CN110695359A - Hot isostatic pressing device and production process of densified product - Google Patents

Hot isostatic pressing device and production process of densified product Download PDF

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Publication number
CN110695359A
CN110695359A CN201911045247.4A CN201911045247A CN110695359A CN 110695359 A CN110695359 A CN 110695359A CN 201911045247 A CN201911045247 A CN 201911045247A CN 110695359 A CN110695359 A CN 110695359A
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China
Prior art keywords
pressure
isostatic pressing
hot isostatic
degreasing
sintered
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CN201911045247.4A
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Chinese (zh)
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CN110695359B (en
Inventor
陈宏霞
张德明
李阳
叶青
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Gangyan Haopu Technology Co ltd
Qingdao Gangyan Haopu Technology Co ltd
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New Metallurgy Hi Tech Group Co Ltd
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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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing
    • 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
    • B22F3/003Apparatus, e.g. furnaces
    • 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
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing
    • B22F2003/153Hot isostatic pressing apparatus specific to HIP

Abstract

The invention discloses a hot isostatic pressing device and a production process of a densified product, belongs to the technical field of material hot isostatic pressing devices and processes, and solves the problems of repeated heating of materials, long process flow time and high cost in the prior art. The hot isostatic pressing device comprises a degreasing system, a pressure-bearing container and a heating unit; the pressure-bearing container is used for placing a material (1) to be sintered, the degreasing system is used for degreasing the material (1) to be sintered, and the heating unit is arranged in the pressure-bearing container and used for heating the material to be sintered; the degreasing system comprises a binder collector (11) and a mechanical pump set (12); the binder collector (11) is connected with the mechanical pump set (12) through a pipeline; the adhesive collector (11) is connected to the pressure-bearing container. The device and the method are used for preparing densified products and shortening the process flow.

Description

Hot isostatic pressing device and production process of densified product
Technical Field
The invention belongs to the technical field of material hot isostatic pressing devices and processes, and particularly relates to a hot isostatic pressing device and a production process of a densified product.
Background
Hot isostatic pressing is a process technique for densifying a product in a closed container under high-temperature and high-pressure environment. The hot isostatic pressing can greatly improve the mechanical properties of the material, particularly the fatigue property and the reliability, and is widely applied in the fields of aerospace, war industry and the like.
Hot isostatic pressing processes can be divided into hot isostatic pressing without capsule and hot isostatic pressing with capsule according to whether capsules are used, wherein hot isostatic pressing without capsule is to further densify products (relative density > 95%) obtained after forming and sintering other processes in hot isostatic pressing equipment; the hot isostatic pressing process of the sheath is to put the powder into the sheath, seal the powder and put the powder into hot isostatic pressing equipment, and complete the forming and the densification in one step.
The clad hot isostatic pressing process has the characteristic of excellent mechanical property of products, but the design and manufacture difficulty of the clad with the complex shape is high and the cost is high when parts with the complex shape are prepared; the hot isostatic pressing process without a sheath has the advantage of low cost, but cannot be directly prepared, and is required to be combined with other forming processes, such as injection forming, gel casting forming and the like, for producing products with complex shapes. However, because the existing hot isostatic pressing equipment has no degreasing function, the formed green body needs to be subjected to binder removal in a vacuum degreasing sintering furnace, is subjected to vacuum sintering until closed pores are formed, and is further densified through hot isostatic pressing again. The two-step method has the problem of repeated heating, the process flow time is long, if the hot isostatic pressing equipment has the degreasing-vacuum sintering function, the process of the non-sheath hot isostatic pressing process is further shortened, the cost is reduced, and the hot isostatic pressing technology is beneficial to popularization and application.
Disclosure of Invention
In view of the above analysis, the present invention aims to provide a hot isostatic pressing apparatus with degreasing-vacuum sintering function, which can realize carrier gas degreasing function at medium and low temperature stages, and then prepare a product through vacuum sintering-hot isostatic pressing densification, so as to realize a short process.
