JPH0269305A - Nitriding furnace and production of metal nitride - Google Patents
Nitriding furnace and production of metal nitrideInfo
- Publication number
- JPH0269305A JPH0269305A JP63220363A JP22036388A JPH0269305A JP H0269305 A JPH0269305 A JP H0269305A JP 63220363 A JP63220363 A JP 63220363A JP 22036388 A JP22036388 A JP 22036388A JP H0269305 A JPH0269305 A JP H0269305A
- Authority
- JP
- Japan
- Prior art keywords
- furnace
- nitriding
- heat
- reaction
- heat element
- 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.)
- Granted
Links
- 238000005121 nitriding Methods 0.000 title claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 15
- 239000002184 metal Substances 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000011810 insulating material Substances 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 230000005484 gravity Effects 0.000 claims description 14
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 11
- 229910052750 molybdenum Inorganic materials 0.000 claims description 11
- 239000011733 molybdenum Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 17
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 15
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 238000011109 contamination Methods 0.000 abstract description 3
- 239000011261 inert gas Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 239000002657 fibrous material Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 239000000835 fiber Substances 0.000 description 10
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000011449 brick Substances 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000011094 fiberboard Substances 0.000 description 5
- 239000003365 glass fiber Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000012784 inorganic fiber Substances 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 239000011490 mineral wool Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000008542 thermal sensitivity Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910016006 MoSi Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052789 astatine Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/10—Reduction of greenhouse gas [GHG] emissions
- Y02P10/143—Reduction of greenhouse gas [GHG] emissions of methane [CH4]
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、窒化の際の多大な発熱量によって溶融するお
それのある金属の窒化反応炉及びその窒化反応炉を用い
てなる金属窒化物の製造法に関する。このような金属の
具体例としては、ケイ素、アルミニウム、チタン、クロ
ム等があげられるが、以下、ケイ素を例にとって説明す
る。Detailed Description of the Invention [Industrial Application Field] The present invention relates to a nitriding reactor for metals that may be melted due to a large amount of heat generated during nitriding, and a method for producing metal nitrides using the nitriding reactor. Regarding manufacturing methods. Specific examples of such metals include silicon, aluminum, titanium, chromium, etc., and the following description will be made by taking silicon as an example.
窒化ケイ素焼結体は、機械的強度が高く耐スポール性も
あるのでセラミック構造体として今日各方面で注目され
ている。そのため、これらの製造原料である窒化ケイ素
粉末の製造についても種々研究され、特に工業的に有利
なケイ素（Ｓｌ）の直接窒化法の研究は数多くなされて
いる。Silicon nitride sintered bodies have high mechanical strength and spall resistance, so they are currently attracting attention in various fields as ceramic structures. Therefore, various studies have been conducted on the production of silicon nitride powder, which is a raw material for these productions, and in particular, many studies have been conducted on the industrially advantageous direct nitriding method of silicon (Sl).
このＳｉの直接窒化法の最大の焦点は経済性をいかに持
たせるかであり、従来より８１の反応抑制即ちＳｌの直
接窒化に伴う大きな発熱のコントロールと高品位の維持
に研究が注がれている。例えば、特開昭４８−１０２１
００号公報、特開昭５７−９５８１９号公報′、特開昭
６０−１８６４０６号公報、特開昭６１−６８３１０号
公報等である。The main focus of this method of direct nitriding of Si is how to make it economical, and research has traditionally focused on suppressing 81 reactions, that is, controlling the large amount of heat generated by direct nitriding of Sl, and maintaining high quality. There is. For example, JP-A-48-1021
00, JP-A-57-95819', JP-A-60-186406, JP-A-61-68310, and the like.
