JPS63185865A - Manufacture of silicon nitride sintered body - Google Patents
Manufacture of silicon nitride sintered bodyInfo
- Publication number
- JPS63185865A JPS63185865A JP62016644A JP1664487A JPS63185865A JP S63185865 A JPS63185865 A JP S63185865A JP 62016644 A JP62016644 A JP 62016644A JP 1664487 A JP1664487 A JP 1664487A JP S63185865 A JPS63185865 A JP S63185865A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- silicon nitride
- nitride sintered
- silicon
- strength
- 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 12
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 229910000676 Si alloy Inorganic materials 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 5
- 238000005121 nitriding Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000007493 shaping process Methods 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 229910052758 niobium Inorganic materials 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 229910052720 vanadium Inorganic materials 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- 150000002739 metals Chemical class 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 150000004767 nitrides Chemical class 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000007545 Vickers hardness test Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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、高強度、高靭性を有する窒化ケイ素焼結体の
製造法に好適に利用される。DETAILED DESCRIPTION OF THE INVENTION "Field of Industrial Application" The present invention is suitably used in a method for manufacturing a silicon nitride sintered body having high strength and high toughness.
「従来の技術」
窒化ケイ素焼結体の強度、靭性を改善する方法として、
焼結体中にウィスカーを分散させる方法によるもの（％
開開５６−９２１８０号公報）や、他の粒子を分散させ
る方法によるもの（％開開６１−１５８８６７号公報）
が知られており、いずれもヤング率、熱膨張係数等の物
理的籍性において５１ｓＮａと異なる物質が焼結体中に
存在することによシ、焼結体中にマイクロクラックや残
留応力が発生し、高強度化、高靭性化がなされるものと
考えられている。"Conventional technology" As a method to improve the strength and toughness of silicon nitride sintered bodies,
Due to the method of dispersing whiskers in the sintered body (%
JP-A No. 56-92180) or methods of dispersing other particles (JP-A No. 61-158867)
It is known that microcracks and residual stress occur in the sintered body due to the presence of substances in the sintered body that differ from 51sNa in physical properties such as Young's modulus and coefficient of thermal expansion. However, it is believed that higher strength and toughness can be achieved.
「発明が解決しようとする問題点」
しかし、上記従来方法によれば、均−ＶＣ粒子やウィス
カーを分散させるのは非常に困難であり１分散が不十分
であると欠陥を生じやすい。"Problems to be Solved by the Invention" However, according to the above-mentioned conventional method, it is very difficult to uniformly disperse the VC particles and whiskers, and defects are likely to occur if the dispersion is insufficient.
また、粒子等が焼結を抑制するため、緻密化し難いし、
粒子等が大きいとそれ自体が欠陥となって強度を低下さ
せる、などの問題点があった。In addition, particles inhibit sintering, making it difficult to densify.
There is a problem that if the particles are large, they themselves become defects and reduce the strength.
本発明は、かかる問題点を解決し、高強度、高靭性で理
論密度の９５％以上の密度を有する窒化ケイ素焼結体の
製造法を提供することを目的とする。An object of the present invention is to solve these problems and provide a method for manufacturing a silicon nitride sintered body having high strength, high toughness, and a density of 95% or more of the theoretical density.
「問題点を解決するための手段」
その手段は、ケイ素合金を粉砕し、窒素を含む雰囲気中
で加熱窒化し、再粉砕し成形した後焼成するところにあ
る。ここでケイ素合金は、窒化物が安定的に存在しうる
金属（ケイ素を除く）を含むものであることが必要で、
Ｔｉ、Ｖ。"Means for Solving the Problems" The method consists in pulverizing the silicon alloy, heating and nitriding it in an atmosphere containing nitrogen, re-pulverizing it, shaping it, and then firing it. Here, the silicon alloy must contain a metal (excluding silicon) in which nitride can exist stably,
Ti, V.
Ｃｒ ｇ Ｚｒ ＋ Ｎｂ ＋ Ｈｆ及びＴａのうちか
ら選ばれる１ｍ以上０．１〜８０Ｊ［量チを含むものが
望ましい。Cr g Zr + Nb + Hf and Ta selected from 1 m or more and 0.1 to 80 J [including quantity is preferable.
「作用」
加熱窒化により、合金中のケイ素は５ｉｓＮ４となり、
ケイ素以外の金属も窒化物となる。而してケイ素以外の
金属は、もともと合金中に均一に存在しているから、こ
れら金属の窒化物はＳｉ３Ｎ４マトリックス中に均一か
つ微細に分散した状態となる。この状態で再度粉砕し成
形した後、焼成することによｐｌなお一層均一な分散状
態を有する焼結体が得られる。"Effect" By heating nitriding, silicon in the alloy becomes 5isN4,
Metals other than silicon also form nitrides. Since metals other than silicon originally exist uniformly in the alloy, nitrides of these metals are uniformly and finely dispersed in the Si3N4 matrix. By pulverizing the powder again in this state, molding it, and then firing it, a sintered body having even more uniform dispersion of pl can be obtained.
