CN111118583B - Method for preparing oriented CNTs/Cu composite material by electromagnetic field assisted electrophoretic deposition method - Google Patents

Method for preparing oriented CNTs/Cu composite material by electromagnetic field assisted electrophoretic deposition method Download PDF

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CN111118583B
CN111118583B CN202010122893.2A CN202010122893A CN111118583B CN 111118583 B CN111118583 B CN 111118583B CN 202010122893 A CN202010122893 A CN 202010122893A CN 111118583 B CN111118583 B CN 111118583B
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electrophoretic deposition
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CN111118583A (en
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邓丽萍
赖永杰
张越
杜航
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Fuzhou University
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    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • 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
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1655—Process features
    • C23C18/1664—Process features with additional means during the plating process
    • C23C18/1666—Ultrasonics
    • 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
    • C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
    • C23C18/1886—Multistep pretreatment
    • C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
    • B32B2264/10—Inorganic particles
    • B32B2264/107—Ceramic
    • B32B2264/108—Carbon, e.g. graphite particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/02—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/12—Pressure

Abstract

The invention discloses a method for preparing an oriented CNTs/Cu composite material by an electromagnetic field assisted electrophoretic deposition method, which mainly solves the problem of inconsistent orientation of carbon nanotubes electrophoretically deposited on a copper matrix, thereby improving the strengthening efficiency of the carbon nanotubes and further improving the electrical and mechanical properties of the CNTs/Cu composite material. The method comprises the following steps: firstly, respectively carrying out oxidation, sensitization, activation and chemical Ni plating treatment on an original carbon nano tube to make the original carbon nano tube have magnetism; then dispersing the pretreated carbon nanotubes in isopropanol solution while adding Al (NO)3)3Ultrasonically dispersing for 4-6h to form uniformly dispersed suspension; then taking the copper foil as a cathode and the stainless steel sheet as an anode, and carrying out electrophoretic deposition with the assistance of an electromagnetic field; and then stacking the copper foils after electrophoretic deposition layer by layer, packaging in a graphite mold, and performing hot-pressing sintering to obtain the CNTs/Cu composite material with the oriented carbon nano tubes.

