CN103817323A - Nickel-coated graphite electric conduction powder used for electric conduction rubber and manufacturing method thereof - Google Patents
Nickel-coated graphite electric conduction powder used for electric conduction rubber and manufacturing method thereof Download PDFInfo
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- CN103817323A CN103817323A CN201410097071.8A CN201410097071A CN103817323A CN 103817323 A CN103817323 A CN 103817323A CN 201410097071 A CN201410097071 A CN 201410097071A CN 103817323 A CN103817323 A CN 103817323A
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Abstract
The invention concretely discloses a nickel-coated graphite electric conduction powder used for electric conduction rubber and a manufacturing method of the nickel-coated graphite electric conduction powder. The nickel-coated graphite electric conduction powder used for the electric conduction rubber comprises 50-80% of nickel and 20-50% of graphite. The manufacturing method of the nickel-coated graphite electric conduction powder used for the electric conduction rubber mainly includes the four steps of oil removing treatment on graphite powder, acid etching and roughening treatment on the graphite powder, surface activating treatment on the graphite powder and chemical nickel plating. The nickel-coated graphite electric conduction powder has the advantages of pure nickel and pure graphite, is low in cost and not prone to rusting and further can improve the mechanical strength of the electric conduction rubber material. The chemical nickel plating method is easy to operate and simple in technology, plated layers are even and compact, the throwing power is high, plating can be performed on particles in any shape, the covering power is high, and the even, fine and dispersed composite powder can be manufactured.
Description
Technical field
The invention belongs to a kind of electromagnetic shielding conductive powder body and preparation method thereof, be specifically related to a kind of conductive rubber nickel bag graphite conductive powder body and preparation method thereof.
Background technology
In recent years, along with popularizing of various electrical equipment, the extensive uses such as computer, communications satellite, grid and some medical equipments, especially along with the microminiaturization of electronic circuit and element, integrated, lightweight and digitlization, cause electronic product used in everyday to be subject to external electromagnetic wave interference and occur malfunction.Therefore, electromagnetic shielding and absorbing material will become new material in application, and conductive filler is the main raw material(s) that forms high-performance electromagnetic wave shielding and absorbing material.But current conductive filler all exists some defects, for example, copper is coating good conductivity, but non-oxidizability is poor; Silver powder good conductivity, but expensive; Conduction nickel powder has good conductive magneto-conductive combination property, but exist, metal packing density is large, high in cost of production problem, nickel powder is in the time making conductive rubber simultaneously, its surface resistivity is the height of conductive rubber than copper, and being not so good as copper at the shield effectiveness of low frequency range (< 30MHz) is conductive rubber.
Summary of the invention
The present invention proposes for addressing the above problem, and its objective is a kind of conductive rubber nickel bag graphite conductive powder body and preparation method thereof is provided.
The technical solution used in the present invention is:
A kind of conductive rubber nickel bag graphite conductive powder body, component and percentage by weight that nickel bag graphite conductive powder body comprises are as follows:
Nickel 50 ~ 80%
Graphite 20 ~ 50%.
Described graphite powder shape of particle is fibrous, irregular sheet, and the average grain diameter of graphite powder particle is 50 ~ 130 microns, and described nickel is coated on the surface of graphite powder.
A preparation method for nickel bag graphite conductive powder body for conductive rubber, comprises the steps:
(I) powdered graphite oil removal treatment
At ambient temperature, powdered graphite is cleaned with degreasing fluid, scavenging period is 10 ~ 15 minutes;
The roughening treatment of (II) powdered graphite acid etching
Powdered graphite after oil removing is cleaned with clear water, then under the condition of 40 ~ 50 ℃, acid etching roughening treatment is carried out in powdered graphite surface with coarsening solution, coarsening time is 10～20 minutes;
(III) powdered graphite surface activation process
Powdered graphite after alligatoring is cleaned with clear water, then use activating solution to carry out surface activation process, under the condition of 35 ~ 45 ℃, put into powdered graphite, stir 20 minutes;
(IV) chemical nickel plating
Powdered graphite after activation processing is cleaned with clear water, then use chemical nickel-plating liquid to carry out nickel plating, plated and powder has been rinsed to neutral with clear water afterwards, after oven dry, obtain conductive rubber nickel bag graphite conductive powder body.
