CN114406275A - Nano TiB reinforced titanium-based composite powder and preparation method thereof - Google Patents
Nano TiB reinforced titanium-based composite powder and preparation method thereof Download PDFInfo
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- CN114406275A CN114406275A CN202210078260.5A CN202210078260A CN114406275A CN 114406275 A CN114406275 A CN 114406275A CN 202210078260 A CN202210078260 A CN 202210078260A CN 114406275 A CN114406275 A CN 114406275A
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- 239000000843 powder Substances 0.000 title claims abstract description 171
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 239000010936 titanium Substances 0.000 title claims abstract description 58
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 50
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 239000002245 particle Substances 0.000 claims abstract description 33
- 230000002787 reinforcement Effects 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000007731 hot pressing Methods 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 31
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 238000000498 ball milling Methods 0.000 claims description 22
- 238000000889 atomisation Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 15
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 229910033181 TiB2 Inorganic materials 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 2
- 230000003014 reinforcing effect Effects 0.000 abstract description 18
- 239000002905 metal composite material Substances 0.000 abstract 1
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 6
- 239000000320 mechanical mixture Substances 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000009987 spinning Methods 0.000 description 5
- 239000007770 graphite material Substances 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009689 gas atomisation Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification 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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- 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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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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
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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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Abstract
The invention relates to the technical field of metal composite materials, in particular to nano TiB reinforced titanium-based composite powder and a preparation method thereof. The preparation method of the nano TiB reinforced titanium-based composite powder comprises the following steps: step one, uniformly mixing titanium alloy powder and reinforcement powder to obtain a mixture; step two, carrying out vacuum reaction hot-pressing sintering treatment on the mixture to obtain a sintered body; and step three, performing heating rotation treatment on the sintered body to enable the heated and melted sintered body to be screwed out to obtain molten liquid drops, and cooling the molten liquid drops to obtain the nano TiB reinforced titanium-based composite powder. The preparation method of the nano TiB reinforced titanium-based composite powder provided by the invention can ensure that the prepared nano TiB reinforced titanium-based composite powder has high sphericity, narrow particle size range and uniform distribution of internal reinforcing phases.
Description
Technical Field
The invention relates to the technical field of metal-based composite materials, in particular to nano TiB reinforced titanium-based composite powder and a preparation method thereof.
Background
The titanium-based composite material has excellent performances such as high specific strength, high temperature resistance and the like, and is an important material applied to the technical field of aerospace in the future. The titanium-based composite material mainly takes a mechanical mixture of titanium alloy powder and ceramic reinforcement powder as a raw material, but the powder of the mechanical mixture does not contain a ceramic phase inside, and ceramic particles are only attached to the surface of the titanium alloy powder, so that the tissue regulation range of the titanium-based composite material and the reinforcement effect of a ceramic reinforcement are limited, and the plasticity of the material is greatly reduced. In the prior art, if a ceramic reinforcement is introduced into mechanically mixed powder, the ceramic reinforcement is realized by using ultrafine titanium alloy powder as a raw material and adding high ball milling energy, but the material cost is increased, the risk of powder oxidation is increased, finally prepared powder is also deformed due to high energy, and the sphericity is reduced.
Chinese patent publication No. CN110340371A discloses a method for preparing powder for additive manufacturing of particle-reinforced titanium-based composite material, which comprises preparing a titanium-based composite material block material by a smelting method, and preparing titanium-based composite powder by a gas atomization powder preparation method. However, this method has three disadvantages: firstly, the titanium-based composite material has poor uniformity in the smelting process, and a macroscopically uneven tissue is easily formed, so that the uniformity of subsequently prepared titanium-based composite powder is poor; if the uniformity is improved, multiple times of smelting are needed, so that the preparation period is prolonged, the preparation difficulty is improved, and the risk of oxidation of the titanium-based composite material is increased; secondly, the block of the smelted titanium-based composite material needs to be forged and formed and machined into a bar, so that the step of powder preparation is added, and the waste of materials is also caused; thirdly, the cooling rate of the gas atomization powder preparation is low, the prepared powder is easy to form sphere adhesion, the powder quality is low, holes are easy to appear in the powder, and the obtained powder is wide and nonuniform in particle size range.
