JPH02294407A - Hot isostatic pressing method - Google Patents

Abstract

PURPOSE:To manufacture a high density sintered product with good product yield by directing a valve box for vacuum sealing downward after packing raw material powder in a capsule under vacuum, fitting this to a supporting tool having heat insulating material and sintering at thigh temp and high pressure at the time of sintering metal powder, etc., with a hot isostatic pressing apparatus. CONSTITUTION:The treating material 4 of metal powder, etc., is charged into the cylindrical capsule 1 made of mild steel, etc., and on this, difficult-to-sintering ceramic powder 5 of BN, etc., and a net-like filter 6 made of stainless steel are set. To opening end at upper part thereof, the cylindrical valve box 7 is fitted and the inner part in the capsule is evacuated and sealed. Bundle 19 of the capsules 1 is charged into a high pressure vessel 13 with directing the valve box 20 downward, and the valve box part at the lower part of the bundle is stably fixed to the supporting tool 21 including the heat insulating material 22. High pressure gas is introduced from a gas introducing hole 14 in an upper cover 15 of the high pressure vessel 13 and also heated with heaters 18a, 18b, and the capsule bundle 19 is pressurized at high temp. and high pressure to sinter the treating material 4 in the capsule 1 and the high density sintered product is manufactured with good yield.

Description

Detailed Description of the Invention (Industrial Application Field) The present invention applies high gas pressure at high temperatures to sinter processed materials such as metal or ceramic powder or bolus compacts to a high density. This is related to the so-called hot isostatic pressing method (HIP method) used for bonding.More specifically, the above-mentioned treated materials are placed in a gas-impermeable capsule such as metal or glass. After vacuum sealing, HIP
This is related to the so-called capsule HIP method. [Prior Art] First, an overview of the HIP device will be explained. Figure 8 shows
It is a conceptual diagram showing the structure of a complete HIP device. The figure has a high pressure container (49) and a high pressure gas passage (50),
Top to seal the upper opening of the high pressure container (49)! (51)
and the lower It(
Heat insulation 15 (53) is installed in the high pressure chamber formed by
), except for its lower part, and is surrounded by a lower lid (52).
The processing body (55) and the heat insulation ji (53
), an upper heater (54a) and a lower heater (54
b) shows a HIP device with Processing body (55)
is placed under a high pressure of approximately several thousand κgf/d by high pressure medium gas guided through the high pressure gas passage (50), and the upper heater (54a) and lower heater (54
It is heated by b) and placed at a high temperature of several thousand degrees Celsius.

