CN111118324A - Preparation method of TiC reinforced copper-based composite material added with coupling agent - Google Patents
Preparation method of TiC reinforced copper-based composite material added with coupling agent Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
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- B22F3/14—Both compacting and sintering simultaneously
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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- 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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- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract
The invention discloses a preparation method of a TiC reinforced copper-based composite material added with a coupling agent, which comprises the steps of preparing titanium-coated titanium carbide powder by magnetron sputtering; then, ball milling, compacting and sintering are adopted to prepare the titanium carbide reinforced copper-based composite material, and the composite reinforced copper-based composite material is obtained after aging treatment. The titanium carbide particle reinforced copper-based composite material prepared by the method of the invention forms TiC and Cu after being processed4The Ti composite reinforcing effect is realized, the interface bonding strength of the reinforcing body and the copper matrix is high, and the hardness, the strength, the wear resistance and the corrosion resistance are obviously improved while certain conductivity is ensured.
Description
Technical Field
The invention belongs to the technical field of material manufacturing, and particularly relates to a preparation method of a TiC reinforced copper-based composite material added with a coupling agent.
Background
Copper-based composite materials are widely used in many fields such as electric power, national defense, and vehicle members because of their high electrical conductivity, high thermal conductivity, high fusion welding resistance, and corrosion resistance, and their ability to maintain low and stable contact resistance. The copper-based composite material is limited in application due to its low strength, hardness and wear resistance. Therefore, on the basis of keeping high electrical conductivity and high thermal conductivity, research and development of copper-based composite materials with high strength, hardness and wear resistance, certain corrosion resistance, high cost performance and balanced and reliable performance are of great significance.
The research and development of the particle reinforced copper-based composite material are widely applied due to simple process and obvious reinforcing effect, and currently adopted reinforcements mainly comprise reinforcements such as silicon carbide, titanium carbide, boron carbide, tungsten carbide, alumina, silicon nitride, titanium boride, boron nitride, graphite and the like. The titanium carbide has certain thermal conductivity and electrical conductivity due to higher hardness, melting point and chemical stability, and has a positive application prospect in preparing copper-based composite materials.
The prior known technology for preparing the titanium carbide reinforced copper-based composite material comprises the following steps: 1) a autogenous titanium carbide reinforced copper-based composite material and a preparation method thereof (application No. CN201910525771.5, publication No. CN110129607A, published as 2019.08.16); 2) the patent "titanium carbide and titanium diboride two-phase reinforced copper-based composite material and the preparation method thereof" (application No. CN201710657353.2, publication No. CN107586987B, published as 2019.06.18); 3) an in-situ synthesized titanium boride, titanium carbide complex phase ceramic reinforced copper base composite material and a preparation method and application thereof (application No. CN201711397493.7, publication No. CN108118178A, published Japanese 2018.06.05); 4) patent "titanium carbide # titanium diboride two-phase reinforced copper-based composite material and preparation method thereof" (application number CN201710657353.2, publication number CN107586987A, published as 2018.01.16); 5) a method for preparing a titanium carbide ceramic particle-reinforced copper-based composite material (application No. CN201710098004.1, publication No. CN106756177A, published as 2017.05.31); 6) patent "preparation method of titanium carbide/copper-based composite material" (application No. CN201610979908.0, publication No. CN106521223A, published as 2017.03.22); 7) patent "a high-strength titanium carbide particle-reinforced copper-based composite material and a method for producing the same" (application No. cn201510728060.x, publication No. CN105256170A, published 2016.01.20); 8) a high-strength titanium carbide copper-based composite material and a preparation method thereof (application No. CN201510727764.5, publication No. CN105177348A, published as 2015.12.23); 9) patent "a particle-reinforced copper-based composite material" (patent No. CN201110202692.4, publication No. CN102888522A, publication No. 2013.01.23); 10) patent "a method for preparing a titanium carbide dispersion-strengthened copper-based composite material" (patent No. CN200910095170.1, publication No. CN101709397A, published japanese 2010.05.19); 11) patent "self-propagating high-temperature synthesis preparation method of titanium carbide dispersion-strengthened copper-based composite material" (patent No. CN200910095173.5, publication No. CN101709398A, published japanese 2010.05.19); 12) a method for producing a titanium carbide dispersion-strengthened copper-based composite material (application No. CN200910095170.1, publication No. CN101709397A, Kokai No. 2010.05.19). 13) A self-propagating high-temperature synthesis method for preparing a titanium carbide dispersion-strengthened copper-based composite material (application No. CN200910095173.5, publication No. CN101709398A, published as 2010.05.19). 14) An in-situ generated titanium carbide dispersion strengthened copper-based composite material and a preparation method thereof (application No. CN200510045649.6, publication No. CN1804077, published Japanese 2006.07.19).
