JPH07117344B2 - Oxidizing atmosphere pressurized self-combustion synthesizer - Google Patents
Oxidizing atmosphere pressurized self-combustion synthesizerInfo
- Publication number
- JPH07117344B2 JPH07117344B2 JP4186946A JP18694692A JPH07117344B2 JP H07117344 B2 JPH07117344 B2 JP H07117344B2 JP 4186946 A JP4186946 A JP 4186946A JP 18694692 A JP18694692 A JP 18694692A JP H07117344 B2 JPH07117344 B2 JP H07117344B2
- Authority
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- Japan
- Prior art keywords
- heater
- self
- sample
- combustion
- temperature
- Prior art date
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Description
【０００１】[0001]
【産業上の利用分野】本発明は、加圧自己燃焼合成法に
よるセラミックスの合成装置の改良に関し、特に酸化雰
囲気中での加圧自己燃焼合成法により酸化物セラミック
スを合成する装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to improvement of a ceramics synthesizing apparatus by a pressure self-combustion synthesis method, and more particularly to an apparatus for synthesizing oxide ceramics by a pressure self-combustion synthesis method in an oxidizing atmosphere. .
【０００２】[0002]
【従来の技術】材料粉末を自己燃焼させてセラミックス
を合成する自己燃焼合成法が、セラミックスの有力な製
造方法として注目されてきた。特に、圧力ガス媒体中で
材料粉末を加圧しながら自己燃焼させる加圧自己燃焼合
成法は、さらに優れた緻密性を持つセラミックスを製造
することが出来るという利点を有する。2. Description of the Related Art The self-combustion synthesis method, in which material powder is self-combusted to synthesize ceramics, has attracted attention as a promising method for producing ceramics. In particular, the pressurized self-combustion synthesis method, in which the material powder is self-combusted while being pressurized in a pressure gas medium, has the advantage of being able to produce ceramics with even higher density.
【０００３】この加圧自己燃焼合成法において、アルゴ
ン、窒素、酸素など各種圧力ガス媒体を使用することに
よつて、セラミックス材料の安定性および生成セラミッ
クスの特性を制御することが可能であり、高圧下での雰
囲気制御が重要な技術的課題になつている。In this pressurized self-combustion synthesis method, it is possible to control the stability of the ceramic material and the characteristics of the produced ceramic by using various pressure gas media such as argon, nitrogen and oxygen. Atmosphere control below has become an important technical issue.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、この加
圧自己燃焼合成法を実施する装置は、主として熱間等方
圧プレスを改造したものが使われてきた。反応容器には
窒化ホウ素などを使用し、ヒーターにはグラファイトな
どを使用するため、圧力ガス媒体はアルゴン、窒素など
の不活性ガスが使用される。したがつて、炉室内は還元
雰囲気であり、非酸化物系セラミックス等の製造に使用
されてきた。However, as the apparatus for carrying out the pressurized self-combustion synthesis method, a hot hot isostatic press modified is mainly used. Since boron nitride or the like is used for the reaction vessel and graphite or the like is used for the heater, an inert gas such as argon or nitrogen is used as the pressure gas medium. Therefore, the furnace chamber has a reducing atmosphere and has been used for manufacturing non-oxide ceramics and the like.
【０００５】このような加圧自己燃焼合成装置では、酸
化雰囲気で焼結を行う酸化物セラミックスなどを製造す
ることが出来なかつた。With such a pressurized self-combustion synthesizer, it has been impossible to manufacture oxide ceramics or the like that are sintered in an oxidizing atmosphere.
【０００６】本発明の目的は、酸化雰囲気中で加圧自己
燃焼合成法により酸化物セラミックスを合成する装置を
提供することにある。An object of the present invention is to provide an apparatus for synthesizing oxide ceramics by a pressure self-combustion synthesis method in an oxidizing atmosphere.
