JPS6283377A - Manufacture of composite sintered body - Google Patents

Manufacture of composite sintered body

Info

Publication number
JPS6283377A
JPS6283377A JP60221408A JP22140885A JPS6283377A JP S6283377 A JPS6283377 A JP S6283377A JP 60221408 A JP60221408 A JP 60221408A JP 22140885 A JP22140885 A JP 22140885A JP S6283377 A JPS6283377 A JP S6283377A
Authority
JP
Japan
Prior art keywords
sintered body
sintering
composite sintered
whiskers
volume
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
Application number
JP60221408A
Other languages
Japanese (ja)
Inventor
馬場 英俊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Niterra Co Ltd
Original Assignee
NGK Spark Plug Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by NGK Spark Plug Co Ltd filed Critical NGK Spark Plug Co Ltd
Priority to JP60221408A priority Critical patent/JPS6283377A/en
Publication of JPS6283377A publication Critical patent/JPS6283377A/en
Pending legal-status Critical Current

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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」 本発明は切削工具用複合焼結体の製造法に好適に利用さ
れ、高温構造材料、エンジン部品等の製造法にも利用さ
れ得る。
DETAILED DESCRIPTION OF THE INVENTION "Field of Industrial Application" The present invention is suitably used in a method for manufacturing a composite sintered body for a cutting tool, and can also be used in a method for manufacturing high-temperature structural materials, engine parts, and the like.

「従来の技術」 5bN4焼結体は高靭性で耐熱衝撃性に優れていること
から耐熱合金にかわる構造材料や切前工具に使用され始
めている。81sN<は共有結合性の高い難焼結材料で
あるため種々の焼結法によって緻密化が試められている
。代表的な焼結法として反応焼結法、普通焼結法及びホ
ットプレス法が知られているが、反応焼結法では相対密
度86%が限度であり高強度のものは得られず、後二者
では高温で特性が劣化する難点があった。そこで反応焼
結体を更に緻密化するため金属Slに焼結助剤を添加し
て反応焼結後ホットプレスする方法(特表昭59−50
1628号公報)、5isNn焼結体の高温特性改善の
ため5isN4中にSiCのウィスカーと呼ばれるひげ
結晶を分散させる方法(窯業協会誌91 (11:) 
1988 、491 )、5isNa中に5isN4の
ウィスカーを分散させる方法(特開昭56−92180
号公報)などが提案された。
"Prior Art" 5bN4 sintered bodies have high toughness and excellent thermal shock resistance, so they are beginning to be used as structural materials and cutting tools in place of heat-resistant alloys. Since 81sN< is a difficult-to-sinter material with high covalent bonding properties, attempts have been made to make it densified by various sintering methods. Reaction sintering, ordinary sintering, and hot pressing are known as typical sintering methods, but the reaction sintering method has a relative density of 86%, which makes it impossible to obtain high strength, and Both had the disadvantage that their properties deteriorated at high temperatures. Therefore, in order to further densify the reaction sintered body, a sintering aid is added to the metal Sl, and hot pressing is performed after reaction sintering.
1628 Publication), Method of dispersing whisker crystals called SiC whiskers in 5isN4 to improve high-temperature characteristics of 5isNn sintered body (Ceramics Association Journal 91 (11:)
1988, 491), Method for dispersing 5isN4 whiskers in 5isNa (Japanese Patent Application Laid-Open No. 56-92180
Publication No. 2), etc. were proposed.

「発明が解決しようとする問題点」 しかし、特表昭59−501628号公報記載の方法で
は焼結助剤添加により高温特性の劣化を招来し、ウィス
カーを分散させる方法では焼結困難となシ室温における
特性もあまり良くなかった。したがって鋳鉄を高速切削
する場合のように刃先が高温になる切削加工に従来のS
 i sNA系工具を用いるとその寿命がAlzOs 
−Tic系工具よりも短かくなるという問題点があった
"Problems to be Solved by the Invention" However, the method described in Japanese Patent Publication No. 59-501628 causes deterioration of high-temperature properties due to the addition of a sintering aid, and the method of dispersing whiskers makes sintering difficult. The properties at room temperature were also not very good. Therefore, conventional S
i When using sNA type tools, the lifespan of AlzOs
-There was a problem that it was shorter than Tic type tools.

