JPH0371388B2 - - Google Patents
Info
- Publication number
- JPH0371388B2 JPH0371388B2 JP58226778A JP22677883A JPH0371388B2 JP H0371388 B2 JPH0371388 B2 JP H0371388B2 JP 58226778 A JP58226778 A JP 58226778A JP 22677883 A JP22677883 A JP 22677883A JP H0371388 B2 JPH0371388 B2 JP H0371388B2
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- processing
- hours
- nitride ceramics
- ceramics
- 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.)
- Expired - Lifetime
Links
- 239000000919 ceramic Substances 0.000 claims description 13
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 10
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 238000005452 bending Methods 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
- 238000005520 cutting process Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Description
(イ) 技術分野
本発明は窒化ケイ素セラミツクス焼結体の破壊
靭性改善、並びに均質化とくに強度バラツキの少
ない、いわゆるワイブル係数の高い窒化ケイ素セ
ラミツクスを得る方法に関する。
(ロ) 従来技術とその問題点
従来窒化ケイ素セラミツクスは、焼結されたま
まで使用されるものや、更には表面を加工し、所
定の寸法にして使用されている。焼結したままの
窒化ケイ素セラミツクスの表面は凹凸部や曲がり
などがあり、精密部分には用いる事ができない。
そこで表面精度を出すためにダイヤモンド工具
を用いて切削加工、研削加工などが行われて部品
として使用されている。しかしながら、これら加
工方法では窒化ケイ素セラミツクス焼結体の表面
に無数の傷即ち欠陥を導入するため焼結体特性と
くに強度への影響が大きく、強度のバラツキが大
きくなり、ワイブル係数が低いという問題点があ
つた。とくに破壊靭性の低い材料ほど大きな問題
であつた。
このような問題点を解決するために加工後の表
面に他のセラミツクスをコーテイングしたり、あ
るいは、酸化雰囲気で熱処理し、表面に酸化被膜
を形成させるなどして、表面傷の影響をなくす事
が考えられ検討されている。しかしながら、これ
らの方法では、コーテイング膜、酸化膜と母材と
の密着性が良好でなく本来の表面傷の影響をなく
す効果を出すにいたつていないのが現状である。
(ハ) 発明の構成
本発明者らは、上記の従来の問題点に鑑みて、
種々検討を行ない破壊靭性の高い均質性に優れた
窒化ケイ素セラミツクスを製造する方法を見い出
したものである。すなわち、焼結された窒化ケイ
素セラミツクスを加工し、ついで窒素雰囲気中で
熱処理し、均質化させることを特徴とする破壊靭
性に優れた高均質セラミツクスの製造法である。
窒化ケイ素セラミツクスの加工には、切削、研削
等の機械加工および放電や電子ビーム、レーザー
を用いた加工等があり、表面に機械的、熱的に傷
を導入されるすべての方法に対して本発明は有効
である。雰囲気としては窒素が有効である。雰囲
気圧力は、減圧、大気圧（常圧）、高圧いずれの
場合も効果があるが、大気圧（常圧）付近が最も
良好な結果が得られる。また、処理温度は1200℃
以上焼結温度以下の焼結が進行する温度範囲が良
好である。処理温度が1200℃以下では、本発明の
効果がなく、焼結温度以下では、異常粒成長をき
たし、本来の性質が保持できなくなるためこの範
囲が適する。処理時間は少なくとも0.5時間あれ
ばよい。
0.5時間以下では熱処理による均質化の効果が
少なく10時間以上の処理は経済的でない。
本発明の熱処理より均質化される効果は、加工
により生じた（あるいは潜在していた）表面傷の
先端へ物質の移動が生じ、傷の先端を鈍化させる
ために、破壊靭性が高くバラツキの少ない均質な
セラミツクスが得られるものと考えられる。
以下、実施例により詳細に説明する。
実施例 １
90wt％Si3N4（シユタルク社、Lc−12グレード）
および5wt％AlO35wt％MgOをアトライターにて
10時間粉砕混合した、その粉末にパラフイン５％
を添加し、金型プレスにより100×100×25mmの成
形体に型押した。その成形体を窒素ガス中1000℃
で脱パラフインを行なつた。ついで1atmN2雰囲
気下昇温速度10℃／分で1800℃まで昇温し、１時
間キープし、圧力300Kg／cm2でホツトプレスを実
施した。この焼結体をダイヤモンド砥石にて切
断、研削加工により３mm×４mm×40mmの曲げ試験
片60本に加工した。
ついで、この半分の30本を本発明にしたがい
1400℃１時間1atmN2中で熱処理した。これら試
験片を800℃でJIS1601に準じて曲げ試験を行ない
熱処理しない30本と比較しながら平均曲げ強さと
ワイブル係数を把握した。
得られた結果を第１表に示す。
(a) Technical Field The present invention relates to improving the fracture toughness of sintered silicon nitride ceramics and to homogenizing them, particularly to a method for obtaining silicon nitride ceramics with little variation in strength and a so-called high Weibull coefficient. (b) Prior art and its problems Conventionally, silicon nitride ceramics have been used in their sintered state, or their surfaces have been processed to give them predetermined dimensions. The surface of silicon nitride ceramics as-sintered has irregularities and bends, so it cannot be used for precision parts. Therefore, in order to achieve surface precision, diamond tools