Disclosure of Invention
The embodiment of the invention provides nano TiB reinforced titanium-based composite powder and a preparation method thereof, and the provided nano TiB reinforced titanium-based composite powder has high sphericity, narrow particle size range and uniform internal reinforced phase distribution.
In a first aspect, the invention provides a preparation method of nano TiB reinforced titanium-based composite powder, which comprises the following steps:
the method comprises the following steps: uniformly mixing titanium alloy powder and reinforcement powder to obtain a mixture;
step two: carrying out vacuum reaction hot-pressing sintering treatment on the mixture to obtain a sintered body;
step three: and heating and rotating the sintered body to ensure that the heated and melted sintered body is screwed out to obtain molten liquid drops, and cooling the molten liquid drops to obtain the nano TiB reinforced titanium-based composite powder.
Preferably, in the step one, the titanium alloy powder is TC4 titanium alloy powder or TA15 titanium alloy powder, and the reinforcement powder is TiB2Powder or boron powder.
Preferably, the particle size of the titanium alloy powder is 100-200 μm, and the TiB2The particle size of the powder is 3-5 μm, and the particle size of the boron powder is 0.5-1 μm.
Preferably, in step one, the method comprises the following steps:
and performing ball milling treatment on the titanium alloy powder and the reinforcement powder in an argon environment for 4-8h, wherein the rotating speed of the ball milling treatment is 200-250r/min, and the ball-to-material ratio is (3-5): 1.
Preferably, in the second step, the temperature of the vacuum reaction hot-pressing sintering treatment is 1150--2Pa, time is 0.5-2 h.
Preferably, in the third step, the heating temperature of the heating and rotating treatment is 2800-.
Preferably, in step two, the method comprises the following steps: putting the mixture into a matched mould to perform the vacuum reaction hot-pressing sintering;
in step three, the method comprises the following steps: fixing the sintered body on a rotating clamp of plasma rotating electrode atomization powder making equipment, wherein the rotating clamp is used for rotating the sintered body;
the size of the matching die is matched with that of the rotary clamp, so that the sintered body is fixed on the rotary clamp.
Preferably, the matching mold is prepared from graphite.
Preferably, in step three, the method comprises the following steps:
fixing the sintered body on the rotary clamp, and under the argon environment, adjusting the current of the plasma rotary electrode atomization powder making equipment to 600-;
and cooling the molten liquid drop to obtain the nano TiB reinforced titanium-based composite powder.
In a second aspect, the invention provides a nano TiB reinforced titanium-based composite powder prepared according to the preparation method of any one of the first aspect.
Compared with the prior art, the invention at least has the following beneficial effects:
in the invention, titanium alloy powder and reinforcement powder are uniformly mixed, so that the titanium alloy powder and the reinforcement powder are macroscopically and uniformly mixed to obtain a mechanical mixture, and then the mechanical mixture is subjected to vacuum reaction hot-pressing sintering treatment, so that boron in the reinforcement powder and titanium are subjected to in-situ self-generated reaction, and a sintered body containing a micron-sized reinforcement phase is obtained.
In the invention, the sintered body is heated to melt the surface of the sintered body, then the sintered body is rotated to enable the melted sintered body to be thrown out under the action of centrifugal force to form a plurality of molten liquid drops, the molten liquid drops are condensed to obtain the nano TiB enhanced titanium-based composite powder, and the nano TiB enhanced titanium-based composite powder is formed by condensing the molten liquid drops, and the liquid drops are agglomerated into a sphere by surface tension, so that the generated powder is spherical, and the condition of adhesion of a plurality of spheres is avoided; because the particles of the powder are formed by the condensation of the molten liquid drops, the particle size interval of the formed powder is narrow; the molten liquid drops are rapidly cooled at a cooling speed of 103-104When the liquid drops are rapidly condensed, the nucleation rate of the titanium element is high, the titanium element preferentially nucleates and crystallizes, and the B element is pushed to a crystal boundary and reacts to form TiB. Because the cooling speed is high, the size of the enhanced phase is small, and therefore, particles with the nanoscale enhanced phase inside are obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a surface microscopic image of a nano TiB reinforced titanium-based composite powder with a reinforcing phase content of 1 vol% according to an embodiment of the present invention;
FIG. 2 is a surface microscopic image of another nano TiB reinforced titanium-based composite powder with a reinforcing phase content of 1 vol% provided by the embodiment of the present invention;
FIG. 3 is a surface microscopic image of a further nano TiB reinforced titanium-based composite powder with a reinforcing phase content of 1 vol% provided by an embodiment of the present invention;
FIG. 4 is a cross-sectional microscopic image of a nano TiB-reinforced titanium-based composite powder with a reinforcing phase content of 1 vol% according to an embodiment of the present invention;
FIG. 5 is a cross-sectional microscopic image of another nano TiB-reinforced titanium-based composite powder with a reinforcing phase content of 1 vol% provided by the embodiment of the present invention;
FIG. 6 is a cross-sectional microscopic image of a further nano TiB reinforced titanium-based composite powder with a reinforcing phase content of 1 vol% provided by an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer and more complete, the technical solutions in the embodiments of the present invention will be described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention, and based on the embodiments of the present invention, all other embodiments obtained by a person of ordinary skill in the art without creative efforts belong to the scope of the present invention.
