CN114196867A - High-strength high-thermal-conductivity graphene dispersion ODS steel composite material and preparation method thereof - Google Patents
High-strength high-thermal-conductivity graphene dispersion ODS steel composite material and preparation method thereof Download PDFInfo
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- CN114196867A CN114196867A CN202111554271.8A CN202111554271A CN114196867A CN 114196867 A CN114196867 A CN 114196867A CN 202111554271 A CN202111554271 A CN 202111554271A CN 114196867 A CN114196867 A CN 114196867A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 135
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 113
- 239000010959 steel Substances 0.000 title claims abstract description 113
- 239000002131 composite material Substances 0.000 title claims abstract description 82
- 239000006185 dispersion Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 59
- 239000002135 nanosheet Substances 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 238000000875 high-speed ball milling Methods 0.000 claims abstract description 10
- 239000011812 mixed powder Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 11
- 239000002064 nanoplatelet Substances 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000002055 nanoplate Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 239000011159 matrix material Substances 0.000 description 22
- 238000002490 spark plasma sintering Methods 0.000 description 11
- 238000005551 mechanical alloying Methods 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- 238000000713 high-energy ball milling Methods 0.000 description 4
- 238000005411 Van der Waals force Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 229910000797 Ultra-high-strength steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011824 nuclear material Substances 0.000 description 1
- 229910001175 oxide dispersion-strengthened alloy Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention discloses a high-strength high-thermal-conductivity graphene dispersion ODS steel composite material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) mixing the graphene nanosheets and ODS steel powder through low-speed ball milling of a planetary ball mill to obtain mixed powder; (2) carrying out high-speed ball milling on the mixed powder obtained in the step (1) in a planetary ball mill for a period of time to obtain graphene-reinforced ODS steel-based composite powder; (3) and (3) preparing the graphene nanosheet reinforced ODS steel composite material from the composite powder obtained in the step (2) in a discharge plasma sintering manner. The preparation method is adopted to prepare the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material. The tensile strength of the graphene-reinforced ODS steel composite material prepared by the method reaches 1160-1250MPa at room temperature, and the elongation reaches 13-15%. Meanwhile, the heat-conducting property of the ODS steel is further improved.
Description
Technical Field
The invention relates to the technical field of nuclear material preparation processes, in particular to the technical field of ODS-based composite material preparation; in particular to a high-strength high-thermal-conductivity graphene dispersion ODS steel composite material and a preparation method thereof.
Background
Advanced nuclear power systems require structural materials with excellent properties in many respects including high temperature strength, radiation resistance, corrosion resistance, etc., and oxide dispersion strengthened steel (ODS steel) is one of the candidates for advanced nuclear power systems because of its high creep strength and excellent radiation resistance. However, high strength materials generally have the contradictory properties of increased strength and loss of ductility and toughness. The plasticity of the high-strength ODS alloy needs to be further improved, and the ODS alloy has a very fine grain structure, so that the thermal conductivity is lower than that of similar molten steel, and the heat transfer performance is reduced.
Graphene is a two-dimensional plane structure material, is the hardest material with the highest specific strength at present due to the unique two-dimensional honeycomb crystal structure and the extremely high bond strength, has the Young modulus of about 1TPa and the strength of 130GPa, is respectively 6 times and 60 times of the best ultrahigh-strength steel, and has high toughness due to the two-dimensional structure of graphene. Therefore, the graphene is compounded with the ODS steel by utilizing the excellent mechanical and thermal properties of the graphene to prepare the graphene reinforced ODS steel-based composite material, and the high-strength high-thermal-conductivity composite material can be obtained and applied to an advanced nuclear energy system.
Due to the fact that the wettability of graphene and ODS steel is poor, and the large specific surface area of graphene enables van der Waals force to be generated between graphene nano sheets to agglomerate, the reinforcing effect of the graphene is greatly reduced, namely the problems that the graphene nano sheets are uneven in the matrix, the wettability of the graphene nano sheets and the matrix is poor and the like exist.