The purpose of the invention is mainly realized by the following technical scheme:
a hot isostatic pressing device comprises a degreasing system, a pressure-bearing container and a heating unit;
the pressure-bearing container is used for placing materials to be sintered, the degreasing system is used for degreasing the sintering materials, and the heating unit is arranged in the pressure-bearing container and used for heating the materials to be sintered;
the degreasing system comprises a binder collector and a mechanical pump set; the binder collector is connected with the mechanical pump set through a pipeline; the binder collector is connected with the pressure-bearing container.
The pressure-bearing container comprises a cylinder body, a lower plug and an upper plug, wherein the cylinder body is in a cylindrical shape with two open ends, and the two ends are respectively sealed by the upper plug and the lower plug.
The heating unit comprises an electric leading electrode and a heating body, the electric leading electrode is connected with an external power supply, and the heating body is used for generating heat.
The heating body and the material to be sintered are wrapped by the heat insulation base and the heat insulation screen, so that heat diffusion is prevented.
The binder collector comprises a first collecting device and a second collecting device, wherein the second collecting device is a next-stage processing unit of the first collecting device, and the second collecting device is arranged above the first collecting device.
Also comprises a material boat for placing the materials to be sintered.
A production process of a densified product adopts the hot isostatic pressing device, and comprises the following steps:
s1, preparing a material to be sintered;
s2, placing the material to be sintered in the material boat, placing the material to be sintered on a heat insulation base, and closing the upper plug;
s3, degreasing the material to be sintered;
s4, sintering the material to be sintered;
s5, carrying out hot isostatic pressing treatment on the sintered material;
and S6, cooling and releasing the pressure to obtain the hot isostatic pressing densified product.
Step S3 is: vacuumizing and washing the furnace, introducing a small amount of carrier gas, opening a degreasing system, heating, and degreasing for 2-5h at the temperature of 300-.
Step S4 is: and closing the carrier gas and the degreasing system, keeping the pressure-bearing container in vacuum, then heating to the sintering temperature of 500-1300 ℃, and preserving the heat for 1-2 h.
Step S5 is: filling high-pressure gas into the pressure-bearing container, and keeping the pressure-bearing container for 1-2h under the conditions of 100-200MPa and 450-1200 ℃.
Compared with the prior art, the invention can at least realize one of the following technical effects:
1) compared with the prior art, the device integrates the degreasing, vacuum sintering and hot isostatic pressing post-treatment devices of the formed green body, can complete the three-step process by using one set of equipment, improves the utilization rate of the equipment, saves the space occupied by the equipment, reduces the purchase cost of the equipment, and has very high popularization and application prospects.
2) Compared with the existing non-sheath hot isostatic pressing process, the production process of the densified product adopting the device of the invention omits the processes of transferring the space of the formed blank in different stages of degreasing, sintering and hot isostatic pressing, the formed blank does not need to transfer the space, thus the processes of cooling before transferring the space and reheating after transferring the space are omitted, the repeated heating of the formed blank in different processes is avoided, the time of the formed blank in a high-temperature stage is shortened, the growth trend of crystal grains can be weakened, the fine-grained product can be obtained, and the performance of the product is improved.
3) In the prior art, after each process is finished, the temperature needs to be reduced, then the device is transferred, and then the temperature is increased again to the temperature needed by the process for subsequent treatment, so that the post-treatment time is greatly prolonged. The device for degreasing, vacuum sintering and hot isostatic pressing post-treatment is integrated, all processes can be finished in a pressure-bearing container without transferring the device or cooling and then heating again, the time of the post-treatment process of the formed green body is shortened, the production efficiency is improved, and the process cost is reduced.
4) The device and the method of the invention carry out degreasing, vacuum sintering and hot isostatic pressing treatment, thereby omitting the process of transferring the intermediate forming blank body, avoiding the oxidation possibly generated in the material transferring process and improving the product quality.
5) The binder collector of the device is provided with the multi-stage collecting device, so that the binder in carrier gas flowing out of the pressure bearing container in the degreasing process can be efficiently collected, and the binder is prevented from entering the vacuum pump set to damage a vacuum pump or reduce the degreasing efficiency of the vacuum pump set.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims thereof.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, wherein like reference numerals are used to designate like parts throughout.
