CN116117133A - Titanium-based composite powder and method for preparing same by using spin height Wen Zhengxing method - Google Patents
Titanium-based composite powder and method for preparing same by using spin height Wen Zhengxing method Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 172
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000010936 titanium Substances 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 63
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000002245 particle Substances 0.000 claims description 80
- 238000000227 grinding Methods 0.000 claims description 44
- 230000003014 reinforcing effect Effects 0.000 claims description 37
- 239000011159 matrix material Substances 0.000 claims description 31
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- 239000012298 atmosphere Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 8
- 230000001788 irregular Effects 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- PWKWDCOTNGQLID-UHFFFAOYSA-N [N].[Ar] Chemical compound [N].[Ar] PWKWDCOTNGQLID-UHFFFAOYSA-N 0.000 claims description 4
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 239000000654 additive Substances 0.000 description 11
- 230000000996 additive effect Effects 0.000 description 11
- 238000009826 distribution Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000007493 shaping process Methods 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000001746 injection moulding Methods 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001513 hot isostatic pressing Methods 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 238000006356 dehydrogenation reaction Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010288 cold spraying Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 238000012876 topography Methods 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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- C—CHEMISTRY; METALLURGY
- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- 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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention provides a titanium-based composite powder and a method for preparing the same by using a rotation height Wen Zhengxing method.
Description
Technical Field
The invention relates to the technical field of metal material preparation, in particular to titanium-based composite material powder and a method for preparing the same by using a rotation height Wen Zhengxing method.
Background
Titanium and titanium alloy have the advantages of light weight, high strength, good biocompatibility, low elastic modulus and the like, and are attracting general attention of researchers at home and abroad. The method is widely applied to the fields of automobiles, ships, aerospace, medical appliances and the like.
In recent years, however, with the rapid development of modern industry and scientific technology, more stringent requirements are put on high-performance materials such as wear resistance, corrosion resistance, high strength, high toughness and the like. The ceramic reinforced phase particles with excellent strength, hardness and wear resistance are introduced into titanium and titanium alloy matrixes with good plastic toughness, so that the titanium-based composite material can meet the requirements, and the titanium-based composite material becomes one of the most potential structural materials in the fields of aerospace and the like. However, the conventional smelting atomization method is still relied on to prepare the titanium-based composite powder adapting to methods such as additive manufacturing and injection molding, so that the variety of the titanium-based composite is limited, and the development of the application of the titanium-based composite powder is further limited due to high cost.
Therefore, how to overcome the drawbacks of the prior art, and to provide a method for preparing titanium-based composite powder with a wide range of raw materials and low cost is a problem that needs to be solved by those skilled in the art.
Disclosure of Invention
The main purpose of the invention is to provide a titanium-based composite powder and a method for preparing the same by using a rotation height Wen Zhengxing method, wherein the preparation method takes titanium powder or titanium alloy powder and reinforcing phase particles as raw materials, the raw materials are mixed with grinding balls in a certain proportion, the titanium-based composite powder is prepared based on a rotary tube furnace, the powder has good fluidity and controllable gap elements, the requirements of various preparation processes such as additive manufacturing, injection molding, hot isostatic pressing and the like can be met, the raw material range is wide, and the cost is greatly reduced.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a method for preparing a titanium-based composite powder using a spin-height Wen Zhengxing method.
The method for preparing the titanium-based composite powder by using the spin height Wen Zhengxing method comprises the following steps of:
the matrix powder, the reinforcing phase particles and the grinding balls are put into a rotary tube furnace together, the temperature is raised to 200-1000 ℃ under the protection atmosphere, the heat is preserved for 1-36 h, the powder preparation is completed, and the powder is cooled along with the furnace; wherein, the tube furnace is kept to uniformly rotate in the heating and heat preservation process; the matrix powder is titanium or titanium alloy powder;
sieving to obtain the titanium-based composite powder with the required granularity.
Further, the temperature is raised to 400-700 ℃ under the protection atmosphere, and the temperature is kept for 1-5 h.
Further, the temperature rising rate is 1-10 ℃/min, and the rotating speed of the rotary tube furnace is 5-200 r/min; the shielding gas comprises but is not limited to argon, helium, nitrogen, argon-oxygen mixed gas, argon-nitrogen mixed gas and nitrogen, and the gas flow rate is 10-5000 mL/min;
preferably, the rotating speed of the rotary tube furnace is 20-80 r/min.
