JPS63252966A - Manufacture of silicon nitride base ceramic composite body - Google Patents
Manufacture of silicon nitride base ceramic composite bodyInfo
- Publication number
- JPS63252966A JPS63252966A JP62088060A JP8806087A JPS63252966A JP S63252966 A JPS63252966 A JP S63252966A JP 62088060 A JP62088060 A JP 62088060A JP 8806087 A JP8806087 A JP 8806087A JP S63252966 A JPS63252966 A JP S63252966A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- ceramic composite
- sintering
- whiskers
- less
- 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 description 20
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims description 20
- 239000000919 ceramic Substances 0.000 title claims description 16
- 239000002131 composite material Substances 0.000 title claims description 12
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 238000005245 sintering Methods 0.000 claims description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011863 silicon-based powder Substances 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 7
- 238000005121 nitriding Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、窒化ケイ素を主成分とし窒化ケイ素ウィスカ
ーで強化したセラミックス複合体の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing a ceramic composite mainly composed of silicon nitride and reinforced with silicon nitride whiskers.
従来から、窒化ケイ素質セラミックスは靭性に優れしか
も高温における特性劣化が小さいため、セラミックスエ
ンジン等の高温構造部材として期待されてきた。Silicon nitride ceramics have traditionally been expected to be used as high-temperature structural members for ceramic engines and the like because they have excellent toughness and exhibit little property deterioration at high temperatures.
しかし、かかる窒化ケイ素質セラミックスもセラミック
スエンジン等として実用に供されるには信頼性において
未だ不充分であシ、特にその高温特性及び靭性を更に一
層向上させることが必要とされている。However, such silicon nitride ceramics still have insufficient reliability to be put to practical use in ceramic engines, etc., and in particular, it is necessary to further improve their high-temperature properties and toughness.
そこで、窒化ケイ素質セラミックスの高温特性及び靭性
を向上させるために種々の方法が検討され、特に特公昭
６０−３５３１６号等に示されるごとく各種繊維を配合
して強化した複合体に関する研究が数多く行われてきた
。これ等の研究の中でもウィスカーと呼ばれる繊維状単
結晶を用いて強化する方法の開発が急速に進んできてい
る。Therefore, various methods have been investigated to improve the high-temperature properties and toughness of silicon nitride ceramics, and in particular, many studies have been conducted on composites reinforced by blending various fibers, as shown in Japanese Patent Publication No. 35316/1983. It has been. Among these studies, rapid progress has been made in the development of a method for reinforcing materials using fibrous single crystals called whiskers.
しかしながら、窒化ケイ素は焼結が困難であるため、通
常の焼結でも高密度で高強度の焼結体が得がたい上、繊
維やウィスカーを添加すると益々焼結が困難となり、期
待された強度や高温特性及び靭性を得ることができなか
った。従って、窒化ケイ素の繊維強化複合体の焼結には
、これ等の特性を少しでも向上させるためにホットプレ
ス法を採用せざるを得なかった。しかるに、ホットプレ
ス法は製造工程が複雑であって連続焼結が困難なため、
製品コストが非常に高くなる等の欠点があった。However, since silicon nitride is difficult to sinter, it is difficult to obtain a high-density, high-strength sintered body even with normal sintering, and addition of fibers and whiskers makes sintering even more difficult, resulting in lower strength and higher temperatures than expected. characteristics and toughness could not be obtained. Therefore, in order to improve these properties even slightly, it was necessary to adopt the hot press method for sintering a fiber-reinforced composite of silicon nitride. However, the hot press method has a complicated manufacturing process and continuous sintering is difficult.
There were drawbacks such as extremely high product costs.
本発明は、上記した従来の事情に鑑み、ホットプレス法
のような加圧焼結によらなくても、高強度であって、且
つ高温特性及び靭性に優れた窒化ケイ素質セラミックス
複合体を安価に製造できる方法を提供することを目的と
する。In view of the above-mentioned conventional circumstances, the present invention has been made to produce a silicon nitride ceramic composite that has high strength and excellent high-temperature properties and toughness at a low cost without using pressure sintering such as the hot press method. The purpose is to provide a method for manufacturing.