Described degreasing fluid component and concentration are as follows:
Dodecyl Polyoxyethylene Ether sodium sulphate 6～8g/L
NPE 3～4g/L.
Described coarsening solution component and concentration are as follows:
K
2CrO
7 110～120g/L
Dense H
2sO
4400～500g/L.
Described activating solution component and concentration are as follows:
PdCl
2 1.0～1.2g/L
SnCl
2·2H
2O 70～80g/L
Dense HCl 300～320g/L
Na
2SnO
3·7H
2O 7.5～8.0g/L。
Chemical nickel-plating liquid in described step (IV) is by forming in main salt, reducing agent, complexing agent, buffer and stabilizing agent.
Described chemical nickel-plating liquid also comprises PH regulator solution, and described PH regulator solution is dense HCl or ammonium hydroxide.
Main salt in described chemical nickel-plating liquid refers to nickelous sulfate; Reducing agent in described chemical nickel-plating liquid refers to sodium hypophosphite; Complexing agent in described chemical nickel-plating liquid refers to the one in natrium citricum or citric acid; Buffer in described chemical nickel-plating liquid refers to the one in ammonium chloride or sodium acetate; Stabilizing agent in described chemical nickel-plating liquid is plumbi nitras.
In described chemical nickel-plating liquid, the concentration of main salt nickelous sulfate is 20g/L ~ 34g/L; In described chemical nickel-plating liquid, the concentration of reducing agent sodium hypophosphite is 20g/L ~ 30g/L; The concentration of described Complexing Agent in Electroless Nickel Deposition Baths natrium citricum is 10g/L, and the concentration of citric acid is 10g/L; In described chemical nickel-plating liquid, the concentration of buffer sodium acetate is 10 g/L, and the concentration of ammonium chloride is 10 g/L; In described chemical nickel-plating liquid, the concentration of stabilizing agent plumbi nitras is 2.5mg/L ~ 3mg/L.
Nickel bag graphite conductive powder body density in the present invention is low, cost is low and non-corrosive, can also improve the mechanical strength of conductive rubber material.And electroless plating method is easy to operate, technique is simple, coating even compact, covering power are strong, can carry out plating on the particle of any shape, covering power is good, can prepare composite granule even, tiny, dispersion.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the conductive rubber nickel bag flake graphite conducting powder of preparation in the embodiment of the present invention 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of the fibrous graphite powder of conductive rubber nickel bag of preparation in the embodiment of the present invention 2.
The specific embodiment
Referring to drawings and Examples, the present invention will be described in detail:
A kind of conductive rubber nickel bag graphite conductive powder body, component and percentage by weight that nickel bag graphite conductive powder body comprises are as follows:
Nickel 50 ~ 80%
Graphite 20 ~ 50%.
Described graphite powder shape of particle is fibrous, irregular sheet, and the average grain diameter of graphite powder particle is 50 ~ 130 microns, and described nickel is coated on the surface of graphite powder.
A preparation method for nickel bag graphite conductive powder body for conductive rubber, comprises the steps:
(I) powdered graphite oil removal treatment
At ambient temperature, powdered graphite is cleaned with degreasing fluid, scavenging period is 10 ~ 15 minutes;
The roughening treatment of (II) powdered graphite acid etching
Powdered graphite after oil removing is cleaned with clear water, then under the condition of 40 ~ 50 ℃, acid etching roughening treatment is carried out in powdered graphite surface with coarsening solution, coarsening time is 10～20 minutes;
(III) powdered graphite surface activation process
Powdered graphite after alligatoring is cleaned with clear water, then use activating solution to carry out surface activation process, under the condition of 35 ~ 45 ℃, put into powdered graphite, stir 20 minutes;
(IV) chemical nickel plating
Powdered graphite after activation processing is cleaned with clear water, then use chemical nickel-plating liquid to carry out nickel plating, plated and powder has been rinsed to neutral with clear water afterwards, after oven dry, obtain conductive rubber nickel bag graphite conductive powder body.
