CN112045182A - Preparation method of Ni/C composite conductive powder - Google Patents
Preparation method of Ni/C composite conductive powder Download PDFInfo
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- CN112045182A CN112045182A CN202010766752.4A CN202010766752A CN112045182A CN 112045182 A CN112045182 A CN 112045182A CN 202010766752 A CN202010766752 A CN 202010766752A CN 112045182 A CN112045182 A CN 112045182A
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- 239000000843 powder Substances 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 108
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 50
- 239000010439 graphite Substances 0.000 claims abstract description 50
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 36
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 35
- 238000007747 plating Methods 0.000 claims abstract description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 15
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000001509 sodium citrate Substances 0.000 claims abstract description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 62
- 239000011259 mixed solution Substances 0.000 claims description 30
- 239000000706 filtrate Substances 0.000 claims description 21
- 230000007935 neutral effect Effects 0.000 claims description 21
- 238000000967 suction filtration Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 5
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000004020 conductor Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
Abstract
The invention discloses a preparation method of Ni/C composite conductive powder, which comprises the following steps: firstly, calcining graphite to obtain flaky graphite; carrying out oil removal treatment on the flaky graphite by using alkali liquor; then placing the graphite powder into a dilute hydrochloric acid solution, carrying out ultrasonic treatment and washing; then NiSO4·6H2O、Na3C6H5O7、CH4N2S is dissolved in deionized water at room temperature and then NaOH solution is usedAdjusting the pH value to obtain nickel plating solution; and then adding the graphite powder into a nickel plating solution, adding a hydrazine hydrate solution while stirring, carrying out ultrasonic treatment, carrying out hydrothermal reaction, washing and drying to obtain the Ni/C composite conductive powder. The Ni/C composite conductive powder is prepared by a hydrothermal reduction method, the flaky graphite is completely plated, the plating layer is uniform, compact and continuous, the binding force between the nickel plating layer and the graphite substrate is strong, and the conductivity of the material is effectively improved.
Description
Technical Field
The invention belongs to the technical field of conductive material preparation, and particularly relates to a preparation method of Ni/C composite conductive powder.
Background
The metal graphite composite material has excellent lubricating property of graphite, has good electrical conductivity and thermal conductivity of metal, and can provide excellent performance which cannot be obtained by a single material. By coating the graphite powder with nickel, the physical properties such as conductivity, corrosion resistance, hardness, lubricity and the like can be obviously improved, and an excellent composite material is formed.
The Ni/C composite powder can be used as an improved conductive material, and can also be used as a corrosion-resistant and wear-resistant coating, a thermal barrier and sealing coating, a microwave absorbing material and the like. The quality of the coating has very important influence on the performance of the core-shell structure composite particle material, and further influences the use effect of the material, so that the research on the uniformity of the Ni/C particle coating, such as the distribution condition of the coating, the bonding strength of the coating and the coated surface, the thickness of the coating, the density (porosity), the flatness and the like, is very important. At present, most of researches on Ni/C composite powder have the problems of complex process, non-compact coating of a nickel shell layer, high nickel plating cost and the like, so that the application of the Ni/C composite powder is limited.
Disclosure of Invention
The invention aims to provide a preparation method of Ni/C composite conductive powder, and the prepared composite conductive powder has low density, good stability and high conductivity.
The technical scheme adopted by the invention is that the preparation method of the Ni/C composite conductive powder is specifically implemented according to the following steps:
step 1, placing graphite in a muffle furnace for calcining, and preserving heat for a period of time to obtain flaky graphite;
step 2, carrying out oil removal treatment on the flaky graphite by using alkali liquor;
step 3, placing the graphite powder obtained in the step 2 in a dilute hydrochloric acid solution, performing ultrasonic treatment, performing suction filtration, and washing with deionized water until filtrate is neutral;
step 4, mixingNiSO4·6H2O、Na3C6H5O7、CH4N2S is dissolved in deionized water at room temperature, the mixture is uniformly mixed, and then the pH value is adjusted by using a dilute NaOH solution to obtain a nickel plating solution;
step 5, adding the graphite powder obtained in the step 3 into the nickel plating solution in the step 4, continuously stirring, and then adding a hydrazine hydrate solution while stirring to obtain a mixed solution;
and 6, carrying out ultrasonic treatment on the mixed solution for a period of time, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, tightly sealing the reaction kettle, keeping the temperature of the reaction kettle at 100-160 ℃ for 3-8 h, cooling the reaction kettle to room temperature, separating the prepared solid matter from the mixed solution, sequentially washing the solid matter with absolute ethyl alcohol and deionized water until the filtrate is neutral, and drying the solid matter to obtain the Ni/C composite conductive powder.
