JPH06100303A - Production of silicon nitride powder - Google Patents
Production of silicon nitride powderInfo
- Publication number
- JPH06100303A JPH06100303A JP4249063A JP24906392A JPH06100303A JP H06100303 A JPH06100303 A JP H06100303A JP 4249063 A JP4249063 A JP 4249063A JP 24906392 A JP24906392 A JP 24906392A JP H06100303 A JPH06100303 A JP H06100303A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- powder
- nitride powder
- particle size
- phase
- 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
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 39
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000000843 powder Substances 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 6
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 5
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 239000011812 mixed powder Substances 0.000 claims abstract description 4
- 238000005121 nitriding Methods 0.000 claims description 11
- 238000010298 pulverizing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 description 14
- 239000010703 silicon Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- -1 silicon halide Chemical class 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、高強度、高靱性且つ高
信頼性の焼結体を製造することができる窒化けい素粉末
の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a silicon nitride powder capable of producing a sintered body having high strength, high toughness and high reliability.
【０００２】[0002]
【従来の技術】窒化けい素焼結体は、強度、硬度、靱
性、耐熱性、耐食性、耐熱衝撃性、耐衝撃性に優れた材
料であることから、各種産業機構部品、自動車部品、ガ
スタービン部品等での利用が進められている。2. Description of the Related Art Sintered silicon nitride is a material excellent in strength, hardness, toughness, heat resistance, corrosion resistance, thermal shock resistance, and shock resistance, so that it is used in various industrial mechanism parts, automobile parts, gas turbine parts. Etc. are being used.
【０００３】窒化けい素粉末の製造法としては、金属け
い素直接窒化法、シリカ還元法、ハロゲン化けい素法が
工業化されている。これらの製法で得られた粉末は、そ
れぞれ異なった粉体特性を有し、焼結性や焼結体特性に
大きな影響を与えている。As a method for producing silicon nitride powder, a metal silicon direct nitriding method, a silica reduction method, and a silicon halide method have been industrialized. The powders obtained by these manufacturing methods have different powder characteristics, and have a great influence on the sinterability and the characteristics of the sintered body.
【０００４】従来より、結晶性の点からは高α相の窒化
けい素粉末が良いとされ、その観点にたった多くの研究
が行われている。高α相の窒化けい素粉末は、主として
ファインセラミックス用原料に使用されているが、それ
を製造するには非常に精密な窒化反応のコントロールと
長い反応時間が必要であり、β相の粉末に比べて製造コ
ストが高くなることが問題である。From the viewpoint of crystallinity, silicon nitride powder having a high α phase has been conventionally considered to be good, and many studies have been conducted from that viewpoint. High α-phase silicon nitride powder is mainly used as a raw material for fine ceramics, but it requires very precise control of the nitriding reaction and long reaction time to produce it. The problem is that the manufacturing cost is higher.
【０００５】これに対し、高β相含有の窒化けい素粉末
は、その焼結体の製造において微構造制御が容易である
という特徴を有しているが、物性のバラツキ、不純物量
等においてファインセラミックス用原料として使用でき
るレベルではなかった。On the other hand, the silicon nitride powder having a high β-phase content is characterized in that it is easy to control the microstructure in the production of the sintered body, but the variation in physical properties, the amount of impurities, etc. are fine. It was not at a level that could be used as a raw material for ceramics.
【０００６】すなわち、従来の高β相含有の窒化けい素
粉末は、β相が90％程度であり、しかもそのバラツキも
大きかったので、残りのα相窒化けい素の影響を受け、
焼結体の製造において微構造をうまく制御することがで
きなかった。That is, since the conventional β-phase-containing silicon nitride powder has a β phase of about 90% and its variation is large, it is affected by the remaining α-phase silicon nitride.
The microstructure could not be well controlled in the production of sintered bodies.
【０００７】このように、従来技術では、高β相含有窒
化けい素の特徴を十分に発揮させることのできるβ分率
98％以上の窒化けい素粉末を、工業的に安定して製造す
る技術はなく、その出現が待たれていた。As described above, in the prior art, the β fraction capable of sufficiently exerting the characteristics of the high β phase-containing silicon nitride.