Description

Method for preparing oriented CNTs/Cu composite material by electromagnetic field assisted electrophoretic deposition method
Technical Field
The invention belongs to the field of copper-based composite materials, and particularly relates to a method for preparing an oriented CNTs/Cu composite material by an electromagnetic field assisted electrophoretic deposition method.
Background
Copper and copper alloy have excellent electric conduction and heat conduction performance and good plasticity, toughness and ductility, are widely applied to the fields of electronic and electrical industry, mechanical manufacturing industry and the like, and occupy an important position in modern industrial systems. However, the conventional copper and copper alloy materials have the defects of low strength, poor high-temperature performance and the like, and limit further application of the copper and copper alloy. With the rapid development of modern industrial technology, higher requirements are put on the mechanical properties of copper and copper alloys. How to introduce a proper reinforcing phase into copper and copper alloy to prepare a high-performance copper-based composite material and how to better exert the synergistic effect of a matrix and the reinforcing phase become hot issues to be focused on by researchers.
As a typical one-dimensional nano material, Carbon Nanotubes (CNTs) have the characteristics of ultrahigh length-diameter ratio, ultrahigh mechanical property, high electrical conductivity, high thermal conductivity, low thermal expansion coefficient, strong acid and alkali resistance, high-temperature oxidation resistance and the like, and are an ideal reinforcing phase. Methods for combining carbon nanotubes with a copper matrix generally include a powder metallurgy method, an in-situ growth method, a deposition method and the like, and these preparation methods all aim to realize uniform dispersion of the carbon nanotubes in the copper matrix, neglect control of the orientation of the carbon nanotubes in the matrix, and the carbon nanotubes, as a typical one-dimensional material, have axial performance superior to other directions, and if the carbon nanotubes can be uniformly dispersed in the copper matrix and aligned along the axial direction, the reinforcing effect of the carbon nanotubes will be greatly enhanced.
The carbon nanotubes are usually rearranged after being combined with the copper matrix, such as: researchers use a 'die drawing' method to continuously elongate the CNTs/Cu composite material in one direction to form a long strip, thereby promoting the carbon nanotubes to be arranged along the axial direction thereof; researchers also realize the trend that the carbon nano-tubes in the copper matrix are arranged along the axial direction thereof by a method of powder metallurgy and assistance of an external magnetic field. These methods are complicated to implement, the equipment used is expensive, and the rearrangement effect of the carbon nanotubes is not significant. And a magnetic field or an electric field can be applied in the process of combining the carbon nanotubes and the copper matrix, so that the carbon nanotubes in the copper matrix are consistent in orientation, and the carbon nanotube arrangement effect obtained by the method is better. The electrophoretic Deposition (EPD) method has the characteristics of simple equipment, high Deposition rate, simple operation and good uniformity, but the carbon nanotubes in the carbon nanotube film obtained by electrophoretic Deposition are randomly distributed in orientation, so that a magnetic field assisted method can be used in the electrophoretic Deposition process to simply and effectively prepare the carbon nanotube oriented CNTs/Cu composite material.
Chinese patent No. 201210069653.6 discloses a method for preparing a magnetic field assisted electrophoretic deposition metallized carbon nanotube cathode, which is applicable to the field of field emission and can not be used for structural members, and the magnetic field is generated by a permanent magnet and has relatively small and unstable magnetism, so the method changes the process and provides a method for preparing the oriented CNTs/Cu composite material by an electromagnetic field assisted electrophoretic deposition method.
Disclosure of Invention
The invention aims to provide a method for preparing an oriented CNTs/Cu composite material by an electromagnetic field assisted electrophoretic deposition method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing oriented CNTs/Cu composite material by an electromagnetic field assisted electrophoretic deposition method comprises the following steps:
1) pretreatment of the carbon nanotubes: after oxidation, sensitization and activation treatment, the carbon nano tube is subjected to chemical nickel plating treatment on the surface, repeatedly washed, filtered and dried;
2) preparing an electrophoresis solution: 0.06g of the carbon nanotubes treated in step 1) was dissolved in 500ml of isopropanol solution, and 0.06g of Al (NO) was added thereto3)3Carrying out ultrasonic treatment for 4-6h to obtain uniformly dispersed suspension;