【０００７】[0007]
【課題を解決するための手段】前記の目的を達成するた
め、本発明は、耐圧容器中に耐酸化性の断熱炉筒および
断熱炉床を設けて炉室を画設し、かつ炉室中に耐酸化性
の着火ヒーターおよび加熱ヒーターを備えた加圧自己燃
焼合成装置において、前記断熱炉床に設けた試料台の上
に載置した被処理物に接して試料温度測定用熱電対を設
けると共に、炉室中央に加熱ヒーター制御用熱電対を設
けて、これら各熱電対をそれぞれ熱電対取出線を介して
温度表示制御器に配線接続し、前記着火ヒーターに通電
して被処理物の試料を加熱することにより自己燃焼の着
火を行い、さらに試料が着火しにくい場合に前記加熱ヒ
ーターを通電して試料を予熱することにより自己燃焼の
開始を促進するように、前記温度表示制御器を介して試
料の温度および加熱ヒーターの温度制御を行うと共に合
成反応の開始を確認するように構成することを特徴とす
る酸化雰囲気加圧自己燃焼合成装置を提供する。Means for Solving the Problems] was to achieve the object of the
Therefore , the present invention provides a heat- resistant container with an oxidation-resistant heat-insulating furnace tube and a heat-insulating hearth in a pressure-resistant container to define the furnace chamber, and the oxidation- proof property is provided in the furnace chamber .
In the pressure self-combustion synthesis apparatus comprising an ignition heater and heater of, on the sample stage provided in the heat insulating hearth
Install a thermocouple for measuring the sample temperature in contact with the object to be processed placed on the
At the same time, install a thermocouple for controlling the heater in the center of the furnace chamber.
Each of these thermocouples via the thermocouple lead wire.
Wire the temperature display controller and turn on the ignition heater.
Heating the sample of the object to be treated
If the sample is fired and the sample is difficult to ignite,
Of the self-combustion by energizing the heater to preheat the sample
Trial via the temperature display controller to facilitate initiation.
Control the temperature of the material and the temperature of the heater
Provided is an oxidizing atmosphere pressurized self-combustion synthesizer, which is configured to confirm the start of a formation reaction .
【０００８】[0008]
【作用】本発明の装置は、断熱炉筒および断熱炉床を耐
酸化性の多孔質酸化物セラミックスで構成し、かつ着火
ヒーターおよび加熱ヒーターを耐酸化性の白金−ロジウ
ム合金とすることにより、圧力ガス媒体として酸素混合
ガスを使用できる構造となり、炉室内を酸化雰囲気にす
ることにより、酸化物セラミックスの加圧自己燃焼合成
が可能となつた。In the apparatus of the present invention, the heat insulating furnace tube and the heat insulating hearth are made of oxidation resistant porous oxide ceramics, and the ignition heater and the heating heater are made of the oxidation resistant platinum-rhodium alloy. Oxygen mixed gas can be used as a pressure gas medium, and pressurized self-combustion synthesis of oxide ceramics is possible by making the furnace chamber an oxidizing atmosphere.
【０００９】使用し得る圧力ガス媒体の酸素濃度は、好
適には０−２０％である。The oxygen concentration of the pressurized gas medium which can be used is preferably 0-20%.
【００１０】また、断熱筒および炉床断熱材は、耐熱性
と耐熱衝撃性を有する多孔質酸化物セラミックス材を使
用することにより、自己燃焼時の高熱が圧力容器側に放
散することを防止し、かつ自己燃焼時の急激な温度上昇
による高熱襲撃に対応する。Further, the heat insulating cylinder and the hearth heat insulating material use a porous oxide ceramic material having heat resistance and thermal shock resistance to prevent the high heat during self-combustion from radiating to the pressure vessel side. In addition, it responds to a high heat attack due to a rapid temperature rise during self-combustion.
【００１１】加熱ヒーターにより、炉室を高温まで加熱
することができる。使用し得る炉室温度は、好適には０
−１６００℃である。The heater can heat the furnace chamber to a high temperature. The furnace chamber temperature that can be used is preferably 0.
-1600 ° C.
【００１２】本発明の装置は、その構造および材質か
ら、当然に圧力媒体としてアルゴン、窒素などの不活性
ガスを使用することが可能であり、従来通りの炭化物、
ホウ化物、窒化物セラミックスなどの加圧自己燃焼合成
にも利用することが出来る。The apparatus of the present invention can naturally use an inert gas such as argon or nitrogen as a pressure medium due to its structure and material, and it is possible to use a conventional carbide,
It can also be used for pressurized self-combustion synthesis of borides and nitride ceramics.