しかしながら、何れも理論的な発熱量の回避例えば昇温
速度の微調節、Ａｒ、Ｈｅ等の不活性ガスの導入に限ら
れ、炉の構造についてはまったく触れられていない。従
来は、炉内面がシリカ、マグネシア、アルミナキャスタ
デル等のレンガで構成されてなる炉を用いて窒化を行っ
ていたが、このような炉では単位面積当りの蓄熱量が大
きいので、−旦反応の暴走が起こると炉材の熱的感受性
が遅いので反応を制御することは難しく原料Ｓ１が溶融
してしまう欠点があった。そのためα分率の高い窒化ケ
イ素を得るには相当な熟練が必要であるか又は製造する
ことはできなかった。さらには炉の発熱体についても大
部分はカーボン電極が用いられており、そこからの汚染
即ちＨ２又はＮＨ５との反応で生じるＣＨ４ガスと原料
金属Ｓ１との反応によるＳｉＣの生成による汚染につい
ても考慮されていない。However, all of these are limited to theoretical avoidance of calorific value, such as fine adjustment of the heating rate, and introduction of inert gases such as Ar and He, and do not mention the structure of the furnace at all. Conventionally, nitriding was carried out using a furnace whose inner surface was made of bricks made of silica, magnesia, alumina castadel, etc., but since such furnaces store a large amount of heat per unit area, the reaction was When runaway occurs, it is difficult to control the reaction because the thermal sensitivity of the furnace material is slow, and the raw material S1 has the disadvantage of melting. Therefore, considerable skill is required to obtain silicon nitride with a high alpha fraction, or it has not been possible to produce silicon nitride. Furthermore, carbon electrodes are used for most of the heating elements in furnaces, and contamination from them, that is, contamination due to the formation of SiC due to the reaction between CH4 gas generated by reaction with H2 or NH5 and raw metal S1, is also considered. It has not been.
本発明者は、Ｓｉ等の金属の直接窒化法における反応熱
の制御を円滑に行うのに不可欠な炉の構成及びカービン
電極に代替できる発熱体につき種種検討した結果、本発
明を完成したものである。The present inventor has completed the present invention as a result of examining various types of furnace configurations that are essential for smoothly controlling the reaction heat in the direct nitriding method of metals such as Si, and heating elements that can be substituted for carbine electrodes. be.
〔課題を解決するだめの手段〕
すなわち、本発明は、炉内面がカサ比重０．５以下の無
機繊維質断熱材で内張りされてなりしかもモリブデン発
熱体を備えてなることを特徴とする窒化反応炉、及び該
窒化反応炉に金属粉末を装入しそれを窒素及び／又はア
ンモニアを含む雰囲気下で加熱窒化することを特徴とす
る金属窒化物の製造法である。[Means for Solving the Problems] That is, the present invention provides a nitriding reaction characterized in that the inner surface of the furnace is lined with an inorganic fibrous heat insulating material having a bulk specific gravity of 0.5 or less and is equipped with a molybdenum heating element. This method of producing metal nitrides is characterized by charging metal powder into a furnace and the nitriding reactor, and heating and nitriding it in an atmosphere containing nitrogen and/or ammonia.
以下、さらに詳しく本発明について説明する。The present invention will be explained in more detail below.
本発明で使用する炉の断熱材は、カサ比重が０．５以下
のアルミナファイバー セラミックファイバー ロック
ウール、シリカファイバー等の蓄熱量の小さい結晶質又
はガラス質の無機繊維である。カサ比重が０．５よりも
大きい例えばアルミナ、シリカ、マグネシア等のレンガ
で施工された炉においては一旦発熱反応が始まれば電源
のカットは勿論のこと、Ａｒ、Ｈｅ等の不活性ガスを導
入しても反応を抑制させることは非常に難しい。たとえ
抑制できたとしてもその後の復帰に際し、炉材の熱的感
受性が遅く、エネルギーも多く消費するとともに再暴走
を起こさせることが多く、α分率の高い窒化ケイ素粉末
を得ることは困難となる。The heat insulating material of the furnace used in the present invention is a crystalline or glassy inorganic fiber with a small amount of heat storage, such as alumina fiber, ceramic fiber, rock wool, or silica fiber, which has a bulk specific gravity of 0.5 or less. For example, in a furnace made of bricks made of alumina, silica, magnesia, etc. with a bulk specific gravity greater than 0.5, once an exothermic reaction begins, the power supply must be cut off and an inert gas such as Ar or He must be introduced. However, it is extremely difficult to suppress the reaction. Even if it can be suppressed, the thermal sensitivity of the furnace material is slow and energy is consumed during subsequent recovery, and runaway often occurs again, making it difficult to obtain silicon nitride powder with a high α fraction. .
