JPH0544599B2 - - Google Patents
Info
- Publication number
- JPH0544599B2 JPH0544599B2 JP89184973A JP18497389A JPH0544599B2 JP H0544599 B2 JPH0544599 B2 JP H0544599B2 JP 89184973 A JP89184973 A JP 89184973A JP 18497389 A JP18497389 A JP 18497389A JP H0544599 B2 JPH0544599 B2 JP H0544599B2
- Authority
- JP
- Japan
- Prior art keywords
- heating element
- insulating layer
- heat insulating
- heating
- preheating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000010438 heat treatment Methods 0.000 claims description 105
- 239000000463 material Substances 0.000 claims description 16
- 230000003647 oxidation Effects 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- 230000001590 oxidative effect Effects 0.000 claims description 12
- 239000007789 gas Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 description 3
- 239000011224 oxide ceramic Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910000629 Rh alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B30—PRESSES
- B30B—PRESSES IN GENERAL
- B30B11/00—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses
- B30B11/001—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a flexible element, e.g. diaphragm, urged by fluid pressure; Isostatic presses
- B30B11/002—Isostatic press chambers; Press stands therefor
Landscapes
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Description
（産業上の利用分野）
本発明は、酸化雰囲気熱間等方圧加圧装置に係
り、例えば、ZrO2、Al2O3、MgO等のような酸
化物系セラミツクスの被処理物、粉末治金等の被
処理物を、等方圧加圧するのに利用される。
（従来の技術）
従来、HIP装置は、第４図に示すように、高圧
ガスを封入する高圧容器３１と、該容器３１内に
設置された加熱装置３２と、被処理物載置台３３
とから成り、高圧容器３１は上蓋３４と下蓋３５
を備え、加熱装置３２は発熱体３６と電源装置３
７及び断熱層３８を備えている。
この発熱体３６に低温部で電気抵抗の大きい材
料（例えばグラフアイト等）を使用する場合、抵
抗変化が大きいため、常温から有効発熱温度（約
100倍）まで加熱できる電源装置３７を必要とす
る。
このようなHIP装置の雰囲気ガスには、ヒー
タ、被処理物、各部材を保護するために、通常、
アルゴンガスのような不活性ガスが用いられてい
る。
ところが、酸化物系セラミツクスの被処理物を
高温で熱処理すると、該被処理物が酸素分解を生
じてその特性が劣化し、変質、変色、機械的性質
の低下等の不具合がある。
そこで、このような不具合点を解決するため
に、アルゴンガスに酸素ガス（以下O2と略称す
る）を、その被処理物の種類によつて最適な体積
比で混合した雰囲気ガスを使用する酸化性ガス雰
囲気HIP処理装置（以下、O2HIP装置と略称す
る場合がある）が開発されている。
しかし、従来の2000℃級HIP装置ではヒータ材
料としてグラフアイトを用いていたために、酸素
雰囲気下では、容易に酸化されてしまい使用に耐
えないばかりか高温においてこのO2と化合して
酸化ガスとなり、被処理物に悪影響を及ぼすこと
があつた。
そこで、加熱装置３２を予熱装置３９により通
電可能な温度まで予熱するようにしたHIP装置が
提案されている（例えば特開昭63−23732号公報
参照）。
このO2HIP装置は、第５図に示すように、予
熱装置３９が、内層断熱筒４０及び外層断熱筒４
１と、これら内外層断熱筒４０，４１間に配設さ
れた発熱体（金属ヒータ）４２とから構成されて
おり、下蓋３５上に予熱装置３９が載設されると
共に、内層断熱筒４０の内側に位置してセラミツ
クヒータからなる加熱装置３２が載設され、加熱
装置３２上に絶縁板４３を介して被処理物２０が
載置されるようになつている。また、下蓋３５に
は、予熱及び加熱用の導線４４が挿通され、図外
の電源装置に接続されている。
そして、第５図の状態において、加熱装置３２
