CN112408380B - Preparation method for laser in-situ synthesis of submicron spherical graphite - Google Patents
Preparation method for laser in-situ synthesis of submicron spherical graphite Download PDFInfo
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- CN112408380B CN112408380B CN202011194615.4A CN202011194615A CN112408380B CN 112408380 B CN112408380 B CN 112408380B CN 202011194615 A CN202011194615 A CN 202011194615A CN 112408380 B CN112408380 B CN 112408380B
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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Abstract
The invention relates to a preparation method for in-situ synthesis of submicron spherical graphite by laser, which belongs to the technical field of laser processing and material synthesis and comprises the following steps: preparing raw material powder, preparing a metal substrate and preparing submicron spherical graphite by laser in-situ synthesis. The invention utilizes laser processing technology and in-situ synthesis reaction to synthesize submicron spherical graphite in a metal matrix without the assistance of a nucleating agent, and the prepared spherical graphite has uniform dispersion, complete structure and no defect in the metal matrix, and the diameter of the prepared spherical graphite is less than 1 mu m; the adopted raw material powder of the in-situ synthesis reaction has few types, the reaction process is simple and efficient, and mixed powder with different contents can be prepared according to the requirements; by regulating and controlling the processing technological parameters, the spherical graphite without impurities can be synthesized, and the spherical graphite with a special structure and a nano copper metal interlayer can also be synthesized.
Description
Technical Field
The invention relates to a preparation method for in-situ synthesis of submicron spherical graphite by laser, belonging to the technical field of laser processing and material synthesis.
Background
Graphite exists in many forms in metals, including flake graphite, spherical graphite, dense graphite, and star graphite, among others. The basic constituent unit of graphite is a monoatomic graphite layer (graphene), which is a two-dimensional planar structure composed of sp2 hybridized bond carbon atoms. Graphite with different forms is composed of graphene layer by layer, and the stacking mode and the growth direction of the graphene determine the macroscopic morphology of the graphite. The carbon atoms in graphene are arranged in a honeycomb shape, and are divided into an a-axis direction and a c-axis direction. The graphite platelets grow along the tightly bonded a-axis to form graphite flakes, while the graphite platelets grow along the c-axis to form graphite spheres.
The change of graphite form in the graphite-metal composite material obviously affects the performance of the graphite-metal composite material, the stress concentration phenomenon can be caused by the tip of flake graphite or irregular graphite, so that microcracks of the metal material are initiated, the stress concentration of the graphite with spherical morphology in a metal matrix is small, and the strength, toughness and fatigue performance of the material can be obviously improved. The preparation method of the spherical graphite mainly comprises the methods of heat treatment of carbon steel or cast iron, spheroidization of natural graphite, chemical vapor deposition and the like. The spherical graphite prepared by the first two methods has a large diameter, generally more than 10 μm. The spherical graphite prepared by chemical vapor deposition has small size, the diameter can reach below 1 mu m, but the cost is high. The heat treatment process consumes much time and energy, is only suitable for ferrous metals such as carbon steel, cast iron and the like, and is not suitable for non-ferrous metals such as copper, aluminum and the like. The spherical graphite obtained by spheroidizing natural graphite is generally nearly spherical, has low sphericity, and can be screened for many times to obtain a material with uniform size. Moreover, spheroidized natural graphite and spherical graphite prepared by chemical vapor deposition need to be introduced into a metal matrix through an external method, and the external method has the defects that the reinforcement is not easy to disperse uniformly, the interface bonding is weak and the like. In the metal matrix, the spherical graphite with small size, uniform distribution and good combination has excellent strengthening effect.
Therefore, the preparation of submicron spherical graphite in metal and the development of corresponding raw material systems become technical problems which are urgently needed to be solved in the field.
Disclosure of Invention
The invention aims to provide a preparation method for in-situ synthesis of submicron spherical graphite by laser, which utilizes high-energy laser beams to react in situ in a copper melt to generate the submicron spherical graphite so as to improve the strength, toughness and fatigue resistance of a composite material.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method for in-situ synthesis of submicron spherical graphite by laser comprises the following steps:
(1) preparation of raw material powder: the raw material powder comprises matrix powder and reaction powder, wherein the matrix powder is metal Cu powder; the reaction powder consists of metal Zr powder and carbide B4C powder with a molar ratio of Zr to B4C＝2:1；
Accurately weighing the powder, putting the powder into a V-shaped mixer for mixing, and putting the powder into a drying box for drying to obtain raw material powder;
(2) preparation of a metal substrate: selecting a pure copper substrate, firstly polishing the surface of the pure copper substrate by using sand paper to remove stains, oxides and the like on the surface, and then cleaning the surface of the substrate by using absolute ethyl alcohol to obtain a smooth and clean metal substrate;
(3) preparing submicron spherical graphite by laser in-situ synthesis: presetting the raw material powder obtained in the step (1) on the surface of the metal substrate obtained in the step (2), carrying out laser processing in an argon protective atmosphere to melt the raw material powder to form a molten pool, and carrying out in-situ synthesis reaction in the molten pool to generate spherical graphite; the reaction equation is as follows:
2Zr+B4C＝2ZrB2+C
the technical scheme of the invention is further improved as follows: the mass of the reaction powder in the step (1) is 10-50% of that of the raw material powder.