Here, a gas such as argon or nitrogen is used as the pressure medium for the HIP process. Characteristics of these gases include that they are fluids with low thermal conductivity and low viscosity coefficients even under high temperature and high pressure, and that they have extremely large density differences depending on temperature. For this reason, when high-pressure gas is heated in the high-pressure chamber of a HIP device, intense natural convection occurs due to the temperature difference, and high-temperature gas tends to accumulate in the upper part of the high-pressure chamber, and the heat accumulated in the upper part flows to the lower part of the high-pressure chamber. Because it is difficult to decompose, it tends to create a vertical temperature distribution in a high-pressure chamber, with high temperatures at the top and low temperatures at the bottom. If such a temperature distribution occurs, the HIP processing conditions will be different between the upper and lower parts of the high-pressure chamber, making it impossible to maintain product uniformity. Various inventions have been made to reduce such temperature distribution. For example, Japanese Patent Application Laid-Open No. 63-1999 proposed a method of dividing the heater into upper and lower parts and controlling the heating by both heaters independently to maintain a uniform temperature in the high-pressure chamber.
Although disclosed in Japanese Patent No. 197876, the temperature near the bottom of the high-pressure chamber of the HIP device is currently too low to use. Next, the processing body used in the }IIP process will be explained using FIG. 9. FIG. 9 is a sectional view of the processing body disclosed in Japanese Patent Publication No. 52-26482. First, to explain the configuration of each part in Fig. 9, the capsule has a cylindrical capsule body (56).
and a welded part (60) at the lower opening of the capsule body (56).
) welded bottom (57) and capsule body (56)
It consists of a lid part (58) with a hole in the center, which is welded to the upper opening part of the lid part (59) with a weld part (59), and the treated material (
6l). In addition, the capsule has a through hole (63
) and has a threaded outer periphery.
2) is fixed to the lid (58), and the through hole (63) of the degassing pipe (62) is formed by the hole in the center of the lid (58).
It communicates with the inside of the capsule. At the top of the deaeration pipe (62), a bottomed cylindrical connection unit (64) for connecting the inside of the capsule and a vacuum bomb (not shown) is installed, with a washer (66) in between, and the opening of the connection unit (64). The connection unit (64) is placed facing the through hole (63) of the deaeration pipe (62), and the connection unit (64) is connected to the deaeration pipe (6) by a nut (65).
2) is connected. In addition, the connection unit l- (64
) is provided with a connecting pipe (67), and the opening of the connecting unit (64) communicates with the outside through the connecting pipe (67). The connection unit (64) is communicated with the vacuum pump via this connection pipe (67). In addition, at the top of the connection unit (64),
A cylinder (68) having a piston (69) inside is installed, and the tip of the rod of the piston (69) passes through a hole provided in the upper part of the connection unit (64). ) and the degassing pipe (62). A holder (70) made of a magnet or the like is attached to the tip of the rod of this piston {69}, and a degassing pipe (6
The sealing valve (7l) that fits into the through hole (63) of 2) is suspended by magnetic force, and the sealing valve (7l) is attached to the holder (70
) can be attached and detached at will. Next, to explain the operation of each part in FIG. ) to Nantes (65
) is connected to the degassing pipe (62) via the washer (66), and then a vacuum pump is connected to the connecting pipe (67). Thereby, the vacuum pump is communicated with the inside of the capsule via the connecting pipe (67), the connecting unit (64), and the through hole (63) of the degassing pipe (62). Further, at this time, airtightness is maintained during evacuation by the washer (66) and the sealing means in the upper hole of the connection unit (64). In this state, the vacuum bomb is activated to evacuate the inside of the capsule. After the evacuation is completed, the cylinder (68) is operated to push the piston (69) downward, and the sealing valve (71) is inserted into the through hole (63) of the degassing pipe (62).
) and vacuum seal the processing material (6 liters) inside the capsule. After sealing, the magnetic force of the magnet of the holder (70) is cut off to separate the sealing valve (7l) from the piston (69), and the nut (65) is loosened to remove the connection unit (64).
from the degassing pipe (62). At this time, the capsule is filled with the processing material (6 liters) and its opening is sealed with a sealing valve (7 liters) (in this way, the processing material is vacuum sealed inside the capsule). The capsule in the state of
(hereinafter referred to as the treated body, including the sealing part). In addition, the special public
Although it is not explicitly stated in Publication No. 2-26482, as described later, the metal-to-metal seal of the sealing valve (71) is insufficient as a sealing means, so the connection unit (64) is connected from the degassing pipe (62). After removal, the sealing valve (71) and degassing pipe (62) are generally welded together. After this,
The processing body is placed in the HIP device with the sealing valve portion facing upward, and HIP processing is performed. A conventional example of performing HIP processing by placing the processing body inside the HIP device with the sealing valve portion facing down, taking advantage of the fact that the lower part of the HIP device is relatively low temperature, is as shown in Fig. 10. There are known methods. Figure lθ is the Tokko Kosho 5
7-31550 is a cross-sectional view showing an example disclosed in Publication No. 7-31550. In this episode, we will introduce the high pressure container (80) and the high pressure gas passage (8l).
), and has an upper lid (82) that seals the upper opening of the high-pressure container (80), and a nozzle that penetrates the lower lid (83),
A lower lid (83) that seals the lower opening of the high-pressure container (80)
In the high pressure chamber formed by The capsule (84) containing the treatment material (87) is inserted into the lower lid (
83) with the tip of the vent pipe (88) exposed outside the high-pressure chamber through the nozzle of the vent pipe (88), and a safety valve (89) attached to the tip of the vent pipe (88).