Disclosure of Invention
The invention aims to provide a high-strength high-thermal-conductivity graphene dispersion ODS steel composite material and a preparation method thereof, and solves the problems of low tensile strength, elongation and thermal conductivity of the existing composite material caused by uneven dispersibility of graphene nano sheets in a matrix, poor wettability of the graphene nano sheets and the matrix and the like; the preparation method of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material has the characteristics of short preparation period, simple and effective process and the like. According to the high-strength high-heat-conductivity graphene dispersion ODS steel composite material, the prepared graphene nanosheet reinforced ODS steel-based composite material shows improved mechanical and heat-conducting properties, the tensile strength at room temperature reaches 1160-1250MPa, and the elongation rate also reaches 13-15%; meanwhile, the heat-conducting property of the ODS steel is further improved.
The invention is realized by the following technical scheme:
in a first aspect, the invention provides a preparation method of a high-strength high-thermal-conductivity graphene dispersion ODS steel composite material, which comprises the following steps:
(1) mixing the graphene nanosheets and ODS steel powder through low-speed ball milling of a planetary ball mill to obtain mixed powder;
(2) carrying out high-speed ball milling on the mixed powder obtained in the step (1) in a planetary ball mill for a period of time to obtain graphene-reinforced ODS steel-based composite powder;
(3) and (3) preparing the graphene nanosheet reinforced ODS steel composite material from the composite powder obtained in the step (2) in a Spark Plasma Sintering (SPS) mode.
The working principle is as follows: based on the poor wettability of graphene and ODS steel, the graphene nano sheets generate Van der Waals force to agglomerate due to the large specific surface area of the graphene, so that the reinforcing effect of the graphene is greatly reduced, namely the problems of uneven dispersibility of the graphene nano sheets in a matrix, poor wettability of the graphene nano sheets and the matrix and the like exist. Therefore, how to realize the uniform dispersion of the graphene in the matrix and improve the interface strength of the graphene and the matrix become the key points for the graphene to play a role in strengthening phase and the success of preparing the composite material. Among them, mechanical ball milling is a simple and effective method for preparing composite materials. Ball milling may cause damage to the structure of graphene to a certain extent, but effective dispersion of graphene in a matrix can also be achieved by ball milling as long as ball milling parameters are properly controlled.
The invention designs a preparation method of a high-strength high-heat-conductivity graphene dispersion ODS steel composite material, which comprises the steps of taking graphene and ODS steel powder as raw materials, preparing composite powder by pre-ball milling (low-speed ball milling) and high-speed ball milling of a planetary ball mill, and then obtaining the graphene-reinforced ODS steel-based composite material by a Spark Plasma Sintering (SPS) mode. Although the high-energy ball milling utilized by the invention causes a certain damage to the structure of graphene, the graphene-reinforced ODS steel composite material prepared by the high-energy ball milling exhibits remarkable mechanical and thermal properties. The embodiment result shows that compared with the ODS steel without added graphene, the tensile strength and the heat conductivity of the graphene reinforced ODS steel composite material prepared by the method provided by the invention are obviously improved.
Further, the graphene in the step (1) comprises one or more of few-layer graphene, multi-layer graphene or graphene nanosheet.
Further, the ODS steel component of the ODS steel powder in said step (1) is, by mass%, 4.5-5)% Cr, (1.5-2)% W, (4-5)% Al, (0.15-0.2)% V, (0.5-0.6)% Zr, (0.3-0.35)% Y2O3The purity is 99.9 percent, the C, N content is less than 0.1 percent, and the balance is Fe.
Further, the ODS steel powder of the step (1) has an ODS steel composition of, by mass, 5.5% Cr, 1.6% W, 4.5% Al, 0.2% V, 0.58% Zr, 0.35% Y2O3And the balance Fe.
Further, the mass percentages of the graphene nanosheets and the ODS steel powder in the step (1) are as follows:
1-2 wt.% of graphene nanoplatelets (i.e. the mass of graphene is 1-2 wt.% of the total mass of the graphene and the ODS steel), the thickness of the nanoplatelets is 3-10nm, and the average particle size of the nanoplatelets is 3-15 μm;
the average grain diameter of ODS steel powder is about 100-120 mu m, the oxygen content is controlled below 0.04 wt.%, the screening granularity is 50-200 meshes, and the ball-milling spare materials are all in mass percent.
Further, in the step (1), graphene nanosheets and ODS steel powder are mixed by a planetary ball mill at a low speed of 15-25rpm for 1-3h to obtain mixed powder.