FIG. 1 is a schematic view of the structure of a hot isostatic pressing apparatus according to example 1;
FIG. 2 is a schematic view of an adhesive collector configuration;
FIG. 3 is a schematic view of a first condenser tube configuration;
fig. 4 is a schematic diagram illustrating the structure positions of the first condensation pipe and the second condensation pipe.
Reference numerals:
1-a material to be sintered, 2-a material boat, 3-a heat insulation base, 4-a heating body, 5-a heat insulation screen, 6-a cylinder, 7-a lower plug, 8-an upper plug, 9-a power-on electrode, 10-a carrier gas, 11-a binder collector and 12-a mechanical pump set; 13-a first collecting device; 1301-a first condensation pipe; 1302-a second condenser tube; 1303-adhesive collecting box; 1304-a straight tube portion; 1305-bending the tube part; 1306-an air intake line; 1307 air outlet pipeline; 14-a second collecting device; 1401-a third condenser tube; 1402-a condensate inlet; 1403-condensate outlet; 15-a first filter; 16-a second filter; 17-pressure relief valve, 18-closing valve.
Detailed Description
The hot isostatic pressing apparatus and method with degreasing-vacuum sintering function will be described in further detail with reference to specific examples, which are provided for comparison and explanation purposes only, and the present invention is not limited to these examples.
Example 1
A hot isostatic pressing device with degreasing-vacuum sintering function, as shown in figure 1, mainly comprises a degreasing system, a pressure-bearing container and a heating heat-insulating device, wherein the degreasing system comprises a mechanical pump unit 12 and a binder collector 11, and the binder collector 11 is connected with the mechanical pump unit 12 through a pipeline; the binder collector 11 is connected with the pressure-bearing container, and the carrier gas degreasing function is realized at the medium-low temperature stage. The pressure-bearing container comprises a cylinder body 6, a lower plug 7 and an upper plug 8, wherein the cylinder body 6 is in a cylindrical shape with two open ends, and the two ends are respectively sealed by the upper plug 8 and the lower plug 7.
The heating system comprises an electric leading electrode 9 and a heating body 4, the electric leading electrode 9 is connected with an external power supply, the external power supply is connected with the heating body 4 by the electric leading electrode 9, and the heating body 4 generates heat through resistance heating after being electrified so as to heat the equipment.
The heat insulation system comprises a heat insulation base 3 and a heat insulation screen 5, wherein the heat insulation base 3 and the heat insulation screen 5 wrap the heating system to prevent heat from diffusing. 2 is a material boat, 1 is a material to be burnt, 9 is an electric leading electrode, and 10 is a carrier gas. In order to heat the material 1 to be sintered uniformly, the heating body 4 is set to be cylindrical and wraps the material 1 to be sintered; further, a bottom heating unit is arranged on the hot base 3, so that the sintering material 1 is uniformly heated in all directions.
Compared with the prior art, the device integrates the degreasing, vacuum sintering and hot isostatic pressing post-treatment devices of the formed green body, can complete the three-step process by using one set of equipment, improves the utilization rate of the equipment, saves the space occupied by the equipment, reduces the purchase cost of the equipment, and has very high popularization and application prospects.
In order to improve degreasing efficiency during binder removal and fill high-pressure gas into the pressure-bearing container in the hot isostatic pressing stage, the lower plug 7 and the heat insulation base 3 are provided with a carrier gas inlet and a carrier gas outlet. Because the temperature in the pressure-bearing container is higher and the temperature of external carrier gas is very low, the carrier gas 10 is directly introduced, and the carrier gas 10 can reduce the temperature in the pressure-bearing container, so that the temperature is unstable, and the performance of the material to be burnt is influenced. In order to prevent the above situation, in this embodiment, the carrier gas inlet is disposed between the heating element 4 and the material boat 2, after the carrier gas is introduced, the carrier gas 10 is heated in the channel formed by the heating element 4 and the material boat 2, and the temperature of the carrier gas 10 is raised and then contacts the material 1 to be sintered in the material boat 2, so that the temperature of the material 1 to be sintered is not greatly affected.
