CN108385013B - Composite material bar core and preparation method thereof - Google Patents
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- C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
Abstract
The invention discloses a composite material bar core and a preparation method thereof, wherein the composite material bar core comprises a base material and a graphene mixture, wherein the base material comprises the following components: si, Fe, Nb, WC and M metal, wherein the M metal is any one or more of Ni, Cu and Co; the graphene mixture includes: polyoxyethylene lauryl ether, polyvinyl alcohol, ethanol, graphene and rare earth elements. The preparation method comprises the following steps: mixing polyoxyethylene lauryl ether, polyvinyl alcohol and ethanol, then adding graphene powder and rare earth element powder, carrying out ultrasonic treatment, distilling, concentrating and drying, mixing with Si powder, Fe powder, Nb powder, WC particles and M metal powder and excessive ethanol, filtering, drying, ball-milling, pressing and sintering to obtain the composite material.
Description
Technical Field
The invention discloses a composite material bar core and a preparation method thereof, belonging to the field of metal physical property modification.
Background
Graphene is a two-dimensional novel carbon material with a single carbon atom thickness, and has excellent mechanical properties such as high specific strength and rigidity. Meanwhile, graphene has a very large specific surface area, high electrical conductivity and thermal conductivity. Due to the excellent mechanical, thermal and electrical properties of the graphene, the graphene has a wide application prospect in the field of composite materials, especially metal-based composite materials. The graphene can be used for preparing composite materials with various metals (such as Al, Cu, Ni and the like), wherein the aluminum-based composite material is widely applied to aerospace, automobiles, electronics and optical instruments, the comprehensive performance of matrix metal is improved to a great extent by introducing the graphene, the application field of the matrix metal-based composite material is widened, the graphene has great research value, and a foundation is laid for realizing industrial production.
Graphene is a hexagonal honeycomb-shaped planar thin film formed by carbon atoms in sp2 hybridized orbitals, is a two-dimensional material with the thickness of only one carbon atom, is considered as the thinnest and the hardest nano material in the world due to the special structure, is almost completely transparent, has the thermal conductivity coefficient as high as 5300W/m.K, and is a good conductor. The graphene can be compounded with other materials to make up the defects of mechanical property and electric and thermal conductivity of other materials, but the graphene has strong hydrophobicity, so that the compatibility of the graphene in other materials is poor.
Disclosure of Invention
The invention provides a metal-reinforced graphene composite bar core and a preparation method thereof, and the technical scheme is as follows:
the composite material bar core comprises a base material and a graphene mixture, wherein the base material comprises the following components in percentage by mass: 1-5% of Si, 65-85% of Fe, 4-10% of Nb, 2-7% of WC and 5-15% of M metal (the M metal is any one or more of Ni, Cu and Co), wherein the graphene mixture comprises the following components in percentage by mass: 75-80% of polyoxyethylene lauryl ether, 5-15% of polyvinyl alcohol, 2-10% of ethanol, 3-5% of graphene and 0.2-2% of rare earth elements.
The preparation method of the composite material bar core comprises the following specific steps:
(1) firstly, mixing polyoxyethylene lauryl ether, polyvinyl alcohol and ethanol, then adding graphene powder and rare earth element powder, and carrying out ultrasonic treatment to obtain a rare earth mixed graphene dispersion liquid; distilling the graphene dispersion liquid of the mixed rare earth to obtain a concentrated solution, and drying to obtain an activating agent modified graphene mixture of the mixed rare earth;
(2) mixing the graphene mixture modified by the activating agent obtained in the step (1) and a base material (Si powder, Fe powder, Nb powder, WC particles and M metal powder) with ethanol, filtering, drying, and uniformly ball-milling to obtain a primary composite powder body;
(3) and (3) pressing the primary composite powder obtained in the step (2) into a cylinder, and sintering to obtain the composite material bar core.