The technical scheme of the invention is further improved as follows: the average particle size of the metal Cu powder in the step (1) is 53-75 μm, and the purity is 99.9%; the average particle size of the metal Zr powder is 38-75 mu m, and the purity is 99.5%; carbide B4The average particle size of the C powder is 25-48 mu m, and the purity is 99.9%.
The technical scheme of the invention is further improved as follows: in the step (1), the rotating speed of the V-shaped mixer is 15r/min, and the powder mixing time is 2 h.
The technical scheme of the invention is further improved as follows: the drying conditions of the drying box in the step (1) are as follows: the drying temperature is 120 ℃ and the drying time is 1 h.
The technical scheme of the invention is further improved as follows: the laser processing parameters of the step (3) are as follows: the spot size D is 3mm, and the laser scanning spot overlapping rate is 50%; when the laser power P is 1.8-2.3 kW and the scanning speed V is 2-5 mm/s, preparing submicron-grade impurity-free spherical graphite; when the laser power P is 2.4-2.8 kW and the scanning speed V is 6-10 mm/s, the submicron spherical graphite with the copper interlayer is prepared.
The technical scheme of the invention is further improved as follows: and (4) presetting the thickness of the raw material powder in the step (3) to be 0.5-1 mm.
Due to the adoption of the technical scheme, the invention has the following technical effects:
the invention utilizes laser processing technology and in-situ synthesis reaction to synthesize submicron spherical graphite in a metal matrix. The laser processing technology provides a rapidly cooled molten pool environment and provides conditions for the formation of the spherical graphite.
The raw material powder of the in-situ synthesis reaction has few types, the reaction process is simple and efficient, and the mixed powder with different contents can be prepared according to the requirements. The spherical graphite prepared by the invention is uniformly dispersed in a metal matrix, has a complete structure and no defects, and has the diameter of less than 1 mu m; by regulating and controlling the processing technological parameters, the spherical graphite without impurities can be synthesized without the assistance of a nucleating agent, and the spherical graphite with a special structure of a nano copper metal interlayer can also be synthesized. The spherical graphite synthesized in situ is firmly combined with the metal matrix and is not easy to fall off.
Drawings
FIG. 1 is a graph of the morphology of graphite obtained in example 1 of the present invention;
FIG. 2 is a microscopic structure view of the spherical graphite obtained in example 1 of the present invention;
FIG. 3 is a high resolution diagram of transmission electrons of the impurity-free spheroidal graphite obtained in example 1 of the present invention;
FIG. 4 is a high resolution image of transmission electrons of spherical graphite with copper interlayer obtained in example 2 of the present invention.
Detailed Description
The invention will be explained in detail below with reference to the figures and specific examples. It is to be understood that the examples described are merely directed to preferred embodiments of the invention and that variations and modifications in the various components and amounts thereof are possible without departing from the spirit and scope of the invention.
Example 1:
a preparation method for in-situ synthesis of submicron spherical graphite by laser comprises the following steps:
(1) preparation of the starting powder
The raw material powder is composed of a matrixThe powder and the reaction powder, wherein the matrix powder is metal Cu powder; the reaction powder consists of metal Zr powder and carbide B4C powder with a molar ratio of Zr to B4C is 2: 1; the content of the reaction powder in the raw material powder was 10 wt.%.
The average particle size of the Cu powder is 53-75 mu m, and the purity is 99.9%; the average particle size of the Zr powder is 38-75 mu m, and the purity is 99.5%; b is4The average particle size of the C powder is 25-48 mu m, and the purity is 99.9%.
Accurately weighing the components according to the powder proportion by using an electronic scale, adding the components into a V-shaped mixer, mixing for 2 hours at the rotating speed of 15r/min, putting the mixture into a drying box, drying for 1 hour at the temperature of 120 ℃, and removing water in the powder to obtain raw material powder.