炉内面の断熱構造は使用温度や負荷等を考慮して適切に
決定する。高温炉の場合は、通常、鉄皮等のケーシング
にガラスファイバーと結晶質ファイバーを順次内張りし
たものが用いられるが、低温炉の場合には、結晶質ファ
イバーを省略することもできる。また、ケーシングは鉄
皮に限らす上記したレンガの場合もあり、さらには、と
くに炉床等のように負荷がかかるところでは、ガラスフ
ァイバーに変えて又はガラスファイバーの施工に先行し
て上記レンガを使用することもできる。なお、負荷のか
かるところでは、カサ比重０．６５〜０．４５程度のボ
ードを使用することが望ましい。The insulation structure of the inner surface of the furnace should be determined appropriately, taking into account the operating temperature, load, etc. In the case of a high-temperature furnace, a casing such as an iron shell is normally lined with glass fiber and crystalline fiber in sequence, but in the case of a low-temperature furnace, the crystalline fiber can be omitted. In addition, the casing may be made of the above-mentioned bricks, which are limited to iron shells.Furthermore, the above-mentioned bricks may be used instead of glass fibers or in advance of the installation of glass fibers, especially in places where loads are applied, such as hearths. You can also use Note that it is desirable to use a board with a bulk specific gravity of about 0.65 to 0.45 in places where loads are applied.
ここで、ガラスファイバーとは、５ｌｏ２系、５ｉ０２
− Ａｔ２０３− ＭｇＯ系等のガラスファイバーで低
温用無機繊維質断熱材であり、結晶質ファイバーとは、
Ａｔ２０３系、Ａｔ ２０３− Ｓ ｉ Ｏ２系、ゐラ
イト系、Ｓｉ３Ｎ４系、ＡｔＮ系等のファイバーで高温
用無機繊維質断熱材である。Here, glass fiber refers to 5lo2 series, 5i02 series
- At203 - A low-temperature inorganic fiber insulation material made of MgO-based glass fiber, etc., and crystalline fiber is
It is an inorganic fiber heat insulating material for high temperature use made of At203-based, At203-S i O2-based, wilite-based, Si3N4-based, and AtN-based fibers.
本発明で使用する発熱体はモリブデン（ＭＯ）であり、
従来のＭｏ５ｉｚ系やＭｏＳｉ□−８ｉＣ系と異なる。The heating element used in the present invention is molybdenum (MO),
This is different from the conventional Mo5iz series and MoSi□-8iC series.
ＭＯ線純度しては、９９％以上好ましくは９９．８％以
上である。従来のモリブデン系の発熱体であっては、Ｎ
Ｈ３、Ｈ２の還元雰囲気では非常に寿命が短かい。また
、従来のようなカーボン（Ｃ）発熱体やＳｉＣ発熱体に
あっては、カーボンは窒化雰囲気に用いるＮＨ３、Ｈ２
と反応してＣＨ，ガスを発生し、さらにそのＣＨ４ガス
が原料Ｓｉと反応してＳｉＣを生じα−窒化ケイ素粉末
の品位を下げる。The MO line purity is 99% or more, preferably 99.8% or more. In conventional molybdenum-based heating elements, N
In a reducing atmosphere of H3 or H2, the life is very short. In addition, in conventional carbon (C) heating elements and SiC heating elements, carbon is used in the nitriding atmosphere, such as NH3 and H2.
The CH4 gas reacts with the raw material Si to generate SiC and lower the quality of the α-silicon nitride powder.
ＳｉＣはＮＨ３、Ｈ２により還元されＳｉＣ発熱体の寿
綿が短かくなるとともに、還元時にＣＨ４ガスが発生し
同様にα−窒化ケイ素粉末の品位を下げる。本発明で用
いるＭＯ発熱体の仕様は棒状、撚線、ワイヤー状等何れ
であってもよい。ＭＯ以外にＷも施工及び価格に若干の
問題を残すが発熱体としては使用可能である。発熱体は
、通常、炉内面に露出して設置される。窒化反応炉は、
パッチ式、連続式例えばコンベアー炉、プッシャー炉、
竪型炉等のいずれであってもよい。SiC is reduced by NH3 and H2, shortening the lifetime of the SiC heating element, and CH4 gas is generated during reduction, which also lowers the quality of the α-silicon nitride powder. The MO heating element used in the present invention may have any shape such as a rod shape, a stranded wire, or a wire shape. In addition to MO, W can also be used as a heating element, although there are some problems with construction and cost. The heating element is usually installed exposed on the inner surface of the furnace. The nitriding reactor is
Patch type, continuous type e.g. conveyor furnace, pusher furnace,
Any type of furnace such as a vertical furnace may be used.
以上のような窒化反応炉を８１の直接窒化法に用い、窒
素の吸収量を考慮した反応熱制御を行えば、α分率９０
％以上のα−窒化ケイ素粉末が経済的に製造できる。す
ｌ譚わち、微細化されたＳ〕粉末をセラミック質の匣鉢
に入れ、それを窒素及び／又はアンモニアを含む雰囲気
中で１４５０°Ｃ程度の温度まで昇温焼成する。If the above-mentioned nitriding reactor is used in the direct nitriding method of 81 and the reaction heat is controlled in consideration of the amount of nitrogen absorbed, the α fraction can be reduced to 90.