The proposal of the titanium carbide reinforced copper-based composite material is that the titanium carbide is added or other inclusion components are added on the basis of the titanium carbide reinforced copper-based composite material, and the titanium carbide reinforced copper-based composite material is prepared by methods such as ball milling, in-situ reaction, casting, infiltration and the like. The schemes effectively improve the electrical property and the mechanical property of the copper-based electric contact material, but have slightly low reinforcing effect to a certain extent and influence the heat conduction, the electric conductivity and the corrosion resistance of the material.
Disclosure of Invention
The invention aims to provide a preparation method of a TiC reinforced copper-based composite material added with a coupling agent, which is characterized in that titanium is plated on the surface of a TiC reinforcing body through magnetron sputtering, then TiC with a plated film and copper powder are mixed, subjected to ball milling, pressed and sintered, and subjected to aging treatment to prepare the TiC reinforced copper-based composite material, so that the rigidity, the strength, the wear resistance and the corrosion resistance are obviously improved while the conductivity is ensured.
The technical scheme adopted by the invention is that the preparation method of the TiC reinforced copper-based composite material added with the Ti coupling agent comprises the following steps:
step 1: powder coating
Pre-cleaning the surface of TiC powder: carrying out ultrasonic cleaning for 20min by adopting absolute ethyl alcohol for surface degreasing and decontamination treatment, then soaking in hydrofluoric acid with the mass concentration of 20 wt.% for 15min, and then cleaning by using distilled water and drying for 2 hours at the temperature of 60 ℃.
Placing the TiC powder with the cleaned surface in magnetron sputtering coating equipment, and carrying out magnetron sputtering Ti plating treatment at room temperature under an argon atmosphere;
step 2: ball milling and pressing
Adding the TiC powder with the coated surface, the copper powder and the process control agent prepared in the step 1 into a ball mill, and carrying out ball milling under the protection of Ar atmosphere or in a vacuum environment to obtain composite powder; then placing the composite powder in a drying oven, drying for 2 hours at 60 ℃, and prepressing the dried composite powder into a blank;
and step 3: sintering
Placing the blank pressed in the step 2 in a hot-pressing sintering furnace, and adding N2Sintering and cooling to room temperature under the atmosphere protection to obtain a prefabricated copper-based composite material;
and 4, step 4: aging treatment
Placing the fired prefabricated copper-based composite material in an atmosphere furnace again, heating to 400-500 ℃ under the protection of argon, preserving heat for 4 hours, then cooling the furnace to room temperature, taking out a sample, and forming α -Cu on the interface of the copper matrix and the titanium carbide reinforcement4Ti stable phase to obtain the reinforced copper-based composite material.
The present invention is also characterized in that,
and (2) in the step 1, the magnetron sputtering power of Ti plating is 150W, the sputtering time is 3h, and the TiC powder is vibrated at the same time, wherein the argon flow is 10sccm, so that the surface of the TiC powder is uniformly coated.
The process control agent in the step 2 is absolute ethyl alcohol.
And 2, weighing the TiC powder according to 0.45-3% of the total mass of the powder.
The amount of the absolute ethyl alcohol is 5-10% of the total mass of the TiC powder.
2, ball milling time is 2-10 h; the rotating speed of the ball mill is 200-300 r/min.
And 3, in the sintering process, the heating temperature is 1040-1060 ℃, the heat preservation time is 50-60 min, and the pressure of 30-35 MPa is continuously applied in the heat preservation process.
The titanium carbide particle reinforced copper-based composite material prepared by the preparation method of the TiC reinforced copper-based composite material added with the coupling agent is processed to form TiC and α -Cu4The addition of Ti as a coupling agent improves the wettability between the reinforcement TiC and the matrix Cu and produces better interface bonding strength, and α -Cu formed after aging treatment is used4The Ti compound further strengthens the particle reinforcing effect, and simultaneously improves the corrosion resistance of the composite material to a certain extent by the generation of the copper-titanium alloy at the interface of the reinforcing body and the matrix.
Detailed Description
The invention relates to a preparation method of a TiC reinforced copper-based composite material added with a coupling agent, which comprises the following steps:
step 1: powder coating
The surface of TiC powder is pre-cleaned, absolute ethyl alcohol is adopted for ultrasonic cleaning for 20min for surface degreasing and decontamination treatment, then the TiC powder is soaked in hydrofluoric acid (20 wt.%) for 15min, and then the TiC powder is cleaned by distilled water and dried for 2 hours at 60 ℃.