【００１３】本発明の装置は、通常の酸化雰囲気熱間等
方圧プレスとして、１６００℃、２０００ｋｇ／ｃｍ２
にて試料を加圧焼結することも可能である。The apparatus of the present invention is used as a normal hot isostatic press in an oxidizing atmosphere at 1600 ° C. and 2000 kg / cm 2.
It is also possible to pressure sinter the sample.
【００１４】[0014]
【実施例】本発明に係る酸化雰囲気加圧自己燃焼合成装
置について、図１を参照しながら以下詳細に説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An oxidizing atmosphere pressurized self-combustion synthesizer according to the present invention will be described in detail below with reference to FIG.
【００１５】圧力容器（１）中の炉台（９）上に断熱炉
筒（６）および断熱炉床（８）を設けて、炉室を画設す
る。前記炉床（８）に試料台（１０）を設け、その上に
被処理物を載置する。試料台（１０）には加熱ヒーター
（１２）を装着し、被処理物の上方には着火ヒーター
（１１）を装着する。加熱ヒーター（１２）および着火
ヒーター（１１）は、炉台（９）および下蓋（４）を貫
通する配線により、それぞれ加熱ヒーター電極（１４）
および着火ヒーター電極（１３）に接続する。被処理物
に接して試料温度測定用熱電対（１５）を設け、炉室中
央に加熱ヒーター制御用熱電対（１６）を設け、これら
熱電対（１５、１６）をそれぞれ熱電対取出線（１７）
を介して温度表示制御器（図示していない）に配線接続
する。An adiabatic furnace tube (6) and an adiabatic hearth (8) are provided on a furnace table (9) in the pressure vessel (1) to define a furnace chamber . A sample table (10) is provided on the hearth (8) , and an object to be processed is placed thereon . A heating heater (12) is attached to the sample table (10) , and an ignition heater (11) is attached above the object to be treated. The heating heater (12) and the ignition heater (11) are respectively provided with a heating heater electrode (14) by a wiring penetrating the furnace base (9) and the lower lid (4).
And to the ignition heater electrode (13). Thermocouple sample temperature measurement in contact with the object to be treated (15) is provided, furnace chamber center heater control thermocouple (16) is provided, these
Connect the thermocouple (15, 16) to the thermocouple lead wire (17) , respectively.
Through a wired connection <br/> to temperature display controller (not shown).
【００１６】被処理物が位置する炉室中に、下蓋および
炉台を貫通する加圧ガス導入管を介して、酸素濃度最高
２０％の混合アルゴンガス又は混合窒素ガスを２０００
ｋｇ／ｃｍ２まで圧入する。最初に、着火ヒーター電極
から着火ヒーターに通電して、被処理物の試料を加熱す
ることにより、自己燃焼の着火を行う。着火しにくい試
料の場合は（または標準生成熱、断熱温度が共に低い場
合など）、加熱ヒーター電極から加熱ヒーターに通電
し、試料を予熱することにより、自己燃焼の開始を促進
する。この間に、前記試料温度測定用熱電対により試料
の温度を測定すると共に前記加熱ヒーター制御用熱電対
により加熱ヒーターの温度制御を、前記温度表示制御器
を介して行い、前述した予熱時の試料の温度を制御する
よう構成する。さらに、試料の自己燃焼が開始した時に
は、試料の温度が急激に上昇することから、合成反応の
開始を前記温度表示制御器により確認することができ
る。In the furnace chamber in which the object to be treated is located, a mixed argon gas or a mixed nitrogen gas having an oxygen concentration of up to 20% is added through a pressurized gas introduction pipe penetrating the lower lid and the furnace base.