の通電に先立つて、予熱装置３９により加熱装置
３２及び被処理物２０の予熱を行ない、加熱装置
３２の発熱体雰囲気が電力供給可能温度域すなわ
ち通電可能温度になると、加熱装置３２に通電
し、HIP処理温度まで昇温するようになつてい
る。
（発明が解決しようとする課題）
ところで、後者の従来装置にあつては、高圧容
器３１内に、予熱装置３９及び加熱装置３２，３
９を同心円状に収容しているので容器３１の直径
が大きくなり、延いては装置全体が大型化する
し、高圧容器３１内が複雑になる。
また、予熱装置３９の発熱体４２と加熱装置３
２の間に内層断熱筒４０を介装しているので予熱
効率が悪いうえ、処理室内が狭くなるなどの問題
がある。
本発明は、上述のような実状に鑑みてなされた
ものでその目的とするところは、高圧容器内の構
造が簡単で維持管理が容易であり、予熱効率が高
くしかも処理室内を広くしうる酸化雰囲気下で熱
間等方圧加圧成形が可能な装置を提供するにあ
る。
（課題を解決するための手段）
本発明は、発熱体６が低温部で電気抵抗が大き
くかつ耐酸化性の材料からなる加熱装置４を備え
た高圧容器１内で、被処理物１４を酸化雰囲気の
高温下で等方性の高圧を作用させて加圧する装置
において、叙述の目的を達成するために次の技術
的手段を講じている。
すなわち、本発明の耐酸化性の材料からなる加
熱装置４は、発熱体６の外側に倒立コツプ形状の
断熱層５を備え、該断熱層５内の上部側に発熱体
６が収められており、
断熱層５内の下部側でかつ発熱体６の下方に、
予熱発熱体７が収められていることを第１の特徴
とするのである。
更に、本発明は前述した第１の特徴に加えて、
前記発熱体６と倒立コツプ形状の第１断熱層５と
の間に、発熱体６を内包する第２断熱層１０５が
設けられていることを第２の特徴とするものであ
る。
（作用）
本発明の第１の特徴によれば、倒立コツプ形状
の断熱層５内に被処理物１４を収めた状態で、予
熱発熱体７に通電して、加熱装置４を直接予熱
し、発熱体６に通電可能な温度まで昇温させる。
この場合、予熱発熱体７は発熱体６の下方にあ
り、対流利用になり、加熱効率がよくなるととも
に、断熱層５で取囲まれているので、断熱性が向
上する。
加熱装置４を通電可能な温度まで昇温してか
ら、その発熱体６に通電し、被処理物１４は酸化
雰囲気下で等方向性の高圧を作用させるとともに
処理温度まで加熱して成形加工される。
この場合、予熱発熱体７の通電は続行させても
中断させてもよく、いずれにしろ処理室は均熱制
御される。
また、処理室が酸化雰囲気下であつても、発熱
体６及び予熱発熱体７は耐酸化性の材料よりなる
ので処理可能となる。
本発明の第２の特徴によれば、前述した第１の
特徴の作用に加えて、断熱層が第１断熱層５と第
２断熱層１０５との２重構成とされていることか
ら、熱衝撃に弱いセラミツクスを使わざるを得な
い高温用のための第２断熱層１０５が温度変化の
大きい炉内上下方向の途中でどどまることにより
熱衝撃を緩和し、高温用第２断熱層１０５そ長寿
命化が図れる。
また、低温領域には、その温度に見当つた薄さ
の第１断熱層５にすることで、使用可能な直径が
広がり設計的自由度が増す。
（実施例）
以下、本発明の実施例を図面を参照して詳述す
る。
第１図は本発明の第１実施例を示しており、１
は高圧容器であり、その上下開口部にはそれぞれ
上蓋２、下蓋３が図外のシールを介して挿脱自在
に嵌合されている。
４はHIP用加熱装置であり、倒立コツプ形の断
熱層５とこの断熱層５内でその上部側に収めらて
いる発熱体６とからなり、この実施例では下蓋３
に備えた指示架台１７に、断熱層５が支持されて
高圧容器１の上開口部より挿脱自在とされてい
る。
断熱層５及び発熱体６の材料は、例えばZrO2、
つまり、体積固有抵抗の温度係数が負（低温部で
電気抵抗が大きい）でかつ耐酸化性の材料からな
つている。
特に、断熱層５にあつては、発熱耐６に比べて
密度の低いポーラスなZrO2を用いることによつ
て、断熱性を高めるとともに抵抗率を大きくして
電気絶縁物の役割も果たし得るようにするのが望
ましい。
７は予熱発熱体であり、HIP用発熱体６の下方
でかつ断熱層５内の下部側に収められており、こ
の実施例では径大筒部８と径小筒部９とを有する
支持台１０の外周面に、Pt−Ph合金よりなる線
状に加工された発熱線材をラセン状に巻回したも
のが示されている。
なお、予熱発熱体７たる耐酸化性の材料には金
属やセラミツクス等を用いることができるPt−
Ph合金（白金ロジウム合金）を用いると加工も
容易な上、高圧中（2000Kgｆ／cm2）で1600℃程度
までは発熱させることが可能である。
１１は発熱体６用のリード線で白金等よりな
り、１２は予熱発熱体７用のリード線であり、図
外の電源装置に接続されている。
１３は電気絶縁材であり、円筒形状とされて支
持台１０の肩部に支持されて径小筒部９に套嵌さ
れている。
１４は被処理物であり、発熱体６内に収められ
て台１５を介して支持台１０上に載置されてい
る。
リード線（電極棒）１１を発熱体６と接続する
部分では発熱体６の温度が下がることから、これ
を捕うために、発熱体６の下部側と予熱発熱体７
の上側部とを容器軸方向（高さ方向）で重なり代
１６を有しており、これにより、予熱発熱体７に
てHIP処理中も補助加熱して均熱制御を可能とし
ている。
また、発熱体６としては酸化物セラミツクス
に、CaOあるいはY2O3を酸化剤として添加し焼
結したZrO2を用いることもできる。
第２図は本発明の第２実施例を示しており、基
本的には前述の第１実施例と同じであり、共通す
る部分は符号で示しており、HIP用発熱体６がく
