CN112746197A - Preparation method of graphene-reinforced nickel-based nano composite powder metallurgy material - Google Patents

Preparation method of graphene-reinforced nickel-based nano composite powder metallurgy material Download PDF

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Publication number
CN112746197A
CN112746197A CN202011578406.XA CN202011578406A CN112746197A CN 112746197 A CN112746197 A CN 112746197A CN 202011578406 A CN202011578406 A CN 202011578406A CN 112746197 A CN112746197 A CN 112746197A
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graphene
nickel
nano
preparation
powder metallurgy
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区炳显
许晨旭
王勤生
熊立斌
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Special Equipment Safety Supervision Inspection Institute of Jiangsu Province
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Special Equipment Safety Supervision Inspection Institute of Jiangsu Province
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1005—Pretreatment of the non-metallic additives
    • 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
    • C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
    • C23C18/1855—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by mechanical pretreatment, e.g. grinding, sanding
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/54—Electroplating of non-metallic surfaces

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a preparation method of a graphene reinforced nickel-based nano composite powder metallurgy material, belonging to the technical field of graphene reinforced nickel-based nano composite powder metallurgy materials, and the preparation method of the graphene reinforced nickel-based nano composite powder metallurgy material comprises the following specific preparation steps: s1: and (3) graphene dispersion: cutting graphite into sheets, and grinding the sheets until graphite particles are in a nano level to obtain nano-level graphene; s2: graphene surface treatment: and (4) reacting the nano-scale graphene with the surface attached with the dispersing agent obtained in the step S2 with nickel. The raw materials are ground and dispersed by graphite flakes to primarily disperse graphite, and the nickel is conveniently and uniformly covered on the surface of graphene through the subsequent multiple mixing and dispersing effects, so that the quality of the material is ensured; due to the composite effect of the nano-grade graphene and the nickel, the obtained finished product has various optimized characteristics and a wide application range.