There is no technology to produce 98% or more of silicon nitride powder in an industrially stable manner, and its appearance has been awaited.
【０００８】[0008]
【発明が解決しようとする課題】本発明の目的は、上記
要望に応えたものであって、β相が98％以上をも可能と
する窒化けい素粉末を工業的に安定して製造する方法を
提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to meet the above-mentioned needs, and to provide a method for industrially stably producing a silicon nitride powder having a β phase of 98% or more. To provide.
【０００９】[0009]
【課題を解決するための手段】すなわち、本発明は、粒
度295 μm 以下の金属シリコン粉末50重量％以上と、β
相90％以上で粒度295 μm 以下の窒化けい素粉末50重量
％以下（0 は含まず）との混合粉末により嵩密度1.5 ｇ
／cm3 以下の成型体を成形し、それを温度1200℃以上に
維持しながら窒素及び／又はアンモニア雰囲気中で窒化
してインゴットを製造した後、それを粉砕することを特
徴とする窒化けい素粉末の製造方法である。[Means for Solving the Problems] That is, the present invention comprises 50% by weight or more of metallic silicon powder having a particle size of 295 μm or less and β
Bulk density of 1.5 g by mixing powder with 90% or more phase and 50% by weight or less (not including 0) of silicon nitride powder with a particle size of 295 μm or less
A silicon nitride characterized by forming a molded body of not more than 1 cm 3 / cm 3 and nitriding it in a nitrogen and / or ammonia atmosphere while maintaining the temperature at 1200 ° C. or more to produce an ingot, and then crushing it. It is a method for producing powder.
【００１０】以下、本発明をさらに詳しく説明する。The present invention will be described in more detail below.
【００１１】本発明では、原料として、金属シリコンを
微粉砕し48メッシュ篩（295 μm ）好ましくは65メッシ
ュ篩（208 μm ）にて分級し全通したものに、β相が90
％以上で粒度が295 μm 以下である窒化けい素粉末（以
下、骨材という）50重量％以下（0 は含まず）、反応の
均一化及び経済性を考慮して、好ましくは10〜40重量％
を混合したものを用いる。金属シリコンと骨材はできる
だけ高純度であることが好ましいが、いずれも95重量％
程度もあれば十分である。In the present invention, as a raw material, metallic silicon is finely pulverized and classified with a 48-mesh sieve (295 μm), preferably a 65-mesh sieve (208 μm), and passed through the whole to obtain a β-phase of 90.
% Or more and a particle size of 295 μm or less and silicon nitride powder (hereinafter referred to as aggregate) 50% by weight or less (0 is not included), considering the homogenization of reaction and economy, preferably 10 to 40% by weight %
A mixture of is used. It is preferable that the metallic silicon and the aggregate have the highest possible purity, but both are 95% by weight.
A degree is enough.
【００１２】金属シリコンの粒度が295 μm よりも大き
いと、内部まで速やかに反応せず金属シリコンが残留す
る。一方、骨材の粒度が295 μm よりも大きかったり、
骨材を混合しないと、窒化反応時に発生する反応熱がこ
もり、融着が起こって未反応金属シリコンの残留につな
がる。骨材のβ相が90％未満では強度のばらつきを示す
ワイブル係数が小さくなる。If the particle size of the metallic silicon is larger than 295 μm, the metallic silicon remains without reacting rapidly to the inside. On the other hand, the particle size of the aggregate is larger than 295 μm,
If the aggregate is not mixed, the reaction heat generated during the nitriding reaction is retained, and fusion occurs, resulting in the unreacted metallic silicon remaining. When the β phase of the aggregate is less than 90%, the Weibull coefficient showing the variation in strength becomes small.