Further, in the step (2), the graphene nanoplatelets and the ODS steel powder in the step (1) are sequentially filled into a ball milling tank, and are flushed with argon for protection; carrying out high-speed ball milling in a planetary ball mill under the protection of argon (Ar gas), wherein the ball milling parameters are as follows: the ball milling method comprises the steps of ball milling a steel tank and stainless steel balls for ball milling, wherein the ball-material ratio is 10:1, the ball milling medium is the stainless steel balls, the rotating speed is 350-.
Further, in the step (3), the graphene nanosheet reinforced ODS steel-based composite material with high strength and high thermal conductivity is prepared in a Spark Plasma (SPS) sintering manner; the sintering system is as follows: the sintering temperature is 1000-1100 ℃, the temperature is kept for 4-6min, and the sintering pressure is 40-60 MPa.
Further, the room-temperature tensile strength of the graphene nanosheet reinforced ODS steel composite material prepared in the step (3) is 1160-1250MPa, and the elongation is 13-15%; the heat conductivity coefficient of the composite material is improved by 25 percent.
In a second aspect, the invention also provides a high-strength high-thermal-conductivity graphene dispersion ODS steel composite material which is a finished product prepared by the preparation method.
Further, the room-temperature tensile strength of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material is 1160-1250MPa, and the elongation is 13-15%; the heat conductivity coefficient of the composite material is improved by 25 percent.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention optimizes the mixing process of graphene and ODS steel, and provides a method and a way for improving the mechanical property and the thermal conductivity of ODS steel. By adopting the ball milling parameters of the invention, 400 plus 500rpm and 24h of ball milling, the reaction of graphene and a matrix can be reduced, and the function of the self-reinforcing phase can be actively exerted.
2. The tensile strength of the graphene-reinforced ODS steel composite material prepared by the method reaches 1160-1250MPa at room temperature, and the elongation reaches 13-15%. Meanwhile, the heat-conducting property of the ODS steel is further improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a powder diagram of example 2 of the present invention after mechanical alloying.
FIG. 2 is a drawing result chart of dispersion-strengthened steel obtained in example 2 of the present invention.
FIG. 3 is a diagram showing the thermal conductivity of dispersion-strengthened steel obtained in example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one of ordinary skill in the art that: it is not necessary to employ these specific details to practice the present invention. In other instances, well-known structures, circuits, materials, or methods have not been described in detail so as not to obscure the present invention.
Throughout the specification, reference to "one embodiment," "an embodiment," "one example," or "an example" means: the particular features, structures, or characteristics described in connection with the embodiment or example are included in at least one embodiment of the invention. Thus, the appearances of the phrases "one embodiment," "an embodiment," "one example" or "an example" in various places throughout this specification are not necessarily all referring to the same embodiment or example. Furthermore, the particular features, structures, or characteristics may be combined in any suitable combination and/or sub-combination in one or more embodiments or examples. Further, those of ordinary skill in the art will appreciate that the illustrations provided herein are for illustrative purposes and are not necessarily drawn to scale. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1
The invention discloses a preparation method of a high-strength high-thermal-conductivity graphene dispersion ODS steel composite material, which comprises the following steps:
(1) mixing the graphene nanosheets and ODS steel powder through low-speed ball milling of a planetary ball mill to obtain mixed powder;
(2) carrying out high-speed ball milling on the mixed powder obtained in the step (1) in a planetary ball mill for a period of time to obtain graphene-reinforced ODS steel-based composite powder;
(3) and (3) preparing the graphene nanosheet reinforced ODS steel composite material from the composite powder obtained in the step (2) in a Spark Plasma Sintering (SPS) mode.
Specifically, the graphene in the step (1) contains one or more of few-layer graphene, multi-layer graphene or graphene nanosheet.
Specifically, the ODS steel composition of the ODS steel powder in said step (1) is (4.5-5)% Cr, (1.5-2)% W, (4-5)% Al, (0.15-0.2)% V, (0.5-0.6)% Zr, (0.3-0.35)% Y2O3The purity is 99.9 percent, the C, N content is less than 0.1 percent, and the balance is Fe. Specifically, the ODS steel powder of the step (1) has ODS steel components of, by mass, 5.5% Cr, 1.6% W, 4.5% Al, 0.2% V, 0.58% Zr, and 0.35% Y2O3And the balance Fe. The above are all mass percentages.
