CN105682442A - Preparation method for light-weight graphite fiber foam nickel electromagnetic shielding material - Google Patents
Preparation method for light-weight graphite fiber foam nickel electromagnetic shielding material Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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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
- C23C18/285—Sensitising or activating with tin based compound or composition
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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
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- 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
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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- H—ELECTRICITY
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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
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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Abstract
The invention relates to a preparation method for a light-weight graphite fiber foam nickel electromagnetic shielding material and belongs to the field of electronic material preparation. The method is characterized by obtaining graphite fiber after carrying out two steps of carbonization and graphitization with polyacrylonitrile fibre being a raw material; then, carrying out chemical nickel plating with porous polyurethane foam being as a substrate to obtain foam nickel; and finally, depositing the graphite fiber to the foam nickel through electrophoretic deposition to obtain the electromagnetic shielding material. In the method, the high-conductivity graphite fiber and the high-permeability metal nickel are utilized as the raw materials, so that a combined shielding effect is achieved; the graphite fiber is utilized to replace metal materials, and the nickel is plated on the polyurethane foam, so that the problems that since conventional metal electromagnetic shielding materials are large in density, cost is expensive and it is difficult to meet the requirement for light weight, and the material is separated out from the substrate easily are solved after compounding; and the method is simple in preparation process, low in cost and suitable for large-scale production and application.
Description
Technical field
The preparation method that the present invention relates to a kind of light weight type graphite fibre nickel foam electromagnetic shielding material, belongs to electronic material preparation field.
Background technology
Developing rapidly of modern electronic technology provides a great convenience to the life of people, also brings serious electromagnetic pollution simultaneously. It not only endangers the healthy of people, also the information security of electronic equipment and the system stability of surrounding devices is constituted a threat to. Developing high performance electromagnetic shielding material is the effective way solving the problems referred to above. In recent years, for adapting to the development trend of electronic equipment lightness and Highgrade integration, lightweight breathable type electromagnetic shielding material is increasingly becoming new study hotspot.
Electromagnetic radiation is ubiquitous, and continue atmospheric pollution, and water pollutes, and is acknowledged as the fourth-largest pollution after noise pollution. Electromagnetic radiation not only results in electromagnetic interference, destroys the properly functioning of electronic electric equipment, and can health be threatened. The electromagnetic shielding material with good shielding has become as the focus of current research, and various countries do a lot of work in the research of Novel shielding material. Filled-type composite electromagnetic shield materials receives much concern due to superior performance, and domestic research in this respect far lags behind abroad, and therefore research novel electromagnetic shielding composite material has important realistic meaning. Electromagnetic shielding refers to electromagnetic pollution source to the electromagnetic wave propagation pathway disruption specified between region, thus reducing or eliminate the harmful effect that the polluter sensitive equipment to specifying in region, device or human body produce. Operation principle according to shielding is different, can be classified as electrostatic screen, magnetic shield and electromagnetic shielding three major types.
Carbon fiber filled polymer can make composite have electric conductivity and good mechanical property, but shield effectiveness is bad, in order to obtain good capability of electromagnetic shielding in broad frequency range, electromagnetic shielding material should be high magnetic permeability and the combination of high conductivity material.
