CN110714137A - Preparation method of graphene-reinforced titanium-based composite material - Google Patents
Preparation method of graphene-reinforced titanium-based composite material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- B22—CASTING; POWDER METALLURGY
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Abstract
The invention relates to a preparation method of a graphene-reinforced titanium-based composite material, which comprises the following steps: adding titanium alloy powder and graphene nanosheets into a planetary ball mill according to a certain mass ratio, and carrying out ball milling to obtain composite powder; and carrying out vacuum hot-pressing sintering on the composite powder to obtain a prefabricated body, and carrying out hot processing treatment on the prefabricated body to obtain the graphene titanium-based composite material. The invention solves the problems of low density and directional distribution of graphene of the graphene-based composite material.
Description
Technical Field
The invention belongs to the field of titanium alloy materials, and particularly relates to a preparation method of a graphene-reinforced titanium-based composite material.
Background
The titanium alloy has the advantages of small density, high specific strength, heat resistance, corrosion resistance and the like, is widely applied to the fields of aerospace and the like, and has higher and higher requirements on the performance of the titanium alloy along with the development of aerospace aircrafts and the requirement on structural function integration. One effective solution to this problem is the development of titanium-based composites. Compared with traditional reinforcements such as titanium carbide, titanium boride and silicon carbide, the graphene has more excellent mechanical, thermal and electrical properties. The modulus of the composite material reaches 1TPa, the breaking strength is about 125GPa, the thermal conductivity is 5000W/(mK), the graphene is used as a reinforcement, the titanium-based composite material with more excellent mechanical property is expected to be obtained, the thermal conductivity of the composite material is improved, and the problems of difficult processing of the titanium alloy and the like are solved.
The preparation difficulty of the graphene titanium-based composite material mainly lies in the following three aspects: (1) due to the addition of the graphene, the composite material is difficult to form, low in density and low in performance. (2) Graphene and titanium are easy to chemically react in a large temperature range to generate titanium carbide, so that the added graphene is easy to completely react, can only play a role of a carbon source, and cannot exert the excellent performance of the added graphene. (3) The graphene is difficult to uniformly disperse in the titanium matrix due to small density and large aspect ratio, and the agglomerated graphene cannot exert the excellent performance of the graphene, and the defect is easily formed by large agglomeration, so that the mechanical property of the composite material is reduced.
Disclosure of Invention
The invention solves the technical problems that the composite material is difficult to form, the density is low and the graphene is easy to agglomerate.
The invention is realized by the following technical scheme:
a preparation method of a graphene titanium-based composite material comprises the following steps:
the method comprises the following steps: preparing composite powder: adding titanium alloy powder and graphene nanosheets into a planetary ball mill according to a certain mass ratio, and carrying out ball milling to obtain composite powder;
step two: preparing a composite material preform: performing vacuum hot-pressing sintering on the composite powder obtained in the step one to obtain a composite material preform, wherein the sintering temperature is 400 ℃ below the alpha-beta phase transition temperature of the titanium alloy, the pressure is 20-200MPa, the time is 0.5-5h, the temperature and the pressure are increased, the temperature and the time are measured, and the composite material preform is cooled along with a furnace;
step three: preparing a graphene titanium-based composite material: and D, carrying out hot working treatment on the composite material preform obtained in the step two.
It is preferable that: the mass ratio of the graphene nanosheet to the titanium alloy powder is 0.01: 99.9-5:95.
It is preferable that: in the first step, a zirconia ball-milling tank and grinding beads are used for ball milling, the ball-material ratio is 1:1-20, the rotating speed is 100-.
It is preferable that: the ball milling atmosphere adopts a vacuum or argon protection method, and the outer wall of the ball milling tank is cooled by circulating water or an intermittent method.
It is preferable that: the hot working is hot extrusion or hot forging, the temperature is within 100 ℃ above and below the alpha-beta phase transition temperature of the titanium alloy, and the deformation is 50-1000%.
It is preferable that: the hot working step requires the application of lubricating oil to the preform surface and the mold surface.
It is preferable that: the heat treatment mode is hot rolling, and the hot rolling step comprises the following steps: preparing a sheath, and filling the preform into the sheath for welding, sealing and hot rolling at the temperature of 100 ℃ above and below the alpha-beta phase transition temperature of the titanium alloy, wherein the deformation is 10-50%.
It is preferable that: the sheath is made of titanium alloy.