Specifically, the mass percentages of the graphene nanosheets and the ODS steel powder in the step (1) are as follows:
1-2 wt.% of graphene nanoplatelets (i.e. the mass of graphene is 1-2 wt.% of the total mass of the graphene and the ODS steel), the thickness of the nanoplatelets is 3-10nm, and the average particle size of the nanoplatelets is 3-15 μm;
the average grain diameter of ODS steel powder is about 100-120 mu m, the oxygen content is controlled below 0.04 wt.%, the screening granularity is 50-200 meshes, and the ball-milling spare materials are all in mass percent.
Specifically, in the step (1), graphene nanosheets and ODS steel powder are mixed through a planetary ball mill at a low speed of 15-25rpm for 1-3h to obtain mixed powder. In specific implementation, the rotating speed of the ball-milling dispersed graphene is 17 rpm/min.
Specifically, in the step (2), the graphene nanoplatelets and ODS steel powder in the step (1) are sequentially filled into a ball milling tank, and argon gas is filled into the ball milling tank for protection; carrying out high-speed ball milling in a planetary ball mill under the protection of argon (Ar gas), wherein the ball milling parameters are as follows: the ball milling method comprises the steps of ball milling a steel tank and stainless steel balls for ball milling, wherein the ball-material ratio is 10:1, the ball milling medium is the stainless steel balls, the rotating speed is 350-. In specific implementation, the rotation speed of ball-milling dispersed graphene is 400rpm/min, the ball-milling time is 24 hours, and the ball-material ratio is 10: 1.
Specifically, in the step (3), the graphene nanosheet reinforced ODS steel-based composite material with high strength and high thermal conductivity is prepared in a Spark Plasma (SPS) sintering manner; the sintering system is as follows: the sintering temperature is 1000-1100 ℃, the temperature is kept for 4-6min, and the sintering pressure is 40-60 MPa. In specific implementation, the sintering temperature is 1050 ℃, the applied pressure is 50MPa, and the heat preservation time is 5 min.
Specifically, the room-temperature tensile strength of the graphene nanosheet reinforced ODS steel composite material prepared in the step (3) is 1160-1250MPa, and the elongation is 13-15%; the heat conductivity coefficient of the composite material is improved by 25 percent.
The working principle is as follows: based on the poor wettability of graphene and ODS steel, the graphene nano sheets generate Van der Waals force to agglomerate due to the large specific surface area of the graphene, so that the reinforcing effect of the graphene is greatly reduced, namely the problems of uneven dispersibility of the graphene nano sheets in a matrix, poor wettability of the graphene nano sheets and the matrix and the like exist. Therefore, how to realize the uniform dispersion of the graphene in the matrix and improve the interface strength of the graphene and the matrix become the key points for the graphene to play a role in strengthening phase and the success of preparing the composite material. Among them, mechanical ball milling is a simple and effective method for preparing composite materials. Ball milling may cause damage to the structure of graphene to a certain extent, but effective dispersion of graphene in a matrix can also be achieved by ball milling as long as ball milling parameters are properly controlled.
The invention designs a preparation method of a high-strength high-heat-conductivity graphene dispersion ODS steel composite material, which comprises the steps of taking graphene and ODS steel powder as raw materials, preparing composite powder by pre-ball milling (low-speed ball milling) and high-speed ball milling of a planetary ball mill, and then obtaining the graphene-reinforced ODS steel-based composite material by a Spark Plasma Sintering (SPS) mode. Although the high-energy ball milling utilized by the invention causes a certain damage to the structure of graphene, the graphene-reinforced ODS steel composite material prepared by the high-energy ball milling exhibits remarkable mechanical and thermal properties. The embodiment result shows that compared with the ODS steel without added graphene, the tensile strength and the heat conductivity of the graphene reinforced ODS steel composite material prepared by the method provided by the invention are obviously improved.