Summary of the invention
The technical problem that present invention mainly solves: mostly be metal system for electromagnetic shielding material traditional at present, and metal based material to there is density big, expensive, be difficult to meet the requirement of light weight, and be prone to from matrix and precipitate out, defect contrary with the development trend of electronic equipment lightness and Highgrade integration, it is provided that the preparation method of a kind of light weight type graphite fibre nickel foam electromagnetic shielding material.The method prepares graphite fibre with polyacrylonitrile fibre for raw material after two-step carbonization and graphitization, carry out chemical nickel plating with cellular polyurethane foam for substrate again and prepare nickel foam, graphite fibre prepares electromagnetic shielding material on electrophoretic deposition to nickel foam the most at last, the present invention makes raw material with the graphite fibre of high conductivity and the metallic nickel of high magnetic permeability, play associating shield effectiveness, wherein replace metal based material with graphite fibre, nickel is plated in polyurethane foam, conventional metals system electromagnetic shielding material density is solved big after composite, expensive, it is difficult to meet the requirement of light weight, and be prone to from matrix precipitate out problem, and preparation process is simple, with low cost, it is suitable for large-scale production to use.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) weigh 500～600g polyacrylonitrile fibre and load oxidation furnace, pre-oxidation 45～60min it is incubated under the oxidizing temperature of 250～300 DEG C, again the fiber after pre-oxidation is moved into retort, first it is warming up to 300～500 DEG C of low-temperature carbonization 15～25min with 5 DEG C/min rate program, again with 10 DEG C/min ramp to 900～1000 DEG C, high temperature carbonization 10～20min, obtains polyacrylonitrile carbon fiber;
(2) above-mentioned prepared polyacrylonitrile carbon fiber is proceeded to graphitizing furnace, in stove, pass into argon with 10mL/min speed until displacement come out of the stove in after all air, graphitization processing 2～3min at the temperature of 2500～3000 DEG C, obtains graphite fibre after discharging, standby;
(3) take 100～200g polyurethane foam put in pulverizer pulverize after cross 50 mesh standard sieves, polyurethane foam particles after sieving is immersed in the potassium permanganate sulfuric acid solution that 400～500mL mass concentration is 10%, stirring alligatoring 3～5min, foam beads and 20～30g stannic chloride mixing addition 100～200mL concentration are 0.1mol/L hydrochloric acid after terminating by alligatoring, stir sensitization 10～15min;
(4) foam beads after above-mentioned sensitization is soaked 3～5min with 500～600mL formaldehyde and the potassium dihydrogen phosphate that isopyknic mass concentration is 30% respectively, finally with namely obtaining pretreated foam beads after deionized water rinsing 10～20min;
(5) measuring 1～2L mass concentration is that 40% nickel sulfate solution is poured in electroless plating tank, sequentially add 10～20g ammonium chloride and 3～5g sodium citrate, after stirring again with mass concentration be 25% ammonia regulate pH to 8～9, pour above-mentioned for 200～300g pretreated foam beads into coating bath again, adding thermal plating bath temperature to 25～35 DEG C, startup Vltrasonic device is cleaned with deionized water and dries after carrying out chemical nickel plating 20～30min, prepare nickel foam, standby;
(6) pour in 200～300mL acetone after weighing 10～20g graphite fibre and 10～15g magnesium nitrate powder mix homogeneously, after disperseing 2～3h with ultrasonic disperse instrument with 200～300W power ultrasonic, join to obtain graphite fibre electrophoresis liquid;
(7) above-mentioned prepared electrophoresis liquid is loaded in electrophoresis tank, using the metal platinized platinum of 20mm × 2mm × 1mm as anode, again standby nickel foam it is hot pressed into the specification of 20mm × 5mm × 2mm and it can be used as negative electrode, distance between regulating YIN and YANG two-stage is 2～3cm, start DC source electrophoretic deposition under 50～60V voltage to process after 1～2h, take out the nickel foam after deposited graphite fiber, put into baking oven dry 2～3h at 105～110 DEG C, obtain light weight type graphite fibre nickel foam electromagnetic shielding material.
The concrete application process of the present invention: electronic component, circuit, combination gold, cable or whole system interference source are coated with by the electromagnetic shielding material prepared by the present invention, after testing, in 8～12GHz frequency, the electromagnetic shielding material that the present invention prepares is with absorption loss for main shielding mechanism, its electromagnet shield effect is between 12～14dB, than shielding properties up to 128～130dB cm3·g-1。
The invention has the beneficial effects as follows: the present invention makes raw material with the graphite fibre of high conductivity and the metallic nickel of high magnetic permeability, play associating shield effectiveness, wherein replace metal based material with graphite fibre, nickel is plated in polyurethane foam, solves conventional metals system electromagnetic shielding material density after composite big, expensive, be difficult to meet the requirement of light weight, and be prone to from matrix precipitate out problem, and preparation process is simple, with low cost, it is suitable for large-scale production and uses.