The present invention is also characterized in that,
in the step 1, the heating temperature of the muffle furnace is 350-400 ℃, and the heat preservation time is 1-3 h.
In the step 2, the method specifically comprises the following steps: putting the flaky graphite in alkali liquor, performing ultrasonic treatment, performing suction filtration, and washing with deionized water until filtrate is neutral;
the average granularity of the flaky graphite is 4-15 mu m, and the purity is more than 98 percent;
the mass ratio of the flaky graphite to the deionized water is 1: 70-180 parts; the mass concentration of the alkali liquor is 80-160 g/L; the ultrasonic treatment time is 35-65 min, and the temperature is 60-85 ℃.
In the step 3, the mass ratio of the graphite powder to the dilute hydrochloric acid solution is 1: 80-160 parts; the mass concentration of the dilute hydrochloric acid is 5-10 ml/L; the ultrasonic treatment time is 30-50 min, and the temperature is 25-40 ℃.
In step 4, the specific method comprises the following steps: under the condition of normal temperature, mixing the raw materials in the following order and proportion to prepare the nickel plating solution:
after dissolving and stirring uniformly, the pH value of the solution is adjusted to 11-13 by adding NaOH.
In the step 5, the mass ratio of the graphite powder to the nickel plating solution to the hydrazine hydrate solution is 1-3: 1000: 4-10; the stirring speed is 300-400 r/min.
In the step 6, the ultrasonic treatment time is 0.5 h-2 h; the drying temperature is 70-95 ℃.
The invention has the beneficial effects that:
according to the preparation method of the Ni/C composite conductive powder, the Ni/C composite conductive powder is prepared by a hydrothermal reduction method, wherein the flaky graphite is completely plated, the plating layer is uniform, compact and continuous, the binding force between the nickel plating layer and the graphite substrate is strong, and the conductivity of the material is effectively improved; in addition, the process flow is simple, the operation is convenient and the cost is low.
Drawings
FIG. 1 is an SEM image of the Ni/C composite conductive powder prepared in example 2 according to the method of the present invention;
FIG. 2 is an XRD spectrum of the Ni/C composite conductive powder prepared in example 2 of the method of the present invention;
fig. 3 is an SEM image of flaky graphite.
Detailed Description
The present invention will be described in detail with reference to the following detailed description and accompanying drawings.
The invention relates to a preparation method of Ni/C composite conductive powder, which is specifically implemented according to the following steps:
step 1, placing graphite in a muffle furnace for calcining, and preserving heat for a period of time to obtain flaky graphite;
the heating temperature of the muffle furnace is 350-400 ℃, and the heat preservation time is 1-3 h;
step 2, carrying out oil removal treatment on the flaky graphite by using alkali liquor;
the method specifically comprises the following steps: putting the flaky graphite in alkali liquor, performing ultrasonic treatment, performing suction filtration, and washing with deionized water until filtrate is neutral;
the average granularity of the flaky graphite is 4-15 mu m, and the purity is more than 98 percent;
the mass ratio of the flaky graphite to the deionized water is 1: 70-180 parts; the mass concentration of the alkali liquor is 80-160 g/L; the ultrasonic treatment time is 35-65 min, and the temperature is 60-85 ℃.
Step 3, placing the graphite powder obtained in the step 2 in a dilute hydrochloric acid solution, performing ultrasonic treatment, performing suction filtration, and washing with deionized water until filtrate is neutral;
the mass ratio of the graphite powder to the dilute hydrochloric acid solution is 1: 80-160 parts; the mass concentration of the dilute hydrochloric acid is 5-10 ml/L; the ultrasonic treatment time is 30-50 min, and the temperature is 25-40 ℃;
step 4, adding NiSO4·6H2O、Na3C6H5O7、CH4N2S is dissolved in deionized water at room temperature, the mixture is uniformly mixed, and then the pH value is adjusted by using a dilute NaOH solution to obtain a nickel plating solution;
the specific method comprises the following steps: under the condition of normal temperature, mixing the raw materials in the following order and proportion to prepare the nickel plating solution:
after dissolving and stirring uniformly, adding NaOH to adjust the pH value of the solution to 11-13;
step 5, adding the graphite powder obtained in the step 3 into the nickel plating solution in the step 4, continuously stirring, and then adding a hydrazine hydrate solution while stirring to obtain a mixed solution;
the mass ratio of the graphite powder to the nickel plating solution to the hydrazine hydrate solution is 1-3: 1000: 4-10;
the stirring speed is 300-400 r/min;
step 6, carrying out ultrasonic treatment on the mixed solution for a period of time, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, tightly sealing the reaction kettle, keeping the temperature of the reaction kettle at 100-160 ℃ for 3-8 h, then cooling the reaction kettle to room temperature, separating the prepared solid matter from the mixed solution, sequentially washing the solid matter with absolute ethyl alcohol and deionized water until the filtrate is neutral, and drying the solid matter to obtain Ni/C composite conductive powder;
the ultrasonic treatment time is 0.5 h-2 h; the drying temperature is 70-95 ℃.