The innovation points of the invention are as follows: 1) the special mechanical property and physical property of graphene and the processing mode of mixing rare earth elements are utilized, and the previous research does not find; 2) mixing graphene and rare earth elements by using a dispersing agent to obtain a preliminary mixed substance of graphene and rare earth elements; in order to organically combine graphene with other materials, polyoxyethylene lauryl ether is used for modifying the surface of the graphene, and then the graphene is mixed with ethanol to prepare a suspension, wherein on one hand, the polyoxyethylene lauryl ether has good combination performance with other materials such as high polymer materials, and on the other hand, the polyoxyethylene lauryl ether is also considered to improve the agglomeration of the graphene; 3) the bar core substrate contains a large amount of Fe element, so that good interface bonding advantage is provided for the subsequent dissolution of the carbon steel into the bar core during the casting; 4) according to the invention, WC ceramic particles are specially added to improve the mechanical property of the composite material with the bar core; 5) the process of the invention is rigorous in formulation, convenient to implement and low in technical requirement on research personnel. By searching related documents, no similar method and product existence is found, the method has obvious promotion effect on the research of improving the physical and mechanical properties of the carbon steel, has strong auxiliary significance and has good application prospect.
Drawings
FIG. 1 is a flow chart of the preparation process of the present invention.
Detailed Description
In order to enhance the understanding of the present invention, the following detailed description of the present invention is given with reference to the following examples and the accompanying drawings, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
Example 1
The composite material bar core comprises a base material and a graphene mixture, wherein the base material comprises the following components in percentage by mass: si 3%, Fe 75%, Nb 6%, WC (tungsten carbide) 7%, Co 4% and Ni 5%; the graphene mixture comprises the following components in percentage by mass: 75% of polyoxyethylene lauryl ether, 13% of polyvinyl alcohol, 5% of ethanol, 5% of graphene and 2% of rare earth element (lanthanum) powder.
The preparation method comprises the following steps:
1) firstly, mixing polyoxyethylene lauryl ether, polyvinyl alcohol and ethanol, then adding graphene powder (the length and the width are respectively 1-300 mu m, the thickness is 5-12 nm) and rare earth element powder (lanthanum powder, the granularity is 500 meshes/the purity is 99.999%), and treating for 20min by using ultrasonic waves (the frequency is 50kHz, the power is 1kW, and the temperature is 20 ℃) to obtain a graphene dispersion liquid of mixed rare earth; distilling the graphene dispersion liquid of the mixed rare earth (70 ℃, 30 min) to obtain a concentrated solution, and drying to obtain an activator-modified graphene mixture of the mixed rare earth;
2) mixing the graphene mixture of the mixed rare earth modified by the activating agent obtained in the step 1) with a base material (Si powder, Fe powder, Nb powder, WC particles, Co powder and Ni powder, wherein the powder granularity and purity are as follows: mixing Si powder with the granularity of 100 meshes/purity of 99.999 percent, Fe powder with the granularity of 300 meshes/purity of 99.99 percent, Nb powder with the granularity of 500 meshes/purity of 99.999 percent, WC particles with the granularity of 100 meshes/purity of 99.999 percent, Co powder with the granularity of 300 meshes/purity of 99.999 percent and Ni powder with the granularity of 300 meshes/purity of 99.999 percent by using ethanol, filtering and drying (50 ℃, 5 hours), and then uniformly ball-milling (Ar protection, 300r/min and 7 hours) to obtain a primary composite powder body;
3) and (3) pressing (hot isostatic pressing forming, 20 MPa) the primary composite powder obtained in the step 2) into a cylinder, and then sintering (discharge plasma sintering, wherein the vacuum degree is-0.01 MPa, the temperature is 1000 ℃, the axial pressure is 100MPa, the time is 0.5h, and the discharge current is 80A) to obtain the composite powder.
Example 2
The composite material bar core comprises a base material and a graphene mixture, wherein the base material comprises the following components in percentage by mass: si 2%, Fe 83%, Nb 5%, WC 4%, Ni 4% and Cu 2%; the graphene mixture comprises the following components in percentage by mass: 75% of polyoxyethylene lauryl ether, 13% of polyvinyl alcohol, 6% of ethanol, 4% of graphene and 2% of rare earth elements (cerium + praseodymium + yttrium + erbium).