Example 2
As shown in fig. 1 to fig. 3, the present embodiment is different from embodiment 1 in that the preparation method of the high-strength high-thermal-conductivity graphene-dispersed ODS steel composite material of embodiment 1 is performed as follows:
(1) preparing 2 wt.% of graphene nanosheets, wherein the thickness of each graphene nanosheet is 3-10nm, the average particle size of each graphene nanosheet is about 10 microns, the balance is ODS steel powder, the oxygen content is controlled to be below 0.04 wt.%, the particle size is screened to be 50-200 meshes, and the ball-milling spare materials are all in percentage by mass;
mixing the prepared graphene nanosheets and ODS steel powder by a planetary ball mill at a low speed of 15-25rpm for 1-3 h;
(2) sequentially filling the ball-milling standby materials in the step (1) into a ball-milling tank, and filling argon for protection; the parameters of ball milling are as follows: the ball-material ratio is 10:1, the ball-milling medium is stainless steel balls, the rotating speed is 400r/min, the ball-milling is carried out for a plurality of times in a way of cooling for 1 hour after ball-milling for 1 hour, the ball-milling time is 24 hours, and the mechanical alloying powder with the average particle size of 183 mu m is obtained;
(3) adopting a Spark Plasma Sintering (SPS) mode, wherein the sintering system is as follows: the sintering temperature is 1000 ℃, the temperature is kept for 4-6min, the sintering pressure is 40MPa, and the graphene reinforced ODS steel composite material is prepared, wherein the room-temperature tensile strength of the composite material is 1241MPa, and the elongation is 14.1%.
FIG. 1 is a powder diagram of example 2 after mechanical alloying; FIG. 2 is a graph showing the drawing results of the dispersion-strengthened steel obtained in example 2, wherein the abscissa of FIG. 2 represents the strain range and the ordinate represents the tensile strength; FIG. 3 is a graph showing the thermal conductivity of the dispersion-strengthened steel obtained in example 2, and the ordinate of FIG. 3 shows the thermal conductivity; it can be seen from fig. 3 that the thermal conductivity of the composite material is further improved.
The invention belongs to the technical field of ODS-based composite material preparation, and solves the problems of uneven dispersity of graphene nano sheets in a matrix, poor wettability of the graphene nano sheets and the matrix and the like. The method comprises the following steps: firstly, mechanically ball-milling and mixing powder, and selecting low-speed ball milling at 15-25rpm for 1-3h for mixing; carrying out high-speed ball milling on alloy powder and graphene nanosheets under the protection of Ar gas, wherein the ball milling parameters are as follows: the ball-material ratio is 10:1, the ball-milling medium is stainless steel balls, the rotating speed is 350-; second, discharge plasma sintering densification; and (3) placing the mechanical alloying powder into SPS equipment for curing and sintering, wherein the sintering environment is vacuum, the temperature is 1100 ℃, the heat preservation time is 4-6min, and the pressure is 40-60MPa, and the final graphene-reinforced ODS steel is obtained through SPS sintering to obtain the composite material. The room temperature tensile strength is up to 1160-1250MPa, and the elongation is 13-15%. Meanwhile, the heat-conducting property of the composite material is further improved.
Example 3
The difference between the present embodiment and embodiment 1 is that the preparation method of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material in embodiment 1 is as follows:
(1) preparing 2 wt.% of graphene nanosheets, wherein the thickness of each graphene nanosheet is 3-10nm, the average particle size of each graphene nanosheet is about 10 microns, the balance is ODS steel powder, the oxygen content is controlled to be below 0.04 wt.%, the particle size is screened to be 50-200 meshes, and the ball-milling spare materials are all in percentage by mass;
and carrying out low-speed ball milling on the graphene nanosheets and the ODS steel powder for 1-3h at 15-25rpm by a planetary ball mill, and mixing;
(2) sequentially filling the ball-milling standby materials in the step (1) into a ball-milling tank, and filling argon for protection; the parameters of ball milling are as follows: the ball-material ratio is 10:1, the ball-milling medium is stainless steel balls, the rotating speed is 500r/min, the ball-milling is carried out for a plurality of times in a way of cooling for 1 hour after ball-milling for 1 hour, the ball-milling time is 24 hours, and the mechanical alloying powder with the average particle size of 183 mu m is obtained;
(3) adopting a spark plasma sintering mode (SPS), wherein the sintering system is as follows: the sintering temperature is 1100 ℃, the temperature is kept for 4-6min, the sintering pressure is 40MPa, and the graphene reinforced ODS steel composite material is prepared, wherein the room-temperature tensile strength of the composite material is 1167MPa, and the elongation is 13.2%.
The composite material prepared by the method disclosed by the invention is simple in process and can be produced industrially in large batch, the uniform dispersibility of graphene in a matrix is improved, the interface bonding state between the graphene and the matrix is improved, the double strengthening effect is achieved by simultaneously introducing the graphene and the nano particles which are dispersed in the matrix, and the strength and the heat conductivity of the ODS steel are improved.