And placing the TiC powder with the cleaned surface in magnetron sputtering coating equipment, and performing Ti plating treatment at room temperature under an argon atmosphere. The magnetron sputtering power is 150W, the sputtering time is 3h, the argon flow is 10sccm, and the TiC powder is vibrated so as to ensure that the surface of the TiC powder is uniformly coated.
Step 2: ball milling and pressing
Adding the powder weighed in the step 1 and a process control agent into a ball mill, weighing TiC powder according to 0.45-3% of the total weight of the powder, and carrying out ball milling under the protection of Ar atmosphere or in a vacuum environment; then drying the composite powder and prepressing into a blank; in the step 2, the process control agent is absolute ethyl alcohol, and the using amount of the process control agent is 5-10% (Wt%) of the total powder mass; the ball milling time is 2h, 5h and 10 h; the rotating speed of the ball mill is 200r/min, 250r/min or 300 r/min;
and step 3: sintering
Placing the blank pressed in the step 2 in a hot-pressing sintering furnace, and adding N2Sintering and cooling to room temperature under the atmosphere protection to obtain the TiC reinforced Cu-based composite material; and 3, in the sintering process in the step 3, the heating temperature is 1040-1060 ℃, the heat preservation time is 50-60 min, and the pressure of 30-35 MPa is continuously applied in the heat preservation process.
And 5: aging treatment
Putting the fired material into an atmosphere furnace again, heating to 400-500 ℃ under the protection of argon, preserving the heat for 4 hours, then cooling the furnace to room temperature, taking out the sample to form α -Cu4Ti stable phase, further strengthening the copper-based composite material.
Example 1
The surface of TiC powder is pre-cleaned, absolute ethyl alcohol is adopted for ultrasonic cleaning for 20min for surface degreasing and decontamination treatment, then the TiC powder is soaked in hydrofluoric acid (20 wt.%) for 15min, and then the TiC powder is cleaned by distilled water and dried for 2 hours at 60 ℃. And placing the TiC powder with the cleaned surface in magnetron sputtering coating equipment, and performing Ti plating treatment at room temperature under an argon atmosphere. The magnetron sputtering power is 150W, the sputtering time is 3h, the argon flow is 10sccm, and the TiC powder is vibrated so as to ensure that the surface of the TiC powder is uniformly coated.
Adding the prepared TiC powder, copper powder and 10 Wt% of absolute ethyl alcohol process control agent into a ball mill, wherein the TiC powder is weighed according to 0.45% of the total mass of the powder, and carrying out ball milling for 2 hours under the protection of Ar atmosphere or in a vacuum environment, and the rotating speed of the ball mill is 200 r/min; and then drying the composite powder and prepressing the composite powder into a blank. Placing the pressed blank in a hot-pressing sintering furnace, and performing sintering in a nitrogen atmosphere2Sintering and cooling to room temperature under the protection of atmosphere to obtain the TiC reinforced copper-based composite material, wherein the heating temperature is 1060 ℃, the heat preservation time is 50min, the pressure of 35MPa is continuously applied in the heat preservation process, the fired material is placed in an atmosphere furnace again, the temperature is increased to 500 ℃ under the protection of argon, the heat preservation is carried out for 4 hours, then the furnace is cooled to room temperature, a sample is taken out, α -Cu is formed on the interface of the copper matrix and the titanium carbide reinforcement body4Ti stable phase, further strengthening the copper-based composite material.
Example 2
The surface of TiC powder is pre-cleaned, absolute ethyl alcohol is adopted for ultrasonic cleaning for 20min for surface degreasing and decontamination treatment, then the TiC powder is soaked in hydrofluoric acid (20 wt.%) for 15min, and then the TiC powder is cleaned by distilled water and dried for 2 hours at 60 ℃. And placing the TiC powder with the cleaned surface in magnetron sputtering coating equipment, and performing Ti plating treatment at room temperature under an argon atmosphere. The magnetron sputtering power is 150W, the sputtering time is 3h, the argon flow is 10sccm, and the TiC powder is vibrated so as to ensure that the surface of the TiC powder is uniformly coated.
