CN111375758A - Sintering method of titanium or titanium alloy powder - Google Patents

Sintering method of titanium or titanium alloy powder Download PDF

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Publication number
CN111375758A
CN111375758A CN202010325032.4A CN202010325032A CN111375758A CN 111375758 A CN111375758 A CN 111375758A CN 202010325032 A CN202010325032 A CN 202010325032A CN 111375758 A CN111375758 A CN 111375758A
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titanium
titanium alloy
powder
alloy powder
heating
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王伟东
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/103Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/142Thermal or thermo-mechanical treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1017Multiple heating or additional steps
    • B22F3/1021Removal of binder or filler
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/11Making porous workpieces or articles
    • B22F3/1121Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/11Making porous workpieces or articles
    • B22F3/1121Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B22F3/1134Inorganic fillers
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/082Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
    • C23C24/085Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/082Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
    • C23C24/085Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • C23C24/087Coating with metal alloys or metal elements only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1051Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1053Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by induction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1054Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave

Abstract

The invention belongs to the field of materials, and particularly relates to a sintering method of titanium or titanium alloy powder. The technical scheme of the invention is as follows: a sintering method of titanium or titanium alloy powder comprises the following steps: 1) preparing powder; 2) the heating body heats the powder; 3) the electromagnetic field heats the powder. According to the sintering method of the titanium or titanium alloy powder, heat is transmitted to the titanium or titanium alloy powder in contact with the heating body through the heating body, the non-conductive titanium dioxide oxide layer on the surface of the titanium or titanium alloy powder in the contact layer is damaged and dissolved, the titanium or titanium alloy powder is mutually connected and conducts electricity, the powder is rapidly heated layer by layer under the action of an alternating electromagnetic field, and finally a complete sintered body is obtained. The method has the advantages of high heating speed, short sintering time, small size shrinkage of the sintered body and simple process, and can be used for preparing porous titanium or titanium alloy and fully-compact titanium or titanium alloy sintered bodies with different pore gas rates.