The processing material (87) is placed under a high pressure of approximately several thousand kgf/c by a high pressure medium gas guided through a high pressure gas passage (8l), and is heated by a heater (86) to a temperature of approximately several thousand degrees Celsius. The HIP process is performed under high temperature conditions. The purpose of this conventional invention is to remove the physically adsorbed gas and chemically adsorbed gas generated from the processing material (87) from the vent pipe (88) during heating, thereby encapsulating the processing material, which is normally done separately. The process of enclosing and HIP
The purpose is to perform the processing steps continuously. Here, the reason why the ventilation pipe (88) is placed in the low temperature section at the bottom of the HIP device is as follows.
This is because it is relatively easy to seal the nozzle portion of the lower m (83) because it is sufficient to seal the relatively low temperature pressure medium gas.

[Problem to be solved by the invention] As mentioned above, inside the HIP device, there is a temperature difference between high temperature at the top and low temperature at the bottom, so the area near the bottom of the high pressure chamber was just a wasted space. ．． In addition, as a method of encapsulating the processed material in capsules,
The prior art shown in FIG. 9 and summarized in Japanese Patent No. 2-26482 has the following problems with the seal. In other words, in this prior art, the deaeration pipe (62) and the connection unit (64) must be removably sealed, so a washer (66) is used to seal them. There was a problem with that. In addition, the sealing valve (
The seal between 71) and the degassing pipe (62) is also achieved by simply fitting the sealing valve (71) into the degassing pipe (62), and the seal is not reliable. In order to increase the reliability of the seal, it is necessary to use an O-ring or adhesive as a sealing member, or to weld the sealing valve (7l) and degassing pipe (62). Sealing materials such as adhesives (especially resin-based O-rings and resin-based adhesion rules often used in -71) are thermally decomposed by the high temperature during HIP processing, so they cannot be used in HIP processing capsules. There wasn't. Furthermore, in the past, since the sealing valve part remained in the form of a protrusion on the processing body, the processing body had to be placed in the high-pressure chamber of the HIP device with the sealing valve part facing upward to maintain the processing body in a stable state. could not. As a result of this, HI
The sealing valve part was placed in a higher temperature area above the high-pressure chamber of the P device, making it more difficult to apply resin-based O-rings and resin-based adhesives. For this reason, welding has traditionally been used as a sealing means, but in addition to the problem that it is not easy to weld the sealing part of the sealing valve (7l), depending on the material being treated, welding There was also the problem that the specified properties could not be obtained due to the influence of the sealing valve, and the problem that the sealing valve part could not be reused if welding was used. In particular, the sealing valve part requires precision machining as described above, and making it disposable is problematic from the economic standpoint of IP processing.

As a conventional example of holding a processing object upside down in a HIP apparatus in order to utilize the low temperature section at the lower part of the HIP apparatus, there is a method described in Japanese Patent Publication No. 57-31550. FIG. 10 is a sectional view of a HIP device showing this conventional example. This conventional example is not based on the idea of performing HIP processing on the processing material housed in a sealed capsule, but instead actively communicates the inside of the capsule with the outside of the HIP device.
The purpose is to discharge or replace gas during P processing, and therefore it is necessary to lead one end of the capsule out of the system by passing through the lower lid. Furthermore, rather than performing HIP processing using a sealed capsule, the condition inside the capsule is adjusted using a valve outside the system, which is a fundamentally different idea. Therefore, this conventional technique has the following problems.

In other words, the inside of the HIP equipment high pressure chamber is several thousand Kgf/c+
1, while the pressure outside the HIP device is atmospheric pressure.
There is an extremely large pressure difference between the two.

For this reason, a thin-walled ventilation pipe (
Not only is it difficult to select the material for the vent pipe (
88) deforms due to pressure difference, it is difficult to ensure airtightness between the nozzle of the lower cover (83) of the HIP device and the ventilation pipe (88), and leakage of pressure medium gas is likely to occur, resulting in safety and workability. There was a problem with this.

