc.)
[Hu et al., Carbon, 2012,50,4596-4599 in terms of the composite material preparation of filler；Yan et al.,
Adv.Fun.Mater.,2015,25,559-566].Carbon system filler is with raw material sources are wide, density is low, environmental stability is good, power
The advantages that have excellent performance.However, since carbon system filler self-conductance rate is not high, and easily reunite in the base, poor dispersion,
Therefore when preparing high electromagnet shield effect composite material, required additive amount is larger.Metal packing has excellent electric conductivity,
But the shortcomings of density is big, of high cost makes its application be extremely restricted.In addition, carbon system filler and the magnetic metal packing of tool
It is also not quite similar to shielding electromagnetic waves mechanism.The conductive network that carbon system filler is formed in the base can by reflection, refraction and
Electromagnetic wave absorption plays the role of electromagnetic shielding；And have magnetic metal packing can be by resistance loss, dielectric loss
And magnetic medium loss is come electromagnetic wave of decaying.
During preparing CPCs, amount of filler is reduced, is worked as with obtaining the composite material with more low excess effusion value
Preceding research emphasis.So far, it is to reduce filler to prepare the conducting polymer composite material (s-CPCs) with isolation structure
Dosage most efficient method [Pang et al., Progress in Polymer Science, 2014,39,1908-1933].
Therefore, preparing can have carbon system filler and the electromagnetic shielding of metal packing advantage multiple simultaneously under low sizing content
Condensation material is of great significance.
Invention content
The present invention has both the electromagnetic screen of carbon system filler and metal packing advantage in order to be obtained while reducing filer content
Performance is covered, a kind of ultra-high molecular weight polyethylene/graphite alkene/nickel composite material and its system with high capability of electromagnetic shielding are provided
Preparation Method.
The present invention is achieved by the following technical solutions：A kind of ultra-high molecular weight polyethylene/graphite alkene/nickel composite wood
Material, it is shell structurre, graphene coated ultra-high molecular weight polyethylene for core that the compound particle for preparing composite material, which is using metallic nickel,
Ni-coated graphite alkene coat ultra-high molecular weight polyethylene particle, the wherein content of graphene coated ultra-high molecular weight polyethylene particle
Content for 97.42vol%~98.91vol%, metallic nickel is 1.09vol%~2.58vol%, and wherein graphene is compound
Content in material is at least 0.028vol%.
In order to prove that composite material of the present invention has highly conductive, high capability of electromagnetic shielding, inventor will be described compound
Particle, nickel plating ultra-high molecular weight polyethylene particle, graphene coated ultra-high molecular weight polyethylene particle, graphene coated nickel plating are super
High molecular weight polyethylene particle is respectively put into mold, and hot pressing 10min is molded at 180 DEG C, 10MPa, then multiple to four kinds
The performance of condensation material is studied, and test result is referring to table 1.It can will become apparent from from table:In the total content of graphene and nickel
In the case of identical, graphene has apparent synergistic effect with metallic nickel for composite system, can make composite material
Conductivity and electromagnet shield effect are obviously improved.
The performance comparison of 1 different type composite material of table
In order to further elaborate the compound particle of composite material of the present invention, the present invention provides nickel plating stones
The preparation method of black alkene cladding ultra-high molecular weight polyethylene particle, concrete technology are：Graphene oxide and super high molecular weight are gathered
Ethylene is distributed in ethanol solution, and heating and constant temperature stirring evaporation after drying, heat through hydrazine hydrate reduction, are filtered, washed, dry
It is dry, obtain the ultra-high molecular weight polyethylene particle of graphene coated；By the graphene coated ultra-high molecular weight polyethylene after drying
Particle is added in chemical plating fluid, at 40-80 DEG C, is stirred in ultrasonic water bath, and reducing agent solution is added dropwise to chemical plating
In liquid, the chemical nickel plating of 30-60min is carried out, is washed, filtered, dried later, finally obtains and prepares above-mentioned composite material
Compound particle；
Chemical plating fluid is the NiCl by 10~50g/L among the above2·6H2O, the C of 30~100g/L6H5Na3O7·2H2O、
The NH of 100~300ml/L3·H2Made of O and distilled water；Reducing agent is the NaH by 20~100g/L2PO2·H2O and steaming
Made of distilled water.