Description

Sintering method of titanium or titanium alloy powder
Technical Field
The invention belongs to the field of materials, and particularly relates to a sintering method of titanium or titanium alloy powder.
Background
The porous material is a structural function integrated material, and due to the existence of pores, the specific surface of the material is increased, the density of the material is reduced, and the porous material has the functional properties of adsorption, filtration, noise reduction, heat insulation and the like. The product is widely applied to the fields of aerospace, medicine, environmental protection, metallurgy, electrochemistry and the like. The existing technology for preparing the porous material has the disadvantages of complex process, long production period, high technical requirement, high production equipment cost and difficult realization.
Titanium and titanium alloys have been widely used as structural materials in aerospace, automotive, diving, medical implants due to their high specific strength, low modulus, excellent biocompatibility, corrosion resistance. The porous titanium and the titanium alloy have the functional properties of high surface area and low modulus by introducing the holes, and the application of the titanium and the titanium alloy in orthopedic implant materials, battery electrode materials, sound absorption materials and filter materials is extended. The pore structure of porous titanium can be divided into two types: closed cell structures and open cell structures. The closed pore structure porous titanium has the functions of high damping, sound absorption and heat insulation due to the closed pores, and is mainly applied to sound absorption materials and thermal protection materials. The open-pore structure porous titanium has the functional attribute of closed-pore structure porous titanium due to the mutual penetration of the pores, has filtering property, and is mainly applied to orthopedic implant materials, battery electrode materials and filtering materials.
At present, the preparation method of porous titanium and titanium alloy is mainly the traditional powder metallurgy technology, and comprises powder loose sintering, pore-forming agent adding method, organic foam immersion method, freezing casting, fiber sintering and the like. In which I.H.Oh et al (scriptaMaterialia,2003,49,1197) prepared porous titanium with a through-hole structure having a porosity of 37% by vacuum sintering of spherical titanium powder, and its Young's modulus and flexural strength were close to those of human bones. Manonukul et al (Powder Technology,2014,266,129) prepared porous titanium with a porosity of 84% by dipping polyurethane foam in titanium Powder slurry by an organic foam dipping method, degreasing and vacuum sintering, and the Young's modulus of the porous titanium could reach 0.58 GPa. In the preparation technology of the porous titanium, because a compact titanium dioxide oxide film exists on the surface of titanium powder, electron migration between the titanium powder which is in contact with each other is hindered, the titanium powder can not be sintered in a mode of rapid heating through an electromagnetic field, heat can only be conducted to powder through the heating elements to be sintered under a vacuum condition, the heating rate is slow, the temperature rise time is long, the size shrinkage of a sintered body is large, the size of a product is difficult to control, and the preparation technology is not suitable for preparing the porous titanium and the titanium alloy with high porosity.
Disclosure of Invention
The invention provides a sintering method of titanium or titanium alloy powder, which transmits heat to titanium or titanium alloy powder contacted with a heating body through the heating body, destroys and dissolves a non-conductive titanium dioxide oxide layer on the surface of the titanium or titanium alloy powder in a contact layer, so that the titanium or titanium alloy powder is mutually connected and conductive, and the powder is rapidly heated layer by layer under the action of an alternating electromagnetic field, and finally a complete sintered body is obtained. The method has the advantages of high heating speed, short sintering time, small size shrinkage of the sintered body and simple process, and can be used for preparing porous titanium or titanium alloy and fully-compact titanium or titanium alloy sintered bodies with different pore gas rates.
The technical scheme of the invention is as follows:
a sintering method of titanium or titanium alloy powder comprises the following steps:
1) preparing powder; preparing titanium or titanium alloy powder into powder;
2) the heating body heats the powder; under the protective atmosphere of vacuum or inert gas, the powder is contacted with a heating body to be rapidly heated;
3) heating the powder by an electromagnetic field; the heating body heats the powder through heat conduction, and simultaneously, the powder is quickly heated through an electromagnetic field to prepare a sintered body.
Further, in the sintering method of the titanium or titanium alloy powder, the powder preparation mode in the step 1) is as follows: mixing titanium or titanium alloy powder with the granularity of less than 1000 mu m with a pore-forming agent and an organic adhesive, preparing a green body by cold pressing, warm pressing, 3D printing, cold isostatic pressing, cold rolling or injection molding, and degreasing the green body to obtain the titanium or titanium alloy powder.
Further, in the sintering method of the titanium or titanium alloy powder, the powder preparation mode in the step 1) is as follows: adding titanium or titanium alloy powder with the granularity of less than 1000 mu m, a binder, a dispersant, a suspending agent, a defoaming agent, a titrant, water or an organic solvent into a container in proportion, preparing powder slurry by stirring, dipping an organic template into the powder slurry, and carrying out curing and degreasing treatment to obtain the titanium or titanium alloy powder.
Further, in the sintering method of the titanium or titanium alloy powder, the powder preparation mode in the step 1) is as follows: the titanium or titanium alloy powder is directly spread on the heating body.
Further, the sintering method of the titanium or titanium alloy powder comprises the step of sintering the titanium or titanium alloy powder, wherein the pore-forming agent is NaCl, sucrose, magnesium, urea or starch.
Further, the sintering method of the titanium or titanium alloy powder is characterized in that the pressure for preparing the green body by the cold pressing or cold isostatic pressing process is 0.1-1500 MPa; the pressure of the green blank prepared by the warm pressing process is 0.1-1500MPa, and the temperature is 50-500 ℃.
Further, in the sintering method of the titanium or titanium alloy powder, the heating body is made of silicon carbide, silicon nitride, aluminum oxide, graphite, tungsten, molybdenum, steel, copper, titanium or titanium alloy.
Further, in the sintering method of titanium or titanium alloy powder, in the step 2), the vacuum condition is as follows: degree of vacuum 10-2~10-5Pa, inert gas is: argon or helium.
Further, in the sintering method of the titanium or titanium alloy powder, the heating temperature of the heating body is 200-1500 ℃.
Further, the sintering method of the titanium or titanium alloy powder comprises the following electromagnetic field heating modes: microwave heating, induction heating, plasma heating or pulse heating; the heating temperature of the electromagnetic field is 600-1500 ℃, and the heat preservation time is 0.01-2400 minutes.
Further, according to the sintering method of the titanium or titanium alloy powder, the green body is prepared on a pure titanium or titanium alloy heating body, the titanium or titanium alloy powder, a pore-forming agent and an organic adhesive are mixed to obtain a mixture, the pure titanium or titanium alloy heating body is placed at the bottom of a mold, the mixture is placed into the mold, cold press molding is carried out, and a molded body comprises the green body and the pure titanium or titanium alloy heating body.