本発明の窒化ケイ素質セラミックス複合体の製造方法は
、１〜７０重量％のβ型窒化ケイ素ウィスカーと実質的
に残部の金属ケイ素粉末とを混合し、この混合物の成形
体を窒素ガス雰囲気中において１３００〜１５００Ｃで
窒化と同時に焼結することを特徴とするものである。The method for producing a silicon nitride ceramic composite of the present invention involves mixing 1 to 70% by weight of β-type silicon nitride whiskers with substantially the remainder of the metal silicon powder, and molding the mixture into a nitrogen gas atmosphere. It is characterized by nitriding and sintering at 1300 to 1500C at the same time.
本方法では、金属ケイ素粉末の成形体を窒化と同時に焼
結する反応焼結によって、ホットプレス等の加圧焼結に
よらなくても緻密な窒化ケイ素質焼結体が得られる。し
かし、金属ケイ素粉末に予め通常の焼結助剤を少量添加
しておき、上記反応焼結に引き続いてＨｌ等によシ加圧
焼結するか、又は高温焼結を行い、更に加圧緻密化する
ことも可能であシ、本発明の範囲に含まれる。In this method, a dense silicon nitride sintered body can be obtained by reactive sintering in which a molded body of metallic silicon powder is sintered at the same time as nitriding, without using pressure sintering such as hot pressing. However, a small amount of a normal sintering aid is added to the metal silicon powder in advance, and following the reaction sintering described above, pressure sintering is performed using Hl, etc., or high temperature sintering is performed, and then pressure densification is performed. However, it is also possible to change the structure to a different one, and it is within the scope of the present invention.
本発明においては、強化用の繊維としてβ型窒化ケイ素
（β−８ｉ３Ｎ４ ）ウィスカーを使用する。In the present invention, β-type silicon nitride (β-8i3N4) whiskers are used as reinforcing fibers.
β−８ｉ３Ｎ４ウイスカーは高温型でα型（低温型）に
比べて安定であり、反応焼結によっても損傷が少ないた
め、複合体中で本来の特性を維持して十分な補強効果が
得られる。β-8i3N4 whiskers are of the high temperature type and are more stable than the α type (low temperature type), and are less damaged by reaction sintering, so they maintain their original properties in the composite and can provide a sufficient reinforcing effect.
β−３ｉ３Ｎ４ウイスカーの使用量は１〜７０重量％と
する。１重量％未満ではウィスカー添加による補強効果
がほとんどなく、７０重量％をこえると焼結体の緻密化
が困難だからである。又、使用するβ−８ｉ３Ｎ４ウイ
スカーは短径が２μｍ以下及び長さが１騙以下で、アス
被りト比（長さ／短径の比）が１０００以下のものが好
ましい。短径が２μｍをこえるとウィスカーの強度が低
下するので添加による補強効果が小さく、又長さが１０
をこえると金属ケイ素との混合中に損傷を受けやすく取
り扱いが困難だからである。The amount of β-3i3N4 whiskers used is 1 to 70% by weight. This is because if the whisker addition is less than 1% by weight, there is almost no reinforcing effect, and if it exceeds 70% by weight, it is difficult to make the sintered body dense. Further, the β-8i3N4 whiskers used preferably have a minor axis of 2 μm or less, a length of 1 square or less, and an asperity coverage ratio (length/minor axis ratio) of 1000 or less. If the short axis exceeds 2 μm, the strength of the whisker decreases, so the reinforcing effect of addition is small, and the length exceeds 10 μm.
This is because if the amount exceeds 100%, it will be easily damaged during mixing with metal silicon and will be difficult to handle.
