CN117965936A - 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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- CN117965936A CN117965936A CN202410142874.4A CN202410142874A CN117965936A CN 117965936 A CN117965936 A CN 117965936A CN 202410142874 A CN202410142874 A CN 202410142874A CN 117965936 A CN117965936 A CN 117965936A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 30
- 239000010936 titanium Substances 0.000 title claims abstract description 30
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 67
- 238000000227 grinding Methods 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 16
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 238000011049 filling Methods 0.000 abstract 1
- 229910017945 Cu—Ti Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000011156 metal matrix composite Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
-
- 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
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to the technical field of graphene toughening titanium-based composite materials, and particularly relates to a preparation method of a graphene toughening titanium-based composite material, which comprises the following steps: and (3) filling titanium alloy powder into a ball milling tank made of high-purity graphite, adding a certain amount of grinding balls, performing ball milling and mixing powder by controlling frequency, thus obtaining graphene/titanium-based composite powder, and performing sintering by a powder metallurgy process to obtain the graphene-toughened titanium-based composite material. The obtained composite material has high strength and high ductility. The preparation method provided by the invention has low technical requirements, no pollution in the preparation process and easy popularization and implementation.
Description
Technical Field
The invention belongs to the technical field of graphene tenacious titanium-based composite materials, and particularly relates to a preparation method of a graphene tenacious titanium-based composite material.
Background
Graphene has excellent electrical, thermal and mechanical properties, and can be used as a reinforcing phase to obviously improve the comprehensive properties of the metal matrix composite, but serious agglomeration phenomenon, high price, stearic acid added in the mixing process and other process control agents cause great challenges for preparing the graphene reinforced metal matrix composite. To address these problems, in situ synthesized graphene is used in the preparation of graphene reinforced metal matrix composites, such as chemical vapor deposition processes. However, the chemical vapor deposition process is cumbersome and time-consuming, and generally uses an organic material as a carbon source, which inevitably causes environmental pollution, and the process is cumbersome and not suitable for large-scale industrial production.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene toughening titanium-based composite material, which can realize toughening of the titanium-based composite material.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of a graphene toughened titanium-based composite material comprises the following steps: and (3) putting titanium alloy powder and hard grinding balls with certain mass into a ball milling tank made of high-purity graphite, taking out the grinding balls after a certain ball milling time and ball milling frequency, obtaining graphene/titanium-based composite powder with a certain graphene mass fraction, and sintering by using a powder metallurgy process to obtain the graphene toughened titanium-based composite material.
The titanium alloy powder is pure titanium, titanium alloy or alloy containing titanium element, and the grain size of the powder is not more than 200 mu m.
The grinding tank is made of high-purity graphite, the purity of the high-purity graphite is more than 99.9%, the volume is not less than 30mL, and the length-diameter ratio of the grinding tank is 1.2-4.
The grinding balls are hard grinding balls, the mass of each grinding ball is not more than 5g, and the ball-to-material ratio is 1:1-7:1.
In the ball milling process, the frequency of planetary ball milling is 30-95r/min, or the frequency of three-dimensional vibration ball milling is 10-28Hz.
The sintering temperature is 600-1200 ℃, the heating rate is 10-200 ℃/min, the sintering pressure is 20-200MPa, and the highest sintering temperature is kept for 5-60min.
Further, the titanium alloy powder is preferably spherical powder having a particle diameter of 5 to 200. Mu.m.
Further, in order to avoid contamination of the composite powder by the components of the grinding balls, the hard grinding balls are preferably zirconia ceramic grinding balls with a purity of more than 95%, and the diameter of the grinding balls is preferably 4-6mm. The ball-to-material ratio is preferably 4:1-6:1.
Further, the volume of the high purity graphite mill tank is preferably 2-5 times of the total volume of the ball material.
Further, the planetary ball milling frequency in the ball milling process is preferably 40-80r/min, and the three-dimensional vibration ball milling frequency is preferably 15-20Hz.
Further, the ball milling time is distinguished according to the ball milling type, the ball milling time of the planetary ball milling can be estimated according to the adding amount of graphene and t=J 1Mmλ2/3/(d3n2V2/3), the ball milling time of the three-dimensional vibration ball milling can be estimated according to t=J 2Mmf2λ2/3/(d3n2V2/3), wherein M is the adding amount of graphene, n is the rotating speed of the planetary ball milling, f is the ball milling frequency of the three-dimensional vibration ball milling, M is the total mass of the grinding ball, d is the diameter of the grinding ball, V is the volume of a graphite tank, lambda is the length-diameter ratio of the graphite tank, and J1 and J2 are the correlation coefficients of the planetary ball milling and the three-dimensional vibration ball milling respectively.
Further, the sintering temperature is preferably 800-1100 ℃, the sintering pressure is preferably 30-100MPa, the heating rate is preferably 80-150 ℃/min, and the heat preservation time is preferably 5-40min.