The embodiment of the invention provides a preparation method of nano TiB reinforced titanium-based composite powder, which comprises the following steps:
the method comprises the following steps: uniformly mixing titanium alloy powder and reinforcement powder to obtain a mixture;
step two: carrying out vacuum reaction hot-pressing sintering treatment on the mixture to obtain a sintered body;
step three: and heating and rotating the sintered body to ensure that the heated and melted sintered body is screwed out to obtain molten liquid drops, and cooling the molten liquid drops to obtain the nano TiB reinforced titanium-based composite powder.
In the invention, titanium alloy powder and reinforcement powder are uniformly mixed firstly, so that the titanium alloy powder and the reinforcement powder are uniformly mixed macroscopically to obtain a mechanical mixture, and then the mechanical mixture is subjected to vacuum reaction hot-pressing sintering treatment, so that in-situ self-generation reaction is carried out on non-metal elements in the reinforcement powder and titanium elements, and a sintered body containing a micron-sized reinforcement phase is obtained.
In the invention, the sintered body is heated to melt the surface of the sintered body, then the sintered body is rotated to enable the melted sintered body to be thrown out under the action of centrifugal force to form a plurality of molten liquid drops, the molten liquid drops are condensed to obtain the nano TiB enhanced titanium-based composite powder, and the nano TiB enhanced titanium-based composite powder is formed by condensing the molten liquid drops, and the liquid drops are agglomerated into a sphere by surface tension, so that the generated powder is spherical, and the condition of adhesion of a plurality of spheres is avoided; because the particles of the powder are formed by the condensation of the molten liquid drops, the particle size interval of the formed powder is narrow; the molten liquid drops are rapidly cooled at a cooling speed of 103-104When the liquid drops are rapidly condensed, the nucleation rate of the titanium element is high, the titanium element preferentially nucleates and crystallizes, and the B element is pushed to a crystal boundary and reacts to form TiB. Because the cooling speed is high, the size of the enhanced phase is small, and therefore, particles with the nanoscale enhanced phase inside are obtained.
It is noted that the method provided by the application can be used for preparing the nano TiB reinforced titanium-based composite powder with the content of the reinforcing phase of 0.001-10 vol%. The mass ratio of the titanium alloy powder to the reinforcement powder in the mixture is adjusted according to the content of the prepared reinforcement phase.
According to some preferred embodiments, in the step one, the titanium alloy powder is TC4 titanium alloy powder or TA15 titanium alloy powder, and the reinforcement powder is TiB2Powder or boron powder.
In the invention, TC4 titanium alloy powder or TA15 titanium alloy powder is selected as a matrix of the composite material, wherein the TA15 titanium alloy has excellent high-temperature resistance, and the type of the titanium alloy powder can be selected according to the use requirement.
In the invention, the boron-containing reinforcement and the titanium alloy can undergo in-situ self-generation reaction to form a stable TiB reinforcing phase in the condensation process after being mixed and melted.
According to some preferred embodiments, the titanium alloy powder has a particle sizeIs 100-200 μm (e.g., may be 100 μm, 110 μm, 120 μm, 130 μm, 140 μm, 150 μm, 160 μm, 170 μm, 180 μm, 190 μm or 200 μm), and the TiB2The particle size of the powder is 3 to 5 μm (for example, may be 3 μm, 4 μm or 5 μm), and the particle size of the boron powder is 0.5 to 1 μm (for example, may be 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm or 1 μm).