びれ部６４を介して下方に延伸されており、予熱
発熱体７は円筒蛇行形状とされ、電気絶縁材１３
がこの上で支持されており、これによれば、処理
室の下方域まで均熱できる。
ここで、第１実施例及び第２実施例において、
HIP用発熱体６の材質と予熱発熱体７の材質の組
合せ例と使用条件を下表に示す。
次 葉
(Industrial Application Field) The present invention relates to an oxidizing atmosphere hot isostatic pressurizing device, and is used to process objects such as oxide-based ceramics such as ZrO 2 , Al 2 O 3 , MgO, etc., and powder treatment. It is used to apply isostatic pressure to objects such as gold. (Prior Art) Conventionally, as shown in FIG. 4, a HIP apparatus includes a high-pressure container 31 that seals high-pressure gas, a heating device 32 installed in the container 31, and a workpiece mounting table 33.
The high-pressure container 31 consists of an upper lid 34 and a lower lid 35.
The heating device 32 includes a heating element 36 and a power supply device 3.
7 and a heat insulating layer 38. If a material with high electrical resistance (such as graphite) is used for the heating element 36 at a low temperature, the change in resistance will be large, so the effective heat generation temperature (approximately
100 times) is required. The atmospheric gas of such HIP equipment usually contains a
An inert gas such as argon gas is used. However, when an oxide ceramic workpiece is heat-treated at high temperatures, the workpiece undergoes oxygen decomposition and its properties deteriorate, resulting in problems such as deterioration, discoloration, and deterioration of mechanical properties. Therefore, in order to solve these problems, we have developed an oxidation method that uses an atmosphere gas that is a mixture of argon gas and oxygen gas (hereinafter referred to as O 2 ) in the optimal volume ratio depending on the type of the object to be processed. BACKGROUND ART A reactive gas atmosphere HIP processing device (hereinafter sometimes abbreviated as an O 2 HIP device) has been developed. However, since conventional 2000℃ class HIP equipment uses graphite as the heater material, it is easily oxidized in an oxygen atmosphere, making it unusable, and it also combines with this O 2 at high temperatures to form oxidizing gas. , which had an adverse effect on the objects to be treated. Therefore, a HIP device has been proposed in which the heating device 32 is preheated by a preheating device 39 to a temperature at which current can be applied (see, for example, Japanese Patent Laid-Open No. 63-23732). In this O 2 HIP device, as shown in FIG.
