CN116393695A - Titanium-based composite powder with shell-core structure and preparation method of composite material - Google Patents
Titanium-based composite powder with shell-core structure and preparation method of composite material Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 195
- 239000010936 titanium Substances 0.000 title claims abstract description 148
- 239000002131 composite material Substances 0.000 title claims abstract description 136
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 132
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 46
- 239000002184 metal Substances 0.000 claims abstract description 40
- 229910052751 metal Inorganic materials 0.000 claims abstract description 39
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000000280 densification Methods 0.000 claims abstract description 24
- 239000011159 matrix material Substances 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 238000011065 in-situ storage Methods 0.000 claims abstract description 8
- 239000006104 solid solution Substances 0.000 claims abstract description 8
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 63
- 239000000126 substance Substances 0.000 claims description 19
- 239000010949 copper Substances 0.000 claims description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 14
- 238000007747 plating Methods 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 10
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- 239000002994 raw material Substances 0.000 claims description 7
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- 238000006243 chemical reaction Methods 0.000 claims description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 6
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- 239000011733 molybdenum Substances 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
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- 238000003917 TEM image Methods 0.000 description 1
- 229910004353 Ti-Cu Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 239000008367 deionised water Substances 0.000 description 1
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- 238000001035 drying Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
- ZPZCREMGFMRIRR-UHFFFAOYSA-N molybdenum titanium Chemical compound [Ti].[Mo] ZPZCREMGFMRIRR-UHFFFAOYSA-N 0.000 description 1
- 229910001000 nickel titanium Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
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- 238000010587 phase diagram Methods 0.000 description 1
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- 238000002490 spark plasma sintering Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- MAKDTFFYCIMFQP-UHFFFAOYSA-N titanium tungsten Chemical compound [Ti].[W] MAKDTFFYCIMFQP-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- 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
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- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- 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
- B22F3/15—Hot isostatic pressing
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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
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- 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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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Abstract
The invention discloses a preparation method of a titanium-based composite powder with a shell-core structure and a composite material, which comprises the following steps: 1. selecting matrix powder and a coating precursor; 2. pouring matrix powder into a vibration tank to serve as an anode by taking a metal target of a coating precursor as a cathode, uniformly vibrating and rolling in the vibration tank, and performing magnetron sputtering to obtain titanium-based composite powder with a shell-core structure; 3. and (3) densification sintering to obtain the nano-phase in-situ authigenic reinforced titanium-based composite material. The invention is based on the principle of magnetron sputtering, combines the control of bias voltage, power and time of magnetron sputtering, precisely controls the uniformity and thickness of the shell of the titanium-based composite powder with a shell-core structure, realizes solid solution precipitation of nanoscale intermetallic compound particles/whiskers in the titanium-based powder and dispersion strengthening of alpha or beta phases by regulating and controlling densification sintering process parameters, improves the strong plasticity matching level of titanium-based alloy and composite materials, is simple to operate, is environment-friendly, and has wide industrial production prospect.
Description
Technical Field
The invention belongs to the technical field of metal material processing, and particularly relates to a titanium-based composite powder with a shell-core structure and a preparation method of the composite material.