得られた焼結体は、５ｉｓＮａと、熱膨張係数、ヤング
率等の特性の異なる金属窒化物とが混在したものである
から、焼結後の冷却過程において又はその後に応力が加
わった場合にマイクロクラックや残留応力が発生する。The obtained sintered body is a mixture of 5isNa and metal nitrides with different properties such as coefficient of thermal expansion and Young's modulus, so it does not react well when stress is applied during or after the cooling process after sintering. Microcracks and residual stress occur.
そしてこれらマイクロクラックや残留応力がクラックの
進展を防止し、又はその進行方向を変える作用をするの
であるが、上記の通シ分散状態が均一であるから、かか
る作用も焼結体内部で均等にはたらき、高強度化、高靭
性化をもたらすのである。These microcracks and residual stress act to prevent the propagation of cracks or change their propagation direction, but since the above-mentioned through-dispersion state is uniform, this effect is evenly distributed inside the sintered body. This results in increased strength and toughness.
合金として上記１櫨以上の金属を０．１〜３０重ｉ１重
含１ものが望ましいとしたのは、これら金属の窒化物が
Ｓｉ３Ｎ４と混在すると・きに最適のマイクロクラック
又は残留応力を発生せしめるからである。但し、その量
が０．１％に満たないと十分に作用せず、３０％を超え
ると焼結全体としての強度が低下するので０．１〜３０
重ｔ％に限定した。The reason why it is desirable to use 0.1 to 30 to 30% of the above-mentioned metals as an alloy is that when the nitrides of these metals are mixed with Si3N4, optimal microcracks or residual stress are generated. It is from. However, if the amount is less than 0.1%, it will not work sufficiently, and if it exceeds 30%, the strength of the sintered whole will decrease.
It was limited to weight t%.
なお、合金の中には上記１楓以上の金属の他に希土類金
属が含まれていてもよく、本発明の作用を妨げることは
ない。In addition, the alloy may contain rare earth metals in addition to the above-mentioned one or more metals, without interfering with the effects of the present invention.
「実施例」
純度９９％のＳｔ粉末と第１表に示す金属の粉末を混合
し、加熱溶解し、冷却してケイ素合金を作った。このケ
イ素合金を粗粉砕し、さらに５ｉａＮａ製ボーμミμを
用いて平均粒径１μｍになるまで粉砕し、Ｓｉ３Ｎ４製
さや内に入れ、Ｎ。"Example" St powder with a purity of 99% and metal powder shown in Table 1 were mixed, heated and melted, and cooled to produce a silicon alloy. This silicon alloy was coarsely ground, further ground to an average particle size of 1 μm using a 5iaNa Bommiμ, placed in a Si3N4 sheath, and heated with N.
とＨ２の混合ガス雰囲気中温度１０００〜１５００℃で
加熱することによシ窒化した。窒化粉末を粗粉砕し、６
重量％のＹｚＯｓと４３ｉｔ％のＡ １２０ｓを院加し
、５ｉｓＮ４製ボー〃ミルを用いて平均粒径０、６μｍ
になるまで粉砕し、２ｔｏｎ／ｄの圧力でラバープレス
成形した後、ＮＺガス圧５０ａｔｍ温度１９００“Ｃで
焼成することによシ、窒化ケイ素焼結体Ｎａ１〜宛８を
製造した。Nitriding was carried out by heating at a temperature of 1000 to 1500° C. in a mixed gas atmosphere of and H2. Coarsely crush the nitriding powder,
% by weight of YzOs and 43 it% of A 120s were added, and the average particle size was 0.6 μm using a 5isN4 bow mill.
Silicon nitride sintered bodies Na1 to No.8 were produced by pulverizing them until they were pulverized, rubber press-molding them at a pressure of 2 tons/d, and then firing them at a NZ gas pressure of 50 atm and a temperature of 1900"C.
比較の丸めに純度９８％、平均粒径０．７μｍの５Ｓｓ
ＮｉにＴＩＮ 、ＹｘＯｓ及びＡｈＯｓ’に混合し、Ｎ
！ガス圧５０ ａｔｍ ｓ温度１９００℃で焼成するこ
とにより、完全窒化されたと仮定した場合の焼結体−２
と同一の組成を有する窒化ケイ素焼結体Ｎ１９を製造し
た。For comparison purposes, 5Ss with a purity of 98% and an average particle size of 0.7 μm
Ni is mixed with TIN, YxOs and AhOs', and N
! Sintered body-2 assuming that it is completely nitrided by firing at a gas pressure of 50 atm s and a temperature of 1900°C
A silicon nitride sintered body N19 having the same composition was manufactured.