【００１３】本発明では、上記金属シリコンと骨材との
混合粉末を嵩密度1.5 ｇ／cm3 以下好ましくは1.4 ｇ／
cm3 以下の成型体に成形し、それを窒素及び／又はアン
モニアを含む雰囲気中で窒化する。ここで成型体の嵩密
度が1.5 ｇ／cm3 をこえると、成型体内部に反応ガスが
行き届かなかったり、反応熱がこもって内部に未反応の
金属シリコンが残留する。In the present invention, the mixed powder of the above-mentioned metallic silicon and the aggregate has a bulk density of 1.5 g / cm 3 or less, preferably 1.4 g / cm 3.
A molded body having a size of cm 3 or less is formed and nitrided in an atmosphere containing nitrogen and / or ammonia. Here, if the bulk density of the molded body exceeds 1.5 g / cm 3 , the reaction gas does not reach the inside of the molded body or the reaction heat remains and unreacted metallic silicon remains inside.
【００１４】また、成型体の多数を一度に窒化する場合
は、それらの成型体間に適当な間隔がないと、同様にし
て未反応の金属シリコンが残留したり、α相が増加した
りして目標とするβ分率が得られなくなる。未反応の金
属シリコンの存在は、窒化けい素粉末の特性を著しく損
なうので、好ましくはその量を0.3 重量％以下に抑える
ように配慮する。Further, when a large number of molded bodies are nitrided at a time, unreacted metallic silicon may remain or the α phase may increase in the same manner if there is no proper space between the molded bodies. As a result, the target β fraction cannot be obtained. Since the presence of unreacted metallic silicon seriously impairs the properties of the silicon nitride powder, it is preferable to control the amount thereof to 0.3% by weight or less.
【００１５】そのためには、成型体一個の厚みはあまり
厚くせず、具体的には厚みが50mm程度以下の直方体とす
るのが望ましい。成型体の多数を一度に窒化する場合
は、成型体間に十分窒化ガスが流れるよう5 〜50mm程度
の間隔を設けるのがよい。For that purpose, it is desirable that the thickness of one molded body is not so thick, and specifically, it is a rectangular parallelepiped having a thickness of about 50 mm or less. When nitriding a large number of molded products at one time, it is preferable to provide an interval of about 5 to 50 mm between the molded products so that the nitriding gas can flow sufficiently.
【００１６】嵩密度1.5 ｇ／cm3 以下の成型体を成形す
るには、あまり圧力をかけずに成形するか、または樹脂
バインダーを用いて成形した後脱脂することよって行う
ことができる。A molded product having a bulk density of 1.5 g / cm 3 or less can be molded by applying less pressure, or by molding with a resin binder and then degreasing.
【００１７】本発明においては、窒化反応温度は常に12
00℃以上にする必要がある。1200℃よりも低い温度で成
型体を窒化炉に投入し窒化を開始した場合は、低温で安
定なα相窒化けい素が生成しやすくなり、目標とする高
β相含有の窒化けい素が得られなくなる。なお、成型体
を投入した際に炉内温度が若干低下するので、その補充
は外部加熱により行う。外部加熱によっても温度制御が
追いつかない場合は、1200℃よりも高温たとえば1300℃
程度に保持された炉に成型体を投入する。In the present invention, the nitriding reaction temperature is always 12
It is necessary to raise the temperature above 00 ℃. If the molded body is put into a nitriding furnace at a temperature lower than 1200 ° C and nitriding is started, stable α-phase silicon nitride is easily generated at a low temperature, and the target silicon nitride containing a high β-phase is obtained. I will not be able to. Since the temperature inside the furnace is slightly lowered when the molded body is charged, the replenishment is performed by external heating. If the temperature control cannot keep up with external heating, the temperature is higher than 1200 ℃, for example 1300 ℃.
The molded body is put into a furnace maintained at a certain degree.
【００１８】原料成型体の搬入と製造された窒化けい素
インゴットの搬出は、バッチ式、半連続式及び連続式の
いずれの手段でも行うことができる。窒化ガスとして
は、窒素及び／又はアンモニアを含むガスが用いられ
る。The raw material compacts can be carried in and the manufactured silicon nitride ingot can be carried out by any means of batch type, semi-continuous type and continuous type. A gas containing nitrogen and / or ammonia is used as the nitriding gas.