In the invention, the particle sizes of the titanium alloy powder and the reinforcement powder are selected from the range, so that the titanium alloy powder and the reinforcement powder can be uniformly mixed after low-energy ball milling treatment.
According to some preferred embodiments, in the step one, the method comprises the following steps:
and performing ball milling treatment on the titanium alloy powder and the reinforcement powder in an argon atmosphere for 4-8h (for example, 4h, 5h, 6h, 7h or 8h), wherein the rotation speed of the ball milling treatment is 200-250r/min (for example, 200r/min, 210r/min, 220r/min, 230r/min, 240r/min or 250r/min), and the ball-to-material ratio is (3-5):1 (for example, 3:1, 4:1 or 5: 1).
In the invention, the titanium alloy powder and the reinforcement powder can be fully and uniformly mixed by utilizing ball milling treatment, and the titanium alloy powder and the reinforcement powder can be protected from being oxidized in an argon environment.
It should be noted that, in the solution of the present invention, the low-energy ball milling process at the rotation speed of 200-. Of course, the invention can also select high-energy ball milling treatment, but on the premise that the low-energy ball milling treatment can meet the use requirement, the low-energy ball milling treatment is selected in the step according to the principle of saving cost.
According to some preferred embodiments, in the second step, the temperature of the vacuum reaction hot pressing sintering process is 1150-1300 ℃ (for example, 1150 ℃, 1200 ℃, 1250 ℃ or 1300 ℃), the pressure is 20-30Mpa (20Mpa, 21Mpa, 22Mpa, 23Mpa, 24Mpa, 25Mpa, 26Mpa, 27Mpa, 28Mpa, 29Mpa or 30Mpa), and the vacuum degree is less than 5 × 10 Mpa- 2Pa for a period of 0.5 to 2h (e.g., 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h, or 2 h).
In the present invention, the mixture is subjected to 1150-1300 deg.C, 20-30MPa and vacuum degree of less than 5X 10-2In the Pa environment, vacuum reaction hot-pressing sintering treatment is carried out for 0.5-2h, so that the prepared sintered body has excellent density, the risk of oxidation is reduced, and the uniformity is improved; meanwhile, in the process of vacuum reaction hot-pressing sintering, the non-metal elements in the reinforcing phase powder and the titanium elements in the titanium alloy undergo in-situ self-generation reaction to obtain the micron-sized reinforcing phase.
According to some preferred embodiments, in step three, the heating temperature of the heating rotation treatment is 2800-.
In the present invention, the surface of the sintered body can be melted by heating the sintered body to the above temperature, and the molten sintered body can be thrown out as droplets by the centrifugal force by rotating the sintered body at the above speed.
According to some preferred embodiments, in step two, the method comprises: putting the mixture into a matched mould to perform the vacuum reaction hot-pressing sintering;
in step three, the method comprises the following steps: fixing the sintered body on a rotating clamp of plasma rotating electrode atomization powder making equipment, wherein the rotating clamp is used for rotating the sintered body;
the size of the matching die is matched with that of the rotary clamp, so that the sintered body is fixed on the rotary clamp.
According to the invention, the size of the matching mold is matched with that of the rotary clamp, and the mixture is filled into the matching mold to be subjected to vacuum reaction hot-pressing sintering to obtain the sintered body, so that the prepared sintered body can be directly filled and fixed on the rotary clamp without processing, the step of secondary processing is omitted, the waste of raw materials is avoided, and the preparation process of the nano TiB reinforced titanium-based composite powder is further simplified.
In the present invention, before the third step, after the second step, the method further comprises: the surface of the sintered body is polished to remove contaminants from the surface and smooth the surface.
It should be noted that the sintered body obtained in the second step may not be immediately subjected to the treatment in the third step, so that contaminants may exist on the surface of the sintered body stored for a period of time, and in order to avoid contamination of the subsequently prepared nano-TiB reinforced titanium-based composite powder, the surface of the sintered body needs to be subjected to a polishing treatment before the third step is performed.
According to some preferred embodiments, the matching mold is made of graphite.
In the invention, graphite is selected as a manufacturing material of the matching die, the graphite has excellent heat-conducting property and thermal stability, and certainly, steel can be selected as a material for preparing the matching die, but the cost of the graphite is lower than that of the steel.