Considering that the carrier gas 10 may be pumped out directly through the carrier gas outlet after flowing from the top after being filled into the pressure-bearing container from the carrier gas inlet, so as to reduce the degreasing efficiency, a fan is arranged on the top of the heat shield 5 to blow the carrier gas into the material boat 2, and the adhesive is taken away through the flowing of the carrier gas 10, so that the degreasing efficiency is improved.
The existing degreasing device easily causes the problem that carrier gas cannot be degreased completely, so that lipid substances such as binders enter the mechanical pump unit 12 along with the carrier gas to pollute the vacuum pump, further the vacuumizing effect and the service life of the vacuum pump are influenced, the degreasing efficiency is reduced, and vicious circle is caused.
In order to prevent the adhesive from entering the mechanical pump unit 12 during degreasing, the adhesive collector 11 of the present embodiment is shown in fig. 2 to 4, and the adhesive collector 11 includes a first collecting means 13 and a second collecting means 14.
The first collecting device 13 comprises a first condensation pipe 1301 and a second condensation pipe 1302, as shown in fig. 3 and 4, the first condensation pipe 1301 and the second condensation pipe 1302 are both arranged in a serpentine shape, that is, a plurality of S-shaped connected structures, each of the first condensation pipe 1301 and the second condensation pipe 1302 comprises a straight pipe portion 1304 and a bent pipe portion 1305, the pipe diameters of the straight pipe portion 1304 and the bent pipe portion 1305 are the same, the pipe diameters of the first condensation pipe 1301 and the second condensation pipe 1302 are the same, and the distance d between two adjacent straight pipes is equal to the pipe diameter; the second condensation pipe 1302 is arranged above the first condensation pipe 1301, the second condensation pipe 1302 and the first condensation pipe 1301 are arranged in a staggered mode, and a straight pipe of the second condensation pipe 1302 is arranged in a vacant area between two straight pipes of the first condensation pipe 1301. All the gas entering the first collecting device 13 can be cooled by the condensation pipe.
The first collection device 13 further comprises an inlet duct 1306 and an outlet duct 1307, the inlet duct 1306 being arranged at the lower end of the first collection device 13 to enable the incoming carrier gas to pass through the first condensation duct 1301 and the second condensation duct 1302; the air inlet pipeline 1306 is provided with a closing valve 18, the pressure-bearing container is still in a vacuum state after degreasing is finished, vacuum sintering is needed subsequently, in order to prevent the binder in the binder collector 11 from reversely entering the pressure-bearing container, and the closing valve 18 is closed after degreasing is finished. The outlet duct 1307 is arranged above the first collecting device 13 and is connected with the second collecting device 14.
The first collecting device 13 further comprises an adhesive collecting box 1303, and the adhesive collecting box 1303 is arranged at the bottom end of the first collecting device 13 and is used for collecting the adhesive which is solidified and falls after cooling. The air intake pipe 1306 is disposed below the first condensation duct 1301 and above the adhesive collecting box 1303. An outlet is provided at a position corresponding to the adhesive collecting case 1303 for replacement of the adhesive collecting case 1303.
Still be the negative pressure in the binder collector 11 after the degrease finishes, in order to facilitate the clearance of binder collector 11 and the change of binder collection box 1303, set up relief valve 17 on first collection device 13, relief valve 17 sets up the upper end at first collection device 13, the top of second condenser pipe 1302 promptly, the carrier gas of second condenser pipe 1302 top has passed through the cooling of first condenser pipe 1301 and second condenser pipe 1302, the binder is mostly detached, prevent the binder shutoff relief valve 17 in the carrier gas, cause unable pressure release.
The second collecting device 14 comprises a third condensation pipe 1401, a condensate inlet 1402 and a condensate outlet 1403, the third condensation pipe 1401 is connected with an air outlet pipeline 1307, the third condensation pipe 1401 rises spirally in the second collecting device 14, the contact time of the carrier gas and the condensate is prolonged, and the carrier gas is further cooled to remove the adhesive. The condensate inlet 1402 is provided at the second collection device 14 and the condensate outlet 143 is provided at the upper end of the second collection device 14. The adhesive in the carrier gas entering the second collecting device 14 is cooled and condensed, then slides downwards in the third condensation pipe 1401, enters the first collecting device 13 along the air outlet pipeline 1307, and finally enters the adhesive collecting box 1303.