【００１９】得られた窒化けい素インゴットは、比表面
積2 ｍ2/ｇ以上の粉末度に粉砕することが望ましい。粉
砕機としては、ロールクラッシャー、ボールミル等が使
用される。It is desirable that the obtained silicon nitride ingot be pulverized to have a specific surface area of 2 m 2 / g or more. A roll crusher, a ball mill or the like is used as the crusher.
【００２０】本発明において、窒化けい素粉末の結晶相
の割合は、α相のＩ102 とＩ201 及びβ相のＩ101 とＩ
210 の回折ピーク強度比をＸ線回折法により求め、次式
によって算出することができる。In the present invention, the crystal phase ratio of the silicon nitride powder is I 102 and I 201 of α phase and I 101 and I of β phase.
The diffraction peak intensity ratio of 210 can be obtained by the X-ray diffraction method and calculated by the following equation.
【００２１】β分率(%) ＝｛（Ｉβ101 ＋Ｉβ210)／
（Ｉα102 ＋Ｉα201 ＋Ｉβ101 ＋Ｉβ210)｝× 100Β fraction (%) = {(Iβ 101 + Iβ 210 ) /
(Iα 102 + Iα 201 + Iβ 101 + Iβ 210 )} × 100
【００２２】[0022]
【実施例】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。EXAMPLES The present invention will be described in more detail with reference to Examples and Comparative Examples.
【００２３】実施例１ 金属シリコンをボールミルで粉砕後、振動篩（65メッシ
ュ）にて分級し 208μm 下の金属シリコン（純度97重量
％）粉末を得た。この金属シリコン粉末60重量部と、骨
材としてβ相が95％で粒度が50μm 以下の窒化けい素粉
末40重量部(40重量％）とをＶ型混合機で１時間混合し
た。得られた混合粉末を底面積が100 ×100mm の金型を
用いて成型体の最も厚い部分が40mmである嵩密度1.4 ｇ
／cm3 の成型体を成形した。Example 1 Metallic silicon was pulverized with a ball mill and then classified with a vibrating sieve (65 mesh) to obtain metallic silicon (purity 97% by weight) powder having a particle size of 208 μm. 60 parts by weight of this metallic silicon powder and 40 parts by weight (40% by weight) of silicon nitride powder having a β phase of 95% and a particle size of 50 μm or less as an aggregate were mixed for 1 hour with a V-type mixer. The obtained mixed powder was used in a mold having a bottom area of 100 × 100 mm, and the thickest part of the molded body was 40 mm. Bulk density 1.4 g
A molded body of / cm 3 was molded.
【００２４】上記成型体を黒鉛製棚板の上に30mmの間隔
を設けて並べ、温度1300℃に保持された炉内に搬入し
た。炉内は、窒素雰囲気であり、原料成型体搬入の際に
空気が入らぬよう若干加圧（大気圧＋100 mm H2O程度）
されている。The above-mentioned molded products were arranged on a graphite shelf plate at intervals of 30 mm, and loaded into a furnace maintained at a temperature of 1300 ° C. The furnace is in a nitrogen atmosphere, and is slightly pressurized (atmospheric pressure + 100 mm H 2 O) so that air does not enter when the raw material compacts are loaded.
Has been done.
【００２５】温度1300℃で成型体を搬入してから外部加
熱及び自己発熱により1450℃まで昇温させその温度で５
時間保持した後自然冷却した。得られたインゴットを炉
から取り出して粉砕し窒化けい素粉末を製造した。After the molded body was carried in at a temperature of 1300 ° C., the temperature was raised to 1450 ° C. by external heating and self-heating, and at that temperature, 5
After holding for a time, it was naturally cooled. The obtained ingot was taken out of the furnace and pulverized to produce a silicon nitride powder.
【００２６】実施例２ 粒度295 μm 下（48メッシュ篩) の金属シリコン粉末を
用いたこと、及び骨材の配合量を60重量部（50重量％）
としたこと以外は、実施例１と同様にして窒化けい素粉
末を製造した。Example 2 Metallic silicon powder having a particle size of 295 μm (48 mesh sieve) was used, and the amount of the aggregate was 60 parts by weight (50% by weight).