(2) Preparation of Metal substrates
Selecting pure copper substrate with the size of 50 multiplied by 15mm3. Firstly, the surface of a pure copper substrate is polished by using sand paper, surface stains, oxides and the like are removed, and then the surface of the substrate is cleaned by using absolute ethyl alcohol.
(3) Preparation of laser in-situ synthesized submicron spherical graphite
The laser head is fixed on a six-axis mechanical arm, in an argon protective atmosphere, the laser scanning speed is 2mm/s, the laser power is 1.8kW, the semiconductor fiber laser emits a high-energy laser beam with the wavelength of 1.064 mu m, the laser spot diameter is 3mm, raw material powder is preset on the surface of a metal substrate, the thickness of the preset powder layer is 1mm, the laser scanning spot overlapping rate is 50%, and submicron-grade impurity-free spherical graphite is synthesized in situ in a copper metal substrate by laser.
And after the laser processing is finished, air cooling to room temperature.
Using an electric spark cutting machine, the sample is cut to the size required for detection.
Zr and B4C is as 2Zr + B4C＝2ZrB2+ C reaction with B4C, decomposing the generated carbon atoms, and synthesizing spherical graphite in the molten pool.
FIG. 1 is a morphology of laser in-situ synthesized graphite, which is observed to be spherical, uniformly distributed in a metal matrix, and having a diameter of less than 1 μm. In fig. 2, the structural integrity of the spheroidal graphites can be observed without significant defects. Fig. 3 is a high resolution diagram of transmission electrons of spherical graphite, a typical graphite layer structure can be observed, and the interplanar spacing of the graphite layer thickness is determined to be 0.3610nm through fast fourier transform and measurement of interplanar spacing.
Example 2:
a preparation method for in-situ synthesis of submicron spherical graphite by laser comprises the following steps:
(1) preparation of the starting powder
The raw material powder consists of matrix powder and reaction powder, wherein the matrix powder is metal Cu powder; the reaction powder consists of metal Zr powder and carbide B4C powder with a molar ratio of Zr to B4C is 2: 1; the content of the reaction powder in the raw material powder was 30 wt.%.
The average particle size of Cu powder is 53-75 mu m, and the purity is 99.9%; the average particle size of the Zr powder is 38-75 mu m, and the purity is 99.5%; b is4The average particle size of the C powder is 25-48 mu m, and the purity is 99.9%.
Accurately weighing the components according to the powder proportion by using an electronic scale, adding the components into a V-shaped mixer, mixing the components for 2 hours at the rotating speed of 15r/min, putting the mixture into a drying box, drying the mixture for 1 hour at the temperature of 120 ℃, and removing water in the powder to obtain raw material powder.
(2) Preparation of Metal substrates
Selecting pure copper substrate with the size of 50 multiplied by 15mm3. Firstly, polishing the surface of a pure copper substrate by using sand paper, and removing surface stains, oxides and the like; and then using absolute ethyl alcohol to clean the surface of the substrate.
(3) Preparation of laser in-situ synthesized submicron spherical graphite
The laser head is fixed on a six-axis mechanical arm, and the laser scanning speed is 6mm/s in the argon protective atmosphere. The laser power is 2.4kW, the semiconductor fiber laser emits a high-energy laser beam with the wavelength of 1.064 μm, the laser spot diameter is 3mm, the raw material powder is preset on the surface of the metal substrate, the thickness of the preset powder layer is 0.5mm, the laser scanning spot overlapping rate is 50%, and the submicron spherical graphite with the copper interlayer is synthesized in situ by laser in the copper metal substrate.
And after the laser processing is finished, air cooling to room temperature.
Using an electric spark cutting machine, the sample is cut to the size required for detection.
In the spheroidal graphites obtained in this example, dark stringy phases were observed. FIG. 4 is a high resolution diagram of transmission electrons of the spherical graphite with copper interlayer obtained in the present example, and it was determined that the phase was Cu and the interplanar spacing of the [111] crystal direction of Cu was 0.2091nm by measuring the interplanar spacing and the fast Fourier transform. The spherical graphite with the copper metal interlayer can be prepared by the preparation method.
Example 3:
a preparation method for in-situ synthesis of submicron spherical graphite by laser comprises the following steps:
(1) preparation of the starting powder
The raw material powder consists of matrix powder and reaction powder, wherein the matrix powder is metal Cu powder; the reaction powder consists of metal Zr powder and carbide B4C powder with a molar ratio of Zr to B4C is 2: 1; the content of the reaction powder in the raw material powder was 50 wt.%.
The average particle size of Cu powder is 53-75 mu m, and the purity is 99.9%; the average particle size of the Zr powder is 38-75 mu m, and the purity is 99.5%; b is4The average particle size of the C powder is 25-48 mu m, and the purity is 99.9%.