The invention has the advantages that:
1. The ball milling tank made of the high-purity graphite is a carbon source of graphene in a composite material, in the ball milling process, the hard grinding balls obtain certain mechanical energy, the graphene is peeled off from the inner wall of the ball milling tank by virtue of shearing action, and the graphene with certain quality is obtained by controlling the size of the grinding balls, the number of the grinding balls, the ball milling time and the ball milling frequency;
2. The preparation and the cladding of the graphene are carried out simultaneously, and in the ball milling process, after the graphene is stripped from the inner wall of the ball milling tank, the graphene can be immediately and mechanically mixed with the alloy powder, so that the in-situ preparation and uniform mixing of the graphene are realized, and the high-purity hard ceramic grinding balls are selected, so that the pollution of the grinding ball components to the composite powder can be effectively avoided; the process control agents such as stearic acid and the like are not needed in the powder mixing process, so that the method has obvious cost advantages and is environment-friendly, and more importantly, the agglomeration of graphene can be effectively inhibited, and the uniformity and comprehensive mechanical properties of the composite material are obviously improved;
3. In the ball milling process, the selection of the ball milling frequency is very important, the ball milling process is low-energy ball milling, but the ball milling frequency is within a certain range: the too low ball milling frequency enables the kinetic energy of the grinding balls to be low, so that the interlayer bonding energy of the graphene can not be overcome, and the graphene can not be effectively stripped to obtain the graphene, the ball milling time is greatly prolonged, and the preparation efficiency is reduced; the excessive ball milling frequency easily causes the grinding balls to have higher kinetic energy, the impact and the shearing of higher energy enable the products peeled from the wall of the ball milling tank to be graphite particles instead of graphene, and meanwhile, the higher ball milling energy easily damages the integrity of the grinding balls and pollutes the composite powder;
4. the addition amount of the graphene is related to the addition amount of the grinding balls, the size of the grinding balls and the ball milling frequency and the ball milling time. By adjusting the addition amount of the grinding balls and the size of the grinding balls and adjusting the ball milling frequency and the ball milling time, composite powder with different graphene addition amounts can be obtained.
Drawings
Fig. 1 is an SEM image of graphene/TC 4 composite powder with mass fraction of 0.06% and EDS results of Ti, al, V and C elements.
Fig. 2 is a laser raman spectrum of 0.06 wt% graphene toughened TC4 composite.
Detailed Description
Example 1
A preparation method of a graphene reinforced titanium-based composite material specifically comprises the following steps: 30g of TC4 titanium alloy powder with the average particle size of 80 mu m is mixed with zirconia grinding balls with the purity of 99% and the diameter of 5mm in a ball-milling ratio of 5:1, the mixture is put into a ball-milling tank which is made of high-purity graphite with the purity of 99.99% and the length-diameter ratio of 1.5 and has the capacity of 100mL, the ball-milling tank performs low-energy planetary ball milling in a planetary ball mill at the rotating speed of 50r/min, and graphene/TC 4 composite powder with the mass fraction of 0.06% is obtained after the calculation for 87min, and the actual time consumption is 95min. The element distribution of the powder surface is shown in figure 1. The composite powder is sintered by discharge plasma, the sintering temperature is 950 ℃, the sintering pressure is 35MPa, the vacuum degree is 3 multiplied by 10 -3 Pa, the heating rate is 100 ℃/min, the heat preservation time is 10min, and the graphene toughening TC4 composite material with 0.06: 0.06 wt.% is obtained after furnace cooling, and the laser Raman spectrum is shown in figure 2.
Comparative example 1
30G of TC4 titanium alloy powder with an average particle diameter of 80 μm was mixed with zirconia milling balls with a purity of 99% and a diameter of 5mm in a ball-material ratio of 5:1, charged into a conventional agate milling pot, and 0.018g of graphene nanoplatelets (0.06 wt%) were added, and subjected to high-energy ball milling in a planetary ball mill at a rotational speed of 200r/min for 30 min. After ball milling is finished, taking out the grinding balls, carrying out spark plasma sintering on the composite powder, wherein the sintering temperature is 950 ℃, the sintering pressure is 35MPa, the vacuum degree is 3×10 -3 Pa, the heating rate is 100 ℃/min, the heat preservation time is 10min, and the graphene reinforced TC4 composite material with 0.06 wt percent is obtained after furnace cooling.