% or more of α-silicon nitride powder can be economically produced. The finely divided S] powder is placed in a ceramic pot and fired at a temperature of about 1450° C. in an atmosphere containing nitrogen and/or ammonia.
本発明は、上記したＳ１以外に反応の暴走によって溶融
するおそれのあるＡｔ、 Ｔｉ、Ｃｒ等の金属にも適用
される。The present invention is also applicable to metals other than the above-mentioned S1, such as At, Ti, and Cr, which may melt due to runaway reaction.
以下、実施例と比較例をあげてさらに具体的に本発明を
説明する。Hereinafter, the present invention will be explained in more detail with reference to Examples and Comparative Examples.
実施例１
鉄皮より順にカサ比重が０．１３のロックウール、０．
１６のセラミックファイバーフェルト、０．１６のアル
ミナファイバーボードで内張シされてなり、市販の棒状
ＭＯ発熱体（純度９９．８ ％ ）を炉内面に露出させ
てなる内容積が０−５ ｍ３の窒化反応炉に、４４μｍ
下の８１粉末１００ｇを入れたＡｔｚ０３製匣鉢１ヶを
挿入し、Ｎ２／ ＮＨ３＝ ２／１のモル比で１１ｓｏ
’ｃから５°Ｑ／Ｈｒの速度で１４５０°Ｃまで昇温し
ながら窒化させた。その後、冷却し得られた窒化ケイ素
のα分率を測定したところ９３チであった。Example 1 Rock wool with a bulk specific gravity of 0.13, 0.13 in order from iron shell,
It is lined with 0.16 ceramic fiber felt and 0.16 alumina fiber board, and a commercially available rod-shaped MO heating element (purity 99.8%) is exposed on the inside of the furnace, with an internal volume of 0-5 m3. 44 μm in the nitriding reactor
Insert one Atz03 sagger containing 100g of 81 powder shown below, and make 11so at a molar ratio of N2/NH3=2/1.
Nitriding was carried out while increasing the temperature from 'c to 1450°C at a rate of 5°Q/Hr. Thereafter, the alpha fraction of the silicon nitride obtained after cooling was measured and found to be 93.
実施例２
カサ比重が０．１６のアルミナファイバーボードのかわ
りにカサ比重０．１０の８１３Ｎ４フアイバーボー１を
用いたこと以外は実施例１と全く同様にして窒化ケイ素
を製造したところ、そのα分率は９５％であった。Example 2 Silicon nitride was produced in the same manner as in Example 1 except that 813N4 fiberboard 1 with a bulk specific gravity of 0.10 was used instead of alumina fiberboard with a bulk specific gravity of 0.16. The rate was 95%.
実施例６
炉壁及び天井は鉄皮よシ順にカサ比重が０．１６のロッ
クウール、０．１６のセラミックファイバーフェル１−
１０．１６のアルミナファイバーボードで内張すされて
なシ、シかも炉床は下部鉄皮面にカサ比重が０．９６の
多孔゛質しンガと０．１６のセラミックファイバーフェ
ルトとの組合せ層を設けさらにその上面にカサ比重０．
２５のアルミナファイバーボードで覆、ってな、シ（炉
床全体のカサ比重は０．３５）、市販の棒状ＭＯ発熱体
（粋度９９．８％ ）が炉内面に露出してなる内容積が
２．３の窒化反応炉内に、４４ μｍ下の８１粉末５０
０ｇを入れたＡｔ２０３製匣鉢５０ケを挿入し、Ｎ２
／ ＮＨ３＝ ２／ 、のモル比で１１５０℃から５°
Ｑ ／ Ｈｒの速度で１４５０℃まで昇温しながら窒化
させた。得られた窒化ケイ素のα分率は９３％であった
。Example 6 The furnace walls and ceiling were made of rock wool with a bulk specific gravity of 0.16 and ceramic fiber felt 1- with a bulk specific gravity of 0.16 in order from the iron shell to the iron shell.
The hearth may not be lined with 10.16 alumina fiberboard, but the hearth has a combination layer of porous material with a bulk specific gravity of 0.96 and ceramic fiber felt with a bulk density of 0.16 on the lower steel surface. Furthermore, a bulk specific gravity of 0.