Accurately weighing the components according to the powder proportion by using an electronic scale, adding the components into a V-shaped mixer, mixing the components for 2 hours at the rotating speed of 15r/min, putting the mixture into a drying box, drying the mixture for 1 hour at the temperature of 120 ℃, and removing water in the powder to obtain raw material powder.
(2) Preparation of Metal substrates
Selecting pure copper substrate with the size of 50 multiplied by 15mm3Firstly, the surface of a pure copper matrix is polished by using sand paper, surface stains, oxides and the like are removed, and then the surface to be clad is cleaned by using absolute ethyl alcohol.
(3) Preparation of laser in-situ synthesized submicron spherical graphite
The laser head is fixed on a six-axis mechanical arm, and the laser scanning speed is 10mm/s in the argon protective atmosphere. The laser power is 2.8kW, the semiconductor fiber laser emits a high-energy laser beam with the wavelength of 1.064 μm, the laser spot diameter is 3mm, the raw material powder is preset on the surface of the metal substrate, the thickness of the preset powder layer is 1mm, the laser scanning spot overlapping rate is 50%, and the submicron spherical graphite is synthesized in situ by laser in the copper metal substrate.
And after the laser processing is finished, air cooling to room temperature.
In light of the foregoing description, it will be apparent to those skilled in the art from this disclosure that various changes and modifications can be made in the embodiment without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, but is determined according to the scope of the claims.
Claims (5)
1. A preparation method for in-situ synthesis of submicron spherical graphite by laser is characterized by comprising the following steps:
(1) preparation of raw material powder: the raw material powder comprises matrix powder and reaction powder, wherein the matrix powder is metal Cu powder; the reaction powder consists of metal Zr powder and carbide B4C powder with a molar ratio of Zr to B4C =2: 1; the mass of the reaction powder is 10-50% of that of the raw material powder;
accurately weighing the powder, putting the powder into a V-shaped mixer for mixing, and putting the powder into a drying box for drying to obtain raw material powder;
(2) preparation of a metal substrate: selecting a pure copper substrate, firstly polishing the surface of the pure copper substrate by using sand paper to remove stains, oxides and the like on the surface, and then cleaning the surface of the substrate by using absolute ethyl alcohol to obtain a smooth and clean metal substrate;
(3) preparing submicron spherical graphite by laser in-situ synthesis: presetting the raw material powder obtained in the step (1) on the surface of the metal substrate obtained in the step (2), carrying out laser processing in an argon protective atmosphere to melt the raw material powder to form a molten pool, and carrying out in-situ synthesis reaction in the molten pool to generate spherical graphite; the laser processing technological parameters are as follows: the spot size D is 3mm, and the laser scanning spot overlapping rate is 50%; when the laser power P is 1.8-2.3 kW and the scanning speed V is 2-5 mm/s, preparing submicron-grade impurity-free spherical graphite; when the laser power P is 2.4-2.8 kW and the scanning speed V is 6-10 mm/s, preparing the submicron spherical graphite with the copper interlayer; the reaction equation is:
2Zr+B4C=2ZrB2+C。
2. the method for preparing submicron spherical graphite by laser in-situ synthesis according to claim 1, characterized in that: the average particle size of the metal Cu powder in the step (1) is 53-75 μm, and the purity is 99.9%; the average particle size of the metal Zr powder is 38-75 mu m, and the purity is 99.5%; carbide B4The average particle size of the C powder is 25-48 mu m, and the purity is 99.9%.
3. The method for preparing submicron spherical graphite by laser in-situ synthesis according to claim 1, characterized in that: in the step (1), the rotating speed of the V-shaped mixer is 15r/min, and the powder mixing time is 2 h.
4. The method for preparing submicron spherical graphite by laser in-situ synthesis according to claim 1, characterized in that: the drying conditions of the drying box in the step (1) are as follows: the drying temperature is 120 ℃ and the drying time is 1 h.
5. The method for preparing submicron spherical graphite by laser in-situ synthesis according to claim 1, characterized in that: and (4) presetting the thickness of the raw material powder in the step (3) to be 0.5-1 mm.
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Effective date of registration: 20230531 Address after: No. 15 Tianjin Street, Industrial Park, Yongji Economic Development Zone, Yongji County, Jilin City, Jilin Province, 132100 Patentee after: Jilin Juneng new carbon material Co.,Ltd. Address before: 066004 No. 438, Hebei Avenue, seaport District, Hebei, Qinhuangdao Patentee before: Yanshan University |