Example 1
A preparation method of Ni/C composite conductive powder is specifically implemented according to the following steps:
step 1, placing graphite in a muffle furnace, calcining at 350 ℃ and preserving heat for 2.5 hours;
step 2, placing the flaky graphite in alkali liquor for ultrasonic treatment, then performing suction filtration and washing with deionized water until filtrate is neutral, wherein the mass ratio of the flaky graphite to the deionized water is 1:70, the ultrasonic temperature is 65 ℃, the treatment time is 35min, and the mass concentration of the alkali liquor is 80 g/L;
and 3, placing the graphite powder obtained in the step 2 in a dilute hydrochloric acid solution for ultrasonic treatment, then performing suction filtration and washing with deionized water until the filtrate is neutral, wherein the mass ratio of the graphite powder to the dilute hydrochloric acid solution is 1: 90, the mass concentration of the dilute hydrochloric acid is 6ml/L, the ultrasonic treatment time is 30min, and the temperature is 25 ℃;
and 4, mixing the raw materials in the following sequence and proportion at normal temperature to prepare the nickel plating solution:
wherein, the pH value of the solution is adjusted to 11-13 by adding NaOH;
step 5, adding the pretreated graphite powder into a nickel plating solution, continuously stirring, and then adding a hydrazine hydrate solution while stirring at a stirring speed of 300r/min to obtain a mixed solution;
wherein the mass ratio of the graphite powder to the nickel plating solution to the hydrazine hydrate solution is 1: 1000: 4;
step 6, carrying out ultrasonic treatment on the mixed solution for 0.5h, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, tightly sealing the reaction kettle, keeping the temperature of the reaction kettle at 110 ℃ for 7h, and then cooling the reaction kettle to room temperature; separating the prepared powder from the product mixed solution, washing with absolute ethyl alcohol and deionized water until the filtrate is neutral, and drying at 75 ℃ to obtain the Ni/C composite conductive powder.
Example 2
A preparation method of Ni/C composite conductive powder is specifically implemented according to the following steps:
step 1, placing graphite in a muffle furnace, calcining at 360 ℃ and preserving heat for 2 hours;
step 2, putting the flaky graphite into alkali liquor for ultrasonic treatment, then performing suction filtration and washing with deionized water until filtrate is neutral, wherein the mass ratio of the flaky graphite to the deionized water is 1:120, the ultrasonic temperature is 70 ℃, the treatment time is 45min, and the mass concentration of the alkali liquor is 100 g/L;
and 3, placing the graphite powder obtained in the step 2 into a dilute hydrochloric acid solution for ultrasonic treatment, then performing suction filtration and washing with deionized water until the filtrate is neutral, wherein the mass ratio of the graphite to the dilute hydrochloric acid solution is 1: 100, wherein the mass concentration of dilute hydrochloric acid is 7ml/L, the ultrasonic treatment time is 35min, and the temperature is 30 ℃;
and 4, mixing the raw materials in the following sequence and proportion at normal temperature to prepare the nickel plating solution:
wherein, the pH value of the solution is adjusted to 11-13 by adding NaOH.
Step 5, adding the pretreated graphite powder into a nickel plating solution, continuously stirring, and then adding a hydrazine hydrate solution while stirring at a stirring speed of 350r/min to obtain a mixed solution;
wherein the mass ratio of the graphite powder to the nickel plating solution to the hydrazine hydrate solution is 2: 1000: 5;
and 6, carrying out ultrasonic treatment on the mixed solution for 1h, placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, tightly sealing the reaction kettle, keeping the temperature of the reaction kettle at 120 ℃ for 6h, cooling the reaction kettle to room temperature, separating the prepared powder from the product mixed solution, washing the obtained powder with absolute ethyl alcohol and deionized water until the filtrate is neutral, and drying the obtained powder at 85 ℃ to obtain the Ni/C composite conductive powder.