To further remove the binder in the carrier gas, a filter, preferably a first filter 15 and a second filter 16 arranged in series, is provided between the second collection device 14 and the mechanical pump group 12, carrying out a secondary filtration of the carrier gas.
In another preferred mode of this embodiment, the first filter 15 and the second filter 16 are disposed in parallel, and a valve is disposed at each of two ends of the first filter 15 and the second filter 16, one of the filters is used during degreasing, when the filter is blocked and needs to be replaced, the valve of the other filter is directly opened, and then the valves at two ends of the blocked filter are closed, so that the filter can be replaced without shutdown, the operation is convenient, and the time is saved.
When the binder collector 11 needs to be cleaned, hot fluid may be introduced into the first condensation pipe 1301, the second condensation pipe 1302, and the second collection device 14 to heat the first collection device 13 and the second collection device 14, so that the binder melts and automatically falls off, and then flows into the binder collection box 1303. When the pressure release valve 17 is blocked, the adhesive blocking the pressure release valve 17 can be peeled off by heating, so that the pressure release valve 17 is smooth.
The degreasing system of the device can greatly improve the binder removal efficiency, and the binder collection device is combined with the filter to remove the binder in the carrier gas, so that the binder is prevented from entering the vacuum pump unit, the service life of the vacuum pump unit is prolonged, and the degreasing efficiency is improved. The existing degreasing system cannot completely remove the binder, so that the binder enters a vacuum pump set, the working efficiency of the vacuum pump is reduced, and the service life of the vacuum pump is prolonged.
Example 2
The invention also provides a use method of the hot isostatic pressing device with the degreasing-vacuum sintering function, which comprises the following steps:
s1, preparing a material to be burnt 1;
s2, placing the material 1 to be burnt in the material boat 2, placing the material on the heat insulation base 3, and closing the upper plug 8;
s3, after vacuumizing and washing the furnace, starting a mechanical pump set of a degreasing system to work under the condition of introducing a small amount of carrier gas, then heating, degreasing for 2-5h at the temperature of 600 ℃ at 300-;
the specific operation of vacuumizing and washing the furnace comprises vacuumizing to remove air, filling inert gas, vacuumizing, and washing the furnace repeatedly; introducing a small amount of carrier gas to maintain micro-positive pressure in the pressure-bearing container, wherein the carrier gas flow is 30-50mbar for example;
s4, after degreasing, closing the carrier gas and the degreasing system, keeping vacuum in the pressure-bearing container, then heating to the sintering temperature of 450-1300 ℃, and preserving heat for 1-2 h;
s5, after the vacuum sintering is finished, filling high-pressure gas into the pressure-bearing container, and further densifying under the conditions of 200MPa for 100 and 1200 ℃ for 1-2 h;
and S6, cooling and releasing the pressure to obtain the hot isostatic pressing densified product.
The device integrating degreasing, vacuum sintering and hot isostatic pressing post-treatment is adopted, the process that the material to be sintered is transferred to the space at different stages of degreasing, sintering and hot isostatic pressing is omitted, the formed blank does not need to be transferred to the space, the process that the material needs to be cooled before being transferred to the space and then is reheated after being transferred to the space is omitted, in the embodiment, the degreasing is carried out at the temperature of 600 ℃ plus 300 ℃, the sintering temperature is 1300 ℃ plus 450 ℃, the hot isostatic pressing is carried out at the temperature of 1200 ℃ plus 500 ℃, the temperature requirement can be met by carrying out a small amount of temperature adjustment, the repeated heating when the formed blank is carried out by different processes is avoided, the time of the formed blank at the high-temperature stage is shortened, the growth trend of crystal grains can be weakened, the fine-.