1, and a heating element (metal heater) 42 disposed between these inner and outer heat insulating cylinders 40 and 41, a preheating device 39 is mounted on the lower lid 35, and A heating device 32 made of a ceramic heater is placed inside the heating device 32, and the object to be processed 20 is placed on the heating device 32 with an insulating plate 43 interposed therebetween. Further, a conductive wire 44 for preheating and heating is inserted through the lower lid 35 and connected to a power supply device (not shown). Then, in the state shown in FIG. 5, the heating device 32
Prior to energization, the heating device 32 and the workpiece 20 are preheated by the preheating device 39, and when the atmosphere of the heating element of the heating device 32 reaches a temperature range that allows power supply, that is, a temperature that allows energization, the heating device 32 is energized, The temperature is now raised to the HIP processing temperature. (Problem to be Solved by the Invention) By the way, in the latter conventional device, a preheating device 39 and heating devices 32, 3 are installed in the high pressure container 31.
9 are housed concentrically, the diameter of the container 31 becomes large, which in turn increases the size of the entire device and complicates the interior of the high-pressure container 31. In addition, the heating element 42 of the preheating device 39 and the heating device 3
Since the inner heat insulating cylinder 40 is interposed between the two, there are problems such as poor preheating efficiency and a narrow inside of the processing chamber. The present invention was made in view of the above-mentioned circumstances, and its purpose is to provide an oxidation system that has a simple structure inside a high-pressure container, is easy to maintain, has high preheating efficiency, and can enlarge the processing chamber. An object of the present invention is to provide an apparatus capable of hot isostatic pressing under an atmosphere. (Means for Solving the Problems) The present invention provides a method for oxidizing a workpiece 14 in a high-pressure vessel 1 equipped with a heating device 4 in which a heating element 6 is made of a material having high electrical resistance and oxidation resistance in a low temperature region. The following technical measures have been taken to achieve the stated purpose in a device that applies isotropic high pressure in a high temperature atmosphere. That is, the heating device 4 made of an oxidation-resistant material of the present invention includes an inverted cup-shaped heat insulating layer 5 on the outside of the heat generating element 6, and the heat generating element 6 is housed in the upper side of the heat insulating layer 5. , on the lower side of the heat insulating layer 5 and below the heating element 6,
The first feature is that a preheating heating element 7 is housed therein. Furthermore, in addition to the first feature described above, the present invention also has the following features:
A second feature is that a second heat insulating layer 105 containing the heat generating body 6 is provided between the heat generating body 6 and the first heat insulating layer 5 having an inverted cup shape. (Function) According to the first feature of the present invention, with the workpiece 14 housed in the inverted cup-shaped heat insulating layer 5, the preheating heating element 7 is energized to directly preheat the heating device 4, The heating element 6 is heated to a temperature at which it can be energized. In this case, the preheating heating element 7 is located below the heating element 6 and utilizes convection to improve heating efficiency, and since it is surrounded by the heat insulating layer 5, the heat insulation properties are improved. After raising the temperature of the heating device 4 to a temperature at which it can be energized, the heating element 6 is energized, and the workpiece 14 is molded by applying isodirectional high pressure in an oxidizing atmosphere and heating it to the processing temperature. Ru. In this case, the energization of the preheating heating element 7 may be continued or interrupted, and in either case, the temperature of the processing chamber is controlled to be uniform. Furthermore, even if the processing chamber is under an oxidizing atmosphere, processing is possible because the heating element 6 and the preheating heating element 7 are made of oxidation-resistant materials. According to the second feature of the present invention, in addition to the effect of the first feature described above, since the heat insulating layer has a double structure of the first heat insulating layer 5 and the second heat insulating layer 105, The second heat insulating layer 105 for high temperature use, which requires the use of impact-resistant ceramics, reduces thermal shock by staying midway in the vertical direction inside the furnace, where temperature changes are large, and the second heat insulating layer 105 for high temperature use Longer life can be achieved. Furthermore, in the low temperature region, by making the first heat insulating layer 5 thin enough to match the temperature, the usable diameter increases and the degree of freedom in design increases. (Example) Hereinafter, an example of the present invention will be described in detail with reference to the drawings. FIG. 1 shows a first embodiment of the present invention.