The invention has the beneficial effects that: the invention transmits heat to the titanium or titanium alloy powder contacted with the heating body, can effectively destroy and dissolve the titanium dioxide oxide layer on the surface of the titanium or titanium alloy powder, and realizes the rapid heating of the powder under the action of the alternating electromagnetic field. The obtained sintered body has a porosity of 0.01-99%, and is suitable for preparing fully compact or porous titanium or titanium alloy products, and a porous titanium or titanium alloy coating can be prepared on a titanium or titanium alloy heating body. The method has the advantages that the heating speed can reach 1000 degrees per minute, the shrinkage rate of the sintered product is 0.1-90 percent, and the pore structure, the pore size, the pore rate and the size deviation of the sintered body of the porous titanium and the titanium alloy can be accurately controlled. The invention has simple production equipment, low raw material cost and controllable process, can realize large-scale industrial production, and can be widely applied to the fields of biomedical implants, photocatalysis, filtration, adsorption, noise reduction, heat insulation and the like.
Drawings
FIG. 1 is a cross-sectional gold phase diagram of porous titanium in example 1;
FIG. 2 is a cross-sectional gold phase diagram of porous titanium in example 2;
FIG. 3 is a metallographic structure chart of a fully dense titanium sintered body in example 2.
Detailed Description
Example 1
A method of sintering titanium powder comprising the steps of:
step 1: uniformly mixing pure titanium powder with the particle size of less than 45 mu m and urea particles with the particle size of less than 70 mu m according to the volume ratio of 3:7, putting 100 g of the mixture into a mold, cold-pressing the mixture into a green body with the diameter of 30 mm under the pressure of 100MPa, and putting the green body under the vacuum condition and the vacuum degree of less than 10-2Pa, degreasing to remove urea to obtain powder, wherein the degreasing temperature is 350 ℃, the heating rate is 10 ℃/min, and the degreasing time is 2 h.
Step 2: and placing the powder on a silicon carbide heating body, and heating the silicon carbide heating body under a vacuum condition, wherein the surface temperature of the silicon carbide heating body reaches 1000 ℃, and the heating rate is 500 ℃/min.
And step 3: the powder is heated to 1000 ℃ by pulse current, and the temperature is kept for 5 minutes to prepare porous titanium, wherein the cross section metallographic structure of the porous titanium is shown in figure 1; the porosity of the porous titanium is 68 percent, and the through porosity is 100 percent.
Example 2
A sintering method of titanium alloy powder comprises the following steps:
step 1: spreading spherical Ti-6Al-4V titanium alloy powder with the particle size of less than 149 microns on a silicon nitride heating body, placing the silicon nitride heating body in an induction heating coil, heating the silicon nitride heating body under the protection of argon gas, wherein the oxygen content is less than 100ppm, and the surface temperature of the silicon nitride heating body reaches 900 ℃, and the heating rate is 450 ℃/min.
And step 3: introducing induction current, heating the powder to 900 ℃ through an alternating electromagnetic field in the induction coil, and preserving heat for 10 minutes to prepare porous titanium, wherein the cross section metallographic structure of the porous titanium is shown in figure 2; the porosity of the porous titanium is 32%, and the through porosity is 100%.
Example 3
A sintering method of titanium alloy powder comprises the following steps:
step 1: heating polypropylene, polyethylene glycol and carnauba wax to 150 ℃ according to the mass ratio of 25:70:5, uniformly mixing to prepare a binder, mixing the binder and spherical Ti-6Al-4V titanium alloy powder with the same volume and the particle size of less than 44 mu m, heating to 150 ℃, uniformly mixing, heating the mixture to 150 ℃ through an injection molding machine, performing injection molding to obtain a green body with the diameter of 20 mm, and performing vacuum injection on the green body under the vacuum condition with the vacuum degree of less than 10-2Pa, heating to 900 ℃, preserving heat for 1 hour, degreasing and removing the binder to obtain powder, wherein the heating rate is 10 ℃/min.
Step 2: and placing the powder on a graphite heating body with the diameter of 40 mm, heating the graphite heating body under the argon protective atmosphere, wherein the oxygen content is lower than 100ppm, and the surface temperature of the graphite heating body reaches 1000 ℃, and the heating rate is 500 ℃/min.
And step 3: heating the powder to 1100 ℃ by using plasma, and preserving the heat for 2 hours to prepare a fully-compact titanium sintered body, wherein the cross section metallographic structure of the fully-compact titanium sintered body is shown in a figure 3; the relative density was 99%.
Example 4
A sintering method of titanium alloy powder comprises the following steps:
step 1: uniformly mixing Ti-6Al-4V titanium alloy powder with the particle size of less than 45 mu m, PVA, a dispersing agent and water in a mass ratio of 75:1:1:23 by a magnetic stirrer to prepare titanium powder slurry, soaking organic foam with the thickness of 20 mm in the slurry, repeating the soaking step for multiple times until the organic foam is completely coated by the slurry, taking out the organic foam, placing the organic foam in air, standing at room temperature for 24 hours until the organic foam is solidified, and placing the organic foam under a vacuum condition with the vacuum degree of less than 10-2Pa, heating to 600 ℃, preserving heat for 2 hours, degreasing and removing organic foam to obtain powder, wherein the heating rate is 10 ℃/min.
Step 2: placing the powder on a tungsten heating body with the area of 400 square centimeters, wherein the vacuum degree is lower than 10 under the vacuum condition-2Pa, heating the tungsten heating body, wherein the surface temperature of the tungsten heating body reaches 1100 ℃, and the heating rate is 500 ℃/min.
And step 3: heating the powder to 1100 ℃ by microwave, and keeping the temperature for 5 minutes to prepare porous titanium; the porosity of the porous titanium is 90%, and the through porosity is 100%.
Example 5
A method of sintering titanium powder comprising the steps of:
step 1: uniformly mixing pure titanium powder with the particle size of less than 45 mu m and NaCl particles with the particle size of less than 2mm according to the volume ratio of 3:7, placing a pure titanium heating body with the diameter of 30 mm at the center position at the bottom of a mould with the diameter of 30 mm, wherein the thickness of the pure titanium heating body is 20 mm, pouring 10 g of the mixture of the pure titanium powder and the NaCl particles into the mould, carrying out cold press molding on the mould under the pressure of 800MPa, coating the surface of the pure titanium heating body with the mixture of the pure titanium powder and the NaCl particles, removing NaCl from the molded body including a coating layer and the titanium heating body in deionized water, and placing the molded body at room temperature for 48 hours, and replacing the deionized.
Step 2: and (2) introducing pulse current to heat the coating layer and the titanium heating body, keeping the temperature of the titanium heating body to 1000 ℃, heating at the rate of 100 ℃/min, keeping the temperature until the temperature of the coating layer reaches 1000 ℃, and stopping heating to prepare the porous titanium coating on the pure titanium heating body, wherein the porosity of the porous titanium is 69% and the porosity of the through hole is 100%.
The above description describes only a few embodiments of the invention, and does not limit the scope of the invention. All changes and modifications that come within the spirit of the invention are desired to be protected.