Described degreasing fluid component and concentration are as follows:
Dodecyl Polyoxyethylene Ether sodium sulphate 6～8g/L
NPE 3～4g/L.
Described coarsening solution component and concentration are as follows:
K
2CrO
7 110～120g/L
Dense H
2sO
4400～500g/L.
Described activating solution component and concentration are as follows:
PdCl
2 1.0～1.2g/L
SnCl
2·2H
2O 70～80g/L
Dense HCl 300～320g/L
Na
2SnO
3·7H
2O 7.5～8.0g/L。
Chemical nickel-plating liquid in described step (IV) is by forming in main salt, reducing agent, complexing agent, buffer and stabilizing agent.
Described chemical nickel-plating liquid also comprises PH regulator solution, and described PH regulator solution is dense HCl or ammonium hydroxide.
Main salt in described chemical nickel-plating liquid refers to nickelous sulfate; Reducing agent in described chemical nickel-plating liquid refers to sodium hypophosphite; Complexing agent in described chemical nickel-plating liquid refers to the one in natrium citricum or citric acid; In chemical nickel-plating liquid, buffer refers to the one in ammonium chloride or sodium acetate; Stabilizing agent in described chemical nickel-plating liquid is plumbi nitras.
Main salt in described chemical nickel-plating liquid can also be any one in nickel chloride or nickel acetate; Reducing agent in described chemical nickel-plating liquid can also be one or more in hydrazine hydrate, sodium borohydride, amido borine or hydrazine sulfate; Complexing agent in described chemical nickel-plating liquid can also be one or more in glycolic, lactic acid, malic acid, propionic acid, glycine or aminoacetic acid; Buffer in described chemical nickel-plating liquid can also be in ammonium borate; Stabilizing agent in described chemical nickel-plating liquid can also be one or more in thiocarbamide, Potassiumiodate or maleic acid.
In described chemical nickel-plating liquid, the concentration of main salt nickelous sulfate is 20g/L ~ 34g/L; In described chemical nickel-plating liquid, the concentration of reducing agent sodium hypophosphite is 20g/L ~ 30g/L; The concentration of described Complexing Agent in Electroless Nickel Deposition Baths natrium citricum is 10g/L, and the concentration of citric acid is 10g/L; In described chemical nickel-plating liquid, the concentration of buffer sodium acetate is 10 g/L, and the concentration of ammonium chloride is 10 g/L; In described chemical nickel-plating liquid, the concentration of stabilizing agent plumbi nitras is 2.5mg/L ~ 3mg/L.
Embodiment 1
A kind of conductive rubber nickel bag graphite conductive powder body, the component and the percentage by weight that comprise are as follows:
Nickel 50%
Graphite 50%.
The average grain diameter of graphite powder particle is 50 microns, and graphite powder shape of particle is irregular sheet, and described nickel is coated on the surface of graphite powder.
A kind of conductive rubber comprises the steps: by the preparation method of nickel bag graphite conductive powder body
(I) powdered graphite oil removal treatment
At ambient temperature, get the flake graphite powder of 50 microns of the average grain diameters of 10 grams, to Dodecyl Polyoxyethylene Ether sodium sulphate 6g/L for powdered graphite, the degreasing fluid 500ml that NPE 3g/L is mixed with cleans, and scavenging period is 10 minutes;
The roughening treatment of (II) powdered graphite acid etching
Distilled water for powdered graphite after oil removing is cleaned 3 minutes, then under the condition of 40 ~ 50 ℃, the K that is 110g/L by volumetric concentration
2crO
7, the dense H that volumetric concentration is 400g/L
2sO
4the coarsening solution 500ml being mixed with, carries out acid etching roughening treatment to the powdered graphite surface after oil removing, and coarsening time is 10～20 minutes;
(III) powdered graphite surface activation process
Powdered graphite after alligatoring is cleaned 3 minutes with distilled water, with the PdCl of volumetric concentration 1.0g/L
2, the SnCl of volumetric concentration 70g/L
22H
2o, the dense HCl of volumetric concentration 300g/L and the Na of volumetric concentration 7.5g/L
2snO
37H
2the activating solution 500ml that O is mixed with, under the condition of 35 ~ 45 ℃, puts into the powdered graphite after roughening treatment, stirs 20 minutes;
(IV) chemical nickel plating
The preparation of chemical nickel-plating liquid: take the nickelous sulfate of 282 grams, the sodium hypophosphite of 160 grams, the citric acid of 80 grams, the plumbi nitras of the sodium acetate of 80 grams and 20 milligrams, dissolves with a small amount of distilled water respectively; Then by consoluet nickel salt solution, under constantly stirring, be poured in the solution containing citric acid; Add again sodium hypophosphite solution, and continuous vigorous stirring; Then add successively lead nitrate solution, SAS; Then with distilled water diluting to 8 liter, finally with dense HCl, the pH value of solution is adjusted to 4.5, and stand-by after filtering with filter.