Further, the mass of the reinforcing phase particles is within 20% of the total mass of the matrix powder and the reinforcing phase particles.
Further, according to the mass of the grinding ball: ball-to-material ratio of the matrix powder and the reinforcing phase particles with the total mass of x:y is used for weighing grinding balls, wherein: x and y are natural numbers;
preferably, the ball to material ratio is 1:1, 2:1 or 1:2.
Preferably, the grinding balls are zirconium oxide, stainless steel and aluminum oxide grinding balls.
Further, the diameter of the grinding ball is less than or equal to 30mm; preferably, grinding balls with different diameters are selected for mixing;
preferably, a grinding ball with the diameter of 5mm is selected to be mixed with a grinding ball with the diameter of 10mm in a ratio of 1:1;
preferably, the diameter of the grinding balls is 10mm.
Further, the matrix powder is spherical powder or irregular powder;
preferably, the titanium powder includes, but is not limited to, hydrogenated dehydrogenated titanium powder, pure titanium powder; the titanium alloy powder includes, but is not limited to, ti-6Al-4V titanium alloy powder.
Further, the granularity of the matrix powder is less than or equal to 200 mu m;
preferably, the particle size of the matrix powder is 15 to 60 μm, 0 to 40 μm or 50 to 150 μm.
Further, the reinforcing phase particles include, but are not limited to, tiB 2 、TiB、TiC、CaC、CaB 6 SiC particles;
preferably, the particle size of the reinforcing phase particles is 0.2 to 50 μm;
preferably, the reinforcing phase particles have a particle size of 0.2 to 20. Mu.m.
In order to achieve the above object, according to a second aspect of the present invention, there is provided a titanium-based composite powder.
The titanium-based composite material powder prepared by the preparation method comprises matrix powder and reinforcing phase particles coated on the surface of the matrix powder; the matrix powder is titanium or titanium alloy powder; the reinforcing phase particles include, but are not limited to, tiB 2 、TiB、TiC、CaC、CaB 6 SiC particles;
preferably, the titanium-based composite powder includes, but is not limited to, ti/TiB 2 Ti/TiC, ti/CaC and Ti/SiC composite powder.
The invention has the beneficial effects that:
1. the titanium-based composite material powder provided by the invention can prevent the phenomena of agglomeration, adhesion and the like of mixed powder, has good powder fluidity, controllable gap elements, firm combination of titanium or titanium alloy powder and reinforcing phase particles, and is beneficial to the subsequent injection molding, additive manufacturing and other processes. According to different application ranges, 15-53 mu m composite material powder manufactured by laser additive is adapted, the fluidity is less than 55s/50g, the oxygen content is less than 2200ppm, and the nitrogen content is less than 500ppm on the premise of not adding additional gap elements; the powder of the composite material with the particle size of 0-40 mu m is formed by injection, the fluidity is less than 70s/50g, the oxygen content is less than 2400ppm and the nitrogen content is less than 600ppm on the premise of not adding additional gap elements; the fluidity of the 53-150 mu m composite material powder which is suitable for the hot isostatic pressing technology is less than 40s/50g, the oxygen content is less than 1800ppm, and the nitrogen content is less than 400ppm on the premise of not adding additional gap elements.
2. The raw material powder can adopt hydrogenated and dehydrogenated titanium powder and reinforced phase particles, so that the cost can be greatly reduced, and compared with the traditional smelting atomization method for preparing the powder, the cost can be reduced by more than 60%. The raw material range is wide, the particle size distribution before and after shaping is not greatly changed, the yield can reach more than 90%, and the titanium-based composite material powder with more diversity and different reinforcing phase contents can be prepared.