A silicon nitride powder was produced in the same manner as in Example 1 except that the above was adopted.
【００２７】比較例１ 粒度495 μm 下（32メッシュ篩) の金属シリコン粉末を
用いたこと以外は実施例１と同様にして窒化けい素粉末
を製造した。Comparative Example 1 Silicon nitride powder was produced in the same manner as in Example 1 except that metallic silicon powder having a particle size of 495 μm (32 mesh sieve) was used.
【００２８】比較例２ 粒度１mm以下の骨材を用いたこと以外は実施例１と同様
にして窒化けい素粉末を製造した。Comparative Example 2 A silicon nitride powder was produced in the same manner as in Example 1 except that an aggregate having a grain size of 1 mm or less was used.
【００２９】比較例３ 嵩密度1.7 ｇ／cm3 の成型体を用いたこと以外は実施例
１と同様にして窒化けい素粉末を製造した。Comparative Example 3 Silicon nitride powder was produced in the same manner as in Example 1 except that a molded body having a bulk density of 1.7 g / cm 3 was used.
【００３０】比較例４ 成型体搬入時の炉内温度を1100℃としたこと以外は実施
例１と同様にして窒化けい素粉末を製造した。Comparative Example 4 Silicon nitride powder was produced in the same manner as in Example 1 except that the temperature inside the furnace at the time of carrying the molded body was 1100 ° C.
【００３１】比較例５ 骨材を用いなかったこと以外は実施例１と同様にして窒
化けい素粉末を製造した。Comparative Example 5 A silicon nitride powder was produced in the same manner as in Example 1 except that the aggregate was not used.
【００３２】比較例６ β分率が50％の骨材を用いたこと以外は実施例１と同様
にして窒化けい素粉末を製造した。Comparative Example 6 Silicon nitride powder was produced in the same manner as in Example 1 except that aggregate having a β fraction of 50% was used.
【００３３】上記実施例１〜２と比較例１〜６における
窒化けい素粉末の製造条件及び得られた窒化けい素粉末
のβ分率と未反応のシリコン（Si）量の測定結果を表１
に示す。Table 1 shows the production conditions of the silicon nitride powder in Examples 1 and 2 and Comparative Examples 1 to 6 and the measurement results of the β fraction of the obtained silicon nitride powder and the amount of unreacted silicon (Si).
Shown in.
【００３４】なお、β分率は上記方法により、また、未
反応のSi量は、プレス成型した試料をＸ線回折装置によ
り測定し、２θ＝27〜30°間でのSi（111)面のピーク面
積（積分強度）を求め、あらかじめ同一条件で作成され
た検量線により算出した。The β fraction was measured by the above method, and the unreacted Si amount was measured by a press-molded sample by an X-ray diffractometer, and the Si (111) plane of 2θ = 27 to 30 ° was measured. The peak area (integrated intensity) was obtained and calculated from a calibration curve prepared under the same conditions in advance.
【００３５】[0035]
【表１】 [Table 1]
【００３６】上記で得られた窒化けい素粉末92重量％、
平均粒径1.5 μm のＹ2 Ｏ3 粉末5重量％及び平均粒径
0.8 μm のＡｌ2 Ｏ3 粉末3 重量％を配合し、1,1,1-ト
リクロロエタン中で4 時間ボールミルで混合し乾燥した
後、100 Kg/cm2の圧力で6 ×10×60mmの成型体を成形
し、それを圧力2700Kg/cm2でＣＩＰ成形した。92% by weight of the silicon nitride powder obtained above,
5% by weight of Y 2 O 3 powder having an average particle size of 1.5 μm and an average particle size
3 μ% by weight of 0.8 μm Al 2 O 3 powder was mixed, mixed in 1,1,1-trichloroethane for 4 hours in a ball mill and dried, and then a 6 × 10 × 60 mm compact was formed at a pressure of 100 Kg / cm 2. Was molded and CIP molded at a pressure of 2700 Kg / cm 2 .