3) electrophoretic deposition: cutting the copper foil into 45mm multiplied by 45mm, cleaning the surface of the copper foil with acetone to be used as a cathode, and performing an electrophoretic deposition process on the suspension obtained in the step 2) by using a stainless steel sheet as an anode, wherein the electrophoretic voltage is 60V, the electrophoretic time is 60s, and the electrode distance is 5 cm. Electrophoretic deposition is carried out in an electromagnetic field: when the switch is closed, the electrified solenoid generates a stable electromagnetic field due to the passing of direct current, the electrophoresis device is positioned in the center of the solenoid, the magnetic field is stable, the magnetic field line is vertical to the electrode, and the magnetic field intensity is 1T-2T.
4) Hot-pressing and sintering: stacking and packaging 100 copper foils obtained in the step 3) in a graphite mold layer by layer, and performing a hot-pressing sintering process under the conditions of 950 ℃ and 50MPa to obtain the oriented CNTs/Cu composite material.
Further, the pretreatment of the carbon nanotubes is specifically: 1g of carbon nanotubes was dissolved in V (H)2SO4):V(HNO3) Oxidizing in a mixed acid solution of =3:1 for 4 hours, filtering, washing to neutrality and drying; and (3) sensitization: placing the oxidized carbon nano tube in SnCl2Carrying out ultrasonic treatment for 30min in a mixed solution of (0.1mol/L) and HCl (10ml/L), carrying out suction filtration, washing and drying; and (3) an activation process: placing the sensitized carbon nano tube in PdCl2Carrying out ultrasonic treatment in a mixed solution of (0.25g/L) and HCl (5ml/L), carrying out suction filtration, washing and drying; chemical Ni plating process: 0.5g of sensitized carbon nano tube is dissolved in NiSO4(0.1mol/L)、NaH2PO2(0.15mol/L)、Na3C6HO7(0.15mol/L) and NH4And (3) carrying out ultrasonic treatment on the mixed solution of Cl (0.2mol/L) for 10min, then plating in a constant-temperature water bath at 85 ℃ for 30min, carrying out suction filtration, washing to be neutral, and drying for later use.
The invention has the following advantages: firstly, the equipment adopted by the invention is simpler, and the operation process is not complex; secondly, the method adopted by the invention can simply and effectively ensure that the carbon nano tubes are directionally arranged on the copper matrix along the axial direction of the copper matrix, thereby improving the axial strength; plating Ni on the carbon nanotube can make the carbon nanotube magnetic and form Ni on the interface between the carbon nanotube and the copper matrix3And C, facilitating the interface connection of the two.
Drawings
FIG. 1 is a schematic diagram of electromagnetic field assisted electrophoretic deposition;
in the figure: 1-electrophoresis apparatus, 2-copper foil, 3-stainless steel sheet, 4-suspension, 5-switch, 6-coil a, 7-magnetic line, 8-coil b, 9-DC power supply.
Detailed description of the invention
For further disclosure, but not limitation, the invention is described in further detail below with reference to specific embodiments.
Example 1
A method for preparing a directional CNTs/Cu composite material by an electromagnetic field assisted electrophoretic deposition method specifically comprises the following steps:
1) 1g of carbon nanotubes was dissolved in V (H)2SO4):V(HNO3) Oxidizing in a mixed acid solution of =3:1 for 4 hours, filtering, washing to neutrality and drying; and (3) sensitization: placing the oxidized carbon nano tube in SnCl2Carrying out ultrasonic treatment for 30min in a mixed solution of (0.1mol/L) and HCl (10ml/L), carrying out suction filtration, washing and drying; and (3) an activation process: placing the sensitized carbon nano tube in PdCl2Carrying out ultrasonic treatment in a mixed solution of (0.25g/L) and HCl (5ml/L), carrying out suction filtration, washing and drying; chemical Ni plating process: 0.5g of sensitized carbon nano tube is dissolved in NiSO4(0.1mol/L)、NaH2PO2(0.15mol/L)、Na3C6HO7(0.15mol/L) and NH4Performing ultrasonic treatment on a mixed solution of Cl (0.2mol/L) for 10min, then plating in a constant-temperature water bath at 85 ℃ for 30min, performing suction filtration, washing to be neutral, and drying for later use;
2) 0.06g of the carbon nanotubes obtained in step 1) was dissolved in 500ml of isopropanol solution, and 0.06g of Al (NO) was added3)3Carrying out ultrasonic treatment for 6h to form uniformly dispersed suspension;
3) cutting a copper foil into 45mm multiplied by 45mm, cleaning the copper foil with acetone, taking the copper foil as a cathode, taking a stainless steel sheet as an anode, and performing electromagnetic field assisted electrophoretic deposition in the suspension prepared in the step 2), wherein the electrophoretic voltage is 60V, the electrophoretic time is 60s, the electrode spacing is 5cm, the magnetic line of force of an electromagnetic field in an electrophoretic tank is perpendicular to the electrodes, and the magnetic field intensity is 2T;
4) stacking and packaging 100 copper foils obtained after the electrophoretic deposition in the step 3) in a graphite mold, and performing hot-pressing sintering at 950 ℃ and under 50MPa to obtain the oriented CNTs/Cu composite material.
Comparative example 1
A blank control bulk material was prepared using the same preparation method as in example 1 except that there was no electromagnetic field assistance during electrophoretic deposition.
The samples prepared with the aid of electromagnetic field and without the aid of electromagnetic field are respectively subjected to axial tensile test and conductivity test, and the average tensile strength and the conductivity of the samples are respectively improved by about 15 percent and 9.0 percent compared with the average tensile strength and the conductivity of the samples prepared with the aid of electromagnetic field. .
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (4)