本発明は上記の問題点を解決し、従来の5isN4系工
具やAltos −Tic系工具よシも高温強度及び高
温硬度に優れた複合焼結体の製造法を提供することを目
的とする。
It is an object of the present invention to solve the above-mentioned problems and provide a method for producing a composite sintered body that has superior high-temperature strength and high-temperature hardness compared to conventional 5isN4-based tools and Altos-Tic-based tools.

「問題点を解決するための手段」 その手段は、Si粉末60〜90重量%及び焼結助剤4
0〜10重量%よりなる粉末20〜90体積チと、ウィ
スカー40〜5体積−と、硬質物質40〜5体積チとを
混合し成形し、窒化後に焼結するところにある。
"Means for solving the problem" The means consists of 60 to 90% by weight of Si powder and 4% of the sintering aid.
20 to 90 volumes of powder consisting of 0 to 10% by weight, 40 to 5 volumes of whiskers, and 40 to 5 volumes of hard material are mixed, molded, and sintered after nitriding.

ここでウィスカーとは、直径0.1〜0.15μ肩のひ
げ結晶をいい、材質としては5iCs 5isNa等の
セラミックスが望ましいものである。硬質物質とは、そ
れ自体の高温における硬度が5lsNaのそれと同等か
又はよシ高いものをいう。
Here, the term "whisker" refers to a whisker crystal having a diameter of 0.1 to 0.15 μm, and the material thereof is preferably ceramic such as 5iCs 5isNa. A hard substance refers to a substance whose hardness at high temperatures is equal to or higher than that of 5lsNa.

「作用」 焼結助剤は、窒化によシ生成した5LlN4の焼結を促
進し緻密化するものであるが、その含有量がウィスカー
と硬質物質とを除く原料中10重量%に満九表いと緻密
化せず、40重量%を超えると高温特性を劣化させるこ
とからその含有量を40〜10重量%に限定した。焼結
助剤の種類はAbOs r AIN * YxOs +
 MgO+ Zr(h及び希土類元素の酸化物のうち一
種以上が望ましく、Alums / Yz0gモル比V
a 〜VxのAhOs 5Y203混合物が好適である
"Function" The sintering aid promotes the sintering and densification of 5LlN4 produced by nitriding, but its content is less than 10% by weight of the raw material excluding whiskers and hard substances. If it exceeds 40% by weight, the high-temperature properties deteriorate, so the content was limited to 40 to 10% by weight. The types of sintering aids are AbOs r AIN * YxOs +
MgO + Zr (preferably one or more of oxides of h and rare earth elements, Alums / Yz0g molar ratio V
AhOs 5Y203 mixtures from a to Vx are preferred.

Sl粉末は窒化によりS i sNaに変化するが、こ
の際成形体の相対密度が75%程度にまで達することか
ら、SimNnとウィスカーとの混合物の相対密度が5
5チ程度にしか達しないのと異なり、焼結時の収縮変形
がほとんど生じないうえ、密接し九5lsNa同志が焼
結することから焼結し易くなる。窒化は1100〜14
00℃の窒素気流中又は窒素、水素及び不活性ガスの混
合気流中層が高温で軟化しても5isN4粒子間をつな
ぎ止めることにより焼結体の高温特性の劣化を防止する
ほか、ウィスカー同志のからみ合いによって成形体中に
多数の開気孔を生ぜしめて窒化時の窒素拡散を容易にし
窒化を促進する。この開気孔はSlがSimNnに窒化
される時の体積膨張や5isN4の気相拡散によシ小さ
くなるので、焼結体の強度に悪影響を及ぼすことはない
。ウィスカーは、成形体中の添加量が5体積チに満たな
いと上記作用に乏しく、40体積ciIを超えると成形
、緻密化共に困難となるのでその添加量を40〜6体積
チに限定した。
Sl powder changes to Si sNa by nitriding, but at this time, the relative density of the compact reaches about 75%, so the relative density of the mixture of SimNn and whiskers is 5%.
Unlike the case where the thickness reaches only about 5cm, almost no shrinkage deformation occurs during sintering, and the 95lsNa sinters in close contact with each other, making it easier to sinter. Nitriding is 1100-14
Even if the middle layer of a nitrogen stream at 00℃ or a mixture of nitrogen, hydrogen, and inert gas softens at high temperatures, it prevents the deterioration of the high-temperature properties of the sintered body by binding the 5isN4 particles together, and also prevents the entanglement of whiskers. This creates a large number of open pores in the molded body, facilitates nitrogen diffusion during nitriding, and promotes nitriding. Since these open pores become smaller due to the volumetric expansion when Sl is nitrided to SimNn and the vapor phase diffusion of 5isN4, they do not adversely affect the strength of the sintered body. When the amount of whiskers added in the molded article is less than 5 volume ciI, the above effect is poor, and when it exceeds 40 volume ciI, both molding and densification become difficult, so the amount added was limited to 40 to 6 volume ciI.