Detailed description of the invention
Weigh 500～600g polyacrylonitrile fibre and load oxidation furnace, pre-oxidation 45～60min it is incubated under the oxidizing temperature of 250～300 DEG C, again the fiber after pre-oxidation is moved into retort, first it is warming up to 300～500 DEG C of low-temperature carbonization 15～25min with 5 DEG C/min rate program, again with 10 DEG C/min ramp to 900～1000 DEG C, high temperature carbonization 10～20min, obtains polyacrylonitrile carbon fiber; Above-mentioned prepared polyacrylonitrile carbon fiber is proceeded to graphitizing furnace, in stove, pass into argon with 10mL/min speed until displacement come out of the stove in after all air, graphitization processing 2～3min at the temperature of 2500～3000 DEG C, obtain graphite fibre after discharging, standby; Take 100～200g polyurethane foam put in pulverizer pulverize after cross 50 mesh standard sieves, polyurethane foam particles after sieving is immersed in the potassium permanganate sulfuric acid solution that 400～500mL mass concentration is 10%, stirring alligatoring 3～5min, foam beads and 20～30g stannic chloride mixing addition 100～200mL concentration are 0.1mol/L hydrochloric acid after terminating by alligatoring, stir sensitization 10～15min; Foam beads after above-mentioned sensitization is soaked 3～5min with 500～600mL formaldehyde and the potassium dihydrogen phosphate that isopyknic mass concentration is 30% respectively, finally with namely obtaining pretreated foam beads after deionized water rinsing 10～20min; Measuring 1～2L mass concentration is that 40% nickel sulfate solution is poured in electroless plating tank, sequentially add 10～20g ammonium chloride and 3～5g sodium citrate, after stirring again with mass concentration be 25% ammonia regulate pH to 8～9, pour above-mentioned for 200～300g pretreated foam beads into coating bath again, adding thermal plating bath temperature to 25～35 DEG C, startup Vltrasonic device is cleaned with deionized water and dries after carrying out chemical nickel plating 20～30min, prepare nickel foam, standby; Pour in 200～300mL acetone after weighing 10～20g graphite fibre and 10～15g magnesium nitrate powder mix homogeneously, after disperseing 2～3h with ultrasonic disperse instrument with 200～300W power ultrasonic, join to obtain graphite fibre electrophoresis liquid; Above-mentioned prepared electrophoresis liquid is loaded in electrophoresis tank, using the metal platinized platinum of 20mm × 2mm × 1mm as anode, again standby nickel foam it is hot pressed into the specification of 20mm × 5mm × 2mm and it can be used as negative electrode, distance between regulating YIN and YANG two-stage is 2～3cm, start DC source electrophoretic deposition under 50～60V voltage to process after 1～2h, take out the nickel foam after deposited graphite fiber, put into baking oven dry 2～3h at 105～110 DEG C, obtain light weight type graphite fibre nickel foam electromagnetic shielding material.
Example 1
Weigh 500g polyacrylonitrile fibre and load oxidation furnace, pre-oxidation 45min it is incubated under the oxidizing temperature of 250 DEG C, again the fiber after pre-oxidation is moved into retort, first it is warming up to 300 DEG C of low-temperature carbonization 15min with 5 DEG C/min rate program, again with 10 DEG C/min ramp to 900 DEG C, high temperature carbonization 10min, obtains polyacrylonitrile carbon fiber; Above-mentioned prepared polyacrylonitrile carbon fiber is proceeded to graphitizing furnace, in stove, pass into argon with 10mL/min speed until displacement come out of the stove in after all air, graphitization processing 2min at the temperature of 2500 DEG C, obtain graphite fibre after discharging, standby; Take 100g polyurethane foam put in pulverizer pulverize after cross 50 mesh standard sieves, polyurethane foam particles after sieving is immersed in the potassium permanganate sulfuric acid solution that 400mL mass concentration is 10%, stirring alligatoring 3min, it is 0.1mol/L hydrochloric acid that foam beads and 20g stannic chloride are mixed addition 100mL concentration after terminating by alligatoring, stirs sensitization 10min; Foam beads after above-mentioned sensitization is soaked 3min with 500mL formaldehyde and the potassium dihydrogen phosphate that isopyknic mass concentration is 30% respectively, finally with namely obtaining pretreated foam beads after deionized water rinsing 10min; Measuring 1L mass concentration is that 40% nickel sulfate solution is poured in electroless plating tank, sequentially add 10g ammonium chloride and 3g sodium citrate, after stirring again with mass concentration be 25% ammonia regulate pH to 8, pour above-mentioned for 200g pretreated foam beads into coating bath again, adding thermal plating bath temperature to 25 DEG C, startup Vltrasonic device is cleaned with deionized water and dries after carrying out chemical nickel plating 20min, prepare nickel foam, standby; Pour in 200mL acetone after weighing 10g graphite fibre and 10g magnesium nitrate powder mix homogeneously, after disperseing 2h with ultrasonic disperse instrument with 200W power ultrasonic, join to obtain graphite fibre electrophoresis liquid; Above-mentioned prepared electrophoresis liquid is loaded in electrophoresis tank, using the metal platinized platinum of 20mm × 2mm × 1mm as anode, again standby nickel foam it is hot pressed into the specification of 20mm × 5mm × 2mm and it can be used as negative electrode, distance between regulating YIN and YANG two-stage is 2cm, start DC source electrophoretic deposition under 50V voltage to process after 1h, take out the nickel foam after deposited graphite fiber, put into baking oven dry 2h at 105 DEG C, obtain light weight type graphite fibre nickel foam electromagnetic shielding material.