Background
In recent years, the rapid development of aerospace industry and the updating of weaponry in China have put higher demands on the development of light, high-strength and high-reliability materials. The titanium-based composite material is a new material obtained by carrying out physical-chemical compounding on a titanium alloy matrix and a reinforcing phase with excellent performance in an external or autogenous mode, and has the characteristics of high specific strength, specific rigidity, high temperature resistance and the like. Many factors affecting the performance of the titanium-based composite material, such as the characteristics, distribution, types and content of the reinforcing phase, and the most important problem affecting the material performance in the powder metallurgy technology is the problem of spatial distribution and interface bonding of the reinforcing body. In order to solve the problem, researchers have improved the interface problem by physical and chemical techniques, mainly coating nano or micro reinforcing phases on the surface of titanium alloy powder by ball milling dispersion or the like, however, ball milling treatment usually grinds metals with better ductility such as copper or nickel or the like into pieces, resulting in uneven distribution on the titanium alloy powder, difficult control of thickness, and difficulty in obtaining titanium alloy materials with excellent properties by introducing impurities and increasing oxygen content during ball milling. On the other hand, the adoption of the electroless plating surface modified titanium alloy powder can cause uneven distribution of the modified reinforcement on the surface of the titanium alloy and serious pollution of the adopted reagent, which is unfavorable for the purity of the titanium alloy composite powder (Vacuum, 2021:110330.). Meanwhile, formaldehyde and the like are used as reducing agents in chemical plating, formaldehyde is a potential carcinogen, the plating solution is unstable and is not beneficial to environmental protection, the important strategy of green sustainable development in China is not met, the surface of the composite powder prepared by the method is uneven, a large amount of copper oxide exists on the surface, and the existence of the oxide can influence the performance of the composite material. Therefore, the regulation and optimization of the uniformity of the powder is important to the improvement of the performance of the composite material.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a shell-core structure titanium-based composite powder and a composite material aiming at the defects of the prior art. The method adopts a magnetron sputtering process to modify, so that metal atoms of an anode metal target are uniformly sputtered on the surface of spherical titanium-based powder which uniformly vibrates and rolls in a cathode, and the titanium-based composite powder with a shell-core structure taking metal as a shell and spherical titanium-based powder as a core is obtained, thereby realizing the precise control on the uniformity and thickness of the shell, further carrying out densification, sintering and solid solution precipitation on nanoscale intermetallic compound particles/whiskers and dispersing and strengthening alpha or beta phases, improving the strong plasticity matching level of a titanium alloy material, and solving the problems of uneven distribution and thickness, agglomeration and disturbance of strong plasticity of the composite material in the traditional preparation of the titanium-based composite material by powder metallurgy.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the shell-core structure titanium-based composite powder and the composite material is characterized by comprising the following steps:
step one, raw material selection: spherical titanium-based powder prepared by a rotary electrode method is selected as matrix powder, and metal which has solid solution reaction with titanium alloy is selected as a precursor of film plating on the surface of the matrix powder; the spherical titanium-based powder is titanium or titanium alloy powder;
preparing titanium-based composite powder with a shell-core structure: pouring the spherical titanium-based powder of the substrate powder selected in the step one into a vibration tank of a magnetron sputtering device and integrally taking the spherical titanium-based powder of the substrate powder as an anode, adjusting the vibration frequency and the vibration amplitude of the anode, keeping the spherical titanium-based powder uniformly vibrated and rolled in the vibration tank, and simultaneously adjusting and controlling bias voltage, power and time to perform magnetron sputtering, so that metal atoms sputtered by the cathode metal target are uniformly coated on the surface of the spherical titanium-based powder, and obtaining metal-titanium alloy shell-core structure composite powder with the thickness of nanometer or micrometer, namely the shell-core structure titanium-based composite powder;
step three, preparing a composite material: and (3) performing densification sintering on the titanium-based composite powder with the shell-core structure obtained in the step two to obtain the nano-phase in-situ autogenous reinforced titanium-based composite material.
The invention is based on the principle of magnetron sputtering, firstly, spherical titanium-based powder is put into a vibration tank of the magnetron sputtering equipment and is integrally used as an anode, a metal target is used as a cathode, the vibration frequency and the vibration amplitude of the anode are regulated, the spherical titanium-based powder is kept uniformly vibrated and rolled in the vibration tank, the surface of the spherical titanium-based powder is fully exposed in the range of the metal target, and atoms of the metal target are ionized from Ar in sputtering gas such as argon + The energy is obtained under bombardment, when the energy is larger than the threshold value, metal atoms are separated from the metal target material and fly to the anode, and the metal atoms are uniformly coated on the surface of the spherical titanium-based powder to form a metal coating, so that the shell-core structure titanium-based composite powder taking metal as a shell and spherical titanium-based powder as a core is obtained, and meanwhile, the uniformity and thickness of the shell-core structure titanium-based composite powder, namely the metal coating, are regulated and controlled by regulating and controlling the bias voltage, the power and the time of magnetron sputtering. Further, the invention compacts and sinters the titanium-based composite powder with the shell-core structure to obtain the nano phaseIn the densification sintering process, according to the characteristics of plating metal and titanium alloy matrix, a shell metal plating layer uniformly coated in the shell-core structure titanium-based composite powder is subjected to solid solution precipitation reaction along the alpha or beta phase of the core spherical titanium-based powder, and the reaction product is selectively precipitated along the alpha or beta phase to form nano-phase intermetallic compound particles which are unevenly distributed in the matrix, so that excellent strengthening effect is exerted, and the strong plasticity matching level of the composite material is improved. For example, the preparation method of the invention is adopted to evenly plate a metal copper film on the surface of TC4 titanium alloy powder, and Ti is precipitated along the beta phase solid solution of the dual-phase titanium alloy in the densification sintering process by utilizing the Ti-Cu eutectoid reaction principle 2 Cu nanoparticles, formed Ti 2 The Cu nano particles/whiskers have excellent strengthening effect and good corrosion resistance, and meanwhile, the strong plastic matching level of the composite material is improved.