更に、本発明においては、原料粉末として金属ケイ素の
粉末を使用し、窒化と同時に焼結する反応焼結を採用し
ている。この反応焼結は窒素ガス雰囲気中において１３
００〜１５００Ｃで行う。反応温度が１３００Ｃ未満で
は窒化反応が十分に進行せず、逆に温度が１５００Ｃを
こえるとケイ素の溶融等の問題が生じるからである。又
、使用する金属ケイ素粉末は、粗粒粉末では窒化反応が
進行し難い為、平均粒径が２μｍ以下の微粉末が好まし
い。Further, in the present invention, metallic silicon powder is used as the raw material powder, and reaction sintering is employed in which sintering is performed simultaneously with nitriding. This reaction sintering is carried out in a nitrogen gas atmosphere.
It is carried out at 00-1500C. This is because if the reaction temperature is less than 1300C, the nitriding reaction will not proceed sufficiently, whereas if the temperature exceeds 1500C, problems such as melting of silicon will occur. Further, the metal silicon powder used is preferably a fine powder with an average particle size of 2 μm or less, since the nitriding reaction does not easily proceed with coarse powder.
下表に示す配合比でβ−８ｉ３Ｎ４ウイスカー （短径
０．５μｍ、長さ５０μｍ）を金属Ｓｉ粉末（平均粒径
２μｍ）に添加し、十分に混合した後、静水圧プｖｙ、
して１０ｊＩＩｘｌＯｊＩＩ＋×４０ＩＩＩＩの成形体
を得た。β-8i3N4 whiskers (minor diameter 0.5 μm, length 50 μm) were added to metal Si powder (average particle size 2 μm) at the mixing ratio shown in the table below, and after thorough mixing, hydrostatic pressure was applied.
A molded article of 10jIIxlOjII+×40III was obtained.
この成形体を１気圧の窒素ガス雰囲気中において１３５
０Ｃの温度で１０時間窒化させると同時に焼結して反応
焼結体を夫々製造した。This molded body was placed in a nitrogen gas atmosphere of 1 atm at 135°C.
Reactive sintered bodies were manufactured by nitriding at a temperature of 0C for 10 hours and sintering at the same time.
比較例として、上記実施例と同様に実施したが、β−８
ｉ３Ｎ４ウイスカーの代りにα−８ｉ３Ｎ４ウイスカー
（短径及び長さは上記β型と同様）を４０重量％添加し
た比較例ａ、及びβ−８ｉ３Ｎ４ウイスカーを添加しな
い比較例すを夫々製造した。As a comparative example, it was carried out in the same manner as in the above example, but β-8
Comparative Example A in which 40% by weight of α-8i3N4 whiskers (breadth axis and length are the same as the above β type) instead of i3N4 whiskers, and Comparative Example S in which β-8i3N4 whiskers were not added were prepared.
得られた各実施例及び比較例について、相対密度（％）
、室温及び高温（１３００Ｃ）での強度（ｋｙ／−）、
並びにシャルピー衝撃値（ｋｙ・ｍ／ｃｔｌ）を測定し
、その結果を下表に併せて示した。Relative density (%) for each example and comparative example obtained
, strength at room temperature and high temperature (1300C) (ky/-),
In addition, the Charpy impact value (ky·m/ctl) was measured, and the results are also shown in the table below.
（注）表中の試料ａ及びｂ、並びに＊印を付した試料ｌ
及び７は比較例である。(Note) Samples a and b in the table, and samples l marked with *
and 7 are comparative examples.
上記の表から、本発明のセラミックス複合体はシャルピ
ー衝撃値が非常に高く、し、かも高温強度のも優れてい
ることがわかる。又、含有されるウィスカーがα−８ｉ
３Ｎ４の場合には、強度及びシャルピー衝撃値ともに著
しく劣ることがわかる。From the above table, it can be seen that the ceramic composite of the present invention has a very high Charpy impact value and is also excellent in high temperature strength. In addition, the whiskers contained are α-8i
It can be seen that in the case of 3N4, both the strength and the Charpy impact value are significantly inferior.