3. The invention has the advantages that the raw material range is wide, the component regulation and control are convenient, compared with the traditional smelting-atomizing method for preparing the composite material powder, the more wide type of reinforced phase particles and the addition amount can be selected, meanwhile, the gap elements such as the argon-oxygen mixed gas and the argon-nitrogen mixed gas can be added to promote the O content and the N content by changing the atmosphere in the rotary shaping process, and the physical performance index of the powder can be customized by regulating and controlling the gap elements, thereby being beneficial to the implementation of the performance regulation and control scheme.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to designate like parts throughout the figures. In the drawings:
FIG. 1 shows the Ti/TiB composition of example 1 according to the present invention 2 Comparing the morphology of the powder before and after the high-temperature shaping of the composite powder; wherein (a) and (c) represent the morphology of the hydrogenated and dehydrogenated titanium powder before shaping, and (b) and (d) represent the Ti/TiB after shaping 2 A topography of the composite powder, with (a) and (b) being an enlarged view of (c) and (d), respectively;
fig. 2 and 3 are graphs showing comparison of powder particle size distribution of hydrogenated dehydrogenated titanium powder and Ti/TiC composite powder before and after rotational high temperature shaping in example 2 provided by the present invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
According to the specific embodiment of the invention, the method for preparing the titanium-based composite material powder by using the rotation height Wen Zhengxing method is provided, and the prepared titanium-based composite material powder has good fluidity and can meet the requirements of various preparation processes such as additive manufacturing, hot isostatic pressing and the like.
The method for preparing the titanium-based composite material powder by using the rotation height Wen Zhengxing method specifically comprises the following steps:
s1, weighing matrix powder and reinforcing phase particles according to mass ratio; wherein the matrix powder is titanium powder or titanium alloy powder, and the mass of the reinforcing phase particles is within 20% of the total mass of the matrix powder and the reinforcing phase particles.
In embodiments of the present invention, titanium powders include, but are not limited to, hydrogenated dehydrogenated titanium powders, pure titanium powders; titanium alloy powders include, but are not limited to, ti-6Al-4V titanium alloy powders; the titanium powder or the titanium alloy powder may be spherical powder or irregular powder.
In the embodiment of the invention, the granularity of the matrix powder is less than or equal to 200 mu m, and the powder with the corresponding granularity range can be selected according to practical application, for example, the granularity of the titanium powder or the titanium alloy powder which is suitable for laser additive manufacturing is 15-60 mu m, the granularity of the titanium powder or the titanium alloy powder which is suitable for injection molding technology is 0-40 mu m, the granularity of the titanium powder or the titanium alloy powder which is suitable for hot isostatic pressing technology is 50-150 mu m, and the granularity of the titanium powder or the titanium alloy powder which is suitable for cold spraying technology is 0-40 mu m. Of course, other application ranges may be selected based on the desired particle size of the target powder.
In embodiments of the invention, the reinforcing phase particles include, but are not limited to, tiB 2 、TiB、TiC、CaC、CaB 6 SiC particles; the particle size of the reinforcing phase particles is 0.2-50 mu m.
As a specific embodiment of the present invention, the particle size of the reinforcing phase particles may be 0.2 to 20. Mu.m, and a more excellent effect may be achieved.
S2, according to the mass of the grinding ball: ball-to-material ratio of matrix powder and reinforcing phase particles with total mass of x:y is used for weighing grinding balls, wherein: x and y are natural numbers, i.e. the matrix powder can be mixed with reinforcing phase particles in any mass ratio; wherein, the grinding ball can be zirconia, stainless steel or alumina grinding ball.
As a specific embodiment of the invention, the ball-to-material ratio can be 1:1, 2:1 or 1:2 to obtain better effect.
In the embodiment of the invention, the diameter of the grinding balls is less than or equal to 30mm, and the grinding balls with different diameters can be selected for mixing according to the needs in actual work so as to obtain better effect.
As a specific embodiment of the invention, a grinding ball with a diameter of 5mm is selected for 1:1 mixing with a grinding ball with a diameter of 10mm.
As a specific embodiment of the invention, the diameter of the grinding balls is 10mm.
S3, loading titanium powder or titanium alloy powder, reinforcing phase particles and grinding balls into a rotary tube furnace, heating to 200-1000 ℃ under a protective atmosphere, preserving heat for 1-36 h, and completing powder preparation and cooling along with the furnace; wherein, the tube furnace is kept to uniformly rotate in the heating and heat preservation processes, and the rotating speed is 5-200 r/min; the temperature rising rate is 1-10 ℃/min, and the protective gas comprises but is not limited to argon, helium, nitrogen, argon-oxygen mixed gas, argon-nitrogen mixed gas and nitrogen, and the gas flow rate is 10-5000 mL/min.