The preparation method of the shell-core structure titanium-based composite powder and the composite material is characterized in that the particle size of the spherical titanium-based powder in the first step is 15-150 mu m, the chemical components of the spherical titanium-based powder meet the requirements of national standard GB/T3620.1-2016 for titanium and titanium alloy brands and chemical components, and satellite powder and hollow powder are not contained. More preferably, the particle size of the spherical titanium-based powder is 75 μm to 150 μm. Because the magnetron sputtering has directionality, the metal plating can be realized only on the surface facing the sputtering target surface, so the particle size of the spherical titanium-based powder is controlled to be 15-150 mu m, and each part of the surface of the spherical titanium-based powder can be exposed in the sputtering environment with equal probability in the uniform vibration rolling process in the vibration groove, thereby obtaining uniform metal plating on the surface of the spherical titanium-based powder, and realizing the regulation and control of the uniformity of the metal plating.
The preparation method of the shell-core structure titanium-based composite powder and the composite material is characterized in that the metal which is subjected to solid solution reaction with the titanium alloy in the first step is copper, nickel, tungsten or molybdenum.
The preparation method of the titanium-based composite powder and the composite material with the shell-core structure is characterized in that the mass purity of the metal target in the second step is more than 99.995%. By adopting the high-purity metal target, the phenomenon that impurities are plated on the surface of the spherical titanium-based powder so as to generate impurity products in the sintering process and influence the structure and mechanical properties of the composite material is avoided.
The preparation method of the titanium-based composite powder and the composite material with the shell-core structure is characterized in that the bias voltage of the magnetron sputtering in the second step is 0V-200V, the power is 100W-300W, and the time is 0.5 h-4 h. The invention controls the thickness and uniformity of the shell metal coating by controlling the parameters of magnetron sputtering, especially the time.
The preparation method of the titanium-based composite powder and the composite material with the shell-core structure is characterized in that the densification sintering temperature in the third step is 800-1100 ℃, the heat preservation time is 5-120 min, and the pressure is 30-150 MPa.
The preparation method of the titanium-based composite powder and the composite material with the shell-core structure is characterized in that the densification sintering in the third step is plasma sintering, hot-press sintering or hot isostatic pressing sintering.
The preparation method of the titanium-based composite powder and the composite material with the shell-core structure is characterized in that the densification sintering is plasma sintering, the temperature of the plasma sintering is 1000 ℃, the heat preservation time is 5min, and the pressure is 40MPa.
Compared with the prior art, the invention has the following advantages:
1. the invention is based on the magnetron sputtering principle, and the spherical titanium-based powder in the cathode is controlled to keep uniform vibration and rolling, so that metal atoms of the anode metal target are uniformly sputtered on the surface of the spherical titanium-based powder to form a metal coating, the shell-core structure titanium-based composite powder taking metal as a shell and the spherical titanium-based powder as a core is obtained, and the bias voltage, the power and the time of the magnetron sputtering are controlled, so that the uniformity and the thickness of the shell-core structure titanium-based composite powder are precisely controlled, and the technical problems of easy deformation and uneven distribution when the soft metal strengthens the titanium alloy in the traditional ball milling process are solved.