本発明によれば、高密度で高強度であって、高温特性や
靭性にも優れた窒化ケイ素質セラミックス複合体を安価
に提供することができる。According to the present invention, a silicon nitride ceramic composite having high density, high strength, and excellent high-temperature properties and toughness can be provided at a low cost.
従って、この窒化ケイ素質セラミックス複合体はガスタ
ービン部材やセラミックスエンジン部材等の高温強度並
びに高信頼性を要求される用途に好適なばかりか、切削
用工具等の耐摩耗部材としても優れた性能を発揮するも
のである。Therefore, this silicon nitride ceramic composite is not only suitable for applications that require high-temperature strength and high reliability, such as gas turbine components and ceramic engine components, but also has excellent performance as a wear-resistant component for cutting tools, etc. It is something that can be demonstrated.
Claims (3)
質的に残部の金属ケイ素粉末とを混合し、この混合物の
成形体を窒素ガス雰囲気中において１３００〜１５００
℃で窒化と同時に焼結することを特徴とする窒化ケイ素
質セラミックス複合体の製造方法。(1) 1 to 70% by weight of β-type silicon nitride whiskers and substantially the remainder of the metal silicon powder are mixed, and a molded product of this mixture is heated to 1300 to 1500% by weight in a nitrogen gas atmosphere.
A method for producing a silicon nitride ceramic composite characterized by nitriding and sintering simultaneously at ℃.
及び長さが１ｍｍ以下であることを特徴とする特許請求
の範囲（１）記載の窒化ケイ素質セラミックス複合体の
製造方法。(2) The method for producing a silicon nitride ceramic composite according to claim (1), wherein the β-type silicon nitride whisker has a short axis of 2 μm or less and a length of 1 mm or less.
とを特徴とする特許請求の範囲（１）記載の窒化ケイ素
質セラミックス複合体の製造方法。(3) The method for producing a silicon nitride ceramic composite according to claim (1), wherein the metal silicon powder has an average particle size of 2 μm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62088060A JPS63252966A (en) | 1987-04-10 | 1987-04-10 | Manufacture of silicon nitride base ceramic composite body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62088060A JPS63252966A (en) | 1987-04-10 | 1987-04-10 | Manufacture of silicon nitride base ceramic composite body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63252966A true JPS63252966A (en) | 1988-10-20 |
| JPH0545551B2 JPH0545551B2 (en) | 1993-07-09 |
Family
ID=13932303
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62088060A Granted JPS63252966A (en) | 1987-04-10 | 1987-04-10 | Manufacture of silicon nitride base ceramic composite body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63252966A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01252583A (en) * | 1988-03-31 | 1989-10-09 | Aisin Seiki Co Ltd | High tough ceramics |
| EP0650943A1 (en) * | 1993-10-25 | 1995-05-03 | Bayer Ag | Process for producing dense silicon nitride materials |
| JP2011063497A (en) * | 2009-09-18 | 2011-03-31 | Kubota Corp | Ceramic filter, and method for producing ceramic filter |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627672A (en) * | 1985-07-04 | 1987-01-14 | 株式会社 香蘭社 | Manufacture of fiber reinforced silicon nitride ceramic |
-
1987
- 1987-04-10 JP JP62088060A patent/JPS63252966A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627672A (en) * | 1985-07-04 | 1987-01-14 | 株式会社 香蘭社 | Manufacture of fiber reinforced silicon nitride ceramic |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01252583A (en) * | 1988-03-31 | 1989-10-09 | Aisin Seiki Co Ltd | High tough ceramics |
| EP0650943A1 (en) * | 1993-10-25 | 1995-05-03 | Bayer Ag | Process for producing dense silicon nitride materials |
| JP2011063497A (en) * | 2009-09-18 | 2011-03-31 | Kubota Corp | Ceramic filter, and method for producing ceramic filter |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0545551B2 (en) | 1993-07-09 |
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