Claims (10)

1. A method for sintering titanium or titanium alloy powder, characterized by comprising the steps of:
1) preparing powder; preparing titanium or titanium alloy powder into powder;
2) the heating body heats the powder; under the protective atmosphere of vacuum or inert gas, the powder is contacted with a heating body to be rapidly heated;
3) heating the powder by an electromagnetic field; the heating body heats the powder through heat conduction, and simultaneously, the powder is quickly heated through an electromagnetic field to prepare a sintered body.
2. The method for sintering titanium or titanium alloy powder according to claim 1, wherein the powder is prepared in the following manner in the step 1): mixing titanium or titanium alloy powder with the granularity of less than 1000 mu m with a pore-forming agent and an organic adhesive, preparing a green body by cold pressing, warm pressing, 3D printing, cold isostatic pressing, cold rolling or injection molding, and degreasing the green body to obtain the titanium or titanium alloy powder.
3. The method for sintering titanium or titanium alloy powder according to claim 1, wherein the powder is prepared in the following manner in the step 1): adding titanium or titanium alloy powder with the granularity of less than 1000 mu m, a binder, a dispersant, a suspending agent, a defoaming agent, a titrant, water or an organic solvent into a container in proportion, preparing powder slurry by stirring, dipping an organic template into the powder slurry, and carrying out curing and degreasing treatment to obtain the titanium or titanium alloy powder.
4. The sintering method for preparing porous titanium by sintering titanium or titanium alloy powder according to claim 1, wherein the powder preparation mode in the step 1) is as follows: the titanium or titanium alloy powder is directly spread on the heating body.
5. The method for sintering titanium or titanium alloy powder according to claim 2, wherein the pore-forming agent is NaCl, sucrose, magnesium, urea, or starch.
6. The method for sintering titanium or titanium alloy powder according to claim 2, wherein the pressure at which the green body is prepared by the cold pressing or cold isostatic pressing process is between 0.1 and 1500 MPa; the pressure of the green blank prepared by the warm pressing process is 0.1-1500MPa, and the temperature is 50-500 ℃.
7. The method for sintering titanium or titanium alloy powder according to claim 1, wherein the heater is made of silicon carbide, silicon nitride, alumina, graphite, tungsten, molybdenum, steel, copper, titanium or titanium alloy.
8. The method for preparing porous titanium by sintering titanium or titanium alloy powder according to claim 1, wherein in the step 2), the vacuum condition is as follows: degree of vacuum 10-2~10-5Pa, inert gas is: argon or helium, wherein the heating temperature of the heating body is 200-1500 ℃.
9. The method for sintering titanium or titanium alloy powder according to claim 1, wherein the electromagnetic field heating means is: microwave heating, induction heating, plasma heating or pulse heating; the heating temperature of the electromagnetic field is 600-1500 ℃, and the heat preservation time is 0.01-2400 minutes.
10. The method for sintering titanium or titanium alloy powder according to claim 2, wherein the green body is prepared on a pure titanium or titanium alloy heating body, the titanium or titanium alloy powder is mixed with a pore-forming agent and an organic binder to obtain a mixture, the pure titanium or titanium alloy heating body is placed at the bottom of the mold, the mixture is placed into the mold, and cold press molding is performed, wherein a molded body comprises the green body and the pure titanium or titanium alloy heating body.
CN202010325032.4A 2020-04-23 2020-04-23 Sintering method of titanium or titanium alloy powder Pending CN111375758A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112692287A (en) * 2021-01-14 2021-04-23 昆明理工大学 Preparation method of ordered porous titanium in three-dimensional communicated latticed distribution
WO2022011951A1 (en) * 2020-07-14 2022-01-20 苏州大学 Tungsten-doped titanium-based composite porous material and preparation method therefor