In the preparation method of above-mentioned Ni-coated graphite alkene cladding ultra-high molecular weight polyethylene particle, the superelevation point of graphene coated
The step of sub- weight northylen particle is known steps, and parameter known in the art can be used in parameter, therefore herein no longer in detail
It repeats.
When it is implemented, graphene coated ultra-high molecular weight polyethylene particle copes with particle before carrying out nickel chemical plating technology
Surface preparation is carried out, which includes 2 procedure of sensitized treatment and activation process.And according to routine, the technology of this field
Personnel include roughening treatment, sensitized treatment and activation process to needing the material for carrying out chemical plating to generally require the pretreatment of progress
3 procedures.But the graphene layer in graphene coated ultra-high molecular weight polyethylene of the present invention greatly improves superelevation
The surface-active of molecular weight polyethylene need not carry out roughening treatment, greatly simplify chemical plating process.
Preferably, the present invention provides a kind of preparation method of ultra-high molecular weight polyethylene/graphite alkene/nickel composite material,
Concrete technology is：Above-mentioned compound particle is put into mold, hot pressing 5-10min is molded at 180-200 DEG C, 10-15MPa,
Obtain that there is the ultra-high molecular weight polyethylene/graphite of isolation structure and high capability of electromagnetic shielding alkene/nickel electromagnetic shielding composite wood
Material.In mold process, the high viscosity of ultra-high molecular weight polyethylene in the molten state limits the diffusion of shell metallic nickel, rises
Good pile-up and isolation effect are arrived, while Flexible graphene layer compensates for the deficiency of brittleness nickel layer easy fracture, it is final to obtain
With the controllable ultra-high molecular weight polyethylene/graphite alkene/nickel composite material of isolation structure, capability of electromagnetic shielding.
The present invention is by composite material of the preparation with isolation structure, in the extremely low situation of metallic nickel and graphene content
Under, the conductivity and capability of electromagnetic shielding of composite material can be significantly improved, realizes that composite material is highly conductive, high electromagnetic shielding
The target of performance, meanwhile, by changing nickel content, the conductivity and capability of electromagnetic shielding of composite material can be adjusted, is obtained
Ultra-high molecular weight polyethylene/graphite alkene/nickel of conductivity and capability of electromagnetic shielding stabilization, favorable reproducibility is electromagnetically shielded composite wood
Material.
Description of the drawings
Fig. 1 is the conductivity and nickel content graph of relation of ultra-high molecular weight polyethylene/graphite alkene/nickel composite material.From
It can be seen from the figure that, with the increase of nickel content in material, the conductivity of composite material increases therewith, and shows typically to lead
Electric percolation.The conductivity highest of composite material can reach 2679S/m.
Fig. 2 is respectively graphene coated ultra-high molecular weight polyethylene particle and Ni-coated graphite alkene cladding superhigh molecular weight polyethylene
The stereoscan photograph of alkene compound particle (graphene content is 0.1vol%, nickel content 2.58vol%).It can from figure (a)
To find out, the graphene nonwoven fabric from filaments of fold is covered on ultra-high molecular weight polyethylene surface, it can be seen that passing through from figure (b)
Plating is learned, the nickel layer of uniformly continuous densification is formd on the surface of ultra-high molecular weight polyethylene/graphite alkene compound particle.Scheme c, d divides
A, the partial enlarged view of b Wei not schemed.
Fig. 3 be prepared ultra-high molecular weight polyethylene/graphite alkene/nickel composite material (graphene content is 0.1vol%,
Nickel content is 2.58vol%) stereoscan photograph.It can be seen that conductive nickel layer is not all sent out in process from figure a
It gives birth to displacement and falls off, be still located at particle interface, and form perfect conductive network, figure b is the partial enlarged view for scheming a.
Fig. 4 is the electromagnet shield effect and frequency of prepared ultra-high molecular weight polyethylene/graphite alkene/nickel composite material
Relation curve.It can be seen from the figure that when graphene content is 0.1vol%, the electromagnet shield effect of composite material is with nickel
The increase of content and be stepped up, highest can reach 88.16dB.