are used to perform cutting and grinding processes before use as parts. However, these processing methods introduce countless scratches or defects on the surface of the silicon nitride ceramic sintered body, which has a large effect on the properties of the sintered body, especially the strength, which leads to large variations in strength and a low Weibull coefficient. It was hot. This was especially a problem for materials with low fracture toughness. To solve these problems, it is possible to eliminate the effects of surface scratches by coating the surface after processing with other ceramics, or by heat-treating it in an oxidizing atmosphere to form an oxide film on the surface. It is thought and considered. However, these methods currently have poor adhesion between the coating film, oxide film, and base material, and are not effective in eliminating the effects of inherent surface scratches. (c) Structure of the invention In view of the above-mentioned conventional problems, the present inventors have
After conducting various studies, we discovered a method for manufacturing silicon nitride ceramics with excellent homogeneity and high fracture toughness. That is, this is a method for producing highly homogeneous ceramics with excellent fracture toughness, which is characterized by processing sintered silicon nitride ceramics and then heat-treating them in a nitrogen atmosphere to homogenize them.
Processing of silicon nitride ceramics includes mechanical processing such as cutting and grinding, and processing using electric discharge, electron beams, and lasers. The invention is valid. Nitrogen is effective as the atmosphere. The atmospheric pressure can be reduced, atmospheric pressure (normal pressure), or high pressure, all of which are effective, but the best results can be obtained near atmospheric pressure (normal pressure). In addition, the processing temperature is 1200℃
A temperature range above the sintering temperature in which sintering progresses is favorable. If the treatment temperature is below 1200°C, the present invention will not be effective, and if it is below the sintering temperature, abnormal grain growth will occur and the original properties cannot be maintained, so this range is suitable. The processing time should be at least 0.5 hours. If the heat treatment is less than 0.5 hours, the effect of homogenization by heat treatment is small, and if the treatment is more than 10 hours, it is not economical. The homogenizing effect of the heat treatment of the present invention is that material transfers to the tips of surface scratches caused by processing (or that were latent) and blunts the tips of the scratches, resulting in high fracture toughness and less variation. It is thought that homogeneous ceramics can be obtained. Hereinafter, it will be explained in detail using examples. Example 1 90wt%Si 3 N 4 (Syuutark, Lc-12 grade)
and 5wt%AlO 3 5wt%MgO in attritor
Pulverized and mixed for 10 hours, 5% paraffin added to the powder
was added and pressed into a molded body of 100 x 100 x 25 mm using a mold press. The molded body was heated to 1000℃ in nitrogen gas.