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3779747A (en) * 1972-09-05 1973-12-18 Gleason Works Process for heating and sintering ferrous powder metal compacts
JPS5964702A (en) * 1982-09-30 1984-04-12 Toyota Motor Corp High-frequency sintering method of compressed body of metal powder
CN1049623A (en) * 1989-08-22 1991-03-06 五十铃汽车有限公司 Porous sintered body and manufacture method thereof
US5034186A (en) * 1985-11-20 1991-07-23 Permelec Electrode Ltd. Process for providing titanium composite having a porous surface
CN102747245A (en) * 2012-07-06 2012-10-24 淮阴工学院 Preparation method of medical porous titanium and titanium alloy
CN105506375A (en) * 2015-12-22 2016-04-20 上海理工大学 Method for rapidly preparing medical titanium alloy
CN107096919A (en) * 2016-02-19 2017-08-29 泰克纳里阿研究与创新基金 The equipment for sintering the method for conductive powder and performing methods described

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3779747A (en) * 1972-09-05 1973-12-18 Gleason Works Process for heating and sintering ferrous powder metal compacts
JPS5964702A (en) * 1982-09-30 1984-04-12 Toyota Motor Corp High-frequency sintering method of compressed body of metal powder
US5034186A (en) * 1985-11-20 1991-07-23 Permelec Electrode Ltd. Process for providing titanium composite having a porous surface
CN1049623A (en) * 1989-08-22 1991-03-06 五十铃汽车有限公司 Porous sintered body and manufacture method thereof
CN102747245A (en) * 2012-07-06 2012-10-24 淮阴工学院 Preparation method of medical porous titanium and titanium alloy
CN105506375A (en) * 2015-12-22 2016-04-20 上海理工大学 Method for rapidly preparing medical titanium alloy
CN107096919A (en) * 2016-02-19 2017-08-29 泰克纳里阿研究与创新基金 The equipment for sintering the method for conductive powder and performing methods described

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
周静,沈杰,赵春霞,祁琰媛》: "《近代材料科学研究技术进展》", 31 December 2012, 武汉理工大学出版社 *
张克立,袁良杰,冯传启: "《无机合成化学第2版》", 31 January 2012, 武汉大学出版社 *
张华诚: "《粉末冶金实用工艺学》", 30 September 2004, 冶金工业出版社 *
曾晓苑: "《锂空气电池高性能催化剂的制备与应用》", 30 April 2019, 冶金工业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022011951A1 (en) * 2020-07-14 2022-01-20 苏州大学 Tungsten-doped titanium-based composite porous material and preparation method therefor
CN112692287A (en) * 2021-01-14 2021-04-23 昆明理工大学 Preparation method of ordered porous titanium in three-dimensional communicated latticed distribution

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