JPH02167864A - Method for heat-treating calcined sialon body - Google Patents
Method for heat-treating calcined sialon bodyInfo
- Publication number
- JPH02167864A JPH02167864A JP63322179A JP32217988A JPH02167864A JP H02167864 A JPH02167864 A JP H02167864A JP 63322179 A JP63322179 A JP 63322179A JP 32217988 A JP32217988 A JP 32217988A JP H02167864 A JPH02167864 A JP H02167864A
- Authority
- JP
- Japan
- Prior art keywords
- strength
- calcined
- sialon
- oxygen gas
- containing oxygen
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001882 dioxygen Inorganic materials 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 3
- 238000011282 treatment Methods 0.000 abstract description 12
- 238000010791 quenching Methods 0.000 abstract description 9
- 230000000171 quenching effect Effects 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000035939 shock Effects 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- 238000005452 bending Methods 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000007423 decrease Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005468 ion implantation Methods 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910001719 melilite Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はサイアロン焼結体の強度を改善する熱処理方法
に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a heat treatment method for improving the strength of a sialon sintered body.
〔従来の技術］
一般にセラミック焼結体は破壊靭性に乏しくセラミック
製部品の強度は機械加工等により表面にクラックが導入
されると著しく低下する。先に特許出願したサイアロン
焼結体（特願昭６３−１３０３３９号）も通常６０〜８
０ｋｇｆ／ｍ２の曲げ強度を有するが、仕上げ加工が悪
いと４０ｋｇｆ／ｍｍ”に低下し、また強度のバラツキ
も大きくなる。そこで、最終加工を施したセラミック焼
結体の強度上昇を目的とした処理方法にはイオン注入や
ＰＶＤＳＣＶＤを利用し異材料をコーティングするなど
の表面改質方法が広く知られている。[Prior Art] Ceramic sintered bodies generally have poor fracture toughness, and the strength of ceramic parts is significantly reduced when cracks are introduced into the surface due to machining or the like. The Sialon sintered body (Patent Application No. 63-130339), for which a patent application was previously applied, is usually 60 to 8
It has a bending strength of 0 kgf/m2, but if the finishing process is poor, the bending strength decreases to 40 kgf/mm'', and the variation in strength becomes large.Therefore, a treatment aimed at increasing the strength of the ceramic sintered body after final processing is carried out. Widely known methods include surface modification methods such as coating with different materials using ion implantation and PVDSCVD.
一方、ａｉｚｏｘやＳｉ、Ｎ、焼結体では酸化処理する
と強度上昇することが知られており、サイアロン焼結体
に関しても酸化処理すると表面クランクが鈍化し、未処
理体と比べて強度上昇を示すことが反答用らによって報
告されている（窯業協会誌：８９（１０） １９８１ｐ
５３３）。On the other hand, it is known that oxidation treatment increases the strength of aizox, Si, N, and sintered bodies, and oxidation treatment of Sialon sintered bodies also dulls the surface crank and shows an increase in strength compared to untreated bodies. This has been reported by Hanshayo et al. (Ceramic Industry Association Journal: 89 (10) 1981p.
533).
前述のイオン注入や異材料をコーティングするなどの表
面改質方法は、特殊な装置を必要とし、また量産部品へ
の適用は困難である。The aforementioned surface modification methods such as ion implantation and coating with different materials require special equipment and are difficult to apply to mass-produced parts.
一方、従来の酸化処理による強度上昇は処理前と比べて
約１．２〜１．５倍程度であり、かつ１２００℃で１５
日、１３００℃で３日という長時間の処理を必要として
いた。On the other hand, the strength increase due to conventional oxidation treatment is approximately 1.2 to 1.5 times that before treatment, and
This required a long treatment time of 3 days at 1300°C.
本発明はこれらの問題点を解決したサイアロン焼結体の
強度を改善する方法を提供するべくなされたものであり
、サイアロン焼結体を酸素ガスを含む雰囲気中で１００
０−１３００℃で１０〜３０時間加熱し、さらに酸素ガ
スを含む雰囲気中で４００〜５００℃で１〜１０分間保
ち、その後５０℃／分以上の速度で冷却することを特徴
とする熱処理方法によってこの目的を達成したものであ
る。The present invention has been made to provide a method for improving the strength of sialon sintered bodies that solves these problems.
By a heat treatment method characterized by heating at 0-1300°C for 10-30 hours, further holding at 400-500°C for 1-10 minutes in an atmosphere containing oxygen gas, and then cooling at a rate of 50°C/min or more. This purpose has been achieved.