is a high-pressure container, and an upper lid 2 and a lower lid 3 are removably fitted into the upper and lower openings of the container via seals (not shown), respectively. Reference numeral 4 denotes a heating device for HIP, which consists of an inverted cup-shaped heat insulating layer 5 and a heating element 6 housed in the upper side of this heat insulating layer 5. In this embodiment, the lower lid 3
A heat insulating layer 5 is supported on an indicator pedestal 17 that is provided at the top of the high-pressure vessel 1 and can be inserted into and removed from the upper opening of the high-pressure vessel 1. The materials of the heat insulating layer 5 and the heating element 6 include, for example, ZrO 2 ,
In other words, it is made of a material that has a negative temperature coefficient of volume resistivity (electrical resistance is large in low temperature areas) and is oxidation resistant. In particular, for the heat insulating layer 5, by using porous ZrO 2 , which has a lower density than the heat-generating layer 6, it increases the heat insulating property and increases the resistivity so that it can also play the role of an electrical insulator. It is desirable to do so. Reference numeral 7 denotes a preheating heating element, which is housed below the HIP heating element 6 and on the lower side of the heat insulating layer 5. In this embodiment, a support base 10 having a large-diameter cylindrical part 8 and a small-diameter cylindrical part 9 A heating wire made of a Pt-Ph alloy and processed into a linear shape is wound in a helical shape around the outer circumferential surface of the device. The oxidation-resistant material of the preheating heating element 7 can be made of metal, ceramics, etc.
Ph alloy (platinum rhodium alloy) is easy to process and can generate heat up to about 1600° C. under high pressure (2000 Kgf/cm 2 ). 11 is a lead wire for the heating element 6 made of platinum or the like, and 12 is a lead wire for the preheating heating element 7, which is connected to a power supply device (not shown). Reference numeral 13 denotes an electrical insulating material, which has a cylindrical shape, is supported by the shoulder of the support base 10, and is fitted into the small diameter cylindrical portion 9. Reference numeral 14 denotes an object to be processed, which is housed within the heating element 6 and placed on the support stand 10 via the stand 15. Since the temperature of the heating element 6 drops at the part where the lead wire (electrode rod) 11 is connected to the heating element 6, in order to catch this, the lower side of the heating element 6 and the preheating heating element 7 are connected.
There is an overlap margin 16 in the axial direction (height direction) of the container with the upper side of the container, and thereby, the preheating heating element 7 performs auxiliary heating even during the HIP process, making it possible to control the temperature uniformity. Further, as the heating element 6, it is also possible to use ZrO 2 which is obtained by adding CaO or Y 2 O 3 as an oxidizing agent to oxide ceramics and sintering the same. FIG. 2 shows a second embodiment of the present invention, which is basically the same as the first embodiment described above, and common parts are indicated by symbols. The preheating heating element 7 has a cylindrical meandering shape, and the electrical insulating material 13