Fig. 3 is an SEM image of 30000 times magnification of the flake graphite, from which it can be seen that the surface of the graphite is smooth and no particles are attached, fig. 1 is an SEM image of 120000 times magnification of the Ni/C composite conductive powder, and it can be known from fig. 1 that the surface of the graphite sheet is coated with a complete nickel plating layer, and the plating layer is dense and continuous and has no exfoliation phenomenon, which indicates that the plating layer has strong binding force. FIG. 2 is an XRD pattern of the Ni/C composite conductive powder, which is compared with JCPDS No.08-0415 card of graphite and JCPDS No.04-0850 card of nickel to obtain a (002) crystal plane diffraction peak of graphite, and the three crystal plane diffraction peaks (111), (200) and (220) correspond to a typical diffraction peak of nickel, which shows that the Ni/C composite conductive powder is composed of two phases of metallic nickel and graphite, has no other impurity phase, and a plating layer on the graphite is pure nickel.
Example 3
A preparation method of Ni/C composite conductive powder is specifically implemented according to the following steps:
step 1, placing graphite in a muffle furnace, calcining at 370 ℃ and preserving heat for 1.5 h;
and 2, placing the flaky graphite in alkali liquor for ultrasonic treatment, then performing suction filtration and washing with deionized water until filtrate is neutral, wherein the mass ratio of the graphite to the deionized water is 1: 150, the ultrasonic temperature is 75 ℃, the processing time is 55min, and the mass concentration of the used alkali liquor is 120 g/L;
and 3, placing the graphite powder obtained in the step 2 into a dilute hydrochloric acid solution for ultrasonic treatment, then performing suction filtration and washing with deionized water until the filtrate is neutral, wherein the mass ratio of the graphite to the dilute hydrochloric acid solution is 1:120, the mass concentration of dilute hydrochloric acid is 9ml/L, the ultrasonic treatment time is 45min, and the temperature is 35 ℃;
and 4, mixing the raw materials in the following sequence and proportion at normal temperature to prepare the nickel plating solution:
wherein, the pH value of the solution is adjusted to 11-13 by adding NaOH.
Step 5, adding the pretreated graphite powder into a nickel plating solution, continuously stirring, and then adding a hydrazine hydrate solution while stirring at a stirring speed of 400r/min to obtain a mixed solution;
wherein the mass ratio of the graphite powder to the nickel plating solution to the hydrazine hydrate solution is 2.5: 1000, parts by weight; 6;
and 6, carrying out ultrasonic treatment on the mixed solution for 1.5h, placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, tightly sealing the reaction kettle, keeping the temperature of the reaction kettle at 130 ℃ for 5h, cooling the reaction kettle to room temperature, separating the prepared powder from a product mixed solution, washing the obtained product mixed solution with absolute ethyl alcohol and deionized water until the filtrate is neutral, and drying the obtained product mixed solution at 90 ℃ to obtain the Ni/C composite conductive powder.
Example 4
A preparation method of Ni/C composite conductive powder is specifically implemented according to the following steps:
step 1, placing graphite in a muffle furnace, calcining at 400 ℃, and preserving heat for 1 h;
and 2, placing the flaky graphite in alkali liquor for ultrasonic treatment, then performing suction filtration and washing with deionized water until the filtrate is neutral, wherein the mass ratio of the flaky graphite to the deionized water is 1: 170, the ultrasonic temperature is 80 ℃, the processing time is 65min, and the mass concentration of the used alkali liquor is 150 g/L;
and 3, placing the graphite powder obtained in the step 2 into a dilute hydrochloric acid solution for ultrasonic treatment, then performing suction filtration and washing with deionized water until the filtrate is neutral, wherein the mass ratio of the graphite to the dilute hydrochloric acid solution is 1: 150, wherein the mass concentration of the dilute hydrochloric acid is 10ml/L, the ultrasonic treatment time is 50min, and the temperature is 40 ℃;
and 4, mixing the raw materials in the following sequence and proportion at normal temperature to prepare the nickel plating solution:
wherein, the pH value of the solution is adjusted to 11-13 by adding NaOH.