In view of the problems of the prior art, the present invention provides an economical solution that enables reliable sealing using a sealing member when vacuum sealing a processing material in a capsule and during IIP processing, and allows reuse of the sealing valve part. The purpose is to provide a standard HIP processing method. [Means for Solving the Problems] The present invention has been made to solve the above-mentioned problems of the prior art. After filling the treatment material and vacuum degassing through the opening, and then sealing the opening to produce a treatment body, the treatment body is subjected to a hot isostatic pressurization device with the sealed portion facing down. The hot isostatic pressing process is carried out in a state in which the sealed part is supported by a supporting member having a heat insulating material provided in the lower low temperature part of the hot isostatic pressing apparatus. Further, the feature of the invention described in claim 2 is that after filling the processing material into a capsule having an open end, the capsule has a cylindrical shape with a communicating hole in which one end is inside the capsule and the other end is open to the atmosphere. A valve seat portion is formed in a part of the communication hole, and
A valve box is provided on the opposite side of the capsule from the valve seat portion and has a deaeration hole that communicates the above-mentioned through hole with an external vacuum pump, and a valve box that moves forward and backward into the communication hole through the atmosphere side opening of the valve box. an on-off valve that is freely fitted and whose tip has a shape corresponding to the valve seat, and a first sealing member between the atmospheric opening of the communication hole of the valve box and the on-off valve; Further, a second sealing member is attached to the valve seat portion and/or the tip of the on-off valve, respectively, and the tip of the valve box on the side opposite to the on-off valve is sealed to the capsule opening via the third sealing member. mated,
After the inside of the capsule is evacuated with a vacuum pump connected to the degassing hole while maintaining a gap between the tip of the on-off valve and the valve seat, the on-off valve is advanced to hit the valve seat. After making a treatment body by sealing the communicating hole with the second sealing member, the body is subjected to hot isostatic pressurization with the valve box portion facing down, and hot isostatic pressurization is performed. The hot isostatic pressurization process is carried out in a state in which the valve box portion is supported while being bent by a support having a heat insulating material provided in the lower low temperature part of the apparatus.

[Effect]

In the invention described in claim 1, after filling the treatment material,
The completed vacuum-sealed processing body is placed in the H
The IP device is supported by a support placed at the bottom of the high-pressure chamber. Therefore, even though the valve box part has an on-off valve, deaeration hole, etc. and has a complicated shape, it cannot be placed stably in the high-pressure chamber of the HIP device even with the sealed part facing down. can.

After this, during HIP processing, the treated body is heated to several thousand degrees Celsius and weighs several thousand kg.
It is placed under high temperature and pressure of f/cj. At this time, the temperature of the sealed part is not only that the lower part of the high pressure chamber of the HIP device is relatively lower than the upper part, but also because it is surrounded by the heat insulating material of the support. The temperature is even lower than the lower part of the high pressure chamber of some HIP devices. Therefore, even at high temperatures during HIP processing, the sealing member does not thermally decompose due to overheating, and the airtightness of the processing body can be maintained.

Furthermore, after the HIP process, the first seal member can be easily removed from the capsule, and since it is not exposed to high temperatures during the HIP process, it will not be thermally deformed and the seal will be sealed. Parts can be reused, and resin-based O-rings and resin-based adhesives can also be used as sealing members. In the invention described in claim 1, first, a processing material such as a metal or ceramic powder or a bolus molded body is filled into a capsule from the opening of the capsule. Next, the valve box is hermetically fitted into the opening of the capsule via the third sealing member. At this time, the third sealing member plays the role of maintaining airtightness between the opening of the capsule and the valve box.

After this, connect the vacuum pump to the deaeration hole in the valve box with the on-off valve open. Thereby, the inside of the capsule is communicated with the vacuum pump through the deaeration hole and the communication hole. In this state, operate the vacuum pump to evacuate the inside of the capsule.
At this time, the first sealing member plays a role of maintaining airtightness between the opening to the atmosphere of the communication hole of the valve box and the on-off valve.

After evacuation, the tip of the on-off valve of the valve box is brought into contact with the valve seat of the communication hole, and the communication hole of the valve box is sealed via the second sealing member. By this sealing, the processing material is completely sealed within the capsule, and the processing body is completed.

At this time, the second seal member plays a role of maintaining airtightness between the communication hole in the valve seat portion of the valve box and the on-off valve.

〔Example〕

Embodiments of the present invention will be described using FIGS. 1 to 6.