Description

Preparation method of graphene-reinforced nickel-based nano composite powder metallurgy material
Technical Field
The invention relates to the technical field of graphene reinforced nickel-based nano composite powder metallurgy materials, in particular to a preparation method of a graphene reinforced nickel-based nano composite powder metallurgy material.
Background
The graphene is sp2The hybridized and connected carbon atoms are tightly packed into a new material with a single-layer two-dimensional honeycomb lattice structure. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. The graphene is added into the nickel matrix to prepare the graphene reinforced nickel-based composite material, so that the mechanical property of the matrix can be improved to a great extent, and the graphene reinforced nickel-based composite material has a wide application prospect.
The wettability of graphene and a metal matrix is poor, so that the graphene and nickel are mixed unevenly, the nickel on the graphene is distributed unevenly, and the material performance is reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene reinforced nickel-based nano composite powder metallurgy material, and aims to solve the problems that due to poor wettability of graphene and a metal matrix, the graphene and nickel are mixed unevenly, so that nickel on the graphene is distributed unevenly, and the material performance is reduced.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a graphene reinforced nickel-based nano composite powder metallurgy material comprises the following specific preparation steps:
s1: and (3) graphene dispersion: cutting graphite into sheets, and grinding the sheets until graphite particles are in a nano level to obtain nano-level graphene;
s2: graphene surface treatment: taking out the nano-graphene obtained in the step S1, adding a dispersing agent into the nano-graphene, placing the nano-graphene and the dispersing agent into a centrifuge, and driving the nano-graphene and the dispersing agent to centrifugally rotate and mix by the centrifuge so that the nano-graphene and the dispersing agent are contacted and blended to obtain the nano-graphene with the surface attached with the dispersing agent;
s3: compounding graphene and nickel to prepare a finished product: and (4) reacting the nano-graphene with the surface attached with the dispersing agent obtained in the step (S2) with nickel, so that the nickel uniformly covers the surface of the nano-graphene, and the finished product graphene reinforced nickel-based nano composite powder metallurgy material is obtained.
Preferably, the flake graphite is ground in step S1 by a ball mill, and the rotation speed of the ball mill is set to 200-300 r/min.
Preferably, in step S2, the nano-sized graphene and the dispersant are respectively 10: 2 to 3.
Preferably, the dispersing agent is graphene DMF dispersing agent, and the graphene tube DMF dispersing agent comprises 80-90% of active agent and 10-20% of water.
Preferably, the specific manner of the reaction between the nano-graphene and the nickel in step S3 is as follows: adding a plating solution into a reaction container in advance, wherein the plating solution uses nickel sulfate as a main salt and hypophosphite as a reducing agent, and performing operation in an acid solution at 90 ℃ to chemically plate nickel and phosphorus on the surface of the nano-scale graphene.
Preferably, the specific manner of the reaction between the nano-graphene and the nickel in step S3 is as follows: the preparation method comprises the following steps of uniformly mixing the nanoscale graphene and the metal nickel powder through a stirrer, and shaping the nanoscale graphene and the metal nickel powder in a sintering mode, wherein the nanoscale graphene and the metal nickel powder are respectively prepared from the following components in parts by mass: nano-graphene: 10-20% of metallic nickel powder: 80-90.
Preferably, the specific manner of the reaction between the nano-graphene and the nickel in step S3 is as follows: in the electroplating mode, nickel sulfate is used as electroplating main salt, nano-scale graphene is used as a cathode plated material and is placed in an electroplating pool, and an electroplating solution is continuously stirred in the electroplating process.
Compared with the prior art, the invention has the beneficial effects that:
1) the raw materials are ground and dispersed by graphite flakes to primarily disperse graphite, and the nickel is conveniently and uniformly covered on the surface of graphene through the subsequent multiple mixing and dispersing effects, so that the quality of the material is ensured;
2) due to the composite effect of the nano-grade graphene and the nickel, the obtained finished product has various optimized characteristics and a wide application range.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a graphene reinforced nickel-based nano composite powder metallurgy material comprises the following specific preparation steps:
s1: and (3) graphene dispersion: cutting graphite into sheets, and grinding the sheets until graphite particles are in a nano level to obtain nano-level graphene;
s2: graphene surface treatment: taking out the nano-graphene obtained in the step S1, adding a dispersing agent into the nano-graphene, placing the nano-graphene and the dispersing agent into a centrifuge, and driving the nano-graphene and the dispersing agent to centrifugally rotate and mix by the centrifuge so that the nano-graphene and the dispersing agent are contacted and blended to obtain the nano-graphene with the surface attached with the dispersing agent;
s3: compounding graphene and nickel to prepare a finished product: and (4) reacting the nano-graphene with the surface attached with the dispersing agent obtained in the step (S2) with nickel, so that the nickel uniformly covers the surface of the nano-graphene, and the finished product graphene reinforced nickel-based nano composite powder metallurgy material is obtained.
Further, in the step S1, the flake graphite is ground by a ball mill, and the rotation speed of the ball mill is set to 200-300 r/min.
Further, in the step S2, the nano-sized graphene and the dispersant are respectively 10: 2 to 3.
Further, the dispersing agent is graphene DMF dispersing agent, and the graphene tube DMF dispersing agent comprises 80-90% of active agent and 10-20% of water.
Further, the specific manner of the reaction between the nano-scaled graphene and the nickel in step S3 is as follows: adding a plating solution into a reaction container in advance, wherein the plating solution uses nickel sulfate as a main salt and hypophosphite as a reducing agent, and performing operation in an acid solution at 90 ℃ to chemically plate nickel and phosphorus on the surface of the nano-scale graphene.
Further, the specific manner of the reaction between the nano-scaled graphene and the nickel in step S3 is as follows: the preparation method comprises the following steps of uniformly mixing the nanoscale graphene and the metal nickel powder through a stirrer, and shaping the nanoscale graphene and the metal nickel powder in a sintering mode, wherein the nanoscale graphene and the metal nickel powder are respectively prepared from the following components in parts by mass: nano-graphene: 10-20% of metallic nickel powder: 80-90.