2. The invention creatively plates metal which can be dissolved and precipitated on the surface of the spherical titanium-based powder as a coating precursor, calculates and combines a solution precipitation mechanism by utilizing a metal-titanium binary phase diagram, realizes solution precipitation of nano-scale metal particles in the titanium-based powder and dispersion strengthening of alpha or beta phase by regulating and controlling densification sintering process parameters, and improves the strong plasticity matching level of the titanium alloy material.
3. Compared with other titanium alloy powder modification methods such as chemical plating, ball milling and the like, the magnetron sputtering process is simple to operate, green and environment-friendly, and the prepared shell-core structure titanium-based composite powder has high purity, controllable uniformity and high quality, and has wide industrial production prospect.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a distribution diagram of cross-sectional elements of a copper-TC 4 titanium alloy core-shell structure composite powder prepared in example 1 of the present invention.
Fig. 2 is a TEM image of the titanium matrix composite prepared in example 1 of the present invention.
Fig. 3 is an SEM image of the titanium-based composite powder prepared in comparative example 2 of the present invention.
Fig. 4 is an SEM image of the titanium-based composite powder prepared in comparative example 3 of the present invention.
FIG. 5 is a graph showing engineering stress-strain curves of the titanium-based composite materials prepared in example 1 and comparative examples 2 to 3 and TC4 titanium alloy prepared in comparative example 1.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, raw material selection: spherical TC4 titanium alloy powder prepared by a rotary electrode method is selected as matrix powder, and copper is selected as a precursor for coating the surface of the matrix powder; the particle size of the spherical TC4 titanium alloy powder is 75-150 mu m, the chemical components of the spherical TC4 titanium alloy powder meet the requirements of national standard GB/T3620.1-2016 (brand and chemical components of titanium and titanium alloy), and satellite powder and hollow powder are avoided;
preparing titanium-based composite powder with a shell-core structure: the method comprises the steps of taking a copper target with the mass purity of 99.995% as a cathode, pouring the spherical TC4 titanium alloy powder selected in the first step into a vibration groove of magnetron sputtering equipment and taking the whole as an anode, adjusting the vibration frequency and the vibration amplitude of the anode, keeping the spherical TC4 titanium alloy powder uniformly vibrated and rolled in the vibration groove, and simultaneously adjusting the bias voltage to 0V and the power to 200W for magnetron sputtering for 3.0h, so that copper atoms sputtered by the cathode copper target are uniformly coated on the surface of the spherical TC4 titanium alloy powder, and obtaining copper-TC 4 titanium alloy shell-core structure composite powder, namely shell-core structure titanium-base composite powder;
step three, preparing a composite material: performing densification sintering on the titanium-based composite powder with the shell-core structure obtained in the step two to obtain a nano-phase in-situ autogenous reinforced titanium-based composite material; the densification sintering is plasma sintering, the temperature is 1000 ℃, the heat preservation time is 5min, and the pressure is 40MPa.
Fig. 1 is a distribution diagram of cross-section elements of a composite powder with a copper-TC 4 titanium alloy shell-core structure prepared in this example, and as can be seen from fig. 1, cu in the composite powder is uniformly distributed on the periphery of spherical TC4 titanium alloy powder and forms a shell-core structure, the thickness of the Cu shell is uniform, the bonding with the interface between TC4 titanium alloy cores is good, no metallurgical defect exists, and the average size of the composite powder is 1 μm.
FIG. 2 is an SEM image of a titanium-based composite material prepared according to this example, and it can be seen from FIG. 2 that the composite material contains nano-scale Ti 2 Cu is uniformly dispersed in the titanium matrix tissue.