Figures 2a to 2C and Figure 1 show embodiments of the present invention in the order of steps, and Figure 2a is a sectional view showing an example of the structure of a capsule used in the present invention. ．． In this example, the capsule consists of a cylindrical capsule body (1) made of metal and a disc-shaped bottom plate (2) also made of metal that seals the lower opening of the capsule body (1). Part (1) and bottom plate (2) are welded together at weld part (3). The material for the metal capsule used in the present invention includes mild steel, stainless steel, Mo, platinum, etc., and is selected depending on the reactivity with the processing material and the processing temperature. Figure 2b shows a cylindrical treated material (4) molded into a capsule with an inner diameter slightly smaller than the inner diameter of the capsule body (1).
Next, the top of the treated material (4) is filled with a hard-to-sinter ceramic powder (5) such as BN, a mixture of BN and AI, SiiNa, etc., and then a stainless steel mesh is placed on top of it. FIG. 2 is a cross-sectional view of a capsule loaded with a filter (6) such as the above. Here, the hard-to-sinter ceramic powder (5) is the treated material (4).
), which acts as a spacer between the part that is exposed to high temperatures and the part that is kept at a low temperature around the valve box.
The filter (6) has the role of preventing the difficult-to-sinter ceramic powder (5) and the powder of the processing material (4) from being sucked into the vacuum pump during vacuuming. FIG. 2C is a sectional view of the processing body after vacuum sealing the processing material (4) in the capsule, and FIG. 3 is an enlarged sectional view of the valve box portion when vacuum is drawn. In this example, the valve box (7) has a cylindrical shape in which the outer diameter of the tip part is smaller than that of the main body, and a resin-based zero ring is provided along the outer periphery of the small diameter part. The small diameter tip portion is hermetically fitted to the capsule body (1) via a ring AOω (corresponding to the third sealing member recited in claim 2). Further, the cylindrical valve box (7) has a communication hole D, and the diameter of the communication hole D is smaller in the small diameter portion at the tip than in the main body, and the diameter changes smoothly within the main body. (This part where the diameter changes smoothly is called the valve seat.) Further, the valve box (7) has a deaeration hole (9) as a horizontal hole extending from the outer circumferential direction toward the communication hole D in the larger diameter portion of the main body. At the opening on the opposite side of the capsule of the communication hole D in the main body of the valve box (7), a resin O-ring BOD (as described in claim 2) is provided along the inner circumference of the hole. A bolt-shaped on-off valve (8) having a threaded portion (7a) is screwed in through the first sealing member (corresponding to the first sealing member), and is movable forward and backward. In addition, the tip of the on-off valve (8) is shaped like a truncated cone,
The communication hole D of the valve body (7) is connected via a resin-based O-ring CG3 (corresponding to the second seal member described in claim 2) provided annularly along the outer periphery of the conical part. It engages with the valve seat. Next, the function of each part will be explained in order of process. First, when vacuuming, as shown in Fig. 3, the on-off valve (8) is not screwed in yet, and the deaeration hole (9), the communication hole D of the main body of valve n (73), and the Communication hole D is in communication.
A vacuum pump is connected to this deaeration hole (9), and a vacuum pump is connected to the deaeration hole (9).
The communication hole D is used as a passage to evacuate the inside of the capsule. At this time, the O-ring AOω maintains airtightness between the capsule body (1) and the valve box (7), and the O-ring B01) serves as a communication hole between the on-off valve (8) and the main body of the valve box (7). Maintain airtightness with D. After completing the evacuation, turn the on-off valve (8) to engage the truncated conical portion of the tip with the valve seat via the O-ring CG2+. At this time, the 0 ring CG2> is connected to the on-off valve (8) and the valve box (
7) Maintain airtightness between the capsule and the communication hole D at the tip, and block the passage that communicates the inside of the capsule with the vacuum pump. In this way, the processing material (4) is vacuum sealed inside the capsule. FIG. 1 shows a bundle 09 of a plurality of processing bodies in a H11 device.
This figure shows the state in which the valve body is supported with its end portion facing down. To explain the structure of the HIP device in the same figure, there is a high pressure container 0■, an upper lid 0ω that has a high pressure gas passage (b) and seals the upper opening of the high pressure container 031, and a lower opening of the high pressure container 031. A high pressure chamber is formed by the lower lid Oe which is sealed.
Inside this high-pressure chamber, an inverted cup-shaped heat insulating layer 0 is installed, and an upper heater (18a) and a lower heater (18b) are arranged in upper and lower two stages along the inside of the insulating layer θ'I). It is arranged. On the other hand, on the lower lid 061 is a cylindrical capsule support that has an outward facing flange at the bottom! 211 is installed with the flange facing the lower cover Oe. Further, a heat insulating material (2) is attached to the inner surface of the cylindrical portion of this support QD.