Covered with 25mm alumina fiberboard (the bulk specific gravity of the whole hearth is 0.35), the internal volume is created by exposing a commercially available rod-shaped MO heating element (99.8% pureness) to the inside of the furnace. 81 powder 50 μm below 44 μm was placed in a nitriding reactor with
Insert 50 At203 saggers containing 0g of N2
/ NH3 = 2/, molar ratio from 1150℃ to 5°
Nitriding was carried out while increasing the temperature to 1450°C at a rate of Q/Hr. The α fraction of the obtained silicon nitride was 93%.
比較例１
鉄皮より順にカサ比重が０．９６の多孔質レンガ、１．
５６のアルミナレンガで被覆されてなり、発熱体がカー
ボンである内容積が０．２ ｍ’の窒化炉に、４４ μ
ｍ下の８１粉末４ＤＩを入れたＡｔ２０３製匣鉢１ケを
挿入し、Ｎ２ ／ ＮＨ３＝＝ ２／ １のモル比で１
１５０℃から５℃／Ｈｒの速度で１４５０℃まで昇温し
ながら窒化させた。その結果、得られた窒化ケイ素には
β−８ｉＣが同定されるとともに、そのα分率は６５チ
であった。Comparative Example 1 Porous brick with a bulk specific gravity of 0.96 in order from the iron shell, 1.
A nitriding furnace with an inner volume of 0.2 m' was coated with 56 alumina bricks and the heating element was carbon.
Insert one At203 sagger containing 4 DI of 81 powder under m, and add 1 at a molar ratio of N2/NH3==2/1.
Nitriding was carried out while increasing the temperature from 150°C to 1450°C at a rate of 5°C/Hr. As a result, β-8iC was identified in the obtained silicon nitride, and its α fraction was 65.
比較例２
ＭＯ発熱体のかわりに市販のＳｉＣ発熱体を用いたこと
以外は実施例１と全く同様にして窒化ケイ素を製造した
ところ、α分率は８９チであったが表層部には多くのβ
−８ｉＣが認められた。Comparative Example 2 Silicon nitride was produced in exactly the same manner as in Example 1 except that a commercially available SiC heating element was used instead of the MO heating element. β of
-8iC was observed.
なお、実施例及び比較例で用いたα分率の測定と鉱物の
同定は理学電気（株）のガイガー７ラツクスＲＡＤ −
ｎ ＢのＸ＠回折によった。The measurement of α fraction and the identification of minerals used in the Examples and Comparative Examples were performed using Geiger 7 Lux RAD- manufactured by Rigaku Denki Co., Ltd.
By X@ diffraction of nB.
本発明によれば、金属の直接窒化法により、高品位の金
属窒化物を経済的に製造することができる。According to the present invention, high-grade metal nitrides can be economically produced by direct metal nitridation.
特許出願人 電気化学工業株式会社Patent applicant Denki Kagaku Kogyo Co., Ltd.
Claims (1)
内張りされてなりしかもモリブデン発熱体を備えてなる
ことを特徴とする窒化反応炉。 ２、請求項１記載の窒化反応炉に金属粉末を装入しそれ
を窒素及び／又はアンモニアを含む雰囲気下で加熱窒化
することを特徴とする金属窒化物の製造法。[Scope of Claims] 1. A nitriding reactor characterized in that the inner surface of the reactor is lined with an inorganic fibrous heat insulating material having a bulk specific gravity of 0.5 or less and is equipped with a molybdenum heating element. 2. A method for producing metal nitrides, which comprises charging metal powder into the nitriding reactor according to claim 1 and heating and nitriding it in an atmosphere containing nitrogen and/or ammonia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63220363A JPH0718652B2 (en) | 1988-09-05 | 1988-09-05 | Nitriding reactor and method for producing metal nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63220363A JPH0718652B2 (en) | 1988-09-05 | 1988-09-05 | Nitriding reactor and method for producing metal nitride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0269305A true JPH0269305A (en) | 1990-03-08 |
| JPH0718652B2 JPH0718652B2 (en) | 1995-03-06 |
Family
ID=16749963
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63220363A Expired - Lifetime JPH0718652B2 (en) | 1988-09-05 | 1988-09-05 | Nitriding reactor and method for producing metal nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0718652B2 (en) |
-
1988
- 1988-09-05 JP JP63220363A patent/JPH0718652B2/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| CERAMIC BULLETIN=1952 * |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0718652B2 (en) | 1995-03-06 |
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