As a specific embodiment of the invention, the temperature is raised to 400-700 ℃ under the protection atmosphere, and the temperature is kept for 1-5 h.
As a specific embodiment of the invention, the rotating speed of the rotary tube furnace can be 20-80 r/min.
S4, screening out grinding balls through a coarse screen, and screening to obtain titanium-based composite powder with the required granularity.
The invention further provides titanium-based composite material powder, which is prepared by the preparation method.
The titanium-based composite material powder of the invention is prepared from a matrix powderAnd reinforcing phase particles coated on the surface of the powder, wherein the matrix powder and the reinforcing phase particles are firmly combined, which is beneficial to the subsequent injection molding, additive manufacturing and other processes. Wherein the matrix powder may be titanium or titanium alloy powder, and the reinforcing phase particles include but are not limited to TiB 2 、TiB、TiC、CaC、CaB 6 SiC particles.
In an embodiment of the invention, the titanium-based composite powder includes, but is not limited to, ti/TiB 2 Ti/TiC, ti/CaC and Ti/SiC composite powder.
The titanium-based composite powder of the present invention and the method for producing the same will be further described below with reference to specific examples.
Example 1
Step 1: according to hydrogenation dehydrogenation titanium powder and TiB 2 Particle powder mass ratio 95:5 hydrogenated dehydrogenated powder 475g is weighed, tiB is weighed 2 25g of granular powder, the particle size distribution of the selected hydrogenated dehydrogenated titanium powder is d10=16.3 μm, d50=32.4 μm, d90=54.8 μm, and the selected TiB 2 The particle size distribution of the particulate powder was d10=3.1 μm, d50=10.4 μm, d90=15.2 μm;
step 2: weighing 500g of zirconia grinding balls according to the ball material mass ratio of 1:1, wherein the grinding balls with the diameter of 5mm are 250g, and the grinding balls with the diameter of 10mm are 250g;
step 3: all the powder and grinding balls are put into a rotary tube furnace, the temperature is raised to 450 ℃ at 5 ℃/min, the heat is preserved for 1h, the whole process is carried out in an argon protection atmosphere, the argon flow rate is 60mL/min, the furnace is cooled, the argon protection is kept in the whole process, and the rotating speed of the rotary furnace is 60r/min;
step 4: cooling, sieving with 60 mesh sieve to remove grinding balls, placing the powder in an atmosphere vibrating sieve, sieving with 270 mesh sieve under the protection of argon atmosphere to obtain undersize powder, sieving with 800 mesh sieve to obtain upper powder to obtain TiB with required particle diameter 2 Ti/TiB with mass fraction of 5% 2 Composite powder.
Hydrogenation dehydrogenation titanium powder and TiB 2 Under the combined action of mechanical force and high temperature, the powder is spheroidized in irregular shape, uniform in particle size and TiB 2 The particles are fully and evenly coated on the surface of the hydrogenated and dehydrogenated titanium powder, and the Ti/TiB is obtained after cooling 2 The morphology of the composite material powder is shown in figure 1, the powder is nearly spherical, and the irregular acute angles disappear.
Through testing, the fluidity of the composite material powder reaches 48.4s/50g;
the test shows that the bulk density of the composite material powder is 2.13g/cm 3 ；
Through testing, the oxygen content of the composite material powder is 0.213wt%, the nitrogen content is 0.028wt% and the carbon content is 0.013wt%;
the above performance can well meet the requirements of additive manufacturing.
Example 2
Step 1: weighing 490g of hydrogenated and dehydrogenated titanium powder and 10g of TiC particle powder according to the mass ratio of the hydrogenated and dehydrogenated titanium powder to the TiC particle powder of 98:2, wherein the particle size distribution of the hydrogenated and dehydrogenated titanium powder is d10=13.5 μm, d50=30.1 μm, d90=62.2 μm, and the particle size distribution of the TiC powder is d10=5.4 μm, d50=13.1 μm and d90=20.7 μm;
step 2: weighing 250g of zirconia grinding balls with the diameter of 5mm according to the mass ratio of the balls to 2;
step 3: all the powder and grinding balls are put into a rotary tube furnace, the temperature is raised to 160 ℃ at a speed of 5 ℃/min, the heat preservation is carried out for 0.5h, the whole process is carried out in an argon protection atmosphere, the temperature is raised to 550 ℃ at a speed of 5 ℃/min after the heat preservation is finished, the heat preservation is carried out for 2h, the argon flow rate is 60mL/min, the furnace is cooled, the argon protection is kept in the whole process, and the rotating speed of the rotary furnace is 20 r/min;
step 4: and (3) cooling, sieving with a 60-mesh screen to remove grinding balls, placing the powder into an atmosphere vibrating screen, sieving with a 270-mesh screen to obtain undersize powder under the protection of argon atmosphere, sieving with a 800-mesh screen to obtain the screened upper powder, and obtaining the Ti/TiC composite material powder with the required particle size TiC mass fraction of 2%.