The concrete application process of the present invention: electronic component, circuit, combination gold, cable or whole system interference source are coated with by the electromagnetic shielding material prepared by the present invention, after testing, in 8GHz frequency, the electromagnetic shielding material that the present invention prepares is with absorption loss for main shielding mechanism, its electromagnet shield effect is between 12dB, than shielding properties up to 128dB cm3·g-1。
Example 2
Weigh 550g polyacrylonitrile fibre and load oxidation furnace, pre-oxidation 55min it is incubated under the oxidizing temperature of 280 DEG C, again the fiber after pre-oxidation is moved into retort, first it is warming up to 400 DEG C of low-temperature carbonization 20min with 5 DEG C/min rate program, again with 10 DEG C/min ramp to 950 DEG C, high temperature carbonization 15min, obtains polyacrylonitrile carbon fiber; Above-mentioned prepared polyacrylonitrile carbon fiber is proceeded to graphitizing furnace, in stove, pass into argon with 10mL/min speed until displacement come out of the stove in after all air, graphitization processing 2min at the temperature of 2800 DEG C, obtain graphite fibre after discharging, standby; Take 150g polyurethane foam put in pulverizer pulverize after cross 50 mesh standard sieves, polyurethane foam particles after sieving is immersed in the potassium permanganate sulfuric acid solution that 450mL mass concentration is 10%, stirring alligatoring 4min, it is 0.1mol/L hydrochloric acid that foam beads and 25g stannic chloride are mixed addition 150mL concentration after terminating by alligatoring, stirs sensitization 13min;Foam beads after above-mentioned sensitization is soaked 4min with 550mL formaldehyde and the potassium dihydrogen phosphate that isopyknic mass concentration is 30% respectively, finally with namely obtaining pretreated foam beads after deionized water rinsing 15min; Measuring 1L mass concentration is that 40% nickel sulfate solution is poured in electroless plating tank, sequentially add 15g ammonium chloride and 4g sodium citrate, after stirring again with mass concentration be 25% ammonia regulate pH to 8, pour above-mentioned for 250g pretreated foam beads into coating bath again, adding thermal plating bath temperature to 30 DEG C, startup Vltrasonic device is cleaned with deionized water and dries after carrying out chemical nickel plating 25min, prepare nickel foam, standby; Pour in 250mL acetone after weighing 15g graphite fibre and 13g magnesium nitrate powder mix homogeneously, after disperseing 2h with ultrasonic disperse instrument with 250W power ultrasonic, join to obtain graphite fibre electrophoresis liquid; Above-mentioned prepared electrophoresis liquid is loaded in electrophoresis tank, using the metal platinized platinum of 20mm × 2mm × 1mm as anode, again standby nickel foam it is hot pressed into the specification of 20mm × 5mm × 2mm and it can be used as negative electrode, distance between regulating YIN and YANG two-stage is 2cm, start DC source electrophoretic deposition under 55V voltage to process after 1h, take out the nickel foam after deposited graphite fiber, put into baking oven dry 2h at 108 DEG C, obtain light weight type graphite fibre nickel foam electromagnetic shielding material.