According to some preferred embodiments, in step three, the method comprises:
fixing the sintered body on the rotary clamp, adjusting the current of the plasma rotary electrode atomization powder preparation device to 600-800A (for example, 600A, 650A, 700A, 750A or 800A) under the argon atmosphere, setting the rotating speed of the rotary clamp to 20000-30000r/min (for example, 20000r/min, 21000r/min, 22000r/min, 23000r/min, 24000r/min, 25000r/min, 26000r/min, 27000r/min, 28000r/min, 29000r/min or 30000r/min), setting the feeding speed of the sintered body to 1.5-3mm/s (for example, 1.5mm/s, 1.6mm/s, 1.7mm/s, 1.8mm/s, 1.9mm/s, 2 mm/s), 2.1mm/s, 2.2mm/s, 2.3mm/s, 2.4mm/s, 2.5mm/s, 2.6mm/s, 2.7mm/s, 2.8mm/s, 2.9mm/s, or 3mm/s) to cause the sintered body melted by heat to spin out to obtain a molten droplet;
and cooling the molten liquid drop to obtain the nano TiB reinforced titanium-based composite powder.
The molten droplets at high temperature can be naturally and rapidly cooled after being spun out, and the cooling speed is highCan reach 103-104℃/s。
In the invention, a plasma rotating electrode atomization powder making device is selected to heat and rotate the sintered body, the current of the plasma rotating electrode atomization powder making device is adjusted to release high-temperature plasma, the surface of the sintered body is melted by the high-temperature plasma, and the sintered body is rotated by a rotating clamp. Meanwhile, the particle size of the molten droplets can also be controlled by controlling the rotation speed and the feeding speed of the sintered body.
The embodiment of the invention also provides nano TiB reinforced titanium-based composite powder prepared by any one of the preparation methods.
The nano TiB reinforced titanium-based composite powder provided by the invention has high sphericity and narrow particle size range, and the reinforcing phase can be uniformly distributed in the powder.
In order to more clearly illustrate the technical scheme and advantages of the present invention, a nano-TiB reinforced titanium-based composite powder and a preparation method thereof are described in detail by several examples.
Example 1
Mixing 130 μm of TC4 titanium alloy powder and 4 μm of TiB2Performing ball milling treatment on the powder for 5 hours in an argon environment to obtain a mixture; wherein the mass fraction of TC4 titanium alloy powder is 99.4 wt%, and TiB2The mass portion of the raw materials is 0.6 wt%, the rotating speed of ball milling treatment is 220r/min, and the ball-to-material ratio is 5: 1;
placing the mixture in a matching mold made of graphite, and placing the matching mold containing the mixture at 1200 deg.C, 25MPa and vacuum degree of 4 × 10-2Carrying out vacuum reaction hot-pressing sintering treatment for 1.5h in a Pa environment to obtain a sintered body;
polishing the sintered body, fixing the sintered body on a rotary clamp in a plasma rotary electrode atomization powder making device under an argon environment, adjusting the current of the plasma rotary electrode atomization powder making device to 750A to melt the surface of the sintered body, setting the rotating speed of the rotary clamp to 28000r/min to rotate the sintered body, setting the feeding speed of the sintered body to 2.5mm/s, spinning out molten liquid drops from the surface of the molten sintered body under the action of centrifugal force, and obtaining the nano TiB reinforced titanium-based composite powder with the reinforcing phase TiB content of 1 vol% after the molten liquid drops are condensed.
Example 2
180 μm of TA15 titanium alloy powder and 3 μm of TiB2Performing ball milling treatment on the powder for 6 hours in an argon environment to obtain a mixture; wherein the TA15 titanium alloy powder comprises 97.1 wt% of TiB2The mass portion of the raw materials is 2.9 wt%, the rotating speed of ball milling treatment is 200r/min, and the ball-to-material ratio is 3: 1;
placing the mixture in a matched mold made of graphite material, and placing the matched mold containing the mixture at 1180 deg.C, 23MPa and vacuum degree of 4.6 × 10-2Carrying out vacuum reaction hot-pressing sintering treatment for 2h in a Pa environment to obtain a sintered body;
polishing the sintered body, fixing the sintered body on a rotary clamp in a plasma rotary electrode atomization powder making device under an argon environment, adjusting the current of the plasma rotary electrode atomization powder making device to 760A to melt the surface of the sintered body, setting the rotating speed of the rotary clamp to 29000r/min to rotate the sintered body, setting the feeding speed of the sintered body to 2.1mm/s, spinning out molten liquid drops on the surface of the molten sintered body under the action of centrifugal force, and obtaining the nano TiB reinforced titanium-based composite powder with the reinforcing phase content of 5 vol% after the molten liquid drops are condensed.