Adding the prepared TiC powder, copper powder and 5 Wt% of absolute ethyl alcohol process control agent into a ball mill, wherein the TiC powder is weighed according to 3% of the total mass of the powder, and carrying out ball milling for 5 hours under the protection of Ar atmosphere or in a vacuum environment, and the rotating speed of the ball mill is 250 r/min; then drying the composite powder and prepressingAnd (5) preparing a blank. Placing the pressed blank in a hot-pressing sintering furnace, and performing sintering in a nitrogen atmosphere2Sintering and cooling to room temperature under the protection of atmosphere to obtain the TiC reinforced copper-based composite material, wherein the heating temperature is 1040 ℃, the heat preservation time is 60min, the pressure of 30MPa is continuously applied in the heat preservation process, the fired material is placed in an atmosphere furnace again, the temperature is increased to 440 ℃ under the protection of argon, the heat preservation is carried out for 4 hours, then the furnace is cooled to room temperature, a sample is taken out, and α -Cu is formed on the interface of the copper matrix and the titanium carbide reinforcement body4Ti stable phase, further strengthening the copper-based composite material.
Example 3
The surface of TiC powder is pre-cleaned, absolute ethyl alcohol is adopted for ultrasonic cleaning for 20min for surface degreasing and decontamination treatment, then the TiC powder is soaked in hydrofluoric acid (20 wt.%) for 15min, and then the TiC powder is cleaned by distilled water and dried for 2 hours at 60 ℃. And placing the TiC powder with the cleaned surface in magnetron sputtering coating equipment, and performing Ti plating treatment at room temperature under an argon atmosphere. The magnetron sputtering power is 150W, the sputtering time is 3h, the argon flow is 10sccm, and the TiC powder is vibrated so as to ensure that the surface of the TiC powder is uniformly coated.
Adding the prepared TiC powder, copper powder and 10 Wt% of absolute ethyl alcohol process control agent into a ball mill, wherein the TiC powder is weighed according to 3% of the total mass of the powder, and carrying out ball milling for 8 hours under the protection of Ar atmosphere or in a vacuum environment, and the rotating speed of the ball mill is 200 r/min; and then drying the composite powder and prepressing the composite powder into a blank. Placing the pressed blank in a hot-pressing sintering furnace, and performing sintering in a nitrogen atmosphere2Sintering and cooling to room temperature under the protection of atmosphere to obtain the TiC reinforced copper-based composite material, wherein the heating temperature is 1050 ℃, the heat preservation time is 55min, the pressure of 33MPa is continuously applied in the heat preservation process, the fired material is placed in an atmosphere furnace again, the temperature is increased to 450 ℃ under the protection of argon, the heat preservation is carried out for 4 hours, then the furnace is cooled to room temperature, a sample is taken out, α is formed on the interface of the copper matrix and the titanium carbide reinforcement body, Cu4Ti stable phase, further strengthening the copper-based composite material.
Example 4
The surface of TiC powder is pre-cleaned, absolute ethyl alcohol is adopted for ultrasonic cleaning for 20min for surface degreasing and decontamination treatment, then the TiC powder is soaked in hydrofluoric acid (20 wt.%) for 15min, and then the TiC powder is cleaned by distilled water and dried for 2 hours at 60 ℃. And placing the TiC powder with the cleaned surface in magnetron sputtering coating equipment, and performing Ti plating treatment at room temperature under an argon atmosphere. The magnetron sputtering power is 150W, the sputtering time is 3h, the argon flow is 10sccm, and the TiC powder is vibrated so as to ensure that the surface of the TiC powder is uniformly coated.
Adding the prepared TiC powder, copper powder and 10 Wt% of absolute ethyl alcohol process control agent into a ball mill, wherein the TiC powder is weighed according to 2% of the total mass of the powder, and carrying out ball milling for 5 hours under the protection of Ar atmosphere or in a vacuum environment, and the rotating speed of the ball mill is 300 r/min; and then drying the composite powder and prepressing the composite powder into a blank. Placing the pressed blank in a hot-pressing sintering furnace, and performing sintering in a nitrogen atmosphere2Sintering and cooling to room temperature under the protection of atmosphere to obtain the TiC reinforced copper-based composite material, wherein the heating temperature is 1060 ℃, the heat preservation time is 60min, the pressure of 35MPa is continuously applied in the heat preservation process, the fired material is placed in an atmosphere furnace again, the temperature is increased to 500 ℃ under the protection of argon, the heat preservation is carried out for 4 hours, then the furnace is cooled to room temperature, a sample is taken out, and α -Cu is formed on the interface of the copper matrix and the titanium carbide reinforcement body4Ti stable phase, further strengthening the copper-based composite material.