サイアロンは基本となる成分が５ｉＳＡｌ、 ＯｌＮの
４元素からなる焼結体であり、特公昭５１−１５８５０
号公報、特公昭５１−３７６５６号公報、特公昭５１−
３７６５７号公報などに開示されている。また、Ｙ２Ｏ
３添加を前提としたサイアロンの研究もまた盛んに行わ
れており、β′相（Ｓｉｂ−ｚ＾１．０□Ｎ１□）や０
′相（Ｓ ｉ ｚ −ｚＡＩＸＯＩ□Ｎｚ−ｘ）が現在
することも知られている（Ｎ−ｏｎ ０ｘｉｄｅ Ｔｅ
ｃｈ、 Ｅｎｇ、 Ｃｅｒｎｍ、 ＰＰ １〜３０．
ＰＰ１０５〜１１７、“８６〉。さらに、５ｉＪａとＹ
ｚＯｉとＡＩＮを出発物質にしたα−サイアロン（Ｍｘ
（Ｓｉ、 ＡＩ）ｔｚ（０，Ｎ）１６）が存在すること
も知られており、その焼結法についても詳細な報告があ
る（特公昭６１−３０９号公報）。Sialon is a sintered body whose basic components are 5iSAl and OLN, and it is a sintered body made of
Publication No. 37656, Special Publication No. 51-37656, Special Publication No. 51-37656
This is disclosed in JP-A No. 37657 and the like. Also, Y2O
Sialon research based on the addition of 3 is also actively conducted, and β' phase (Sib-z^1.0□N1□) and 0
' phase (S i z -zAIXOI□Nz-x) is also known to exist (N-on Oxide Te
ch, Eng, Cernm, PP 1-30.
PP105-117, “86〉.Furthermore, 5iJa and Y
α-sialon (Mx) using zOi and AIN as starting materials
(Si, AI)tz(0,N)16) is also known to exist, and there is a detailed report on its sintering method (Japanese Patent Publication No. 309/1983).
そのほか、量に多少の差があるものの、Ｙ、０３−５ｉ
Ｏ！ ５ｉ３Ｎｉ ＡｌｚＯｚ系のガラス相、Ｙ２
Ｏ，・Ｓｉ：＋Ｎ４相（メリライト相）、ＹＡＧ相等も
存在する場合がある。In addition, although there are some differences in quantity, Y, 03-5i
O! 5i3Ni AlzOz-based glass phase, Y2
O,.Si:+N4 phase (melilite phase), YAG phase, etc. may also be present.
また、ＡｈＯｉ粉末と５ｉ３Ｎａ粉末とを混合した場合
に鴎高温強度の弱い疑似ムライト相とも言われるＸ′−
サイアロンが生成する（窯業協会誌９３ （１０） １
９８５ ＰＰ ６２９−Ｐ６３５）。サイアロン焼結体
にはこのようにＳｉ、 ＡＩ％ Ｎｓ Ｏの含有比率、
相状態、微量成分、製造方法などに応じて種々存在し、
形状も用途等に応じて種々のものが存在するが、本発明
の方法はそれらを問わず適用できる。In addition, when AhOi powder and 5i3Na powder are mixed, X′-
Generated by Sialon (Ceramic Industry Association Magazine 93 (10) 1
985 PP 629-P635). In this way, the content ratio of Si, AI% Ns O,
There are various types depending on the phase state, trace components, manufacturing method, etc.
There are various shapes depending on the purpose and the like, and the method of the present invention can be applied regardless of the shape.
本発明の方法が適用されるサイアロン焼結体は焼結後さ
らに最終加工が施されたものである。このサイアロン焼
結体を酸素ガスを含む雰囲気、例えば大気中でまず約１
０００〜１３００℃１好ましくは約１１００℃の温度で
約１０〜３０時間、好ましくは約２４時間加熱する。こ
の加熱によって焼結体の加工処理等によって生じたクラ
ック等が鈍化されあるいは消滅する。The sialon sintered body to which the method of the present invention is applied is one that is further subjected to final processing after sintering. This sialon sintered body is first placed in an atmosphere containing oxygen gas, for example, in the air, for about 1 hour.
The mixture is heated at a temperature of 000 to 1300°C, preferably about 1100°C, for about 10 to 30 hours, preferably about 24 hours. This heating blunts or eliminates cracks and the like caused by processing of the sintered body.