Example 2
The embodiment comprises the following steps:
step one, raw material selection: spherical TC4 titanium alloy powder prepared by a rotary electrode method is selected as matrix powder, and copper is selected as a precursor for coating the surface of the matrix powder; the particle size of the spherical TC4 titanium alloy powder is 75-150 mu m, the chemical composition of the spherical TC4 titanium alloy powder meets the requirements of national standard GB/T3620.1-2016 for titanium and titanium alloy brands and chemical compositions, and satellite powder and hollow powder are avoided;
preparing titanium-based composite powder with a shell-core structure: the method comprises the steps of taking a copper target with the mass purity of 99.995% as a cathode, pouring the spherical TC4 titanium alloy powder selected in the first step into a vibration tank of a magnetron sputtering device and taking the whole as an anode, adjusting the vibration frequency and the vibration amplitude of the anode, keeping the spherical titanium-based powder uniformly vibrated and rolled in the vibration tank, and simultaneously adjusting the bias voltage to be 100V and the power to be 100W for magnetron sputtering for 0.5h, so that copper atoms sputtered by the cathode copper target are uniformly coated on the surface of the spherical TC4 titanium alloy powder, and obtaining copper-TC 4 titanium alloy shell-core structure composite powder, namely shell-core structure titanium-based composite powder;
step three, preparing a composite material: performing densification sintering on the titanium-based composite powder with the shell-core structure obtained in the step two to obtain a nano-phase in-situ autogenous reinforced titanium-based composite material; the densification sintering is plasma sintering, the temperature is 800 ℃, the heat preservation time is 15min, and the pressure is 30MPa.
Example 3
The embodiment comprises the following steps:
step one, raw material selection: selecting spherical TC4 titanium alloy powder prepared by a rotating electrode method as matrix powder, and selecting nickel as a precursor for coating a film on the surface of the matrix powder; the particle size of the spherical TC4 titanium alloy powder is 75-150 mu m, the chemical components of the spherical TC4 titanium alloy powder meet the requirements of national standard GB/T3620.1-2016 (brand and chemical components of titanium and titanium alloy), and satellite powder and hollow powder are avoided;
preparing titanium-based composite powder with a shell-core structure: pouring the spherical titanium alloy powder selected in the first step into a vibration tank of a magnetron sputtering device and taking the spherical titanium alloy powder as an anode as a whole, adjusting the vibration frequency and the vibration amplitude of the anode, keeping the spherical titanium-based powder uniformly vibrated and rolled in the vibration tank, and simultaneously adjusting the bias voltage to 200V and the power to 300W for magnetron sputtering for 4.0h, so that nickel atoms sputtered by the cathode nickel target are uniformly coated on the surface of the spherical TC4 titanium alloy powder, and obtaining the nickel-titanium alloy shell-core structure composite powder, namely the shell-core structure titanium-based composite powder;
step three, preparing a composite material: performing densification sintering on the titanium-based composite powder with the shell-core structure obtained in the step two to obtain a nano-phase in-situ autogenous reinforced titanium-based composite material; the densification sintering is hot-pressed sintering, the temperature is 1100 ℃, the heat preservation time is 60min, and the pressure is 60MPa.
Example 4
The embodiment comprises the following steps:
step one, raw material selection: spherical Ti powder prepared by a rotary electrode method is selected as matrix powder, and tungsten is selected as a precursor for coating a film on the surface of the matrix powder; the particle size of the spherical Ti powder is 15-53 mu m, the chemical components of the spherical Ti powder meet the requirements of national standard GB/T3620.1-2016 titanium and titanium alloy brand and chemical components, and satellite powder and hollow powder are avoided;
preparing titanium-based composite powder with a shell-core structure: the tungsten target with the mass purity of 99.995% is used as a cathode, the spherical Ti powder selected in the first step is poured into a vibration tank of a magnetron sputtering device and is integrally used as an anode, the vibration frequency and the vibration amplitude of the anode are regulated, the spherical Ti powder is kept uniformly vibrated and rolled in the vibration tank, and magnetron sputtering is carried out for 0.5h under the condition that the regulating bias voltage is 100V and the power is 100W, so that tungsten atoms sputtered by the cathode tungsten target are uniformly coated on the surface of the spherical Ti powder, and the tungsten-titanium shell-core structure composite powder, namely the shell-core structure titanium-based composite powder is obtained;
step three, preparing a composite material: performing densification sintering on the titanium-based composite powder with the shell-core structure obtained in the step two to obtain a nano-phase in-situ autogenous reinforced titanium-based composite material; the densification sintering is hot isostatic pressing sintering, the temperature is 800 ℃, the heat preservation time is 120min, and the pressure is 150MPa.