Next, the operation of each part in FIG. 1 will be explained in order of process. First, a bundle 09 of a plurality of processing bodies is set inside the heat insulating material 03 of the support QD with its valve box 121 facing down. At this time, if the heat insulating material (2δ) is molded into almost the same shape as the outer periphery of the bundle 09 of the plurality of processing objects, the bundle 09 of the plurality of processing objects can be supported in a stable state. After supporting the bundle 09 of a plurality of processing bodies in this way, high pressure gas is sent into the high pressure chamber through the high pressure gas passage 0, and the upper heater (18a) and the lower heater (18
b) to bring the inside of the high pressure chamber into a high temperature and high pressure state, and
It performs IP processing.

At this time, the temperature of the valve box 121 is determined by the fact that the lower part of the high pressure chamber is relatively lower than the upper part, and also
? ), so the resin-based sealing material 0
The culm is kept at a low temperature so that the ring is not thermally decomposed by overheating.

FIG. 4 is a cross-sectional view of another embodiment of the capsule of the present invention.

In the figure, the capsule has a cylindrical capsule body Q1.
, a bottom plate 4l that seals the lower opening of the capsule body 12m, and a lid Q9 that seals the upper opening of the capsule body 0.
It consists of In addition, a circular hole is provided in the center of the lid (251).A cylindrical deaeration pipe (2 [9) having an outer diameter slightly smaller than the diameter of this hole is inserted into this hole. ing.

The capsule body 12m, the bottom plate a4l, 1 (c), and the degassing pipe 019 are all made of thin metal plates, and the capsule body I2l and the bottom plate (24i are welded parts), and the capsule body 0 and the lid 4 are made of thin metal plates. is welded part am, and M4 and degassing pipe Q old are welded at welded part Q1, respectively.

After filling the powder processing material (30) into this capsule, the second
As in the embodiment shown in the figure, the valve box (31) is hermetically fitted to the end of the degassing pipe (26), and the processing material (30) is vacuum-sealed into the capsule. This embodiment has an advantage over the embodiment shown in FIG. 2 in that a large amount of processing material can be processed at one time. Here, the material of the resin O-ring used in the sealing member of the present invention is preferably one with high heat resistance such as silicone rubber, fluorine rubber, polytetrafluoroethylene, etc.
As for the heat resistance, it can be used as long as it is between 70''C and 80''C, so NBR etc. may also be used. FIG. 5 shows another embodiment of the capsule of the present invention, and is a sectional view of the capsule when a glass capsule is used. In the same figure, the glass capsule (32) is a circle? The i-shaped body has a hemispherical shell-like lid part as a convex part at both ends, and a cylindrical degassing pipe part (33 ) is formed. A spacer (3
4) Fill the hemisphere with the degassing pipe part (33), and place the body and degassing pipe part (33) in the center.
A spacer (35) having a through hole communicating with the two spacers (34) (35) is provided respectively.
) and the body of the glass capsule (32) is filled with a processing material (36). Further, a cylindrical metal support (37) is arranged along the inner circumference of the deaeration pipe section (33). Further, the degassing pipe part (33) of the glass capsule (32) is filled with a hard-to-sinter ceramic powder (38) and a filter (38a) thereon, and the opening thereof is filled with: The valve box (39) is sealed and fitted. The valve box (39) has an on-off valve (40) as in the example shown in FIG.
, deaeration hole (4l), and resin O-ring B (42)
It has However, in this embodiment, instead of using the resin-based O-ring A and the resin-based O-ring C as the sealing members, a resin-based adhesive is used to seal the parts. That is, an adhesive is applied in advance to the outer periphery of the tip of the valve box (39) and to the truncated conical portion of the tip of the on-off valve (40), and then vacuum sealing is performed. As the resin-based adhesive used in the sealing member of the present invention, eboshiki-based resin is favorable from the viewpoint of handling properties. In the cases of FIGS. 2 and 4 in which metal is used as the capsule material, and in the case of FIG. 5 in which glass is used, the locations to be sealed with sealing members are 0-ring A and 0-ring B in FIG. 3. These are the three locations where O-ring C is installed. O-rings may be used or adhesive may be used in the locations where O-rings A and O-rings C are provided.