Specific implementation mode
Embodiment one：
It is 0.1 by volume ratio：99.9 graphene oxide and ultra-high molecular weight polyethylene is distributed in ethanol solution, 90 DEG C
Lower constant temperature stirring evaporation, obtained sample is dried, and then passes through 90 DEG C of stirring reduction 4h of hydrazine hydrate solution, be filtered, washed,
Drying, obtains the ultra-high molecular weight polyethylene particle of graphene coated.
The surface of the ultra-high molecular weight polyethylene particle of graphene coated is pre-processed, including：Sensitization：By graphene
The ultra-high molecular weight polyethylene particle of cladding is added in 100ml sensitizing solutions, and at 30 DEG C, 15min is stirred in ultrasonic water bath, is washed
It washs；Activation：Ultra-high molecular weight polyethylene particle after sensitization is added in 100ml activating solutions, at 30 DEG C, in ultrasonic water bath
15min is stirred, drying for standby is washed.
Wherein sensitizing solution, the process for preparation of activating solution are as follows：
Sensitizing solution：The stannous chloride for weighing 2g is added in 100ml distilled water, and the concentrated hydrochloric acid of the 37wt% of 1ml is added dropwise,
Sensitizing solution is obtained after it is completely dissolved.
Activating solution：The palladium bichloride of 0.1g is dissolved in the concentrated hydrochloric acid of the 37wt% of 1ml, is stirring evenly and then adding into 1000ml
Distilled water stirs evenly until obtaining activating solution after solution clarification.
To the process of the ultra-high molecular weight polyethylene chemistry of particles nickel plating of graphene coated：By the graphite after activation and drying
The ultra-high molecular weight polyethylene particle of alkene cladding is added in the chemical plating fluid of 100ml, at 80 DEG C, is stirred in ultrasonic water bath,
The reducing agent liquid of 10ml is added dropwise in plating solution, the chemical nickel plating of 60min is carried out, washs, filter later, drying, obtaining
The ultra-high molecular weight polyethylene compound particle of metallic nickel and graphene coated.
Chemical plating fluid specifically comprises among the above：The NiCl of 50g/L2·6H2The C of O, 30g/L6H5Na3O7·2H2O,
The NH of 150ml/L3·H2O, solvent are distilled water.Reducing agent liquid specifically comprises：The NaH of 100g/L2PO2·H2O, solvent are
Distilled water.
The ultra-high molecular weight polyethylene particle of obtained metallic nickel and graphene coated is added in mold, 200
DEG C, hot pressing 10min moldings under 15MPa, obtain having the ultra-high molecular weight polyethylene of isolation structure and high capability of electromagnetic shielding/
Graphene/nickel composite material.
Embodiment two：
It is 0.1 by volume ratio：99.9 graphene oxide and ultra-high molecular weight polyethylene is distributed in ethanol solution, 60 DEG C
Lower constant temperature stirring evaporation after drying obtained sample, through 80 DEG C of stirring reduction 3h of hydrazine hydrate solution, is filtered, washed, dries
It is dry, obtain the ultra-high molecular weight polyethylene particle of graphene coated.
The surface of the ultra-high molecular weight polyethylene particle of graphene coated is pre-processed, including：Sensitization：By graphene
The ultra-high molecular weight polyethylene particle of cladding is added in 100ml sensitizing solutions, and at 25 DEG C, 30min is stirred in ultrasonic water bath, is washed
It washs；Activation：Ultra-high molecular weight polyethylene particle after sensitization is added in 100ml activating solutions, temperature is 30 DEG C, in ultrasonic water
30min is stirred in bath, washs drying for standby.
The process for preparation of wherein sensitizing solution, activating solution is as follows：
Sensitizing solution：The stannous chloride for weighing 2g is added in 100ml distilled water, and the concentrated hydrochloric acid of the 37wt% of 1ml is added dropwise,
Sensitizing solution is obtained after it is completely dissolved.
Activating solution：The palladium bichloride of 0.5g is dissolved in the concentrated hydrochloric acid of the 37wt% of 1ml, is stirring evenly and then adding into 1000ml
Distilled water stirs evenly until obtaining activating solution after solution clarification.
To the process of the ultra-high molecular weight polyethylene chemistry of particles nickel plating of graphene coated：By the graphite after activation and drying
The ultra-high molecular weight polyethylene particle of alkene cladding is added in the chemical plating fluid of 100ml, at 60 DEG C, is stirred in ultrasonic water bath,
The reducing agent liquid of 10ml is added dropwise in plating solution, the chemical nickel plating of 60min is carried out, washs, filter later, drying, obtaining
The ultra-high molecular weight polyethylene compound particle of metallic nickel and graphene coated.