Press up to kg / cm 2 . First, by energizing the ignition heater from the ignition heater electrode to heat the sample of the object to be treated, self-combustion ignition is performed. In the case of a sample that is difficult to ignite (or when the standard heat of formation and the adiabatic temperature are both low), the heater is energized from the heater electrode to preheat the sample to accelerate the start of self-combustion. During this time, the sample by the sample temperature measuring thermocouple
For measuring the temperature of the heater and controlling the heating heater
The temperature control of the heater is controlled by the temperature display controller
It carried through, to control the temperature of the sample at the time of preheating the aforementioned
Configure as follows . Furthermore, <br/> when self-combustion of the sample was started, since the temperature of the sample rises rapidly, it is possible to confirm the start of the synthesis reaction by the temperature display controller
It
【００１７】[0017]
【発明の効果】本発明の装置は、加圧自己燃焼セラミッ
クス合成装置の炉室中を酸化雰囲気にすることにより、
従来の装置では合成が出来なかつた酸化物セラミックス
の酸化雰囲気加圧自己燃焼合成が可能となり、高品質の
酸化物セラミックスを製造し得る利点を有する。EFFECT OF THE INVENTION The apparatus according to the present invention is provided with an oxidizing atmosphere in the furnace chamber of the pressurized self-combusting ceramics synthesis apparatus,
The conventional apparatus has the advantage that it is possible to perform self-combustion under pressure in an oxidizing atmosphere while being unable to synthesize oxide ceramics, and to manufacture high-quality oxide ceramics.
【００１８】特に、本発明によれば、前記断熱炉床に設
けた試料台の上に載置した被処理物に接して試料温度測
定用熱電対を設けると共に、炉室中央に加熱ヒーター制
御用熱電対を設けて、これら各熱電対をそれぞれ熱電対
取出線を介して温度表示制御器に配線接続し、前記着火
ヒーターに通電して被処理物の試料を加熱することによ
り自己燃焼の着火を行い、さらに試料が着火しにくい場
合に前記加熱ヒーターを通電して試料を予熱することに
より自己燃焼の開始を促進するように、前記温度表示制
御器を介して試料の温度および加熱ヒーターの温度制御
を行うと共に合成反応の開始を確認するように構成する
ことにより、酸化雰囲気加圧自己燃焼合成を適正かつ円
滑に達成することができる。また、炉室中を酸化雰囲気
にすることにより、加圧ガス中の酸素と被処理物との反
応による酸化雰囲気加圧自己燃焼合成も可能となり、合
成反応の範囲も拡大して、より多種類の製品を得ること
ができる。In particular, according to the invention, the installation in the adiabatic hearth
The sample temperature is measured by touching the object to be processed placed on the sample table.
A constant temperature thermocouple is installed and a heater control is provided in the center of the furnace chamber.
A thermocouple for use is provided and each of these thermocouples is
Ignite the above by connecting to the temperature display controller via the lead wire.
By energizing the heater to heat the sample to be processed,
When self-combustion ignition occurs and the sample is difficult to ignite
In order to preheat the sample by energizing the heater
In order to accelerate the start of self-combustion, the temperature display system
Control of sample temperature and heater temperature via controller
And confirm the start of the synthetic reaction.
By doing so, it is possible to make the self-combustion synthesis under pressure in an oxidizing atmosphere proper and circular.
Can be achieved smoothly . Further, by making the furnace chamber to an oxidizing atmosphere, an oxidizing atmosphere pressure self-combustion synthesis by reaction between oxygen and the object to be treated in the pressurized gas can also be a Do Ri, be expanded range of synthetic reactions, more A wide variety of products can be obtained.
【００１９】本発明の装置は、その構造および材質か
ら、当然に圧力ガス媒体としてアルゴン、窒素などの不
活性ガスを使用することが可能であり、従来通りの炭化
物、ホウ化物、窒化物セラミックスなどの加圧自己燃焼
合成にも利用することが出来る。The apparatus of the present invention can naturally use an inert gas such as argon or nitrogen as a pressure gas medium due to its structure and material, and it is possible to use conventional carbides, borides, nitride ceramics, etc. It can also be used for pressurized self-combustion synthesis of.
【００２０】また、通常の酸化雰囲気熱間等方圧プレス
として、最高１６００℃、２０００ｋｇ／ｃｍ２で試料
を加圧焼結することも可能である。It is also possible to press-sinter the sample at a maximum temperature of 1600 ° C. and 2000 kg / cm 2 as a normal hot isostatic press in an oxidizing atmosphere.
【図１】本発明に係る実施例を示す酸化雰囲気加圧自己
燃焼合成装置の要部断面図である。FIG. 1 is a sectional view of an essential part of an oxidizing atmosphere pressurized self-combustion synthesizer showing an embodiment according to the present invention.