The preparation method comprises the following steps:
1) firstly, mixing polyoxyethylene lauryl ether, polyvinyl alcohol and ethanol, then adding graphene powder (the length and the width are respectively 1-300 mu m, the thickness is 5-12 nm) and rare earth element powder (cerium + praseodymium + yttrium + erbium powder, the granularity is 500 meshes/the purity is 99.999%), and treating for 30min by using ultrasonic vibration (the frequency is 50kHz, the power is 1kW, and the temperature is 50 ℃) to obtain a graphene dispersion liquid of mixed rare earth; distilling the graphene dispersion liquid of the mixed rare earth (120 ℃, 20 min) to obtain a concentrated solution, and drying to obtain an activator-modified graphene mixture of the mixed rare earth;
2) mixing the graphene mixture of the mixed rare earth modified by the activating agent obtained in the step 1) with a base material (Si powder with the granularity of 100 meshes/purity of 99.999%, Fe powder with the granularity of 300 meshes/purity of 99.99%, Nb powder with the granularity of 500 meshes/purity of 99.999%, WC particles with the granularity of 100 meshes/purity of 99.999%, Ni powder with the granularity of 300 meshes/purity of 99.999%) by using ethanol, filtering and drying (150 ℃, 5 h), and then carrying out uniform ball milling (Ar protection, 1200r/min and 12 h) to obtain a primary composite powder body;
3) and (3) pressing (hot isostatic pressing forming, 150 MPa) the primary composite powder obtained in the step 2) into a cylinder, and then sintering (discharge plasma sintering, wherein the vacuum degree is-0.01 MPa, the temperature is 2000 ℃, the axial pressure is 200MPa, the time is 1h, and the discharge current is 350A) to obtain the composite powder.
Example 3
The composite material bar core comprises a base material and a graphene mixture, wherein the base material comprises the following components in percentage by mass: si 4%, Fe 79%, Nb 9%, WC 3%, Co 1% and Cu 4%; the graphene mixture comprises the following components in percentage by mass: 79% of polyoxyethylene lauryl ether, 7% of polyvinyl alcohol, 10% of ethanol, 3% of graphene and 1% of rare earth elements (neodymium, samarium, dysprosium or ytterbium).
The preparation method comprises the following steps:
1) firstly, mixing polyoxyethylene lauryl ether, polyvinyl alcohol and ethanol. Then adding graphene powder (the length and the width are respectively 1-300 mu m, the thickness is 5-12 nm) and rare earth element powder (neodymium or samarium or dysprosium or ytterbium powder, the granularity is 200 meshes/the purity is 99.999%). Treating for 30min by using ultrasonic vibration (the frequency is 30kHz, the power is 1kW, and the temperature is 50 ℃) to obtain a graphene dispersion liquid of the mixed rare earth; distilling the graphene dispersion liquid of the mixed rare earth (80 ℃, 30 min) to obtain a concentrated solution, and drying to obtain an activating agent modified graphene mixture of the mixed rare earth;
2) mixing the graphene mixture of the mixed rare earth modified by the activating agent obtained in the step 1) with a base material (Si powder with the granularity of 100 meshes/purity of 99.999%, Fe powder with the granularity of 300 meshes/purity of 99.99%, Nb powder with the granularity of 500 meshes/purity of 99.999%, WC particles with the granularity of 100 meshes/purity of 99.999%, Co powder with the granularity of 300 meshes/purity of 99.999%) by using ethanol, filtering and drying (100 ℃, 20 h), and then carrying out uniform ball milling (Ar protection, 300r/min and 10 h) to obtain a primary composite powder body;
3) pressing (hot isostatic pressing forming, 30 MPa) the primary composite powder obtained in the step 2) into a cylinder, and then sintering (discharge plasma sintering under the conditions of vacuum degree of-0.01 MPa, temperature of 1000 ℃, axial pressure of 200MPa, time of 1h and discharge current of 100A) to obtain the composite powder.