Under the combined action of mechanical force and high temperature, tiC particles are fully and uniformly wrapped on the surface of the hydrogenated and dehydrogenated titanium powder, and the Ti/TiC composite material powder is obtained by cooling, so that the powder is spheroidized in irregular shape, and compared with the hydrogenated and dehydrogenated titanium powder, the average particle size D50 of the powder is slightly increased, and the particle size of the powder is more concentrated. In addition, the particle size distribution is not greatly changed before and after shaping, as shown in fig. 2, the shaping process has higher yield, and the yield can reach more than 90%.
Through testing, the flowability of the composite material powder reaches 46.0s/50g;
the test shows that the bulk density of the composite material powder is 2.25g/cm 3 ；
The test shows that the oxygen content of the composite material powder is 0.189wt% and the nitrogen content is 0.030wt%;
the composite powder particle size distribution was tested as d10=17.7 μm, d50=33.1 μm, d90=59.3 μm;
the above performance can well meet the requirements of additive manufacturing.
Example 3
Step 1: according to hydrogenation of Ti-6Al-4V powder and CaB 6 Particle powder mass ratio 95:5 hydrogenated dehydrogenated Ti-6Al-4V powder 475g is weighed and CaB is weighed 6 25g of a particulate powder having a particle size distribution d10=16.1 μm, d50=31.9 μm, d90=52.8 μm, selected CaB 6 The particle size distribution of the particulate powder was d10=1.5 μm, d50=5.1 μm, d90=9.3 μm;
step 2: weighing 1000g of zirconia grinding balls with the diameter of 5mm according to the mass ratio of the balls to the materials of 2:1;
step 3: all the powder and grinding balls are put into a rotary tube furnace, the temperature is raised to 550 ℃ at 5 ℃/min, the heat is preserved for 2 hours, the rotating speed is 30r/min, the powder and the grinding balls are cooled along with the furnace, the protection of argon atmosphere is maintained in the whole process, and the flow rate of the argon is 60mL/min;
step 4: cooling, sieving with 60 mesh sieve to remove grinding balls, placing the powder in an atmosphere vibrating sieve, sieving with 270 mesh sieve under the protection of argon atmosphere to obtain undersize powder, sieving with 800 mesh sieve to obtain upper powder to obtain CaB with required particle size 6 5% by mass of Ti-6Al-4V/CaB 6 Composite powder.
Hydrogenation dehydrogenation Ti-6Al-4V powder and CaB 6 Under the combined action of mechanical force and high temperature, the particles are spheroidized and CaB is obtained by irregular shape of powder 6 The particles are fully and uniformly coated on the surface of the hydrogenated and dehydrogenated Ti-6Al-4V powder, and the Ti-6Al-4V/CaB is obtained by cooling 6 Composite powder.
Through testing, the fluidity of the composite material powder reaches 51.8s/50g;
the test shows that the bulk density of the composite material powder is 2.18g/cm 3 ；
The test shows that the oxygen content of the composite material powder is 0.210wt%, the nitrogen content is 0.029wt% and the carbon content is 0.013wt%;
the above performance can well meet the requirements of additive manufacturing.
The invention also carries out comparative analysis on the titanium-based composite powder prepared in the example and the titanium-based composite powder obtained in the prior art so as to further describe the titanium-based composite powder and the preparation method thereof.
The traditional titanium-based composite material powder needs to be prepared in a smelting-atomizing powder making mode, the whole process procedure is long, and the reinforced phase particles are easy to react with titanium in the smelting process due to the fact that titanium belongs to high-activity metal in the smelting process, and component segregation is easy to be caused when the adding amount is large, so that the uniformity of the final powder is affected.