１ 圧力容器 ２ ヨークフレーム ３ 上蓋 ４ 下蓋 ５ ガスシール ６ 断熱筒 ７ 断熱筒支持ケーシング ８ 断熱炉床 ９ 炉台 １０ 試料台 １１ 着火ヒーター １２ 加熱ヒーター １３ 着火ヒーター電極 １４ 加熱ヒーター電極 １５ 試料温度測定用熱電対 １６ 加熱ヒーター制御用熱電対 １７ 熱電対取出線 1 Pressure Vessel 2 Yoke Frame 3 Upper Lid 4 Lower Lid 5 Gas Seal 6 Heat Insulation Cylinder 7 Heat Insulation Cylinder Support Casing 8 Heat Insulation Hearth 9 Furnace Stand 10 Sample Stage 11 Ignition Heater 12 Heating Heater 13 Ignition Heater Electrode 14 Heating Heater Electrode 15 For Measuring Sample Temperature Thermocouple 16 Thermocouple for heating heater control 17 Thermocouple lead wire
フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｆ２７Ｄ 1/00 Ｎ 11/02 Ａ 7727−4Ｋ Continuation of the front page (51) Int.Cl. 6 Identification code Office reference number FI technical display location F27D 1/00 N 11/02 A 7727-4K
Claims (1)
断熱炉床を設けて炉室を画設し、かつ炉室中に耐酸化性
の着火ヒーターおよび加熱ヒーターを備えた加圧自己燃
焼合成装置において、前記断熱炉床に設けた試料台の上に載置した被処理物に
接して試料温度測定用熱電対を設けると共に、炉室中央
に加熱ヒーター制御用熱電対を設けて、これら各熱電対
をそれぞれ熱電対取出線を介して温度表示制御器に配線
接続し 、前記着火ヒーターに通電して被処理物の試料を加熱する
ことにより自己燃焼の着火を行い、さらに試料が着火し
にくい場合に前記加熱ヒーターを通電して試料を予熱す
ることにより自己燃焼の開始を促進するように、前記温
度表示制御器を介して試料の温度および加熱ヒーターの
温度制御を行うと共に合成反応の開始を確認するように
構成する ことを特徴とする酸化雰囲気加圧自己燃焼合成
装置。1. A pressure-resistant container is provided with an oxidation-resistant heat-insulating furnace tube and a heat-insulating hearth to define a furnace chamber, and the oxidation resistance is maintained in the furnace chamber .
In the pressurized self-combustion synthesizer equipped with the ignition heater and the heating heater , the object to be treated placed on the sample table provided in the adiabatic hearth
A thermocouple for measuring the sample temperature was installed in contact with the center of the furnace chamber.
A thermocouple for controlling the heater is installed in the
To each temperature display controller via the thermocouple lead wire
Connect and heat the sample to be processed by energizing the ignition heater.
Self-combustion ignition, which in turn causes the sample to ignite.
If difficult, energize the heater to preheat the sample
Temperature to accelerate the initiation of self-combustion.
Of the sample temperature and heater via the degree display controller
To control the temperature and confirm the start of the synthetic reaction
An oxidizing atmosphere pressurized self-combustion synthesizer characterized by being configured .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4186946A JPH07117344B2 (en) | 1992-07-14 | 1992-07-14 | Oxidizing atmosphere pressurized self-combustion synthesizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4186946A JPH07117344B2 (en) | 1992-07-14 | 1992-07-14 | Oxidizing atmosphere pressurized self-combustion synthesizer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0634276A JPH0634276A (en) | 1994-02-08 |
| JPH07117344B2 true JPH07117344B2 (en) | 1995-12-18 |
Family
ID=16197497
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4186946A Expired - Fee Related JPH07117344B2 (en) | 1992-07-14 | 1992-07-14 | Oxidizing atmosphere pressurized self-combustion synthesizer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07117344B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113390100B (en) * | 2021-05-13 | 2022-07-08 | 张明玉 | Candle seedling type burner |
| JP7852922B2 (en) * | 2022-08-16 | 2026-04-28 | 株式会社燃焼合成 | Combustion synthesis furnace |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02126093A (en) * | 1988-07-30 | 1990-05-15 | Kobe Steel Ltd | Oxidizing atmosphere hot isotropic pressurizer |
-
1992
- 1992-07-14 JP JP4186946A patent/JPH07117344B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0634276A (en) | 1994-02-08 |
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