Further, the specific manner of the reaction between the nano-scaled graphene and the nickel in step S3 is as follows: in the electroplating mode, nickel sulfate is used as electroplating main salt, nano-scale graphene is used as a cathode plated material and is placed in an electroplating pool, and an electroplating solution is continuously stirred in the electroplating process.
Example (b):
the preparation method of the graphene reinforced nickel-based nano composite powder metallurgy material comprises the following specific preparation steps:
s1: and (3) graphene dispersion: cutting graphite into sheets, and grinding the sheets until graphite particles are in a nano level to obtain nano-level graphene;
s2: graphene surface treatment: taking out the nano-scale graphene obtained in the step S1, and adding a dispersing agent into the nano-scale graphene, wherein the mass proportion of the nano-scale graphene to the dispersing agent is respectively 10: 2, the dispersing agent is graphene DMF dispersing agent, the graphene tube DMF dispersing agent comprises 90% of active agent and 10% of water, the nano-scale graphene and the dispersing agent are placed in a centrifuge, the centrifuge drives the nano-scale graphene and the dispersing agent to centrifugally rotate and mix, so that the nano-scale graphene and the dispersing agent are contacted and blended to obtain the nano-scale graphene with the surface attached with the dispersing agent, the dispersing agent is arranged on the surface of the nano-scale graphene, and subsequent nickel can be further dispersed on the surface of the nano-scale graphene through the dispersing agent;
s3: compounding graphene and nickel to prepare a finished product: and (4) reacting the nano-graphene with the surface attached with the dispersing agent obtained in the step (S2) with nickel, adding a plating solution into a reaction container in advance, using nickel sulfate as a main salt and hypophosphite as a reducing agent, operating in an acid solution at 90 ℃, and chemically plating nickel and phosphorus on the surface of the nano-graphene to enable nickel to uniformly cover the surface of the nano-graphene, thereby obtaining the finished product graphene reinforced nickel-based nano composite powder metallurgy material.
The application comprises the following steps:
the graphene reinforced nickel-based nano composite powder metallurgy material is applied to most bearing members and structural materials in the aerospace field, hot end parts of aero-engines and automobile precision parts.
While there have been shown and described the fundamental principles and essential features of the invention and advantages thereof, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. A preparation method of a graphene reinforced nickel-based nano composite powder metallurgy material is characterized by comprising the following steps: the preparation method of the graphene reinforced nickel-based nano composite powder metallurgy material comprises the following specific preparation steps:
s1: and (3) graphene dispersion: cutting graphite into sheets, and grinding the sheets until graphite particles are in a nano level to obtain nano-level graphene;
s2: graphene surface treatment: taking out the nano-graphene obtained in the step S1, adding a dispersing agent into the nano-graphene, placing the nano-graphene and the dispersing agent into a centrifuge, and driving the nano-graphene and the dispersing agent to centrifugally rotate and mix by the centrifuge so that the nano-graphene and the dispersing agent are contacted and blended to obtain the nano-graphene with the surface attached with the dispersing agent;
s3: compounding graphene and nickel to prepare a finished product: and (4) reacting the nano-graphene with the surface attached with the dispersing agent obtained in the step (S2) with nickel, so that the nickel uniformly covers the surface of the nano-graphene, and the finished product graphene reinforced nickel-based nano composite powder metallurgy material is obtained.
2. The preparation method of the graphene reinforced nickel-based nano composite powder metallurgy material according to claim 1, wherein the preparation method comprises the following steps: in the step S1, the flake graphite is ground by a ball mill, and the rotation speed of the ball mill is set to 200-300 r/min.
3. The preparation method of the graphene reinforced nickel-based nano composite powder metallurgy material according to claim 1, wherein the preparation method comprises the following steps: in the step S2, the nano-sized graphene and the dispersant are respectively 10: 2 to 3.
4. The preparation method of the graphene reinforced nickel-based nano composite powder metallurgy material according to claim 3, wherein the preparation method comprises the following steps: the dispersing agent is graphene DMF dispersing agent, and the graphene tube DMF dispersing agent comprises 80-90% of active agent and 10-20% of water.
5. The preparation method of the graphene reinforced nickel-based nano composite powder metallurgy material according to claim 1, wherein the preparation method comprises the following steps: the specific reaction mode of the nano-scale graphene and the nickel in the step S3 is as follows: adding a plating solution into a reaction container in advance, wherein the plating solution uses nickel sulfate as a main salt and hypophosphite as a reducing agent, and performing operation in an acid solution at 90 ℃ to chemically plate nickel and phosphorus on the surface of the nano-scale graphene.
6. The preparation method of the graphene reinforced nickel-based nano composite powder metallurgy material according to claim 1, wherein the preparation method comprises the following steps: the specific reaction mode of the nano-scale graphene and the nickel in the step S3 is as follows: the preparation method comprises the following steps of uniformly mixing the nanoscale graphene and the metal nickel powder through a stirrer, and shaping the nanoscale graphene and the metal nickel powder in a sintering mode, wherein the nanoscale graphene and the metal nickel powder are respectively prepared from the following components in parts by mass: nano-graphene: 10-20% of metallic nickel powder: 80-90.
7. The preparation method of the graphene reinforced nickel-based nano composite powder metallurgy material according to claim 1, wherein the preparation method comprises the following steps: the specific reaction mode of the nano-scale graphene and the nickel in the step S3 is as follows: in the electroplating mode, nickel sulfate is used as electroplating main salt, nano-scale graphene is used as a cathode plated material and is placed in an electroplating pool, and an electroplating solution is continuously stirred in the electroplating process.
CN202011578406.XA 2020-12-28 2020-12-28 Preparation method of graphene-reinforced nickel-based nano composite powder metallurgy material Pending CN112746197A (en)

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Cited By (1)

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