Chemical plating fluid specifically comprises among the above：The NiCl of 40g/L2·6H2The C of O, 50g/L6H5Na3O7·2H2O,
The NH of 100ml/L3·H2O, solvent are distilled water.Reducing agent liquid specifically comprises：The NaH of 50g/L2PO2·H2O, solvent are
Distilled water.
The ultra-high molecular weight polyethylene particle of obtained metallic nickel and graphene coated is added in mold, 180
DEG C, hot pressing 10min moldings under 10MPa, obtain having the ultra-high molecular weight polyethylene of isolation structure and high capability of electromagnetic shielding/
Graphene/nickel composite material.
Embodiment three：
It is 0.1 by volume ratio：99.9 graphene oxide and ultra-high molecular weight polyethylene is distributed in ethanol solution, 70 DEG C
Lower constant temperature stirring evaporation after drying obtained sample, through 90 DEG C of stirring reduction 4h of hydrazine hydrate solution, is filtered, washed, dries
It is dry, obtain the ultra-high molecular weight polyethylene particle of graphene coated.
The surface of the ultra-high molecular weight polyethylene particle of graphene coated is pre-processed, including：Sensitization：By graphene
The ultra-high molecular weight polyethylene particle of cladding is added in 100ml sensitizing solutions, and at 25 DEG C, 60min is stirred in ultrasonic water bath, is washed
It washs；Activation：Ultra-high molecular weight polyethylene particle after sensitization is added in 100ml activating solutions, at 30 DEG C, in ultrasonic water bath
60min is stirred, drying for standby is washed.
The process for preparation of wherein sensitizing solution, activating solution is as follows：
Sensitizing solution：The stannous chloride for weighing 2g is added in 100ml distilled water, and the concentrated hydrochloric acid of the 37wt% of 1ml is added dropwise,
Sensitizing solution is obtained after it is completely dissolved.
Activating solution：The palladium bichloride of 0.5g is dissolved in the concentrated hydrochloric acid of the 37wt% of 1ml, is stirring evenly and then adding into 1000ml
Distilled water stirs evenly until obtaining activating solution after solution clarification.
To the process of the ultra-high molecular weight polyethylene chemistry of particles nickel plating of graphene coated：By the graphite after activation and drying
The ultra-high molecular weight polyethylene particle of alkene cladding is added in the chemical plating fluid of 100ml, at 70 DEG C, is stirred in ultrasonic water bath,
The reducing agent liquid of 10ml is added dropwise in plating solution, the chemical nickel plating of 40min is carried out, is washed, filtered, dried later,
Obtain the ultra-high molecular weight polyethylene compound particle of metallic nickel and graphene coated.
Chemical plating fluid specifically comprises among the above：The NiCl of 30g/L2·6H2The C of O, 100g/L6H5Na3O7·2H2O,
The NH of 200ml/L3·H2O, solvent are distilled water.Reducing agent liquid specifically comprises：The NaH of 80g/L2PO2·H2O, solvent are
Distilled water.
The ultra-high molecular weight polyethylene powder of obtained metallic nickel and graphene coated is added in mold, 190
DEG C, hot pressing 5min moldings under 15MPa, obtain having the ultra-high molecular weight polyethylene of isolation structure and high capability of electromagnetic shielding/
Graphene/nickel composite material.
Example IV：
It is 0.1 by volume ratio：99.9 graphene oxide and ultra-high molecular weight polyethylene is distributed in ethanol solution, 80 DEG C
Lower constant temperature stirring evaporation after drying obtained sample, through 85 DEG C of stirring reduction 3.5h of hydrazine hydrate solution, is filtered, washed, dries
It is dry, obtain the ultra-high molecular weight polyethylene particle of graphene coated.
The surface of the ultra-high molecular weight polyethylene particle of graphene coated is pre-processed, including：Sensitization：By graphene
The ultra-high molecular weight polyethylene particle of cladding is added in 100ml sensitizing solutions, and temperature is 25 DEG C, is stirred in ultrasonic water bath
50min, washing；Activation：Ultra-high molecular weight polyethylene particle after sensitization is added in 100ml activating solutions, temperature is 30 DEG C,
50min is stirred in ultrasonic water bath, washs drying for standby.