is supported on this, and with this, it is possible to uniformly heat the lower part of the processing chamber. Here, in the first example and the second example,
Examples of combinations of the materials of the HIP heating element 6 and the materials of the preheating heating element 7 and usage conditions are shown in the table below. next leaf
【表】
また、高圧ガスとしては、アルゴンのような不
活性ガスに、酸素ガスをその被処理物１４の種類
によつて最適な体積比で混合した雰囲気ガスが使
用され、高圧容器１内は酸化雰囲気とされる。
さらに、加圧処理中の軸力は上蓋２、下蓋３の
上下端面に、台車フレーム、旋回フレームを係合
させることによつて受持つ。
第３図は本発明の第３実施例であつて、低温
（最高温度1200℃以下）または中音（最高温度が
1200℃〜1500℃）用の第１断熱層５は、SUS304
よりなる外層５ＡとSiO2やAl2O3等よりなる内層
５Ｂとの間に、CAAl2O3、SiO2等のセラミツク
フアイバよりなる断熱材５Ｃを備えており、この
第１断熱層５と発熱体６との間に、発熱体６を内
包してジルコニア、イツトリア等を主成分とする
高温用（最高温度1500℃以上）の第２断熱層１０
５を設けたものであり、その他の構成は前述した
第１実施例を共通するので、共通部分は共通符号
で示している。
なお、第３図の第３実施例において、図示省略
したが、前述した第２実施例を付加することもで
きる。
なお、いずれの実施例においても、被処理物１
４、加熱装置４等は上蓋２を取外して高圧容器１
内に出入れされるが、下取出型式としたものであ
つてもよい。
次に、上記実施例、主に、第１実施例において
その作用を説明すると、上蓋２を取外して高圧容
器１の中に、被処理物１４を収め、これの加熱装
置４で取囲むように該加熱装置４を高圧容器１中
に収めて上蓋２を施蓋する。
加熱装置４における発熱体６の通電に先立つ
て、予熱発熱体７に通電することにより、加熱装
置４を通電可能な温度まで昇温する。
この昇温に当つて、断熱層４は断熱性を高め、
対流作用で昇温を早めることになるし、予熱が直
接的となるので効率は向上される。
所定の温度まで昇温されると、発熱体６に通電
することにより、酸化雰囲気下での高温高圧な等
方圧加圧がなされるが、発熱体６、予熱発熱体７
はいずれも耐酸化性の材料からなるので、酸素雰
囲気中でもHIP処理が可能となり、O2と激しく
反応することもなく、被処理物１４は高温で安定
した焼結体に加圧される。
このHIP処理中において、予熱発熱体７の通電
を続行しておくことにより、発熱体６と予熱発熱
体７とによる処理室内の均熱制御が可能となり、
特に、予熱発熱体７による対流で均熱性は向上す
る。
また、発熱体６と予熱発熱体７とを重ね代１６
を有して上下に配置することにより、予熱発熱体
７による補助加熱が確実になされ、処理室の均熱
性は向上する。
所定の処理が完了すると、発熱体６、予熱発熱
体７の通電を止め、加熱装置４を上方より取出し
て焼結体が取出されることになる。
（発明の効果）
本発明は以上の通りであり、次の利点がある。
加熱装置の発熱体及び予熱発熱体はいずれも耐
酸化性の材料からなるので、酸素雰囲気中でも
HIP処理が可能となる。
また、加熱装置の発熱体は倒立コツプ形状の断
熱層の上部側にあり、この発熱体の下方で断熱層
内に予熱発熱体が収められているので、予熱は対
流作用で加熱効率が向上できるばかりか処理室の
均熱制御も可能となり、高温で安定した焼結体を
得ることができる。
更に、発熱体と予熱発熱体とは断熱層内で上下
に配置されているので、処理室は大きくできるに
も拘らず高圧容器の内部構造が簡単でしかも装置
全体をコンパクトにできる。
また本発明は断熱層を２重構成にしたことによ
り熱衝撃に弱いセラミツクスを使わざるを得ない
高温用の第２断熱層が温度変化の大きい炉内上下
方向の途中でとどまることにより熱衝撃を緩和
し、高温用の第２断熱層の長寿命化が図れる。
更に、低温領域には、その温度に見当つた薄さ
の第１断熱層にすることで、使用可能な直径が広
がり設計的自由度を増大することができる。
本発明は以上の利点を有し、従つて、酸化物系
セラミツクス、粉末治金等の被処理物を酸素雰囲
気下でHIP処理するものとして有意義である。[Table] In addition, as the high-pressure gas, an atmospheric gas containing an inert gas such as argon and oxygen gas mixed in an optimal volume ratio depending on the type of the object to be processed 14 is used, and the inside of the high-pressure container 1 is It is assumed to be an oxidizing atmosphere. Furthermore, the axial force during the pressurization process is handled by engaging the upper and lower end surfaces of the upper cover 2 and lower cover 3 with the truck frame and the revolving frame. FIG. 3 shows the third embodiment of the present invention, which shows low-temperature (maximum temperature 1200°C or less) or medium-temperature (maximum temperature
1200℃~1500℃) The first insulation layer 5 is SUS304
A heat insulating material 5C made of ceramic fiber such as CAAl 2 O 3 or SiO 2 is provided between the outer layer 5A made of SiO 2 or Al 2 O 3 and the inner layer 5B made of SiO 2 or Al 2 O 3 . A second heat insulating layer 10 for high temperatures (maximum temperature of 1500°C or higher) containing the heating element 6 and containing zirconia, ittria, etc. as a main component is provided between the heating element 6 and the heating element 6.