焼結体Ｎａｌ〜宛９から、大きさ８Ｘ４Ｘ４０■の試験
片を切り出し、密度、室温強度及び破壊靭性値の測定を
行った。強度はスパン８０ｍの８点曲げ法により、破壊
靭性値はビッカース圧子押し込み法により、それぞれ測
定した。測定結果を第１表に示す。A test piece with a size of 8×4×40 cm was cut out from the sintered body Nal~9, and its density, room temperature strength, and fracture toughness were measured. The strength was measured by the 8-point bending method with a span of 80 m, and the fracture toughness was measured by the Vickers indentation method. The measurement results are shown in Table 1.
第１表から、本発明に係る焼結体Ｎ［Ｌ１〜−７は純ケ
イ素から製造した焼結体嵐８に比べて強度、靭性ともに
高く、象加した副成分余積の蟹化物により強化されてい
ることがわかった。From Table 1, it can be seen that the sintered bodies N [L1 to -7 according to the present invention have higher strength and toughness than the sintered body Arashi 8 manufactured from pure silicon, and are strengthened by the extra volume of the inlaid subcomponent, ie, crabide. It turned out that it was.
また、焼結体−９に比べ焼結体へ２の方が密度、強度、
靭性ともに高く、本発明の製造法が従来法よりも緻密化
が容易でかつ強度、靭性を向上させるのに効果的である
ことがわかった。Also, compared to sintered body 9, sintered body 2 has better density, strength,
Both toughness was high, and it was found that the manufacturing method of the present invention is easier to densify than the conventional method and is effective in improving strength and toughness.
「発明の効果」
緻密で烏強度、高靭性′ｔ−有する窒化ケイ素焼結体を
容易に製造することができる。"Effects of the Invention" It is possible to easily produce a silicon nitride sintered body that is dense, has high strength and high toughness.
Claims (2)
窒化し、再粉砕し成形した後、焼成することを特徴とす
る窒化ケイ素焼結体の製造法。(1) A method for producing a silicon nitride sintered body, which comprises pulverizing a silicon alloy, heating and nitriding it in an atmosphere containing nitrogen, re-pulverizing it, shaping it, and then firing it.
ｆ及びＴａのうちから選ばれる１種以上０．１〜８０重
量％を含有するものである特許請求の範囲第１項記載の
窒化ケイ素焼結体の製造法。(2) Silicon alloy is Ti, V, Cr, Zr, Nb, H
The method for producing a silicon nitride sintered body according to claim 1, which contains 0.1 to 80% by weight of one or more selected from f and Ta.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62016644A JPS63185865A (en) | 1987-01-27 | 1987-01-27 | Manufacture of silicon nitride sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62016644A JPS63185865A (en) | 1987-01-27 | 1987-01-27 | Manufacture of silicon nitride sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63185865A true JPS63185865A (en) | 1988-08-01 |
| JPH0511064B2 JPH0511064B2 (en) | 1993-02-12 |
Family
ID=11922060
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62016644A Granted JPS63185865A (en) | 1987-01-27 | 1987-01-27 | Manufacture of silicon nitride sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63185865A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01115872A (en) * | 1987-10-29 | 1989-05-09 | Kurasawa Opt Ind Co Ltd | Silicon nitride ceramics |
| JPH01226767A (en) * | 1988-03-07 | 1989-09-11 | Hitachi Ltd | Electrically conductive material and production thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5141011A (en) * | 1974-10-03 | 1976-04-06 | Tatsuro Kuratomi | 4 chitsuka 3 keisoseikeitaino seizoho |
| JPS623076A (en) * | 1985-06-28 | 1987-01-09 | 京セラ株式会社 | Manufacture of silicon nitride base sintered body |
-
1987
- 1987-01-27 JP JP62016644A patent/JPS63185865A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5141011A (en) * | 1974-10-03 | 1976-04-06 | Tatsuro Kuratomi | 4 chitsuka 3 keisoseikeitaino seizoho |
| JPS623076A (en) * | 1985-06-28 | 1987-01-09 | 京セラ株式会社 | Manufacture of silicon nitride base sintered body |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01115872A (en) * | 1987-10-29 | 1989-05-09 | Kurasawa Opt Ind Co Ltd | Silicon nitride ceramics |
| JPH01226767A (en) * | 1988-03-07 | 1989-09-11 | Hitachi Ltd | Electrically conductive material and production thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0511064B2 (en) | 1993-02-12 |
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