次に、酸素ガスを含む雰囲気、例えば大気中で約４００
〜５００℃、好ましくは約５００℃の温度で１〜１５分
間程度、好ましくは１０分間程度保つ。その後この温度
から５０℃／分以上、好ましくは１０００℃／分程度の
速度で急冷する。急冷手段としては、例えば水等を掛け
たり、水中に投入したりすればよいが、送風等の手段も
利用することができる。尚、前記の１０００〜１３００
℃の加熱は酸化被膜の形成によるクラックの鈍化、消滅
させるために行うものあるから、この加熱と４００〜５
００℃の加熱との間は連続的に行う必要はなく、必要に
より他の処理を行うこともできる。Next, in an atmosphere containing oxygen gas, for example, the atmosphere, about 400
The temperature is maintained at a temperature of ~500°C, preferably about 500°C, for about 1 to 15 minutes, preferably about 10 minutes. Thereafter, it is rapidly cooled from this temperature at a rate of 50° C./min or more, preferably about 1000° C./min. As the quenching means, for example, pouring water or putting it into water may be used, but means such as blowing air may also be used. In addition, the above 1000 to 1300
Heating at a temperature of 400°C and
It is not necessary to perform the heating at 00° C. continuously, and other treatments can be performed if necessary.
〔作用］
急冷処理を施す前に、１０００〜１３００’Ｃ大気中で
１０〜３０時間の加熱処理を施すと、表面に安定した酸
化被膜が形成される。これにより加工クランクは鈍化し
たり、酸化膜により閉じ、強度上界を生じるとともに、
耐熱衝撃性を高めて急冷開始温度を上昇させることがで
きる。さらに、４００〜５００℃からの急冷処理により
表面に圧縮応力を残留させることにより、未処理物と比
べ強度を約２倍にすることを可能とする。[Function] If heat treatment is performed for 10 to 30 hours in the atmosphere at 1000 to 1300'C before performing the quenching treatment, a stable oxide film is formed on the surface. As a result, the machined crank becomes dull or closed by an oxide film, creating an upper limit on strength.
It is possible to increase the thermal shock resistance and raise the quenching start temperature. Furthermore, by leaving compressive stress on the surface by rapid cooling treatment from 400 to 500°C, it is possible to approximately double the strength compared to untreated material.
大気中加熱処理を施さないサイアロン焼結体は、４００
〜４５０℃から急冷すると熱応力により破壊する。Sialon sintered body without heat treatment in the atmosphere is 400
When rapidly cooled from ~450°C, it breaks due to thermal stress.
また、処理前に加工クラックが存在すると、その程度に
より４００℃以下からの急冷によってもクランクが進展
し、強度低下を招く。Furthermore, if processing cracks exist before treatment, depending on the severity, the cracks may develop even when rapidly cooled from 400° C. or lower, leading to a decrease in strength.
サイアロン焼結体より°通常の部品程度の加工（Ｒｍａ
ｘ １〜３ 即）を施した幅４ｍｍ、高さ３ａｍ、長さ
４９ｍｍの曲げ試験片を作製した。この状態で曲げ強度
を測定したところ、平均曲げ強度は４５ｋｇｆ／ｍｍ２
でワイブル係数は６〜７程度であった。また水中急冷に
よって破壊を生じる急冷開始温度は４００〜４２５℃で
あり、中には３００℃からの象、冷によりクランクを生
じる試験片もあった。Processing of ordinary parts (Rma) from Sialon sintered body
A bending test piece having a width of 4 mm, a height of 3 am, and a length of 49 mm was prepared. When the bending strength was measured in this state, the average bending strength was 45 kgf/mm2
The Weibull coefficient was about 6 to 7. Moreover, the quenching start temperature at which breakage occurs due to quenching in water is 400 to 425°C, and some specimens showed cracks when cooled from 300°C.
この試験片に１０００〜１４００℃大気中で２４時間の
加熱処理を施して得られた加熱処理後の試験片の助げ強
度と加熱処理温度との関係を第１図に実線で示す。また
、同図中の点線は未処理の試験片の強度を示している。This test piece was heat-treated at 1,000 to 1,400° C. in the atmosphere for 24 hours, and the relationship between the support strength of the test piece after the heat treatment and the heat treatment temperature is shown by a solid line in FIG. Furthermore, the dotted line in the figure indicates the strength of the untreated test piece.