Example 3
Performing ball milling treatment on TC4 titanium alloy powder with the particle size of 160 mu m and boron powder with the particle size of 0.6 mu m for 5.5 hours in an argon environment to obtain a mixture; wherein the TA15 titanium alloy powder accounts for 99.8 wt%, the boron powder accounts for 0.2 wt%, the rotation speed of ball milling is 250r/min, and the ball-to-material ratio is 4: 1;
placing the mixture in a matching mold made of graphite material, and placing the matching mold containing the mixture at 1200 deg.C, 25MPa and vacuum degree of 4 × 10-2Carrying out vacuum reaction hot-pressing sintering treatment for 1.5h in a Pa environment to obtain a sintered body;
polishing the sintered body, fixing the sintered body on a rotary clamp in a plasma rotary electrode atomization powder manufacturing device under an argon environment, adjusting the current of the plasma rotary electrode atomization powder manufacturing device to 750A to melt the surface of the sintered body, setting the rotating speed of the rotary clamp to 28000r/min to rotate the sintered body, setting the feeding speed of the sintered body to 2mm/s, spinning out molten liquid drops on the surface of the molten sintered body under the action of centrifugal force, and obtaining the nano TiB reinforced titanium-based composite powder with the reinforcing phase content of 1 vol% after the molten liquid drops are condensed.
Example 4
Example 4 is essentially the same as example 3, except that: the titanium alloy powder is TA15 titanium alloy powder (the particle size is 200 mu m), the TA15 titanium alloy powder accounts for 99.8 wt%, and the boron powder accounts for 0.2 wt%; the particle size of the boron powder was 0.5 μm.
Example 5
Performing ball milling treatment on 100 mu m of TC4 titanium alloy powder and 1 mu m of boron powder for 4 hours in an argon environment to obtain a mixture; wherein the TA15 titanium alloy powder accounts for 99.8 wt%, the boron powder accounts for 0.2 wt%, the rotation speed of ball milling is 250r/min, and the ball-to-material ratio is 5: 1;
placing the mixture in a matched mold made of graphite material, and placing the matched mold containing the mixture at 1150 deg.C, 20MPa and vacuum degree of 4 × 10-2And carrying out vacuum reaction hot-pressing sintering treatment for 0.5h in a Pa environment to obtain a sintered body.
Polishing the sintered body, fixing the sintered body on a rotary clamp in a plasma rotary electrode atomization powder making device under an argon environment, adjusting the current of the plasma rotary electrode atomization powder making device to 600A to melt the surface of the sintered body, setting the rotating speed of the rotary clamp to 20000r/min to rotate the sintered body, setting the feeding speed of the sintered body to 1.5mm/s, spinning out molten liquid drops from the surface of the molten sintered body under the action of centrifugal force, and obtaining the nano TiB reinforced titanium-based composite powder with the reinforcing phase content of 1 vol% after the molten liquid drops are condensed.
Example 6
200 μm of TA15 titanium alloy powder and 5 μm of TiB2Ball milling the powder for 8h under argon atmosphere to obtain a mixtureAn agent; wherein the TA15 titanium alloy powder comprises 97.1 wt% of TiB2The mass portion of the raw materials is 2.9 wt%, the rotating speed of ball milling treatment is 200r/min, and the ball-to-material ratio is 5: 1;
placing the mixture in a matching mold made of graphite material, and placing the matching mold containing the mixture at 1300 deg.C, 30MPa and vacuum degree of 4.9 × 10-2Carrying out vacuum reaction hot-pressing sintering treatment for 2h in a Pa environment to obtain a sintered body;
polishing the sintered body, fixing the sintered body on a rotary clamp in a plasma rotary electrode atomization powder making device under an argon environment, melting the surface of the sintered body by adjusting the current of the plasma rotary electrode atomization powder making device to 800A, setting the rotating speed of the rotary clamp to 30000r/min to rotate the sintered body, setting the feeding speed of the sintered body to 3mm/s, spinning out molten liquid drops on the surface of the molten sintered body under the action of centrifugal force, and obtaining the nano TiB reinforced titanium-based composite powder with the reinforcing phase content of 5 vol% after the molten liquid drops are condensed.