Example 3
Injection molded 316L stainless steel degreasing-vacuum sintering-hot isostatic compaction
(1) Preparing a 316L stainless steel blank by using an injection molding process;
(2) placing the injection-molded 316L stainless steel blank body in a material boat, placing the material boat on a heat insulation base, and closing an upper plug;
(3) after vacuumizing and washing the furnace, starting a mechanical pump set of a degreasing system to work under the condition of introducing a small amount of carrier gas, and then degreasing for 5 hours under the condition of heating to 500 ℃;
(4) after degreasing, closing the carrier gas and the degreasing system, keeping vacuum in the pressure-bearing container, then heating to the sintering temperature of 1200 ℃, and preserving heat for 1 h;
(5) after the vacuum sintering is finished, filling high-pressure gas into the pressure-bearing container, and further densifying under the conditions of 200MPa and 1200 ℃ for 1 h;
(6) and cooling and releasing the pressure to obtain a hot isostatic pressing densified 316L stainless steel product.
In the prior art, after each process is finished, the temperature needs to be reduced, then the device is transferred, and then the temperature is increased again to the temperature needed by the process for subsequent treatment, so that the post-treatment time is greatly prolonged. The device for degreasing, vacuum sintering and hot isostatic pressing post-treatment is integrated, all processes can be completed in a pressure-bearing container, a device does not need to be transferred, and the temperature does not need to be reduced and then raised again. In the embodiment, the degreasing temperature is 500 ℃, the temperature can reach 1200 ℃ of vacuum sintering after being heated, the temperature does not need to be changed, the next hot isostatic pressing treatment can be carried out only by filling high-pressure gas, the time of the post-treatment process of the formed green body is greatly shortened, the production efficiency is improved, and the process cost is reduced. The process of transferring the intermediate forming blank into the space is omitted, the oxidation which may be generated in the material transferring process is avoided, and the product quality is improved.
Example 4
Degreasing-vacuum sintering-hot isostatic pressing densification of press-formed 2024 aluminum alloy
(1) Preparing a 2024 aluminum alloy blank by using a press forming process;
(2) placing the 2024 aluminum alloy blank formed by pressing in a material boat, placing on a heat insulation base, and closing the upper plug;
(3) after vacuumizing and washing the furnace, starting a mechanical pump set of a degreasing system to work under the condition of introducing a small amount of carrier gas, and then degreasing for 2 hours under the condition of heating to 300 ℃;
(4) after degreasing, closing the carrier gas and the degreasing system, keeping vacuum in the pressure-bearing container, then heating to the sintering temperature of 500 ℃, and preserving heat for 2 hours;
(5) after the vacuum sintering is finished, filling high-pressure gas into the pressure-bearing container, and further densifying under the conditions of 100MPa and 450 ℃ for 2 h;
(6) and cooling and releasing the pressure to obtain the hot isostatic pressing densified 2024 aluminum alloy product.
The method saves the processes of transferring the space of the material to be sintered at different stages of degreasing, sintering and hot isostatic pressing, the formed green body does not need to transfer the space, the processes of cooling before transferring the space and reheating after transferring the space are also saved, the repeated heating of the formed green body during different processes is avoided, the time of the formed green body at the high-temperature stage is shortened, the growth trend of crystal grains can be weakened, the fine-grained product can be obtained, and the performance of the product is improved.
Example 5
Degreasing-vacuum sintering-hot isostatic pressing densification of gel film-injection forming FGH95 high-temperature alloy
(1) Preparing an FGH95 high-temperature alloy blank by using a gel film-injection forming process;
(2) placing the FGH95 high-temperature alloy blank in a material boat, placing the material boat on a heat insulation base, and closing an upper plug;
(3) after vacuumizing and washing the furnace, starting a mechanical pump set of a degreasing system to work under the condition of introducing a small amount of carrier gas, and then degreasing for 5 hours under the condition of heating to 600 ℃;
(4) after degreasing, closing the carrier gas and the degreasing system, keeping vacuum in the pressure-bearing container, then heating to the sintering temperature of 1300 ℃, and preserving heat for 1.5 h;
(5) after the vacuum sintering is finished, filling high-pressure gas into the pressure-bearing container, and further densifying under the conditions of 200MPa and 1200 ℃ for 1.5 h;
(6) cooling and releasing the pressure to obtain the hot isostatic pressing densified FGH95 high-temperature alloy product.