Powdered graphite after activation processing is cleaned 3 minutes with distilled water, then use chemical nickel-plating liquid to carry out nickel plating, plated and powder has been rinsed to neutral with clear water afterwards, after 80 ℃ of oven dry, obtain conductive rubber nickel bag graphite conductive powder body.
Fig. 1 is the scanning electron microscope (SEM) photograph of the conductive rubber nickel bag flake graphite conducting powder of preparation in the embodiment of the present invention 1.
Embodiment 2
A kind of conductive rubber nickel bag graphite conductive powder body, the component and the percentage by weight that comprise are as follows:
Nickel 80%
Graphite 20%.
The average grain diameter of graphite powder particle is 130 microns, and graphite powder shape of particle is fibrous, and described nickel is coated on the surface of graphite powder.
A kind of conductive rubber comprises the steps: by the preparation method of nickel bag graphite conductive powder body
(I) powdered graphite oil removal treatment
At ambient temperature, get the deep-fried twisted dough sticks shape powdered graphite of 130 microns of the average grain diameters of 10 grams, to Dodecyl Polyoxyethylene Ether sodium sulphate 8g/L for powdered graphite, the degreasing fluid 500ml that NPE 4g/L is mixed with cleans, and scavenging period is 15 minutes;
The roughening treatment of (II) powdered graphite acid etching
Distilled water for powdered graphite after oil removing is cleaned 3 minutes, then under the condition of 40 ~ 50 ℃, the K that is 120g/L by volumetric concentration
2crO
7, the dense H that volumetric concentration is 500g/L
2sO
4the coarsening solution 500ml being mixed with, carries out acid etching roughening treatment to the powdered graphite surface after oil removing, and coarsening time is 10～20 minutes;
(III) powdered graphite surface activation process
Powdered graphite after alligatoring is cleaned 3 minutes with distilled water, with the PdCl of volumetric concentration 1.2g/L
2, the SnCl of volumetric concentration 80g/L
22H
2o, the dense HCl of volumetric concentration 320g/L and the Na of volumetric concentration 8.0g/L
2snO
37H
2the activating solution 500ml that O is mixed with, under the condition of 35 ~ 45 ℃, puts into the powdered graphite after roughening treatment, stirs 20 minutes;
(IV) chemical nickel plating
The preparation of chemical nickel-plating liquid: take the nickelous sulfate of 300 grams, the sodium hypophosphite of 450 grams, the ammonium chloride of 450 grams, the plumbi nitras of the natrium citricum of 150 grams and 45 milligrams, dissolves with a small amount of distilled water respectively; Then by consoluet nickel salt solution, under constantly stirring, be poured in the solution containing natrium citricum; Add again sodium hypophosphite solution, and continuous vigorous stirring; Then add lead nitrate solution, then regulate pH value to 10 with ammonium hydroxide; Then add ammonium chloride solution, and with distilled water diluting to 15 liter; Finally again with ammonium hydroxide, the pH value of solution is adjusted to 10, and stand-by after filtering with filter.
Powdered graphite after activation processing is cleaned 3 minutes with distilled water, then use chemical nickel-plating liquid to carry out nickel plating, plated and powder has been rinsed to neutral with clear water afterwards, after 80 ℃ of oven dry, obtain conductive rubber nickel bag graphite conductive powder body.