Example 4
The difference between the embodiment and embodiment 1 is that the embodiment provides a high-strength high-thermal-conductivity graphene dispersion ODS steel composite material, which is the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material prepared by the preparation method described in embodiment 1.
Specifically, the room-temperature tensile strength of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material is 1160-1250MPa, and the elongation is 13-15%; the heat conductivity coefficient of the composite material is improved by 25 percent.
According to the invention, the finished product prepared by the preparation method of the embodiment 1 is used, and the problems of uneven dispersibility of the graphene nanosheet in the matrix, poor wettability of the graphene nanosheet and the matrix and the like are solved. The high-strength high-thermal-conductivity graphene dispersion ODS steel composite material prepared by the method disclosed by the invention has the room-temperature tensile strength up to 1160-1250MPa and the elongation percentage of 13-15%. Meanwhile, the heat-conducting property of the composite material is further improved.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a high-strength high-thermal-conductivity graphene dispersion ODS steel composite material is characterized by comprising the following steps:
(1) mixing the graphene nanosheets and ODS steel powder through low-speed ball milling of a planetary ball mill to obtain mixed powder;
(2) carrying out high-speed ball milling on the mixed powder obtained in the step (1) in a planetary ball mill for a period of time to obtain graphene-reinforced ODS steel-based composite powder;
(3) and (3) preparing the graphene nanosheet reinforced ODS steel composite material from the composite powder obtained in the step (2) in a discharge plasma sintering manner.
2. The preparation method of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material according to claim 1, wherein in the step (1), the graphene comprises one or more of few-layer graphene, multi-layer graphene or graphene nanosheets.
3. The preparation method of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material as claimed in claim 1, wherein the ODS steel in step (1)The ODS steel component of the powder is, in mass percent, (4.5-5)% Cr, (1.5-2)% W, (4-5)% Al, (0.15-0.2)% V, (0.5-0.6)% Zr, and (0.3-0.35)% Y2O3The purity is 99.9 percent, the C, N content is less than 0.1 percent, and the balance is Fe.
4. The preparation method of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material of claim 3, wherein the ODS steel powder of the step (1) comprises, by mass, 5.5% Cr, 1.6% W, 4.5% Al, 0.2% V, 0.58% Zr, and 0.35% Y2O3And the balance Fe.
5. The preparation method of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material according to claim 1, wherein the graphene nanoplatelets and ODS steel powder in step (1) are in mass percent:
1-2 wt.% of graphene nanosheets, the thickness of the nanosheets being 3-10nm, and the average particle size of the nanosheets being 3-15 μm;
the ODS steel powder has an average particle size of 100-120 μm, an oxygen content of 0.04 wt.% or less, and a sieve particle size of 50-200 mesh.
6. The preparation method of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material according to claim 1, wherein in the step (2), the graphene nanoplates and ODS steel powder in the step (1) are sequentially filled into a ball mill pot, and are flushed with argon gas for protection; carrying out high-speed ball milling in a planetary ball mill under the protection of argon, wherein the ball milling parameters are as follows: the ball-material ratio is 10:1, the ball-milling medium is stainless steel balls, the rotating speed is 350-.
7. The preparation method of the high-strength high-thermal-conductivity graphene dispersion ODS steel composite material according to claim 1, characterized in that in the step (3), the graphene nanoplate-reinforced ODS steel-based composite material with high-strength high-thermal-conductivity is prepared by discharge plasma (SPS) sintering; the sintering system is as follows: the sintering temperature is 1000-1100 ℃, the temperature is kept for 4-6min, and the sintering pressure is 40-60 MPa.
8. The preparation method of the high-strength and high-thermal-conductivity graphene dispersion ODS steel composite material as claimed in claim 1, wherein the room-temperature tensile strength of the graphene nanoplate-reinforced ODS steel composite material prepared in step (3) is 1160-1250MPa, and the elongation is 13-15%.
9. A high-strength high-thermal-conductivity graphene dispersion ODS steel composite material is characterized by being a finished product prepared by the preparation method of any one of claims 1-8.
10. The ODS steel composite material of claim 9, wherein the ODS steel composite material has a room temperature tensile strength of 1160-1250MPa, and an elongation of 13-15%.
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