Example 4
The composite material bar core comprises a base material and a graphene mixture, wherein the base material comprises the following components in percentage by mass: 5% of Si, 70% of Fe, 6% of Nb, 5% of WC, 8% of Co and 6% of Ni; the graphene mixture comprises the following components in percentage by mass: 79 percent of polyoxyethylene lauryl ether, 12.5 percent of polyvinyl alcohol, 3 percent of ethanol, 5 percent of graphene and 0.5 percent of rare earth elements (europium + promethium + gadolinium).
The preparation method comprises the following steps:
1) firstly, mixing polyoxyethylene lauryl ether, polyvinyl alcohol and ethanol. Then adding graphene powder (the length and the width are respectively 1-300 mu m, the thickness is 5-12 nm) and rare earth element powder (europium + promethium + gadolinium powder, the granularity is 500 meshes/the purity is 99.999%). Treating for 30min by using ultrasonic vibration (the frequency is 30kHz, the power is 1kW, and the temperature is 50 ℃) to obtain a graphene dispersion liquid of the mixed rare earth; distilling the graphene dispersion liquid of the mixed rare earth (80 ℃, 30 min) to obtain a concentrated solution, and drying to obtain an activating agent modified graphene mixture of the mixed rare earth;
2) mixing the graphene mixture of the mixed rare earth modified by the activating agent obtained in the step 1) with a base material (Si powder with the granularity of 100 meshes/purity of 99.999%, Fe powder with the granularity of 300 meshes/purity of 99.99%, Nb powder with the granularity of 1000 meshes/purity of 99.999%, WC particles with the granularity of 100 meshes/purity of 99.999%, Co powder with the granularity of 300 meshes/purity of 99.999% and Ni powder with the granularity of 300 meshes/purity of 99.999%) by using ethanol, filtering and drying (100 ℃, 20 h), and then carrying out uniform ball milling (Ar protection, 300r/min and 10 h) to obtain a primary composite powder body;
3) and (3) pressing (hot isostatic pressing forming, 30 MPa) the primary composite powder obtained in the step 2) into a cylinder, and then sintering (discharge plasma sintering, wherein the vacuum degree is-0.01 MPa, the temperature is 1000 ℃, the axial pressure is 200MPa, the time is 1h, and the discharge current is 100A) to obtain the composite powder.
Example 5
The composite material bar core comprises a base material and a graphene mixture, wherein the base material comprises the following components in percentage by mass: si 1%, Fe 76%, Nb 4%, WC 6%, Co 5%, Ni 6% and Cu 2%; the graphene mixture comprises the following components in percentage by mass: 75% of polyoxyethylene lauryl ether, 8% of polyvinyl alcohol, 10% of ethanol, 5% of graphene and 2% of rare earth elements (holmium or terbium or thulium or lutetium or scandium).
The preparation method comprises the following steps:
1) firstly, mixing polyoxyethylene lauryl ether, polyvinyl alcohol and ethanol. Then adding graphene powder (the length and the width are respectively 1-300 mu m, and the thickness is 5-12 nm) and rare earth element powder (holmium or terbium or thulium or lutetium or scandium powder, and the granularity is 300 meshes/the purity is 99.999%). Treating for 30min by using ultrasonic vibration (the frequency is 30kHz, the power is 1kW, and the temperature is 50 ℃) to obtain a graphene dispersion liquid of the mixed rare earth; distilling the graphene dispersion liquid of the mixed rare earth (80 ℃, 30 min) to obtain a concentrated solution, and drying to obtain an activating agent modified graphene mixture of the mixed rare earth;
2) mixing the graphene mixture of the mixed rare earth modified by the activating agent obtained in the step 1) with a base material (Si powder with the granularity of 100 meshes/purity of 99.999%, Fe powder with the granularity of 300 meshes/purity of 99.99%, Nb powder with the granularity of 1000 meshes/purity of 99.999%, WC particles with the granularity of 100 meshes/purity of 99.999%, Co powder with the granularity of 300 meshes/purity of 99.999%, Ni powder with the granularity of 300 meshes/purity of 99.999%, and Cu powder with the granularity of 100 meshes/99.999%) by using ethanol, filtering and drying (100 ℃, 20 h), and then uniformly ball-milling (Ar protection, 300r/min, 10 h) to obtain a primary composite powder body;
3) and (3) pressing (hot isostatic pressing forming, 30 MPa) the primary composite powder obtained in the step 2) into a cylinder, and then sintering (discharge plasma sintering, wherein the vacuum degree is-0.01 MPa, the temperature is 1000 ℃, the axial pressure is 200MPa, the time is 1h, and the discharge current is 200A) to obtain the composite powder.