Step 5, adding the pretreated graphite powder into a nickel plating solution, continuously stirring, and then adding a hydrazine hydrate solution while stirring at a stirring speed of 400r/min to obtain a mixed solution;
wherein the mass ratio of the graphite powder to the nickel plating solution to the hydrazine hydrate solution is 3: 1000: 8;
and 6, carrying out ultrasonic treatment on the mixed solution for 2 hours, placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, tightly sealing the reaction kettle, keeping the temperature of the reaction kettle at 150 ℃ for 4 hours, cooling the reaction kettle to room temperature, separating the prepared powder from the product mixed solution, washing the obtained powder with absolute ethyl alcohol and deionized water until the filtrate is neutral, and drying the obtained powder at 95 ℃ to obtain the Ni/C composite conductive powder.
Claims (7)
1. The preparation method of the Ni/C composite conductive powder is characterized by comprising the following steps:
step 1, placing graphite in a muffle furnace for calcining, and preserving heat for a period of time to obtain flaky graphite;
step 2, carrying out oil removal treatment on the flaky graphite by using alkali liquor;
step 3, placing the graphite powder obtained in the step 2 in a dilute hydrochloric acid solution, performing ultrasonic treatment, performing suction filtration, and washing with deionized water until filtrate is neutral;
step 4, adding NiSO4·6H2O、Na3C6H5O7、CH4N2S is dissolved in deionized water at room temperature, the mixture is uniformly mixed, and then the pH value is adjusted by using a dilute NaOH solution to obtain a nickel plating solution;
step 5, adding the graphite powder obtained in the step 3 into the nickel plating solution in the step 4, continuously stirring, and then adding a hydrazine hydrate solution while stirring to obtain a mixed solution;
and 6, carrying out ultrasonic treatment on the mixed solution for a period of time, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, tightly sealing the reaction kettle, keeping the temperature of the reaction kettle at 100-160 ℃ for 3-8 h, cooling the reaction kettle to room temperature, separating the prepared solid matter from the mixed solution, sequentially washing the solid matter with absolute ethyl alcohol and deionized water until the filtrate is neutral, and drying the solid matter to obtain the Ni/C composite conductive powder.
2. The preparation method of the Ni/C composite conductive powder according to claim 1, wherein in the step 1, the heating temperature of a muffle furnace is 350-400 ℃, and the heat preservation time is 1-3 h.
3. The method for preparing the Ni/C composite conductive powder according to claim 1, wherein the step 2 specifically comprises: putting the flaky graphite in alkali liquor, performing ultrasonic treatment, performing suction filtration, and washing with deionized water until filtrate is neutral;
the average granularity of the flaky graphite is 4-15 mu m, and the purity is more than 98 percent;
the mass ratio of the flaky graphite to the deionized water is 1: 70-180 parts; the mass concentration of the alkali liquor is 80-160 g/L; the ultrasonic treatment time is 35-65 min, and the temperature is 60-85 ℃.
4. The method for preparing Ni/C composite conductive powder according to claim 1, wherein in the step 3, the mass ratio of the graphite powder to the dilute hydrochloric acid solution is 1: 80-160 parts; the mass concentration of the dilute hydrochloric acid is 5-10 ml/L; the ultrasonic treatment time is 30-50 min, and the temperature is 25-40 ℃.
5. The method for preparing the Ni/C composite conductive powder according to claim 1, wherein in the step 4, the specific method comprises the following steps: under the condition of normal temperature, mixing the raw materials in the following order and proportion to prepare the nickel plating solution:
after dissolving and stirring uniformly, the pH value of the solution is adjusted to 11-13 by adding NaOH.
6. The method for preparing Ni/C composite conductive powder according to claim 1, wherein in the step 5, the mass ratio of the graphite powder to the nickel plating solution to the hydrazine hydrate solution is 1-3: 1000: 4-10; the stirring speed is 300-400 r/min.
7. The method for preparing the Ni/C composite conductive powder according to claim 1, wherein in the step 6, the time of ultrasonic treatment is 0.5h to 2 h; the drying temperature is 70-95 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010766752.4A CN112045182A (en) | 2020-08-03 | 2020-08-03 | Preparation method of Ni/C composite conductive powder |
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| CN114700490A (en) * | 2022-03-15 | 2022-07-05 | 东北大学 | Preparation method of nickel-coated graphite composite particles and application of nickel-coated graphite composite particles in electromagnetic shielding field |
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| CN108277480A (en) * | 2017-10-30 | 2018-07-13 | 浙江三元电子科技有限公司 | A kind of method of graphite nickel plating |
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| CN114700490A (en) * | 2022-03-15 | 2022-07-05 | 东北大学 | Preparation method of nickel-coated graphite composite particles and application of nickel-coated graphite composite particles in electromagnetic shielding field |
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