5, and the other configurations are the same as those of the first embodiment described above, so common parts are indicated by common symbols. Although not shown in the third embodiment shown in FIG. 3, the second embodiment described above can also be added. In addition, in any of the examples, the object to be treated 1
4. Remove the top cover 2 of the heating device 4, etc. and place it in the high pressure container 1.
Although it can be put in and taken out from the inside, it may also be a type that can be taken out from the bottom. Next, to explain the operation of the above embodiment, mainly the first embodiment, the upper lid 2 is removed, the object to be processed 14 is placed in the high pressure container 1, and the object is surrounded by the heating device 4. The heating device 4 is placed in the high-pressure container 1 and the upper lid 2 is closed. Prior to energizing the heating element 6 in the heating device 4, the preheating heating element 7 is energized to raise the temperature to a temperature at which the heating device 4 can be energized. In response to this temperature increase, the heat insulating layer 4 increases its heat insulating properties,
The convection action speeds up the temperature rise, and since preheating is direct, efficiency is improved. When the temperature is raised to a predetermined temperature, the heating element 6 is energized to perform isostatic pressurization at high temperature and high pressure in an oxidizing atmosphere.
Since both are made of oxidation-resistant materials, HIP processing is possible even in an oxygen atmosphere, and the object to be processed 14 is pressurized into a stable sintered body at high temperatures without violently reacting with O 2 . During this HIP process, by continuing to energize the preheating heating element 7, it becomes possible to uniformly control the temperature inside the processing chamber by the heating element 6 and the preheating heating element 7.
In particular, convection by the preheating heating element 7 improves thermal uniformity. Also, the heating element 6 and the preheating heating element 7 are overlapped by 16
By arranging them one above the other, auxiliary heating by the preheating heating element 7 is reliably performed, and the thermal uniformity of the processing chamber is improved. When the predetermined process is completed, the power supply to the heating element 6 and the preheating heating element 7 is stopped, the heating device 4 is taken out from above, and the sintered body is taken out. (Effects of the Invention) The present invention is as described above, and has the following advantages. The heating element of the heating device and the preheating heating element are both made of oxidation-resistant materials, so they can be used even in an oxygen atmosphere.
HIP processing becomes possible. In addition, the heating element of the heating device is located on the upper side of the inverted cup-shaped insulation layer, and the preheating heating element is housed within the insulation layer below this heating element, so preheating can improve heating efficiency through convection. Not only that, it is also possible to control the soaking temperature of the processing chamber, making it possible to obtain a sintered body that is stable at high temperatures. Furthermore, since the heating element and the preheating heating element are arranged one above the other within the heat insulating layer, the internal structure of the high-pressure container is simple and the entire apparatus can be made compact, although the processing chamber can be made larger. In addition, the present invention has a double structure of the heat insulating layer, so that the second heat insulating layer for high temperatures, which necessitates the use of ceramics that are susceptible to thermal shock, stays in the middle of the vertical direction inside the furnace where temperature changes are large, thereby reducing thermal shock. This makes it possible to extend the life of the second heat insulating layer for high temperatures. Furthermore, by providing the first heat insulating layer with a thickness appropriate for the temperature in the low temperature region, the usable diameter can be expanded and the degree of freedom in design can be increased. The present invention has the above-mentioned advantages, and is therefore useful as a method for HIPing objects to be treated such as oxide ceramics and powder metallurgy in an oxygen atmosphere.
第１図は本発明第１実施例の立面断面図、第２
図は本発明第２実施例の立面断面図、第３図は本
発明第３実施例の立面断面図、第４図と第５図は
いずれも従来例の立面断面図である。
１……高圧容器、４……加熱装置、５……第１
断熱層、６……発熱体、７……予熱発熱体、１６
……重なり代、１０５……第２断熱層。
Fig. 1 is an elevational cross-sectional view of the first embodiment of the present invention;
The figure is an elevational sectional view of the second embodiment of the present invention, FIG. 3 is an elevational sectional view of the third embodiment of the invention, and both FIGS. 4 and 5 are elevational sectional views of the conventional example. 1... High pressure container, 4... Heating device, 5... First
Heat insulation layer, 6...Heating element, 7...Preheating heating element, 16
...Overlap allowance, 105...Second heat insulation layer.