Example 5
The surface of TiC powder is pre-cleaned, absolute ethyl alcohol is adopted for ultrasonic cleaning for 20min for surface degreasing and decontamination treatment, then the TiC powder is soaked in hydrofluoric acid (20 wt.%) for 15min, and then the TiC powder is cleaned by distilled water and dried for 2 hours at 60 ℃. And placing the TiC powder with the cleaned surface in magnetron sputtering coating equipment, and performing Ti plating treatment at room temperature under an argon atmosphere. The magnetron sputtering power is 150W, the sputtering time is 3h, the argon flow is 10sccm, and the TiC powder is vibrated so as to ensure that the surface of the TiC powder is uniformly coated.
Adding the prepared TiC powder, copper powder and 8 Wt% of absolute ethyl alcohol process control agent into a ball mill, wherein the TiC powder is weighed according to 1.5% of the total mass of the powder, and carrying out ball milling for 10 hours under the protection of Ar atmosphere or in a vacuum environment, and the rotating speed of the ball mill is 300 r/min; and then drying the composite powder and prepressing the composite powder into a blank. Placing the pressed blank in a hot-pressing sintering furnace, andin N2Sintering and cooling to room temperature under the protection of atmosphere to obtain the TiC reinforced copper-based composite material, wherein the heating temperature is 1040 ℃, the heat preservation time is 50min, the pressure of 30MPa is continuously applied in the heat preservation process, the fired material is placed in an atmosphere furnace again, the temperature is increased to 400 ℃ under the protection of argon, the heat preservation is carried out for 4 hours, then the furnace is cooled to room temperature, a sample is taken out, and α -Cu is formed on the interface of the copper matrix and the titanium carbide reinforcement body4Ti stable phase, further strengthening the copper-based composite material.
Claims (7)
1. A preparation method of a TiC reinforced copper-based composite material added with a coupling agent is characterized by comprising the following steps:
step 1: powder coating
Pre-cleaning the surface of TiC powder: carrying out ultrasonic cleaning for 20min by adopting absolute ethyl alcohol for surface degreasing and decontamination treatment, then soaking in hydrofluoric acid with the mass concentration of 20 wt.% for 15min, and then cleaning by using distilled water and drying for 2 hours at the temperature of 60 ℃.
Placing the TiC powder with the cleaned surface in magnetron sputtering coating equipment, and carrying out magnetron sputtering Ti plating treatment at room temperature under an argon atmosphere;
step 2: ball milling and pressing
Adding the TiC powder with the coated surface, the copper powder and the process control agent prepared in the step 1 into a ball mill, and carrying out ball milling under the protection of Ar atmosphere or in a vacuum environment to obtain composite powder; then placing the composite powder in a drying oven, drying for 2 hours at 60 ℃, and prepressing the dried composite powder into a blank;
and step 3: sintering
Placing the blank pressed in the step 2 in a hot-pressing sintering furnace, and adding N2Sintering and cooling to room temperature under the atmosphere protection to obtain a prefabricated copper-based composite material;
and 4, step 4: aging treatment
Placing the fired prefabricated copper-based composite material in an atmosphere furnace again, heating to 400-500 ℃ under the protection of argon, preserving heat for 4 hours, then cooling the furnace to room temperature, taking out a sample, and forming α -Cu on the interface of the copper matrix and the titanium carbide reinforcement4Ti stable phase to obtain the reinforced copper-based composite material.
2. The preparation method of the TiC reinforced copper-based composite material added with the coupling agent, as recited in claim 1, wherein the magnetron sputtering power for Ti plating in step 1 is 150W, the sputtering time is 3h, and the TiC powder is vibrated at the same time, and the flow of argon gas is 10sccm, so that the surface of the TiC powder is uniformly coated.
3. The method of claim 1, wherein the process control agent in step 2 is absolute ethyl alcohol.
4. The method of claim 1, wherein the TiC powder in step 2 is weighed in an amount of 0.45-3% by weight based on the total weight of the powder.
5. The preparation method of the TiC reinforced copper-based composite material added with the coupling agent, as recited in claim 2, wherein the amount of the absolute ethyl alcohol is 5-10% of the total mass of the TiC powder.
6. The preparation method of the TiC reinforced copper-based composite material added with the coupling agent according to claim 1, wherein the ball milling time in the step 2 is 2-10 hours; the rotating speed of the ball mill is 200-300 r/min.
7. The preparation method of the Couplant-added TiC-reinforced copper-based composite material, according to claim 1, characterized in that in the sintering process in the step 3, the heating temperature is 1040-1060 ℃, the heat preservation time is 50-60 min, and the pressure of 30-35 MPa is continuously applied in the heat preservation process.
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