The process for preparation of wherein sensitizing solution, activating solution is as follows：
Sensitizing solution：The stannous chloride for weighing 2g is added in 100ml distilled water, and the concentrated hydrochloric acid of the 37wt% of 1ml is added dropwise,
Sensitizing solution is obtained after it is completely dissolved.
Activating solution：The palladium bichloride of 1g is dissolved in the concentrated hydrochloric acid of the 37wt% of 1ml, is stirring evenly and then adding into 1000ml steamings
Distilled water stirs evenly until obtaining activating solution after solution clarification.
To the process of the ultra-high molecular weight polyethylene powder chemistry nickel plating of graphene coated：By the graphite after activation and drying
The ultra-high molecular weight polyethylene particle of alkene cladding is added in the chemical plating fluid of 100ml, at 40 DEG C, is stirred in ultrasonic water bath,
The reducing agent liquid of 10ml is added dropwise in plating solution, the chemical nickel plating of 40min is carried out, washs, filter later, drying, obtaining
The ultra-high molecular weight polyethylene compound particle of metallic nickel and graphene coated.
Chemical plating fluid specifically comprises among the above：The NiCl of 10g/L2·6H2The C of O, 30g/L6H5Na3O7·2H2O,
The NH of 100ml/L3·H2O, solvent are distilled water.Reducing agent liquid specifically comprises：The NaH of 20g/L2PO2·H2O, solvent are
Distilled water.
The ultra-high molecular weight polyethylene powder of obtained metallic nickel and graphene coated is added in mold, 185
DEG C, hot pressing 8min moldings under 12MPa, obtain having the ultra-high molecular weight polyethylene of isolation structure and high capability of electromagnetic shielding/
Graphene/nickel composite material.
Embodiment five：
It is 0.028 by volume ratio：99.972 graphene oxide and ultra-high molecular weight polyethylene is distributed in ethanol solution,
Constant temperature stirring evaporation at 80 DEG C after drying obtained sample, through 85 DEG C of stirring reduction 3.5h of hydrazine hydrate solution, is filtered, is washed
It washs, dry, obtain the ultra-high molecular weight polyethylene particle of graphene coated.
The surface of the ultra-high molecular weight polyethylene particle of graphene coated is pre-processed, including：Sensitization：By graphene
The ultra-high molecular weight polyethylene particle of cladding is added in 100ml sensitizing solutions, and temperature is 28 DEG C, is stirred in ultrasonic water bath
50min, washing；Activation：Ultra-high molecular weight polyethylene particle after sensitization is added in 100ml activating solutions, temperature is 25 DEG C,
60min is stirred in ultrasonic water bath, washs drying for standby.
The process for preparation of wherein sensitizing solution, activating solution is as follows：
Sensitizing solution：The stannous chloride for weighing 2g is added in 100ml distilled water, and the concentrated hydrochloric acid of the 37wt% of 1ml is added dropwise,
Sensitizing solution is obtained after it is completely dissolved.
Activating solution：The palladium bichloride of 1g is dissolved in the concentrated hydrochloric acid of the 37wt% of 1ml, is stirring evenly and then adding into 1000ml steamings
Distilled water stirs evenly until obtaining activating solution after solution clarification.
To the process of the ultra-high molecular weight polyethylene chemistry of particles nickel plating of graphene coated：By the graphite after activation and drying
The ultra-high molecular weight polyethylene particle of alkene cladding is added in the chemical plating fluid of 100ml, at 40 DEG C, is stirred in ultrasonic water bath,
The reducing agent liquid of 10ml is added dropwise in plating solution, the chemical nickel plating of 30min is carried out, is washed, filtered, dried later,
Obtain the ultra-high molecular weight polyethylene compound particle of metallic nickel and graphene coated.
Chemical plating fluid specifically comprises among the above：The NiCl of 10g/L2·6H2The C of O, 30g/L6H5Na3O7·2H2O,
The NH of 300ml/L3·H2O, solvent are distilled water.Reducing agent liquid specifically comprises：The NaH of 20g/L2PO2·H2O, solvent are
Distilled water.