Fig. 2 is the scanning electron microscope (SEM) photograph of the fibrous graphite powder of conductive rubber nickel bag of preparation in the embodiment of the present invention 2.
Embodiment 3
The nickel bag graphite conductive powder body that embodiment 1 and embodiment 2 are made is put into laboratory kneader according to the proportioning of table 1 and is mixed and make silica-based conductive rubber material.
The silica-based conductive rubber composition that the nickel bag graphite conductive powder body that table 1 embodiment 1～2 makes is raw material
By the silica-based nickel bag graphite conductive rubber making, thick by within 10 minutes, making 2mm 170 ℃ of mold pressings, the test piece of 12mm × 12mm, record after resistance, and calculating its resistivity, shown in result (in table 2), the silica-based conductive rubber making has good electric conductivity and mechanical property.
The silica-based conductive rubber testing experiment of the nickel bag graphite result that table 2 the present invention makes
Nickel bag graphite conductive powder body density in the present invention is low, cost is low and non-corrosive, can also improve the mechanical strength of conductive rubber material.And electroless plating method is easy to operate, technique is simple, coating even compact, covering power are strong, can carry out plating on the particle of any shape, covering power is good, can prepare composite granule even, tiny, dispersion.
Claims (10)
1. a conductive rubber nickel bag graphite conductive powder body, is characterized in that: component and percentage by weight that nickel bag graphite conductive powder body comprises are as follows:
Nickel 50 ~ 80%
Graphite 20 ~ 50%.
2. a kind of conductive rubber nickel bag graphite conductive powder body according to claim 1, it is characterized in that: described graphite powder shape of particle is fibrous, irregular sheet, the average grain diameter of graphite powder particle is 50 ~ 130 microns, and described nickel is coated on the surface of graphite powder.
3. the preparation method with nickel bag graphite conductive powder body according to a kind of conductive rubber claimed in claim 1, is characterized in that: comprise the steps:
(I) powdered graphite oil removal treatment
At ambient temperature, powdered graphite is cleaned with degreasing fluid, scavenging period is 10 ~ 15 minutes;
The roughening treatment of (II) powdered graphite acid etching
Powdered graphite after oil removing is cleaned with clear water, then under the condition of 40 ~ 50 ℃, acid etching roughening treatment is carried out in powdered graphite surface with coarsening solution, coarsening time is 10～20 minutes;
(III) powdered graphite surface activation process
Powdered graphite after alligatoring is cleaned with clear water, then use activating solution to carry out surface activation process, under the condition of 35 ~ 45 ℃, put into powdered graphite, stir 20 minutes;
(IV) chemical nickel plating
Powdered graphite after activation processing is cleaned with clear water, then use chemical nickel-plating liquid to carry out nickel plating, plated and powder has been rinsed to neutral with clear water afterwards, after oven dry, obtain conductive rubber nickel bag graphite conductive powder body.
4. the preparation method of nickel bag graphite conductive powder body for a kind of conductive rubber according to claim 3, is characterized in that: described degreasing fluid component and concentration are as follows:
Dodecyl Polyoxyethylene Ether sodium sulphate 6～8g/L
NPE 3～4g/L.
5. the preparation method of nickel bag graphite conductive powder body for a kind of conductive rubber according to claim 3, is characterized in that: described coarsening solution component and concentration are as follows:
K
2CrO
7 110～120g/L
Dense H
2sO
4400～500g/L.
6. the preparation method of nickel bag graphite conductive powder body for a kind of conductive rubber according to claim 3, is characterized in that: described activating solution component and concentration are as follows:
PdCl
2 1.0～1.2g/L
SnCl
2·2H
2O 70～80g/L
Dense HCl 300～320g/L
Na
2SnO
3·7H
2O 7.5～8.0g/L。
7. the preparation method of nickel bag graphite conductive powder body for a kind of conductive rubber according to claim 3, is characterized in that: the chemical nickel-plating liquid in described step (IV) is by forming in main salt, reducing agent, complexing agent, buffer and stabilizing agent.