Claims (2)
1. The composite material bar core comprises a base material and a graphene mixture, wherein the base material comprises the following components: si, Fe, Nb, WC and M metal, wherein the M metal is any one or more of Ni, Cu and Co, and the mass percentage of each component in the base material is as follows: 1-5% of Si, 65-85% of Fe, 4-10% of Nb, 2-7% of WC and 5-15% of M metal; the graphene mixture comprises the following components: polyoxyethylene lauryl ether, polyvinyl alcohol, ethanol, graphene and rare earth elements, wherein the graphene mixture comprises the following components in percentage by mass: 75-80% of polyoxyethylene lauryl ether, 5-15% of polyvinyl alcohol, 2-10% of ethanol, 3-5% of graphene and 0.2-2% of rare earth elements.
2. A method of making a composite rod core of claim 1, comprising the steps of:
(1) firstly, mixing polyoxyethylene lauryl ether, polyvinyl alcohol and ethanol, then adding graphene powder and rare earth element powder, and carrying out ultrasonic treatment to obtain a rare earth mixed graphene dispersion liquid; distilling the graphene dispersion liquid of the mixed rare earth to obtain a concentrated solution, and drying to obtain an activating agent modified graphene mixture of the mixed rare earth;
(2) mixing the graphene mixture modified by the activating agent obtained in the step (1) with Si powder, Fe powder, Nb powder, WC particles and M metal powder by using ethanol, filtering, drying, and uniformly ball-milling to obtain a primary composite powder body;
(3) and (3) pressing the primary composite powder obtained in the step (2) into a cylinder, and sintering to obtain the powder.
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| CN102509779A (en) * | 2011-09-30 | 2012-06-20 | 郑州大学 | Rare earth modified grapheme and preparation method |
| CN104846228A (en) * | 2015-04-09 | 2015-08-19 | 浙江泰索科技有限公司 | Method for reinforcing metallic material by graphene |
| CN105110318A (en) * | 2015-07-23 | 2015-12-02 | 深圳市国创新能源研究院 | Graphene aqueous slurry, and preparation method thereof |
| CN106584717A (en) * | 2016-12-13 | 2017-04-26 | 柳州通为机械有限公司 | Door trim panel injection mold |
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Patent Citations (6)
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|---|---|---|---|---|
| CN102509779A (en) * | 2011-09-30 | 2012-06-20 | 郑州大学 | Rare earth modified grapheme and preparation method |
| CN104846228A (en) * | 2015-04-09 | 2015-08-19 | 浙江泰索科技有限公司 | Method for reinforcing metallic material by graphene |
| CN105110318A (en) * | 2015-07-23 | 2015-12-02 | 深圳市国创新能源研究院 | Graphene aqueous slurry, and preparation method thereof |
| CN106584717A (en) * | 2016-12-13 | 2017-04-26 | 柳州通为机械有限公司 | Door trim panel injection mold |
| CN107311466A (en) * | 2017-05-11 | 2017-11-03 | 北京大学 | A kind of in-situ preparation method of Graphene glass |
| CN107557704A (en) * | 2017-09-07 | 2018-01-09 | 苏州浩焱精密模具有限公司 | A kind of hot forming dies materials and preparation method thereof |
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