In the preparation method provided by the invention, matrix powder (titanium or titanium alloy powder) and reinforcing phase particles are uniformly mixed, and after the matrix powder is softened at high temperature, the reinforcing phase particles are inlaid on the matrix powder under the combined action of mechanical force and heat to form metallurgical bonding, so that the preparation of various titanium alloys and reinforcing phase titanium-based alloy powder is realized. In contrast, the invention has low energy consumption, short working procedure, wide raw material range and low cost.
Moreover, compared with the ball milling method which is prepared by a simple mechanical mixing method, the preparation method provided by the invention realizes the tight combination of the titanium alloy matrix powder and the reinforcing phase particles, and better meets the requirements of preparation processes such as additive manufacturing, injection molding and the like.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for preparing titanium-based composite powder by using a spin height Wen Zhengxing method, the method comprising the steps of:
the matrix powder, the reinforcing phase particles and the grinding balls are put into a rotary tube furnace together, the temperature is raised to 200-1000 ℃ under the protection atmosphere, the heat is preserved for 1-36 h, the powder preparation is completed, and the powder is cooled along with the furnace; wherein, the tube furnace is kept to uniformly rotate in the heating and heat preservation process; the matrix powder is titanium or titanium alloy powder;
sieving to obtain the titanium-based composite powder with the required granularity.
2. The preparation method according to claim 1, wherein the temperature is raised to 400-700 ℃ under a protective atmosphere, and the temperature is kept for 1-5 h.
3. The preparation method according to claim 1, wherein the heating rate is 1-10 ℃/min and the rotating speed of the rotary tube furnace is 5-200 r/min; the shielding gas comprises but is not limited to argon, helium, nitrogen, argon-oxygen mixed gas, argon-nitrogen mixed gas and nitrogen, and the gas flow rate is 10-5000 mL/min;
preferably, the rotating speed of the rotary tube furnace is 20-80 r/min.
4. The method of claim 1, wherein the reinforcing phase particles have a mass that is within 20% of the total mass of the matrix powder and the reinforcing phase particles.
5. The method of manufacturing according to claim 1, wherein the grinding balls are of the following mass: ball-to-material ratio of the matrix powder and the reinforcing phase particles with the total mass of x:y is used for weighing grinding balls, wherein: x and y are natural numbers;
preferably, the ball to material ratio is 1:1, 2:1 or 1:2.
Preferably, the grinding balls are zirconium oxide, stainless steel and aluminum oxide grinding balls.
6. The method of claim 1 or 5, wherein the grinding balls have a diameter of 30mm or less; preferably, grinding balls with different diameters are selected for mixing;
preferably, a grinding ball with the diameter of 5mm is selected to be mixed with a grinding ball with the diameter of 10mm in a ratio of 1:1;
preferably, the diameter of the grinding balls is 10mm.
7. The method of manufacturing according to claim 1, wherein the base powder is a spherical powder or an irregular powder;
preferably, the titanium powder includes, but is not limited to, hydrogenated dehydrogenated titanium powder, pure titanium powder; the titanium alloy powder includes, but is not limited to, ti-6Al-4V titanium alloy powder.
8. The method of claim 1, wherein the matrix powder has a particle size of 200 μm or less;
preferably, the particle size of the matrix powder is 15 to 60 μm, 0 to 40 μm or 50 to 150 μm.
9. The method of manufacture of claim 1, wherein the reinforcing phase particles include, but are not limited to TiB 2 、TiB、TiC、CaC、CaB 6 SiC particles;
preferably, the particle size of the reinforcing phase particles is 0.2 to 50 μm;
preferably, the reinforcing phase particles have a particle size of 0.2 to 20. Mu.m.
10. The titanium-based composite powder produced by the production method according to any one of claims 1 to 9, wherein the titanium-based composite powder is composed of a matrix powder and reinforcing phase particles coated on the surface thereof; the matrix powder is titanium or titanium alloy powder; the reinforcing phase particles include, but are not limited to, tiB 2 、TiB、TiC、CaC、CaB 6 SiC particles;
preferably, the titanium-based composite powder includes, but is not limited to, ti/TiB 2 Ti/TiC, ti/CaC and Ti/SiC composite powder.
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