Compared with the prior art, the invention has the following beneficial technical effects:
1. the preparation process is simple, the cost is low, and the density is greatly improved.
2. The composite material is subjected to large plastic deformation in the hot working process, so that the graphene is directionally distributed, and the thermal conductivity and the mechanical property of the composite material are improved simultaneously.
3. The method combines vacuum hot-pressing sintering with directional plastic deformation (hot rolling, hot extrusion and hot forging), and solves the problems of difficult composite material forming, low density, easy graphene agglomeration and directional graphene distribution.
4. The method of combining sintering at a lower temperature (phase transition temperature) with high-temperature short-time plastic deformation is adopted, the reaction of titanium and graphene is inhibited, and the structural integrity of the graphene is improved.
Drawings
FIG. 1 is a scanning electron micrograph of a composite prepared in example one;
FIG. 2 is a scanning electron micrograph of a composite prepared in example one;
FIG. 3 is a scanning electron micrograph of a composite prepared according to example one;
FIG. 4 is an XRD pattern of the composite material prepared in the first example;
FIG. 5 is a Raman spectrum of a composite prepared in the first example;
FIG. 6 is a graph of the compressive properties of the composite prepared in the first example;
fig. 7 is the thermal conductivity of the composite material prepared in the first example.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a detailed description of the present invention will be given below with reference to the accompanying drawings and specific embodiments. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth to provide a thorough understanding of the present invention, and the described embodiments are merely a subset of the embodiments of the present invention, rather than a complete embodiment. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
(1) a preparation method of a graphene titanium-based composite material comprises the following steps:
step 1, preparing composite powder: according to the mass fraction of 2% of graphene, mixing TC4The powder and the graphene nanosheets are added into a planetary ball mill in an argon atmosphere, a zirconia ball milling tank and grinding beads are selected, the zirconia is high in hardness and good in wear resistance, the sample is prevented from being polluted, the ball-material ratio is 1:1, the graphene structure can be effectively protected from being damaged due to low energy, the rotating speed is 180rmp, the ball milling time is 8 hours, the ball milling atmosphere is protected by vacuum or argon, and the temperature of the tank body is prevented from being too high due to the adoption of a circulating water cooling method on the outer wall of the ball milling tank.
Step 3, preparing the graphene titanium-based composite material: preparing a sheath with the same material as the matrix and the wall thickness of the sheath of 10mm according to the size of the preform obtained in the step 2, putting the preform into the sheath, welding, sealing and hot rolling at the hot rolling temperature of 970 ℃, wherein the deformation is 20%, and the graphene titanium-based composite material is obtained after hot rolling.
(2) Comparative test
The specific implementation steps are as follows:
step 1, preparing graphene/TC4Composite powder: according to the mass fraction of 0% of graphene, mixing TC4Adding argon into powder and graphene nanosheet to form an atmosphereThe planetary ball mill adopts a zirconia ball milling tank and milling beads, the ball-material ratio is 1:1, the rotating speed is 180rmp, the ball milling time is 8 hours, and the reverse ball milling is carried out after the milling is stopped for 20 minutes after 10 minutes.
Step 3, preparing the graphene titanium-based composite material: preparing pure TC according to the size of the preform obtained in the step 24And (3) sheathing, wherein the wall thickness of the sheathing is 10mm, placing the prefabricated body into the sheathing, welding, sealing and hot rolling, wherein the hot rolling temperature is 970 ℃, the deformation is 20%, and the graphene titanium-based composite material is obtained after hot rolling.
Test comparison and performance test analysis: in fig. 1, 2 and 3, it can be seen that after ball milling, the graphene is uniformly distributed in TC4Surface of powder, TC4The powder is well combined, and the graphene is directionally distributed in the hot rolling direction after hot rolling, so that the mechanical property and the thermal conductivity of the composite material are improved. As can be seen in fig. 4, the chemical reaction occurs during the preparation of the composite material to produce titanium carbide. Fig. 5 shows that the characteristic peak of graphene in the composite material is obvious, which indicates that graphene does not completely react, and graphene with a good structure is retained. FIG. 6 is the composite compression behavior, and it can be seen that the composite yield strength is compared to pure TC4The improvement is about 22 percent. FIG. 7 is the composite thermal conductivity, and it can be seen that TC is the direction of hot rolling4-2% GNPs composite material vs. matrix TC4Respectively increased by 17%.