The concrete application process of the present invention: electronic component, circuit, combination gold, cable or whole system interference source are coated with by the electromagnetic shielding material prepared by the present invention, after testing, in 10GHz frequency, the electromagnetic shielding material that the present invention prepares is with absorption loss for main shielding mechanism, its electromagnet shield effect is between 13dB, than shielding properties up to 129dB cm3·g-1。
Example 3
Weigh 600g polyacrylonitrile fibre and load oxidation furnace, pre-oxidation 60min it is incubated under the oxidizing temperature of 300 DEG C, again the fiber after pre-oxidation is moved into retort, first it is warming up to 500 DEG C of low-temperature carbonization 25min with 5 DEG C/min rate program, again with 10 DEG C/min ramp to 1000 DEG C, high temperature carbonization 20min, obtains polyacrylonitrile carbon fiber; Above-mentioned prepared polyacrylonitrile carbon fiber is proceeded to graphitizing furnace, in stove, pass into argon with 10mL/min speed until displacement come out of the stove in after all air, graphitization processing 3min at the temperature of 3000 DEG C, obtain graphite fibre after discharging, standby; Take 200g polyurethane foam put in pulverizer pulverize after cross 50 mesh standard sieves, polyurethane foam particles after sieving is immersed in the potassium permanganate sulfuric acid solution that 500mL mass concentration is 10%, stirring alligatoring 5min, it is 0.1mol/L hydrochloric acid that foam beads and 30g stannic chloride are mixed addition 200mL concentration after terminating by alligatoring, stirs sensitization 15min; Foam beads after above-mentioned sensitization is soaked 5min with 600mL formaldehyde and the potassium dihydrogen phosphate that isopyknic mass concentration is 30% respectively, finally with namely obtaining pretreated foam beads after deionized water rinsing 20min; Measuring 2L mass concentration is that 40% nickel sulfate solution is poured in electroless plating tank, sequentially add 20g ammonium chloride and 5g sodium citrate, after stirring again with mass concentration be 25% ammonia regulate pH to 9, pour above-mentioned for 300g pretreated foam beads into coating bath again, adding thermal plating bath temperature to 35 DEG C, startup Vltrasonic device is cleaned with deionized water and dries after carrying out chemical nickel plating 30min, prepare nickel foam, standby; Pour in 300mL acetone after weighing 20g graphite fibre and 15g magnesium nitrate powder mix homogeneously, after disperseing 3h with ultrasonic disperse instrument with 300W power ultrasonic, join to obtain graphite fibre electrophoresis liquid;Above-mentioned prepared electrophoresis liquid is loaded in electrophoresis tank, using the metal platinized platinum of 20mm × 2mm × 1mm as anode, again standby nickel foam it is hot pressed into the specification of 20mm × 5mm × 2mm and it can be used as negative electrode, distance between regulating YIN and YANG two-stage is 3cm, start DC source electrophoretic deposition under 60V voltage to process after 2h, take out the nickel foam after deposited graphite fiber, put into baking oven dry 3h at 110 DEG C, obtain light weight type graphite fibre nickel foam electromagnetic shielding material.
The concrete application process of the present invention: electronic component, circuit, combination gold, cable or whole system interference source are coated with by the electromagnetic shielding material prepared by the present invention, after testing, in 12GHz frequency, the electromagnetic shielding material that the present invention prepares is with absorption loss for main shielding mechanism, its electromagnet shield effect is between 14dB, than shielding properties up to 130dB cm3·g-1。
Claims (1)
1. the preparation method of a light weight type graphite fibre nickel foam electromagnetic shielding material, it is characterised in that concrete preparation process is:
(1) weigh 500～600g polyacrylonitrile fibre and load oxidation furnace, pre-oxidation 45～60min it is incubated under the oxidizing temperature of 250～300 DEG C, again the fiber after pre-oxidation is moved into retort, first it is warming up to 300～500 DEG C of low-temperature carbonization 15～25min with 5 DEG C/min rate program, again with 10 DEG C/min ramp to 900～1000 DEG C, high temperature carbonization 10～20min, obtains polyacrylonitrile carbon fiber;
(2) above-mentioned prepared polyacrylonitrile carbon fiber is proceeded to graphitizing furnace, in stove, pass into argon with 10mL/min speed until displacement come out of the stove in after all air, graphitization processing 2～3min at the temperature of 2500～3000 DEG C, obtains graphite fibre after discharging, standby;