Example 5
The embodiment comprises the following steps:
step one, raw material selection: spherical Ti powder prepared by a rotary electrode method is selected as matrix powder, and molybdenum is selected as a precursor for coating a film on the surface of the matrix powder; the particle size of the spherical Ti powder is 53-75 mu m, the chemical components of the spherical Ti powder meet the requirements of national standard GB/T3620.1-2016 titanium and titanium alloy brand and chemical components, and satellite powder and hollow powder are avoided;
preparing titanium-based composite powder with a shell-core structure: the method comprises the steps of taking a molybdenum target with the mass purity of 99.995% as a cathode, pouring spherical Ti powder selected in the first step into a vibration tank of magnetron sputtering equipment and taking the spherical Ti powder as an anode as a whole, adjusting the vibration frequency and the vibration amplitude of the anode, keeping the spherical Ti powder uniformly vibrated and rolled in the vibration tank, and simultaneously adjusting the bias voltage to be 100V and the power to be 100W for magnetron sputtering for 0.5h, so that molybdenum atoms sputtered by the cathode molybdenum target are uniformly coated on the surface of the spherical Ti powder, and obtaining molybdenum-titanium shell-core structure composite powder, namely shell-core structure titanium-base composite powder;
step three, preparing a composite material: performing densification sintering on the titanium-based composite powder with the shell-core structure obtained in the step two to obtain a nano-phase in-situ autogenous reinforced titanium-based composite material; the densification sintering is isostatic pressing sintering, the temperature is 800 ℃, the heat preservation time is 60min, and the pressure is 100MPa.
Comparative example 1
The specific process of this comparative example is: directly performing spark plasma sintering on spherical TC4 titanium alloy powder with the particle size of 75-150 mu m to obtain TC4 titanium alloy; the sintering temperature of the spark plasma is 1000 ℃, the heat preservation time is 5min, and the pressure is 40MPa.
Comparative example 2
The specific process of this comparative example is: adding spherical TC4 titanium alloy powder and Cu powder with particle diameters of 75-150 mu m into a stainless steel ball grinding tank for ball milling, wherein the ball-to-material ratio is 3:1, rotating at 300rpm, ball milling for 2 hours to obtain titanium-based composite powder, and sintering the titanium-based composite powder to obtain a composite material; the sintering temperature is 1000 ℃, the time is 5min, and the pressure is 40MPa.
Fig. 3 is an SEM image of the titanium-based composite powder prepared in this comparative example, and as can be seen from fig. 3, cu in the titanium-based composite powder is not uniformly distributed on the spherical TC4 titanium alloy powder, an obvious core-shell structure cannot be formed, obvious agglomeration occurs, and the sizes of the agglomerates are different.
Comparative example 3
The specific process of this comparative example is: placing spherical TC4 titanium alloy powder in acetone solution, ultrasonically cleaning for 15min, placing in NaOH solution at 40deg.C for pretreatment for 20min, and placing pretreated spherical TC4 titanium alloy powder in CuSO solution containing 9.75g/L 4 ·5H 2 O、25g/L C 4 H 4 O 6 KNa·4H 2 O、12mL/L CH 2 O、10mg/LC 10 H 8 N 2 Is a solution of (2)Lightly stirring the solution, filtering, washing with deionized water and ethanol, drying in a vacuum oven at 100 ℃ for 20min to obtain titanium-based composite powder, and sintering the titanium-based composite powder to obtain a composite material; the sintering temperature is 1000 ℃, the time is 5min, and the pressure is 40MPa.
Fig. 4 is an SEM image of the titanium-based composite powder prepared in this comparative example, and it can be seen from fig. 4 that Cu agglomerates in the titanium-based composite powder are distributed on the surface of the spherical TC4 titanium alloy powder, and the sizes are different.
Comparing fig. 1 and fig. 3 to 4, it can be seen that, in example 1, a magnetron sputtering modification method is adopted to obtain a copper plating shell with uniform dispersion, uniform thickness and good bonding on the surface of the spherical TC4 titanium alloy powder, so as to obtain a titanium-based composite powder with a shell-core structure.