However, since it is necessary to move the on-off valve after evacuation, it is necessary to use an O-ring at the location where the O-ring B is provided.

Next, the support inside the HIP processing equipment will be explained using FIGS. 6 and 7. FIG. 6 is a cross-sectional view of another embodiment of a support device for supporting the capsule shown in FIG. 4.
In the figure, the same numbers as in Figure 1 or Figure 4 are:
Since this is the same as in the same figure, the explanation will be omitted. In the figure, a bottomed cylindrical base (43) having a hole at the center of its bottom plate is fixed with its opening facing the upper part of the lower lid 0ω. At the top of the bottom slope of this base (43), there is a cylindrical heat insulating material (
44) is mounted with its through hole communicating with the hole in the base (43). In this example, the lid (25) of the capsule is placed on top of the heat insulating material (44) to support the processing body in a stable state, and the heat insulating material (44) also supports the degassing pipe (25) of the capsule. ) Keep the part beyond the part at a low temperature.

In this example, the insulation material (44) itself is also a support for supporting the capsule. Also, at this time, the valve box (
31) is arranged in the space formed between the base (43) and the lower lid Oe. In this example, the space is used as insulation. It should be noted that the material of the heat insulating material in FIGS. 1 and 6 is preferably alumina brick because it is resistant to cracking due to temperature differences. FIG. 7 is a cross-sectional view of another embodiment of the support device, in which the capsule shown in FIG. 2 is thermally protected by an easily filled insulating material. In this figure, the parts with the same numbers as those in FIG. 1 are the same as in the same figure, so their explanation will be omitted. In the same figure, a cylindrical support (45) having an outwardly facing flange at its lower part is installed on the lower 106J, with the flange facing the lower lid Q61,
A plurality of processing bodies (46) are arranged inside this support (45) with their valve boxes (47) facing downward, and these processing bodies (
The space between the support (46) and the support (45) is filled with an easily filled heat insulating material (48). In this case, use ceramic fiber etc. as the heat insulating material. Further, instead of ceramic fibers, ceramic powder or grains having a particle size of 0.1 to 3 mm may be used. Using a heat insulating material that is easy to fill, as in this embodiment, has the advantage that there is no need to mold the heat insulating material to match the shape of the object as shown in FIG. Next, a specific example will be explained below.
Intermetallic compound powder with i-AI of 1:1 (average particle size approximately 20
0 μm) was filled into a pure titanium capsule (wall thickness 2+*m, length 200 l, outer diameter 22 ms) having the shape shown in Fig. 2a, and then BN was filled as a hard-to-sinter ceramic material. Furthermore, a stainless steel M400 mesh was placed as a filter, a valve box having the same structure as in Figure 2C and having an O-ring made of fluorocarbon rubber was tightly attached, and the valve box was connected to a vacuum pump via a vacuum hose. In this state, the end of the capsule containing the treatment material, about 20 mm, is heated to about 300°C and vacuumed, and the vacuum gauge on the vacuum pump side shows that the degree of vacuum is about 10-2 to
When the temperature reached rr, the sealing valve was closed, the vacuum pump was disconnected, and the processing body was fabricated. After that, the processed body was placed in the HIP device shown in Fig. 1, and heated at 1050°C and 1500 kg.
HIP treatment was performed for one hour at f/c+1. At this time,
The temperature of the valve body was approximately 50°C, which was low enough to prevent the O-ring from being thermally decomposed. After the pressure was reduced and the temperature was lowered, the treated body was removed from the HIP device, and it was confirmed that the O-ring had not been thermally decomposed and that the HIP treatment had been performed properly. Thereafter, the valve box was removed by hand, the titanium capsule was removed using a lathe, and the density of the sintered body was measured, and the result was 3.08 g/cj, which confirmed that the sintered body had been sintered to its true density. Next, a second specific example will be described below. Alumina powder (All603G) was processed by the CIP method at a pressure of 2000 Kgf/c- to a diameter of 15 am and a length of 15 mm.
It was molded into a cylindrical shape of 0en. The relative density of the compact at this time was approximately 58%. This molded body was placed in a mild steel capsule in the form shown in Figure 2b. For the hard-to-sinter ceramic powder used for filling, BN powder is heated to 5000 kgf using the CIP method.
/c- pressure, re-grind, and sieve approximately 50
-1000μ so was used. After this, the first
I{IP processing was performed according to the procedure shown in the figure. HIP processing is 1350°C, 1500Kgf/c
After the HIP treatment, the body was removed from the HIP device and the valve box was removed. After this, the alumina sintered body was taken out from the capsule and its density was measured, and it was found to be 3.98 g/cj, which is almost the true density. (Effects of the Invention) According to the present invention, by arranging the valve box surrounded by a heat insulating material in the lower low-temperature part of the HIP device, a resin-based O-ring which is easy to handle and is commonly used can be used. It is now possible to use resin-based adhesives, etc. as a sealing member, and it is possible to seal reliably and easily when vacuum sealing the processing material in the capsule and during HIP processing.
This can contribute to simplifying the processing process and improving product yield. Furthermore, after the HIP treatment, the valve box part can be easily removed from the capsule, and the valve box part can be easily removed from the capsule. ．． Since it does not deform, the valve box can be reused. From the above, the cost of HIP processing can be significantly reduced and the scope of application of HIP processing technology can be expanded.