Compared with the existing non-sheath hot isostatic pressing process, the degreasing-vacuum sintering-hot isostatic pressing method of the device avoids repeated heating of the formed blank in different processes, reduces the time of the formed blank in a high-temperature stage, can weaken the growth trend of crystal grains, is beneficial to obtaining fine-grained products and improves the performance of the products.
In the prior art, after each process is finished, the temperature needs to be reduced, then the device is transferred, and then the temperature is increased again to the temperature needed by the process for subsequent treatment, so that the post-treatment time is greatly prolonged. The device and the method of the invention shorten the time of the post-treatment process of the formed blank, improve the production efficiency and reduce the process cost. The invention omits the process of the transfer space of the intermediate forming blank, avoids the oxidation possibly generated in the material transfer process and improves the product quality.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (10)

1. A hot isostatic pressing device is characterized by comprising a degreasing system, a pressure-bearing container and a heating unit; the pressure-bearing container is used for placing a material (1) to be sintered, the degreasing system is used for degreasing the sintering material (1), and the heating unit is arranged in the pressure-bearing container and used for heating the material to be sintered;
the degreasing system comprises a binder collector (11) and a mechanical pump set (12); the binder collector (11) is connected with a mechanical pump set (12) through a pipeline; the binder collector (11) is connected with the pressure-bearing container.
2. The hot isostatic pressing arrangement according to claim 1, wherein the pressure-containing vessel comprises a barrel (6), a lower plug (7) and an upper plug (8), the barrel (6) being cylindrical in shape with open ends, the barrel (6) being sealed at both ends with the upper plug (8) and the lower plug (7), respectively.
3. The hot isostatic pressing arrangement according to claim 1, wherein the heating unit comprises an electric lead electrode (9) and a heat generating body (4), the electric lead electrode (9) being connected to an external power supply, the heat generating body (4) being adapted to generate heat.
4. The hot isostatic pressing device according to claim 3, further comprising a heat insulation device, wherein the heat insulation device comprises a heat insulation base (3) and a heat shield (5), and the heat insulation base (3) and the heat shield (5) enclose the heating body (4) and the material (1) to be sintered and prevent heat from diffusing.
5. The hot isostatic pressing arrangement according to claim 1, wherein the binder collector (11) comprises a first collector arrangement (13) and a second collector arrangement (14), the second collector arrangement (14) being a next-stage treatment unit of the first collector arrangement (13).
6. The hot isostatic pressing arrangement according to any one of claims 1-5, further comprising a boat (2) for holding the material (1) to be sintered.
7. A process for the production of a densified product, characterized in that a hot isostatic pressing device according to claims 1-6 is used, comprising the steps of:
s1, preparing a material (1) to be sintered;
s2, placing the material (1) to be sintered in the material boat (2), placing the material boat on the heat insulation base (3), and closing the upper plug (8);
s3, degreasing the material (1) to be sintered;
s4, sintering the material (1) to be sintered;
s5, carrying out hot isostatic pressing treatment on the sintered material;
and S6, cooling and releasing the pressure to obtain the hot isostatic pressing densified product.
8. The process for producing a densified product according to claim 7, wherein the step S3 is: vacuumizing and washing the furnace, introducing a small amount of carrier gas, opening a degreasing system, heating, and degreasing for 2-5h at the temperature of 300-.
9. The process for producing a densified product according to claim 7, wherein the step S4 is: and closing the carrier gas and the degreasing system, keeping the pressure-bearing container in vacuum, then heating to the sintering temperature of 500-1300 ℃, and preserving the heat for 1-2 h.
10. Process for the production of a densified product according to any one of claims 7 to 9, wherein step S5 is: filling high-pressure gas into the pressure-bearing container, and keeping the pressure-bearing container for 1-2h under the conditions of 100-200MPa and 450-1200 ℃.
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CN113198797A (en) * 2021-05-21 2021-08-03 萍乡市方兴石化填料有限公司 Regular packing degreasing equipment

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