【００３７】このＣＩＰ成型体をカーボンルツボにセッ
トし、圧力10Kg/cm2のＮ2 ガス雰囲気中、温度1900℃で
4 時間焼成して焼結体を製造した。それを3 ×4 ×40mm
に研削加工後、アルキメデス法による焼結体密度と室温
における4 点曲げ強度を島津製作所社製「オートグラフ
ＡＧ−２０００Ａ」を用いて測定した。それらの結果を
表２に示す。This CIP molded body was set in a carbon crucible, and at a temperature of 1900 ° C. in a N 2 gas atmosphere with a pressure of 10 kg / cm 2.
A sintered body was manufactured by firing for 4 hours. 3 x 4 x 40 mm
After grinding, the density of the sintered body by the Archimedes method and the 4-point bending strength at room temperature were measured using "Autograph AG-2000A" manufactured by Shimadzu Corporation. The results are shown in Table 2.
【００３８】[0038]
【表２】 [Table 2]
【００３９】[0039]
【発明の効果】本発明によれば、β相が98％以上の窒化
けい素粉末を工業的に且つ安定して製造することができ
る。According to the present invention, a silicon nitride powder having a β phase of 98% or more can be industrially and stably produced.
フロントページの続き (72)発明者 広津留 秀樹 福岡県大牟田市新開町１ 電気化学工業株 式会社大牟田工場内 (72)発明者 磯崎 啓 福岡県大牟田市新開町１ 電気化学工業株 式会社大牟田工場内Front page continuation (72) Inventor Hideki Hirotsuru 1 Shinkai-cho, Omuta City, Fukuoka Prefecture Omuta Plant, Electrochemical Industry Co., Ltd. (72) Inventor, Kei Kei Isozaki Omuta Factory, Shinkai-cho, Omuta City, Fukuoka Prefecture Within
Claims (1)
重量％以上と、β相90％以上で粒度295 μm 以下の窒化
けい素粉末50重量％以下（0 は含まず）との混合粉末に
より嵩密度1.5 ｇ／cm3 以下の成型体を成形し、それを
温度1200℃以上に維持しながら窒素及び／又はアンモニ
ア雰囲気中で窒化してインゴットを製造した後、それを
粉砕することを特徴とする窒化けい素粉末の製造方法。1. A metallic silicon powder 50 having a particle size of 295 μm or less.
A molded body having a bulk density of 1.5 g / cm 3 or less is formed by a mixed powder of 50% by weight or more and 50% by weight or less (not including 0) of silicon nitride powder having a β phase of 90% or more and a particle size of 295 μm or less, A method for producing silicon nitride powder, which comprises nitriding it in a nitrogen and / or ammonia atmosphere while maintaining it at a temperature of 1200 ° C. or higher to produce an ingot, and then pulverizing the ingot.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24906392A JP3255302B2 (en) | 1992-09-18 | 1992-09-18 | Method for producing silicon nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24906392A JP3255302B2 (en) | 1992-09-18 | 1992-09-18 | Method for producing silicon nitride powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06100303A true JPH06100303A (en) | 1994-04-12 |
| JP3255302B2 JP3255302B2 (en) | 2002-02-12 |
Family
ID=17187462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24906392A Expired - Fee Related JP3255302B2 (en) | 1992-09-18 | 1992-09-18 | Method for producing silicon nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3255302B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010228836A (en) * | 2009-03-26 | 2010-10-14 | Allied Material Corp | Powder filling method and powder filling apparatus |
| JPWO2023190968A1 (en) * | 2022-03-31 | 2023-10-05 |
-
1992
- 1992-09-18 JP JP24906392A patent/JP3255302B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010228836A (en) * | 2009-03-26 | 2010-10-14 | Allied Material Corp | Powder filling method and powder filling apparatus |
| JPWO2023190968A1 (en) * | 2022-03-31 | 2023-10-05 | ||
| WO2023190968A1 (en) * | 2022-03-31 | 2023-10-05 | 株式会社プロテリアル | Method for producing silicon nitride substrate |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3255302B2 (en) | 2002-02-12 |
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