Example 2
A preparation method of a graphene reinforced titanium-based composite material specifically comprises the following steps: 90g of Cu-Ti (2.0 wt% Ti) prealloyed powder with an average particle size of 43 μm is mixed with zirconia grinding balls with a purity of 99% and a diameter of 5mm in a ball-material ratio of 5:1, the mixture is put into a ball-milling tank which is made of high-purity graphite with a purity of 99.99% and an aspect ratio of 1.2 and has a capacity of 500mL, low-energy vibration ball milling is carried out in a three-dimensional vibration ball mill at a frequency of 20Hz, and graphene/Cu-Ti composite powder with a mass fraction of 0.1% is obtained after calculation for 104min, so that the actual time consumption is 121min. The composite powder is sintered by discharge plasma, the sintering temperature is 850 ℃, the heating rate is 100 ℃/min, the sintering pressure is 35MPa, the vacuum degree is 3 multiplied by 10 -3 Pa, the heat preservation time is 15min, and the graphene toughening Cu-Ti composite material with 0.1: 0.1 wt.% is obtained after furnace cooling.
Comparative example 2
90G of Cu-Ti (2.0 wt% Ti) prealloyed powder with the average particle size of 43 mu m is mixed with zirconia grinding balls with the purity of 99% and the diameter of 5mm in a ball-material ratio of 5:1, the mixture is put into a conventional PP ball-milling tank, 0.09g of graphene nano-sheets (0.1: 0.1 wt%) are added, high-energy vibration ball milling is carried out in a three-dimensional vibration ball mill at the frequency of 30Hz, and the graphene/Cu-Ti composite powder with the mass fraction of 0.1% is obtained after 40 min. The composite powder is sintered by spark plasma, the sintering temperature is 850 ℃, the heating rate is 100 ℃/min, the sintering pressure is 35MPa, the vacuum degree is 3 multiplied by 10 -3 Pa, the heat preservation time is 15min, and the graphene reinforced Cu-Ti composite material with 0.1: 0.1 wt.% is obtained after furnace cooling. Mechanical properties were measured for each of example 1, example 2, comparative example 1, comparative example 2 and the corresponding matrix materials, and the measurement results are shown in table 1.
TABLE 1
Claims (7)
1. A preparation method of a graphene reinforced titanium-based composite material is characterized by comprising the following steps: loading titanium alloy powder and hard grinding balls into a ball milling tank made of high-purity graphite according to the ball material ratio of 1:1-7:1, adopting planetary ball milling or three-dimensional vibration ball milling, wherein the planetary ball milling frequency is 30-95r/min, the ball milling time is calculated according to the graphene addition amount by a formula t=J 1Mmλ2/3/(d3n2V2/3), the three-dimensional vibration ball milling frequency is 10-28Hz, the ball milling time is calculated according to the graphene addition amount by a formula t=J 2Mm f 2λ2/3/(d3n2V2/3), M is the graphene addition amount, n is the rotating speed of the planetary ball milling, f is the ball milling frequency of the three-dimensional vibration ball milling, M is the total mass of the grinding balls, d is the diameter of the grinding balls, V is the volume of the graphite tank, lambda is the length-diameter ratio of the graphite tank, and J 1、J2 is the correlation coefficient of the planetary ball milling and the three-dimensional vibration ball milling respectively; grinding the above steps to obtain graphene/titanium-based composite powder, and sintering the graphene/titanium-based composite powder by using a powder sintering method to obtain the graphene-toughened titanium-based composite material.
2. The method for preparing the graphene-toughened titanium-based composite material according to claim 1, which is characterized by comprising the following steps: the titanium alloy powder is pure titanium, titanium alloy or alloy containing titanium element, preferably spherical powder, and the grain size is 5-200 mu m.
3. The method for preparing the graphene-toughened titanium-based composite material according to claim 2, which is characterized by comprising the following steps: the grinding balls are hard grinding balls, the mass of each grinding ball is not more than 5g, the hard grinding balls are preferably zirconia ceramic grinding balls with the purity of more than 95%, the diameter of each grinding ball is preferably 4-6mm, and the ball-to-material ratio is preferably 4:1-6:1.
4. The method for preparing the graphene-toughened titanium-based composite material according to claim 3, wherein the method comprises the following steps: the sintering temperature of the powder is 600-1200 ℃, the heating rate is 10-200 ℃/min, the sintering pressure is 20-200MPa, and the highest sintering temperature is kept for 5-60min.
5. The method for preparing the graphene-toughened titanium-based composite material according to claim 3, wherein the method comprises the following steps: the grinding tank is made of high-purity graphite, the purity of the high-purity graphite is greater than 99.9%, the volume is not less than 30mL, the volume is preferably 2-5 times of the total volume of the ball material, and the length-diameter ratio of the grinding tank is 1.2-4.
6. The method for preparing the graphene-toughened titanium-based composite material according to claim 1, which is characterized by comprising the following steps: the planetary ball milling frequency is preferably 40-80r/min in the ball milling process, and the three-dimensional vibration ball milling frequency is preferably 15-20Hz.
7. The method for preparing the graphene-toughened titanium-based composite material according to claim 4, which is characterized by comprising the following steps: the sintering temperature of the powder is 800-1100 ℃, the sintering pressure is 30-100MPa, the heating rate is 80-150 ℃/min, and the heat preservation time is 5-40min.
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