The nano TiB reinforced titanium-based composite powder prepared in the examples 1 to 6 is sieved to obtain three powders with different particle sizes of less than 100 meshes, 100 meshes and 200 meshes and more than 200 meshes. Wherein the powder with the particle size less than 100 meshes only accounts for 9 percent of the prepared powder, the powder with the particle size of 100-200 meshes accounts for 56 percent, and the fine powder with the particle size greater than 200 meshes accounts for 35 percent, so that the nano TiB reinforced titanium-based composite powder provided by the application has a narrow particle size interval and high fine powder yield.
FIGS. 1 to 6 are micrographs of the TiB-based composite nanopowder prepared in example 1 having a reinforcing phase content of 1 vol%, and it can be seen from FIGS. 1 to 3 that the TiB-based composite nanopowder is spherical, free from the phenomenon of conglutination of spheres, free from flat particles, uniform in particle size and high in powder quality; meanwhile, as can be seen from fig. 4-6, the cross section of the nano-TiB reinforced titanium-based composite powder has no void defects, and it can be observed in fig. 6 that nano-TiB whiskers are precipitated at the grain boundary, and the length of the whiskers is less than 500nm and the diameter is less than 100 nm.
In order to facilitate observation of the subgrain boundary of the hypoeutectic structure under a mirror, the powder is subjected to corrosion treatment to corrode the subgrain boundary so as to facilitate observation, and the reticular dark cracks are corroded subgrain boundaries in the figure.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of nano TiB reinforced titanium-based composite powder is characterized by comprising the following steps:
the method comprises the following steps: uniformly mixing titanium alloy powder and reinforcement powder to obtain a mixture;
step two: carrying out vacuum reaction hot-pressing sintering treatment on the mixture to obtain a sintered body;
step three: and heating and rotating the sintered body to ensure that the heated and melted sintered body is screwed out to obtain molten liquid drops, and cooling the molten liquid drops to obtain the nano TiB reinforced titanium-based composite powder.
2. The method of claim 1, wherein in step one, the titanium alloy powder is TC4 titanium alloy powder or TA15 titanium alloy powder, and the reinforcement powder is TiB2Powder or boron powder.
3. The method as claimed in claim 2, wherein the titanium alloy powder has a particle size of 100-200 μm, and the TiB powder2The particle size of the powder is 3-5 μm, and the particle size of the boron powder is 0.5-1 μm.
4. The method according to claim 1, wherein the step one comprises:
performing ball milling treatment on the titanium alloy powder and the reinforcement powder in an argon environment for 4-8h, wherein the rotating speed of the ball milling treatment is 200-250r/min, and the ball-to-material ratio is 3-5): 1.
5. The method as claimed in claim 1, wherein in the second step, the temperature of the vacuum reaction hot pressing sintering treatment is 1150--2Pa, time is 0.5-2 h.
6. The method as claimed in claim 1, wherein in step three, the heating temperature of the heating and rotating treatment is 2800-.
7. The production method according to claim 1,
in the second step, the method comprises the following steps: putting the mixture into a matched mould to perform the vacuum reaction hot-pressing sintering;
in step three, the method comprises the following steps: fixing the sintered body on a rotating clamp of plasma rotating electrode atomization powder making equipment, wherein the rotating clamp is used for rotating the sintered body;
the size of the matching die is matched with that of the rotary clamp, so that the sintered body is fixed on the rotary clamp.
8. The method of claim 6, wherein the matching mold is made of graphite.
9. The method according to claim 7, comprising, in step three:
fixing the sintered body on the rotary clamp, and under the argon environment, adjusting the current of the plasma rotary electrode atomization powder making equipment to 600-;
and cooling the molten liquid drop to obtain the nano TiB reinforced titanium-based composite powder.
10. A nano TiB reinforced titanium matrix composite powder prepared according to the method of any one of claims 1 to 9.
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