硬質物質は、焼結体の高温中での硬度を向上させるもの
で、例えばIVa族元素、Va族元素もしくはVIa族
元素の炭化物、窒化物もしくは炭窒化物又はこれらのう
ちから選ばれる二種以上があげられ、特にTie 、 
TIN及びT i CNのうちから選ばれる一種以上が
望ましい。硬質物質は焼結体中の含有量が6体積チに満
たないとその作用に乏しく、40体積チを超えると焼結
を困難にするので、上記の含有量に限定した。
The hard substance improves the hardness of the sintered body at high temperatures, and is, for example, a carbide, nitride, or carbonitride of an IVa group element, Va group element, or VIa group element, or two or more selected from these. are mentioned, especially Tie,
One or more selected from TIN and T i CN are desirable. If the content of the hard substance in the sintered body is less than 6 volume units, its effect will be poor, and if it exceeds 40 volume units, sintering will be difficult, so the content was limited to the above range.

焼結は1〜200気圧の窒素中湿度1650〜2000
℃のガス圧焼結又は100〜800気圧のカーボンモー
ルド中温度1600〜1900℃のホットプレスにて行
われる。
Sintering is performed in nitrogen at 1 to 200 atmospheres with a humidity of 1650 to 2000.
℃ gas pressure sintering or hot pressing at a temperature of 1600-1900°C in a carbon mold at 100-800 atm.

「実施例」 360メツシ工通過、純度99チの81%干均粒径0.
6μm、純度99.9%の(! −AbOs、平均粒径
1μm、純度99チのY2O3、平均粒径1μm1純度
99チのTiC、平均粒径1.5μm1純度99チのT
iN、 SLCウィスカー及び5L3N4ウイスカーを
第1表に示す割合で秤量し、混合し、1ton/aAで
金型プレスし、窒素気流中1800℃で窒化した後、1
800℃、201t/adでホットプレスすることによ
って焼結体A1−威15を製造した。
"Example" Passed through 360 mesh, purity 99%, 81% dry average particle size 0.
6 µm, purity 99.9% (! - AbOs, average particle size 1 µm, purity 99 µm Y2O3, average particle size 1 µm 1 purity 99 µm TiC, average particle size 1.5 µm 1 purity 99 µm T
iN, SLC whiskers and 5L3N4 whiskers were weighed and mixed in the proportions shown in Table 1, pressed into a mold at 1 ton/aA, and nitrided at 1800°C in a nitrogen stream.
A sintered body A1-I15 was produced by hot pressing at 800° C. and 201 t/ad.

焼結体ム1,1B、44.47.ム8.ム11.41B
笈びム14は本発明製造法によって得られたものであり
、他は範囲外品である。
Sintered compact 1, 1B, 44.47. M8. Mu11.41B
The cup 14 was obtained by the manufacturing method of the present invention, and the others are products outside the range.