The ultra-high molecular weight polyethylene particle of obtained metallic nickel and graphene coated is added in mold, 185
DEG C, hot pressing 8min moldings under 12MPa, obtain having the ultra-high molecular weight polyethylene of isolation structure and high capability of electromagnetic shielding/
Graphene/nickel composite material.
The conductivity of composite material obtained by 2 embodiment one of table to embodiment five
Claims (2)
1. a kind of preparation method of Ni-coated graphite alkene cladding ultra-high molecular weight polyethylene particle, which is characterized in that concrete technology is：
Graphene oxide and ultra-high molecular weight polyethylene are distributed in ethanol solution, heating and constant temperature stirring evaporation, after drying, heating
It through hydrazine hydrate reduction, is filtered, washed, dries, the ultra-high molecular weight polyethylene particle of graphene coated is obtained, to graphene coated
Ultra-high molecular weight polyethylene particle carries out surface preparation, which is sensitized treatment and activation process, after activation
Washing, drying for standby；Graphene coated ultra-high molecular weight polyethylene particle after activation and drying is added in chemical plating fluid,
It at 40-80 DEG C, is stirred in ultrasonic water bath, reducing agent solution is added dropwise in chemical plating fluid, carry out the change of 30-60 min
Nickel plating is learned, is washed, filtered, dried later, finally obtain the compound particle for preparing composite material, it is described to prepare composite wood
The compound particle of material is the Ni-coated graphite alkene packet for core using metallic nickel as shell structurre, graphene coated ultra-high molecular weight polyethylene
Cover ultra-high molecular weight polyethylene particle, wherein the content of graphene coated ultra-high molecular weight polyethylene particle be 97.42 vol% ~
The content of 98.91vol%, metallic nickel are the vol% of 1.09vol% ~ 2.58, and the wherein content of graphene in the composite is at least
0.028 vol%；
The group of chemical plating fluid becomes among the above：The NiCl of 10 ~ 50 g/L2·6H2O, the C of 30 ~ 100 g/L6H5Na3O7·2H2O,
The NH of 100 ~ 300 ml/L3·H2O, solvent are distilled water；The group of reducing agent becomes：The NaH of 20 ~ 100 g/L2PO2·H2O, it is molten
Agent is distilled water.
2. a kind of preparation method of ultra-high molecular weight polyethylene/graphite alkene/nickel composite material, which is characterized in that concrete technology is：
The compound particle a kind of Ni-coated graphite alkene described in claim 1 coated in the preparation method of ultra-high molecular weight polyethylene particle is put
Enter into mold, hot pressing 5-10 min are molded at 180-200 DEG C, 10-15MPa, are obtained with isolation structure and high electromagnetism
Ultra-high molecular weight polyethylene/graphite alkene/nickel electromagnetic shielding composite material of shielding properties.
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| CN106883456B (en) * | 2017-02-09 | 2018-11-02 | 华南理工大学 | A kind of preparation method of polyaminopropylsilsesquioxane doping nickel coated graphene |
| CN107333460B (en) * | 2017-06-30 | 2019-05-10 | 河北大学 | A kind of preparation method of graphene-based metal composite absorbing material |
| CN109233141A (en) * | 2018-07-20 | 2019-01-18 | 浙江农林大学 | A kind of manufacturing process of high shielding charcoal mould plate |
| CN109912866A (en) * | 2019-03-04 | 2019-06-21 | 唐山烯鹏石墨烯科技有限公司 | Butylbenzene particle/graphene/aluminum composite material and preparation method |
| CN110591207B (en) * | 2019-10-28 | 2021-08-31 | 株洲时代新材料科技股份有限公司 | Ultrahigh molecular weight polyethylene/graphene oxide composite material and preparation method thereof |
| CN110918980B (en) * | 2019-12-16 | 2021-09-24 | 北京工商大学 | Electromagnetic shielding composite material and preparation method thereof |
| CN111269560B (en) * | 2020-03-19 | 2022-03-29 | 中北大学 | Nylon 6/expanded graphite/nickel composite material for electromagnetic shielding container and preparation method thereof |
| CN113441712B (en) * | 2021-06-15 | 2023-11-21 | 宁波职业技术学院 | Graphene modified Ni-Cu-Pb composite metal material and preparation method thereof |
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