Example 2: a preparation method of a graphene titanium-based composite material comprises the following steps:
the method comprises the following steps: preparing composite powder: adding titanium alloy powder and graphene nanosheets into a planetary ball mill according to the mass fraction of 5% of graphene, performing ball milling to obtain composite powder, wherein the ball milling atmosphere is protected by vacuum or argon, and the outer wall of a ball milling tank is water-cooled by circulating water or in an intermittent manner (ball milling is suspended for 1-30min for 1-3 times of ball milling time). Ball-milling with a zirconia ball-milling tank and grinding beads at a ball-material ratio of 1:10 and a rotation speed of 500rmp for 100 h;
step two: preparing a prefabricated body: and (3) carrying out vacuum hot-pressing sintering on the composite powder obtained in the step one to obtain a preform, wherein the sintering temperature is 960 ℃, the pressure is 200MPa, the time is 5 hours, the temperature and the pressure are reached, the temperature and the pressure are measured, and the preform is cooled along with a furnace.
Step three: preparing a graphene titanium-based composite material: and (3) carrying out hot extrusion on the preform obtained in the step two, wherein the temperature is 1100 ℃, and the deformation is 1000%. And (3) obtaining the graphene titanium-based composite material after hot extrusion, wherein lubricating oil is required to be coated on the surface of the preform and the surface of the die in the hot extrusion process.
Example 3: a preparation method of a graphene titanium-based composite material comprises the following steps:
the method comprises the following steps: preparing composite powder: adding titanium alloy powder and graphene nanosheets into a planetary ball mill according to the mass fraction of 3% of graphene, performing ball milling to obtain composite powder, wherein the ball milling atmosphere is protected by vacuum or argon, and the outer wall of a ball milling tank is water-cooled by circulating water or in an intermittent manner (ball milling is suspended for 1-30min for 1-3 times of ball milling time). Ball-milling with a zirconia ball-milling tank and grinding beads at a ball-material ratio of 1:1 and a rotation speed of 100rmp for 1 h;
step two: preparing a prefabricated body: performing vacuum hot-pressing sintering on the composite powder obtained in the step one to obtain a prefabricated body, wherein the sintering temperature is 960 ℃, the pressure is 20MPa, the time is 0.5h, the temperature and the pressure are increased, the temperature and the pressure are measured, and the prefabricated body is cooled along with a furnace;
step three: preparing a graphene titanium-based composite material: and (3) performing hot forging on the preform obtained in the step two, wherein the hot extrusion temperature is 1100 ℃, and the deformation is 100%. And (3) obtaining the graphene titanium-based composite material after hot forging, wherein lubricating oil is required to be coated on the surface of the prefabricated part and the surface of a die in the hot forging process.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The embodiments given above are preferable examples for implementing the present invention, and the present invention is not limited to the above-described embodiments. Any non-essential addition and replacement made by the technical characteristics of the technical scheme of the invention by a person skilled in the art belong to the protection scope of the invention.
Claims (8)
1. The preparation method of the graphene titanium-based composite material is characterized by comprising the following steps:
the method comprises the following steps: preparing composite powder: adding titanium alloy powder and graphene nanosheets into a planetary ball mill according to a certain mass ratio, and carrying out ball milling to obtain composite powder;
step two: preparing a prefabricated body: performing vacuum hot-pressing sintering on the composite powder obtained in the step one to obtain a prefabricated body, wherein the sintering temperature is within 400 ℃ below the alpha-beta phase transition temperature of the titanium alloy, the pressure is 20-200MPa, the time is 0.5-5h, the temperature and the pressure are increased, the temperature and the time are counted, and the prefabricated body is cooled along with a furnace;
step three: preparing a graphene titanium-based composite material: and D, carrying out hot working treatment on the prefabricated body obtained in the step two to obtain the graphene titanium-based composite material.
2. The preparation method of the graphene titanium-based composite material according to claim 1, wherein the mass ratio of the graphene nanosheets to the titanium alloy powder is 0.01: 99.9-5:95.
3. The preparation method of the graphene titanium-based composite material as claimed in claim 2, wherein in the first step, the ball milling step is performed by using a zirconia ball milling tank and grinding beads, the ball-to-material ratio is 1:1-20, the rotation speed is 100-.
4. The preparation method of the graphene titanium-based composite material according to claim 3, wherein the atmosphere in the ball milling step is protected by vacuum or argon, and the outer wall of a ball milling tank is cooled by circulating water or by a batch method.