同図に示すように、強度上界を生じ、特に１１００’Ｃ
で２４時間の処理を施したものは常温３点曲げ強度が７
０ｋｇｆ／ｍｍ”で未処理の試験片と比べて約１．６倍
に上昇しワイブル係数も１５に増加した。また、１１０
０℃の大気中で２４時間加熱処理した試験片（実線）及
び未処理の試験片（点線）、をさらに各種の温度から水
中急冷し、各試験片の曲げ強度を測定した結果を第２図
に示す。同図に示すように、４００〜５００℃から急冷
したものは常温３点曲げ強度が９１ｋｇｆ／ｍｍ２以上
で未処理の試験片と比べて約２倍に上昇した。また、本
処理により強度低下を示す試験片は皆無であった。As shown in the figure, there is an upper limit on the intensity, especially at 1100'C.
The one treated for 24 hours has a 3-point bending strength of 7 at room temperature.
0 kgf/mm", the Weibull coefficient increased approximately 1.6 times compared to the untreated test piece, and the Weibull coefficient also increased to 15.
Figure 2 shows the results of measuring the bending strength of each test piece after quenching the test piece (solid line) and untreated test piece (dotted line) in the atmosphere at 0°C for 24 hours and quenching them in water from various temperatures. Shown below. As shown in the figure, the three-point bending strength at room temperature of the specimen rapidly cooled from 400 to 500° C. was 91 kgf/mm 2 or more, which was about twice as high as that of the untreated specimen. Furthermore, no test pieces showed a decrease in strength due to this treatment.
本発明の方法によりバラツキの少ない高強度で耐熱衝撃
性に優れたサイアロン焼結体を作ることができる。また
、１３００℃に維持できる大気炉のような単純な設備で
、バッチ処理により多量の熱処理を行うことが可能であ
る。By the method of the present invention, it is possible to produce a sialon sintered body having high strength with little variation and excellent thermal shock resistance. Further, it is possible to perform a large amount of heat treatment by batch processing using simple equipment such as an atmospheric furnace that can maintain a temperature of 1300°C.
第１図はサイアロン焼結体を１０００〜１４００℃大気
中に２４時間加熱処理を施した試験片の強度と加熱温度
の関係を示す。また、第２図は１１００’Ｃで２４時間
大気中で加熱処理を施した試験片および比較として未処
理試験片に水中急冷処理を施したものの強度と急冷開始
温度の関係を示す。
特許出願人 日本調管株式会社
代 理 人 弁理士 国中 政浩FIG. 1 shows the relationship between the strength and heating temperature of a test piece obtained by heating a Sialon sintered body in the atmosphere at 1000 to 1400° C. for 24 hours. Further, FIG. 2 shows the relationship between the strength and the quenching start temperature of a test piece heat-treated at 1100'C for 24 hours in the air and, for comparison, an untreated test piece quenched in water. Patent applicant: Nippon Chokan Co., Ltd. Representative: Masahiro Kuninaka, patent attorney
Claims (1)
０〜１３００℃で１０〜３０時間加熱し、さらに酸素ガ
スを含む雰囲気中で４００〜５００℃で１〜１５分間保
ち、その後５０℃／分以上の速度で冷却することを特徴
とするサイアロン焼結体の熱処理方法The sialon sintered body was heated to 100% in an atmosphere containing oxygen gas.
Sialon sintering characterized by heating at 0 to 1300°C for 10 to 30 hours, further holding at 400 to 500°C for 1 to 15 minutes in an atmosphere containing oxygen gas, and then cooling at a rate of 50°C/min or more. Body heat treatment method
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63322179A JPH02167864A (en) | 1988-12-22 | 1988-12-22 | Method for heat-treating calcined sialon body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63322179A JPH02167864A (en) | 1988-12-22 | 1988-12-22 | Method for heat-treating calcined sialon body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02167864A true JPH02167864A (en) | 1990-06-28 |
Family
ID=18140826
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63322179A Pending JPH02167864A (en) | 1988-12-22 | 1988-12-22 | Method for heat-treating calcined sialon body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02167864A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0679616A2 (en) * | 1994-04-26 | 1995-11-02 | Sumitomo Electric Industries, Ltd. | Method of producing silicon nitride ceramic component |
-
1988
- 1988-12-22 JP JP63322179A patent/JPH02167864A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0679616A2 (en) * | 1994-04-26 | 1995-11-02 | Sumitomo Electric Industries, Ltd. | Method of producing silicon nitride ceramic component |
| EP0679616A3 (en) * | 1994-04-26 | 1995-11-29 | Sumitomo Electric Industries | |
| US5599493A (en) * | 1994-04-26 | 1997-02-04 | Sumitomo Electric Industries, Ltd. | Method of producing silicon nitride ceramic component |
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