[Brief explanation of drawings]

1 to 6 show examples of the present invention, and FIG. 1 is a front cross-sectional view of a HIP device that supports a processing body inside;
Figure 2a is a front sectional view of the capsule, Figure 2b is a front sectional view of the capsule after filling with processing material, Figure 2C is a front sectional view of the processing body after vacuum encapsulation, and Figure 3 is before vacuum encapsulation. 4 is a partially sectional front view showing another embodiment of the capsule, FIG. 5 is a front view showing another embodiment of the capsule, and FIG. 6 is a front view showing another embodiment of the capsule. Front sectional view showing an example of the support device, No. 7
The figures also show a front view showing an example of another support device, the 8th figure is a conceptual diagram showing the structure of a general HIP device, the 9th figure is a front sectional view of a conventional capsule, and the 10th figure is a conventional example. This is the normal cross section shown. (4) One treated material, (7), (To) One valve box, (8) - Opening/closing valve, 0ω - Third resin O-ring A, (l1) - First resin O-ring B, 0 second resin O-ring C, 09 - treated body, RO υ - support, I23 - heat insulating material. Patent Applicant Kobe Steel Co., Ltd. Agent Patent Attorney Shoichi Kanemaru Figure 1 Figure 2 a Figure 2 b Figure 7 Figure 6 Figure 8 b, Figure 9 Figure 10

Claims (2)

[Claims] (1) Fill a processing material into a capsule with an open end, perform vacuum degassing through the opening, then seal the opening to produce a processing body, and then place the processing body with the sealed part facing down. The hot isostatic pressure is applied to a hot isostatic pressurizing device in a state where the sealed portion is bent and supported by a support having a heat insulating material provided in the lower low temperature part of the hot isostatic pressurizing device. A hot isostatic pressing method characterized by pressure treatment. (2) After filling a processing material into a capsule with an open end, the capsule has a cylindrical shape with a communicating hole in which one end is in the capsule and the other end is open to the atmosphere, and a valve seat is provided in a part of the communicating hole. A valve box is formed, and is provided on the side opposite to the capsule from the valve seat part, and is connected to a valve box in which a deaeration hole is formed, which communicates the communication hole with an external vacuum pump, through an atmosphere-side opening of the valve box. an on-off valve that fits into the hole so as to be able to move forward and backward, and whose tip has a shape corresponding to the valve seat; A sealing member and a second sealing member are respectively attached to the valve seat portion and/or the tip of the on-off valve, and a third sealing member is attached to the tip of the valve box on the opposite side of the on-off valve to the capsule opening. After evacuating the inside of the capsule with a vacuum pump connected to the degassing hole while maintaining a gap between the tip of the on-off valve and the valve seat, the on-off valve is closed. Hot isostatic pressurization according to claim 1, characterized in that the treatment body is manufactured by entering the valve seat and making it contact with the valve seat, and sealing the communication hole with the second sealing member. Method.