1. A method for preparing oriented CNTs/Cu composite material by an electromagnetic field assisted electrophoretic deposition method is characterized by comprising the following steps: the method comprises the following steps:
1) pretreatment of the carbon nanotubes: sequentially carrying out oxidation, sensitization and activation treatment on the carbon nano tube, then carrying out chemical nickel plating treatment on the surface of the carbon nano tube, repeatedly washing, filtering and drying;
2) preparing an electrophoretic solution: dissolving the carbon nano tube prepared in the step 1) in isopropanol, adding aluminum nitrate, and carrying out ultrasonic treatment for 4-6h to obtain uniformly dispersed electrophoretic solution;
3) magnetic field assisted electrophoretic deposition: cleaning the surface of the copper foil with acetone, taking the cleaned surface as a cathode, taking a stainless steel sheet as an anode, and carrying out electrophoretic deposition on the electrophoretic solution prepared in the step 2) under the assistance of an electromagnetic field;
4) hot-pressing and sintering: stacking the copper foils obtained after the electrophoretic deposition in the step 3), packaging in a graphite mold, and performing hot-pressing sintering to obtain the oriented CNTs/Cu composite material;
the pretreatment of the carbon nano tube in the step 1) is specifically as follows: dissolving carbon nanotube in V (H)2SO4):V(HNO3) Oxidizing in a mixed acid solution of =3:1 for 4h, filtering, washing to neutrality and drying; then placing the oxidized carbon nano tube in SnCl2Carrying out ultrasonic treatment for 30min in the mixed solution of HCl, carrying out suction filtration, washing and drying; then placing the sensitized carbon nano tube in PdCl2Carrying out ultrasonic treatment in a mixed solution of HCl, carrying out suction filtration, washing and drying; finally dissolving in NiSO4、NaH2PO2、Na3C6HO7And NH4Performing ultrasonic treatment on the mixed solution of Cl for 10min, plating in a constant-temperature water bath at 85 ℃ for 30min, performing suction filtration, washing to be neutral, and drying to obtain a pretreated carbon nano tube; the electromagnetic field assistance in the step 3) is specifically: when the switch is closed, the electrified solenoid generates a stable magnetic field in the electrophoresis tank due to the passing of direct current, the magnetic field line at the center of the magnetic field is vertical to the electrode, and the central magnetic field intensity is 1T-2T; the SnCl2SnCl in mixed solution of HCl and2the concentration is 0.1mol/L, the HCl concentration is 10 ml/L; the PdCl2PdCl in mixed solution with HCl2The concentration is 0.25mol/L, the HCl concentration is 5 ml/L; the NiSO4、NaH2PO2、Na3C6HO7And NH4NiSO in mixed solution of Cl4Concentration of 0.1mol/L, NaH2PO2The concentration is 0.15mol/L, Na3C6HO7Concentration of 0.15mol/L, NH4The Cl concentration was 0.2 mol/L.
2. The method for preparing the oriented CNTs/Cu composite material by the electromagnetic field assisted electrophoretic deposition method according to claim 1, characterized in that: in the step 2), the addition amount of the carbon nano tube and the aluminum nitrate is 0.06g, and the volume of the isopropanol is 500 mL.
3. The method for preparing the oriented CNTs/Cu composite material by the electromagnetic field assisted electrophoretic deposition method according to claim 1, characterized in that: the voltage of the electrophoretic deposition in the step 3) is 60V, the electrophoretic time is 60s, and the electrode distance is 5 cm.
4. The method for preparing the oriented CNTs/Cu composite material by the electromagnetic field assisted electrophoretic deposition method according to claim 1, characterized in that: the copper foil in the step 4) is 100 pieces, the temperature of hot-pressing sintering is 900-.
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CN112373147A (en) * 2020-10-19 2021-02-19 西安工程大学 Preparation method of carbon nano tube and TiC particle hybrid reinforced copper-based composite material
CN114032415A (en) * 2021-11-19 2022-02-11 国网河北能源技术服务有限公司 Preparation method of carbon nano tube reinforced copper-based layered composite material
CN114381782B (en) * 2021-12-29 2022-10-21 江苏诺德新材料股份有限公司 Environment-friendly high-Tg low-dielectric copper-clad plate and preparation process thereof
CN114672865A (en) * 2022-04-26 2022-06-28 昆明理工大学 Preparation method of CNTs/Cu composite board

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