(3) take 100～200g polyurethane foam put in pulverizer pulverize after cross 50 mesh standard sieves, polyurethane foam particles after sieving is immersed in the potassium permanganate sulfuric acid solution that 400～500mL mass concentration is 10%, stirring alligatoring 3～5min, foam beads and 20～30g stannic chloride mixing addition 100～200mL concentration are 0.1mol/L hydrochloric acid after terminating by alligatoring, stir sensitization 10～15min;
(4) foam beads after above-mentioned sensitization is soaked 3～5min with 500～600mL formaldehyde and the potassium dihydrogen phosphate that isopyknic mass concentration is 30% respectively, finally with namely obtaining pretreated foam beads after deionized water rinsing 10～20min;
(5) measuring 1～2L mass concentration is that 40% nickel sulfate solution is poured in electroless plating tank, sequentially add 10～20g ammonium chloride and 3～5g sodium citrate, after stirring again with mass concentration be 25% ammonia regulate pH to 8～9, pour above-mentioned for 200～300g pretreated foam beads into coating bath again, adding thermal plating bath temperature to 25～35 DEG C, startup Vltrasonic device is cleaned with deionized water and dries after carrying out chemical nickel plating 20～30min, prepare nickel foam, standby;
(6) pour in 200～300mL acetone after weighing 10～20g graphite fibre and 10～15g magnesium nitrate powder mix homogeneously, after disperseing 2～3h with ultrasonic disperse instrument with 200～300W power ultrasonic, join to obtain graphite fibre electrophoresis liquid;
(7) above-mentioned prepared electrophoresis liquid is loaded in electrophoresis tank, using the metal platinized platinum of 20mm × 2mm × 1mm as anode, again standby nickel foam it is hot pressed into the specification of 20mm × 5mm × 2mm and it can be used as negative electrode, distance between regulating YIN and YANG two-stage is 2～3cm, start DC source electrophoretic deposition under 50～60V voltage to process after 1～2h, take out the nickel foam after deposited graphite fiber, put into baking oven dry 2～3h at 105～110 DEG C, obtain light weight type graphite fibre nickel foam electromagnetic shielding material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610208973.3A CN105682442A (en) | 2016-04-06 | 2016-04-06 | Preparation method for light-weight graphite fiber foam nickel electromagnetic shielding material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610208973.3A CN105682442A (en) | 2016-04-06 | 2016-04-06 | Preparation method for light-weight graphite fiber foam nickel electromagnetic shielding material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106334562A (en) * | 2016-09-21 | 2017-01-18 | 郑州峰泰纳米材料有限公司 | Photocatalytic material with nano TiO2 loaded on graphene-foamed nickel and preparation method of photocatalytic material |
| CN106391024A (en) * | 2016-09-21 | 2017-02-15 | 郑州峰泰纳米材料有限公司 | Photocatalytic material of carbon nano tube-foam nickel loaded nanometer TiO3 and preparation method thereof |
| CN106517141A (en) * | 2016-12-27 | 2017-03-22 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Novel hair charring method |
| CN110572997A (en) * | 2019-08-13 | 2019-12-13 | 西安理工大学 | preparation method of novel foam carbon electromagnetic shielding composite material |
| CN110820031A (en) * | 2019-11-19 | 2020-02-21 | 有研工程技术研究院有限公司 | Preparation method of miniature getter |
| CN112624104A (en) * | 2021-01-08 | 2021-04-09 | 中国林业科学研究院林产化学工业研究所 | Preparation method of wood fiber-based high-conductivity carbon material |
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2016
- 2016-04-06 CN CN201610208973.3A patent/CN105682442A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106334562A (en) * | 2016-09-21 | 2017-01-18 | 郑州峰泰纳米材料有限公司 | Photocatalytic material with nano TiO2 loaded on graphene-foamed nickel and preparation method of photocatalytic material |
| CN106391024A (en) * | 2016-09-21 | 2017-02-15 | 郑州峰泰纳米材料有限公司 | Photocatalytic material of carbon nano tube-foam nickel loaded nanometer TiO3 and preparation method thereof |
| CN106517141A (en) * | 2016-12-27 | 2017-03-22 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Novel hair charring method |
| CN110572997A (en) * | 2019-08-13 | 2019-12-13 | 西安理工大学 | preparation method of novel foam carbon electromagnetic shielding composite material |
| CN110572997B (en) * | 2019-08-13 | 2020-08-18 | 西安理工大学 | Preparation method of novel foam carbon electromagnetic shielding composite material |
| CN110820031A (en) * | 2019-11-19 | 2020-02-21 | 有研工程技术研究院有限公司 | Preparation method of miniature getter |
| CN112624104A (en) * | 2021-01-08 | 2021-04-09 | 中国林业科学研究院林产化学工业研究所 | Preparation method of wood fiber-based high-conductivity carbon material |
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