Deparaffinization was performed. Then, the temperature was raised to 1800° C. at a rate of 10° C./min in a 1 atmN 2 atmosphere, maintained for 1 hour, and hot pressed at a pressure of 300 Kg/cm 2 . This sintered body was cut with a diamond grindstone and ground into 60 bending test pieces measuring 3 mm x 4 mm x 40 mm. Next, half of these 30 pieces were made according to the present invention.
Heat treatment was performed at 1400° C. for 1 hour in 1 atmN 2 . These test pieces were subjected to a bending test at 800°C according to JIS1601, and the average bending strength and Weibull coefficient were determined by comparing them with 30 pieces that were not heat treated. The results obtained are shown in Table 1.
【表】
実施例 ２
実施例１と同様に、Si3N4焼結体を作成し、試
験片まで加工した。ついでその熱処理条件を変え
その効果を把握した。得られた結果を第２表に示
す。[Table] Example 2 In the same manner as in Example 1, a Si 3 N 4 sintered body was produced and processed into a test piece. Then, the heat treatment conditions were changed and the effects were ascertained. The results obtained are shown in Table 2.
Claims (1)
られた焼結体の表面を加工し、ついで窒素雰囲気
下、大気圧で1200℃以上、焼結温度以下で0.5時
間以上10時間以下加熱処理することを特徴とする
高靭性窒化ケイ素セラミツクスの製造法。1 Sintering silicon nitride ceramic powder, processing the surface of the obtained sintered body, and then heat-treating it in a nitrogen atmosphere at atmospheric pressure at 1200°C or higher and below the sintering temperature for 0.5 hours or more and 10 hours or less. A manufacturing method for high-toughness silicon nitride ceramics.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58226778A JPS60122783A (en) | 1983-12-02 | 1983-12-02 | Manufacture of ceramics |
| DE19843443817 DE3443817A1 (en) | 1983-12-02 | 1984-11-30 | METHOD FOR PRODUCING CERAMICS |
| US06/920,908 US4702869A (en) | 1983-12-02 | 1986-10-17 | Process for the production of ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58226778A JPS60122783A (en) | 1983-12-02 | 1983-12-02 | Manufacture of ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60122783A JPS60122783A (en) | 1985-07-01 |
| JPH0371388B2 true JPH0371388B2 (en) | 1991-11-13 |
Family
ID=16850459
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58226778A Granted JPS60122783A (en) | 1983-12-02 | 1983-12-02 | Manufacture of ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60122783A (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62171977A (en) * | 1986-01-27 | 1987-07-28 | 日本碍子株式会社 | Method of strengthening silicon nitride ceramic body |
| JPS6325275A (en) * | 1986-07-18 | 1988-02-02 | 日本ピラ−工業株式会社 | Sliding member made from super high density silicon carbide sintered body |
| JPS6355180A (en) * | 1986-08-22 | 1988-03-09 | 株式会社東芝 | Ceramic part |
| JPH0723270B2 (en) * | 1992-10-30 | 1995-03-15 | 株式会社東芝 | Silicon nitride ceramic parts |
| JPH07126077A (en) * | 1994-04-13 | 1995-05-16 | Ngk Spark Plug Co Ltd | Production of whisker-containing formed ceramic article, coating method and production of ceramic tool |
| JP4955864B2 (en) * | 2001-05-31 | 2012-06-20 | 日本碍子株式会社 | Method for producing silicon nitride strip |
| JP2007191376A (en) * | 2006-01-23 | 2007-08-02 | Fujifilm Corp | Polycrystalline material and method for heat treating the same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5240326A (en) * | 1975-09-26 | 1977-03-29 | Matsushita Electric Ind Co Ltd | Speaker |
-
1983
- 1983-12-02 JP JP58226778A patent/JPS60122783A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5240326A (en) * | 1975-09-26 | 1977-03-29 | Matsushita Electric Ind Co Ltd | Speaker |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60122783A (en) | 1985-07-01 |
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