Claims (1)
酸化性の材料からなる加熱装置４を備えた高圧容
器１内で、被処理物１４を酸化雰囲気の高温下で
等方性の高圧を作用させて加圧する装置におい
て、 耐酸化性の材料からなる加熱装置４は、発熱体
６の外側に倒立コツプ形状の断熱層５を備え、該
断熱層５内の上部側に発熱体６が収められてお
り、 断熱層５内の下部側でかつ発熱体６の下方に、
予熱発熱体７が収められていることを特徴とする
酸化雰囲気熱間等方圧加圧装置。 ２ 発熱体６が低温部で電気抵抗が大きくかつ耐
酸化性の材料からなる加熱装置４を備えた高圧容
器１内で、被処理物１４を酸化雰囲気の高温下で
等方性の高圧を作用させて加圧する装置におい
て、 耐酸化性の材料からなる加熱装置４は、発熱体
６の外側に倒立コツプ形状の第１断熱層５を備
え、該第１断熱層５内の上部側に発熱体６が収め
られており、 更に、前記発熱体６と第１断熱層５との間に、
発熱体６を内包する第２断熱層１０５が設けら
れ、 前記第１断熱層５内の下部側でかつ発熱体６の
下方に、予熱発熱体７が収められていることを特
徴とする酸化雰囲気熱間等方圧加圧装置。 ３ 発熱体６の下部側と予熱発熱体７の上部側と
が容器軸方向で重なり代１６を有することを特徴
とする請求項１又は２の酸化雰囲気熱間等方圧加
圧装置。[Scope of Claims] 1. In a high-pressure container 1 equipped with a heating device 4 in which the heating element 6 is made of a material with high electrical resistance and oxidation resistance in a low temperature part, the workpiece 14 is heated under a high temperature in an oxidizing atmosphere. In a device that pressurizes by applying directional high pressure, a heating device 4 made of an oxidation-resistant material is provided with an inverted cup-shaped heat insulating layer 5 on the outside of a heating element 6, and an insulating layer 5 on the upper side inside the heat insulating layer 5. A heating element 6 is housed at the lower side of the heat insulating layer 5 and below the heating element 6.
An oxidizing atmosphere hot isostatic pressurizing device characterized by containing a preheating heating element 7. 2. In a high-pressure container 1 equipped with a heating device 4 in which the heating element 6 is a low-temperature part and is made of a material with high electrical resistance and oxidation resistance, an isotropic high pressure is applied to the workpiece 14 in an oxidizing atmosphere at a high temperature. In the device for pressurizing, the heating device 4 made of an oxidation-resistant material is provided with a first heat insulating layer 5 having an inverted cup shape on the outside of the heating element 6, and the heating element is placed on the upper side of the first heat insulating layer 5. 6 is housed therein, and further between the heating element 6 and the first heat insulating layer 5,
An oxidizing atmosphere characterized in that a second heat insulating layer 105 containing a heat generating element 6 is provided, and a preheating heat generating element 7 is housed on the lower side of the first heat insulating layer 5 and below the heat generating element 6. Hot isostatic press equipment. 3. The oxidizing atmosphere hot isostatic pressurizing device according to claim 1 or 2, wherein the lower side of the heating element 6 and the upper side of the preheating heating element 7 have an overlap margin 16 in the axial direction of the container.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP90902829A EP0434839B1 (en) | 1989-07-17 | 1990-02-08 | Oxidizing atmosphere hot isotropic press |
| DE69013657T DE69013657T2 (en) | 1989-07-17 | 1990-02-08 | ISOTROPICAL HOT PRESS UNDER OXYDING ATMOSPHERE. |
| PCT/JP1990/000158 WO1991001474A1 (en) | 1989-07-17 | 1990-02-08 | Oxidizing atmosphere hot isotropic press |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63-191593 | 1988-07-30 | ||
| JP19159388 | 1988-07-30 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02126093A JPH02126093A (en) | 1990-05-15 |
| JPH0544599B2 true JPH0544599B2 (en) | 1993-07-06 |
Family
ID=16277222
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1184973A Granted JPH02126093A (en) | 1988-07-30 | 1989-07-17 | Oxidizing atmosphere hot isotropic pressurizer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02126093A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07117344B2 (en) * | 1992-07-14 | 1995-12-18 | 日機装株式会社 | Oxidizing atmosphere pressurized self-combustion synthesizer |
| JP5500802B2 (en) * | 2008-08-19 | 2014-05-21 | 株式会社神戸製鋼所 | Hot isostatic press |
-
1989
- 1989-07-17 JP JP1184973A patent/JPH02126093A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02126093A (en) | 1990-05-15 |
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