8. the preparation method of nickel bag graphite conductive powder body for a kind of conductive rubber according to claim 7, is characterized in that: described chemical nickel-plating liquid also comprises PH regulator solution, and described PH regulator solution is dense HCl or ammonium hydroxide.
9. the preparation method of nickel bag graphite conductive powder body for a kind of conductive rubber according to claim 7, is characterized in that: described main salt refers to nickelous sulfate; Described reducing agent refers to sodium hypophosphite; Described complexing agent refers to the one in natrium citricum or citric acid; Buffer refers to the one in ammonium chloride or sodium acetate; Described stabilizing agent is plumbi nitras.
10. the preparation method of nickel bag graphite conductive powder body for a kind of conductive rubber according to claim 7, is characterized in that: in described chemical nickel-plating liquid, the concentration of main salt nickelous sulfate is 20g/L ~ 34g/L; In described chemical nickel-plating liquid, the concentration of reducing agent sodium hypophosphite is 20g/L ~ 30g/L; The concentration of described Complexing Agent in Electroless Nickel Deposition Baths natrium citricum is 10g/L, and the concentration of citric acid is 10g/L; In described chemical nickel-plating liquid, the concentration of buffer sodium acetate is 10 g/L, and the concentration of ammonium chloride is 10 g/L; In described chemical nickel-plating liquid, the concentration of stabilizing agent plumbi nitras is 2.5mg/L ~ 3mg/L.
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| CN201410097071.8A CN103817323A (en) | 2014-03-17 | 2014-03-17 | Nickel-coated graphite electric conduction powder used for electric conduction rubber and manufacturing method thereof |
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| CN107452433A (en) * | 2016-06-01 | 2017-12-08 | 益阳市菲美特新材料有限公司 | A kind of all-directional conductive sponge and preparation method thereof |
| CN111408713A (en) * | 2020-03-17 | 2020-07-14 | 苏州逸峰新材料科技有限公司 | Preparation method of nickel-coated graphite composite powder material with high coating rate |
| CN112045182A (en) * | 2020-08-03 | 2020-12-08 | 西安工程大学 | Preparation method of Ni/C composite conductive powder |
| CN114103321A (en) * | 2021-11-17 | 2022-03-01 | 西北工业大学 | High-strength high-conductivity layered silicone rubber composite material and preparation method thereof |
| CN115233137A (en) * | 2022-08-03 | 2022-10-25 | 四川苏克流体控制设备有限公司 | Low-friction supersonic flame spraying wear-resistant coating material, preparation method and application |
| CN115415519A (en) * | 2022-10-11 | 2022-12-02 | 雅安百图高新材料股份有限公司 | Chemical nickel plating solution of graphite micropowder and method for judging nickel plating reaction end point |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107452433A (en) * | 2016-06-01 | 2017-12-08 | 益阳市菲美特新材料有限公司 | A kind of all-directional conductive sponge and preparation method thereof |
| CN107452433B (en) * | 2016-06-01 | 2023-06-02 | 益阳市菲美特新材料有限公司 | Omnibearing conductive sponge and preparation method thereof |
| CN111408713A (en) * | 2020-03-17 | 2020-07-14 | 苏州逸峰新材料科技有限公司 | Preparation method of nickel-coated graphite composite powder material with high coating rate |
| CN112045182A (en) * | 2020-08-03 | 2020-12-08 | 西安工程大学 | Preparation method of Ni/C composite conductive powder |
| CN114103321A (en) * | 2021-11-17 | 2022-03-01 | 西北工业大学 | High-strength high-conductivity layered silicone rubber composite material and preparation method thereof |
| CN115233137A (en) * | 2022-08-03 | 2022-10-25 | 四川苏克流体控制设备有限公司 | Low-friction supersonic flame spraying wear-resistant coating material, preparation method and application |
| CN115415519A (en) * | 2022-10-11 | 2022-12-02 | 雅安百图高新材料股份有限公司 | Chemical nickel plating solution of graphite micropowder and method for judging nickel plating reaction end point |
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Application publication date: 20140528 |