5. The method of claim 1, wherein the hot working is hot extrusion or hot forging, the temperature is within 100 ℃ above and below the α - β phase transition temperature of the titanium alloy, and the deformation is 50-1000%.
6. The method for preparing the graphene titanium-based composite material according to claim 5, wherein the hot working step requires applying a lubricant to the surface of the preform and the surface of the mold.
7. The method for preparing the graphene titanium-based composite material according to claim 1, wherein the heat treatment is hot rolling, and the hot rolling comprises the following steps: preparing a sheath, and filling the preform into the sheath for welding, sealing and hot rolling at the temperature of 100 ℃ above and below the alpha-beta phase transition temperature of the titanium alloy, wherein the deformation is 10-50%.
8. The method for preparing the graphene titanium-based composite material according to claim 7, wherein the sheath is made of titanium alloy.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111644615A (en) * | 2020-06-16 | 2020-09-11 | 西安稀有金属材料研究院有限公司 | Preparation method for realizing high strength and toughness of TC4 titanium alloy by co-strengthening method |
| CN111763849A (en) * | 2020-06-03 | 2020-10-13 | 西北工业大学 | Preparation method of high-thermal-conductivity titanium-based composite material |
| CN111961917A (en) * | 2020-08-25 | 2020-11-20 | 中国石油天然气集团有限公司 | Graphene oxide reinforced titanium alloy and preparation method thereof |
| CN112281088A (en) * | 2020-10-23 | 2021-01-29 | 西北工业大学 | Preparation method of carbon fiber reinforced titanium alloy composite material |
| CN113088735A (en) * | 2021-03-24 | 2021-07-09 | 东北大学 | Method for preparing high-strength plastic titanium-graphene composite material based on grading compounding |
| CN113122746A (en) * | 2021-04-16 | 2021-07-16 | 北京理工大学 | Preparation method of interface-reaction-free graphene/titanium-based nanocomposite |
| CN113789457A (en) * | 2021-09-18 | 2021-12-14 | 西北工业大学 | Method for preparing carbon nano tube reinforced aluminum matrix composite material by solid-liquid method |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111763849A (en) * | 2020-06-03 | 2020-10-13 | 西北工业大学 | Preparation method of high-thermal-conductivity titanium-based composite material |
| CN111644615A (en) * | 2020-06-16 | 2020-09-11 | 西安稀有金属材料研究院有限公司 | Preparation method for realizing high strength and toughness of TC4 titanium alloy by co-strengthening method |
| CN111644615B (en) * | 2020-06-16 | 2022-03-01 | 西安稀有金属材料研究院有限公司 | Preparation method for realizing high strength and toughness of TC4 titanium alloy by co-strengthening method |
| CN111961917A (en) * | 2020-08-25 | 2020-11-20 | 中国石油天然气集团有限公司 | Graphene oxide reinforced titanium alloy and preparation method thereof |
| CN111961917B (en) * | 2020-08-25 | 2021-09-28 | 中国石油天然气集团有限公司 | Graphene oxide reinforced titanium alloy and preparation method thereof |
| CN112281088A (en) * | 2020-10-23 | 2021-01-29 | 西北工业大学 | Preparation method of carbon fiber reinforced titanium alloy composite material |
| CN112281088B (en) * | 2020-10-23 | 2021-07-06 | 西北工业大学 | Preparation method of carbon fiber reinforced titanium alloy composite material |
| CN113088735A (en) * | 2021-03-24 | 2021-07-09 | 东北大学 | Method for preparing high-strength plastic titanium-graphene composite material based on grading compounding |
| CN113088735B (en) * | 2021-03-24 | 2022-04-22 | 东北大学 | Method for preparing high-strength plastic titanium-graphene composite material based on grading compounding |
| CN113122746A (en) * | 2021-04-16 | 2021-07-16 | 北京理工大学 | Preparation method of interface-reaction-free graphene/titanium-based nanocomposite |
| CN113122746B (en) * | 2021-04-16 | 2021-12-31 | 北京理工大学 | Preparation method of interface-reaction-free graphene/titanium-based nanocomposite |
| CN113789457A (en) * | 2021-09-18 | 2021-12-14 | 西北工业大学 | Method for preparing carbon nano tube reinforced aluminum matrix composite material by solid-liquid method |
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