FIG. 5 is a graph showing engineering stress-strain curves of the titanium-based composite material prepared in example 1 and comparative examples 2-3 and the TC4 titanium alloy prepared in comparative example 1, and as can be seen from FIG. 5, the titanium-based composite material prepared in example 1 has a better strong plastic matching level, compared with the TC4 alloy prepared in comparative example 1 by direct powder sintering, the tensile strength is improved to 1070MPa, the elongation is not reduced, particularly the uniform elongation, and meanwhile, the tensile strength of the titanium-based composite material prepared in example 1 is improved to a larger extent than that of the titanium-based composite material prepared in comparative example 2, and the elongation is equivalent, which indicates that the metal modification of the invention has a remarkable improvement on the mechanical property of the titanium alloy; the titanium-based composite material prepared by adopting chemical plating in comparative example 3 has higher tensile strength, but the plasticity of the titanium-based composite material is very poor and is far lower than engineering use requirements due to uneven distribution and obvious agglomeration of copper powder in the preparation process. In conclusion, the preparation method solves the problem of uneven distribution of soft phase metal in the traditional powder metallurgy preparation process of the titanium-based composite material, improves the plasticity of the titanium-based composite material, and realizes good strong plastic matching.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (8)
1. The preparation method of the shell-core structure titanium-based composite powder and the composite material is characterized by comprising the following steps:
step one, raw material selection: spherical titanium-based powder prepared by a rotary electrode method is selected as matrix powder, and metal which has solid solution reaction with titanium alloy is selected as a precursor of film plating on the surface of the matrix powder; the spherical titanium-based powder is titanium or titanium alloy powder;
preparing titanium-based composite powder with a shell-core structure: pouring the spherical titanium-based powder of the substrate powder selected in the step one into a vibration tank of a magnetron sputtering device and integrally taking the spherical titanium-based powder of the substrate powder as an anode, adjusting the vibration frequency and the vibration amplitude of the anode, keeping the spherical titanium-based powder uniformly vibrated and rolled in the vibration tank, and simultaneously adjusting and controlling bias voltage, power and time to perform magnetron sputtering, so that metal atoms sputtered by the cathode metal target are uniformly coated on the surface of the spherical titanium-based powder, and obtaining metal-titanium alloy shell-core structure composite powder with the thickness of nanometer or micrometer, namely the shell-core structure titanium-based composite powder;
step three, preparing a composite material: and (3) performing densification sintering on the titanium-based composite powder with the shell-core structure obtained in the step two to obtain the nano-phase in-situ autogenous reinforced titanium-based composite material.
2. The preparation method of the shell-core structure titanium-based composite powder and the composite material, which are disclosed in claim 1, is characterized in that the particle size of the spherical titanium-based powder in the first step is 15-150 μm, the chemical composition of the spherical titanium-based powder meets the requirements of national standard GB/T3620.1-2016 (brand and chemical composition of titanium and titanium alloy), and no satellite powder and hollow powder exist.
3. The method for preparing titanium-based composite powder and composite material with shell-core structure according to claim 1, wherein the metal which is subjected to solid solution reaction with titanium alloy in the first step is copper, nickel, tungsten or molybdenum.
4. The preparation method of the shell-core structure titanium-based composite powder and the composite material according to claim 1, wherein the mass purity of the metal target in the second step is more than 99.995%.
5. The preparation method of the titanium-based composite powder and the composite material with the shell-core structure, which are disclosed in claim 1, is characterized in that the bias voltage of the magnetron sputtering in the second step is 0-200V, the power is 100-300W, and the time is 0.5-4 h.
6. The preparation method of the titanium-based composite powder and the composite material with the shell-core structure, which are disclosed in claim 1, is characterized in that the densification sintering temperature in the step three is 800-1100 ℃, the heat preservation time is 5 min-120 min, and the pressure is 30-150 MPa.
7. The method for preparing titanium-based composite powder and composite material with shell-core structure according to claim 1, wherein the densification sintering in the third step is plasma sintering, hot-press sintering or hot isostatic pressing sintering.
8. The preparation method of the titanium-based composite powder and the composite material with the shell-core structure, which are disclosed in claim 1, is characterized in that in the third step, densification sintering is performed by plasma sintering, the temperature of the plasma sintering is 1000 ℃, the heat preservation time is 5min, and the pressure is 40MPa.
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