焼結体ムト」14について次に示す測定方法で抗折力、
硬度及び耐摩耗性を評価した結果を第1表に示す。
The transverse rupture strength and
Table 1 shows the results of evaluating hardness and abrasion resistance.

抗折力測定方法 抗折力はJIS規格R1601にしたがって1200℃
における8点曲げ強さを測定した。
Transverse rupture strength measurement method Transverse rupture strength is 1200℃ according to JIS standard R1601
The 8-point bending strength was measured.

硬度は、焼結体を5NGN4B2形状に研削加工し、J
IS規格Z 2245にしたがってロックウエルスーパ
ーフィシャル硬さ45Nを測定した。
The hardness is determined by grinding the sintered body into a 5NGN4B2 shape and J
A Rockwell superficial hardness of 45N was measured according to IS standard Z 2245.

耐摩耗性は、焼結体を5NGN482形状に研摩した後
、第2表に示す条件で切削して逃げ面摩耗VBを測定す
ることによって評価した。
Wear resistance was evaluated by grinding the sintered body into a 5NGN482 shape, cutting it under the conditions shown in Table 2, and measuring flank wear VB.

第    2    表 第1表かられかるように、本発明製造法にしたがって得
られたものは、高温強度、高温硬度が高く、切削性能に
優れていた。
Table 2 As can be seen from Table 1, the products obtained according to the production method of the present invention had high high temperature strength and high temperature hardness, and were excellent in cutting performance.

「発明の効果」 以上のように本発明製造法によれば、切削工具、高温構
造材料、エンジン部品等に適した複合焼結体を得ること
ができる。
"Effects of the Invention" As described above, according to the manufacturing method of the present invention, a composite sintered body suitable for cutting tools, high-temperature structural materials, engine parts, etc. can be obtained.

特許出願人 日本特殊陶業株式会社 代表者 鈴 木 亭 −Patent applicant: Nippon Tokushu Tokugyo Co., Ltd. Representative Suzuki Tei -

Claims (2)

【特許請求の範囲】[Claims] (1)Si粉末60〜90重量%及び焼結助剤40〜1
0重量%よりなる粉末20〜90体積%と、ウィスカー
40〜5体積%と、硬質物質40〜5体積%とを混合し
成形し、窒化後に焼結することを特徴とする複合焼結体
の製造法。
(1) Si powder 60-90% by weight and sintering aid 40-1
A composite sintered body characterized in that 20-90% by volume of powder consisting of 0% by weight, 40-5% by volume of whiskers, and 40-5% by volume of hard material are mixed, molded, and sintered after nitriding. Manufacturing method.
(2)硬質物質がIVa族元素、Va族元素もしくはVIa
族元素の炭化物、窒化物もしくは炭窒化物又はこれらの
うちから選ばれる二種以上である特許請求の範囲第1項
記載の複合焼結体の製造法。
(2) The hard substance is a group IVa element, a group Va element, or a group VIa
2. The method for producing a composite sintered body according to claim 1, wherein the composite sintered body is a carbide, nitride, or carbonitride of a group element, or two or more selected from these.
JP60221408A 1985-10-04 1985-10-04 Manufacture of composite sintered body Pending JPS6283377A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP60221408A JPS6283377A (en) 1985-10-04 1985-10-04 Manufacture of composite sintered body

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP60221408A JPS6283377A (en) 1985-10-04 1985-10-04 Manufacture of composite sintered body

Publications (1)

Publication Number Publication Date
JPS6283377A true JPS6283377A (en) 1987-04-16

Family

ID=16766272

Family Applications (1)

Application Number Title Priority Date Filing Date
JP60221408A Pending JPS6283377A (en) 1985-10-04 1985-10-04 Manufacture of composite sintered body

Country Status (1)

Country Link
JP (1) JPS6283377A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63185864A (en) * 1986-09-05 1988-08-01 株式会社日立製作所 Composite ceramics and their manufacturing method
JPS63233077A (en) * 1986-11-14 1988-09-28 日立金属株式会社 Silicon nitride base composite sintered body

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5860677A (en) * 1981-09-30 1983-04-11 日本特殊陶業株式会社 Manufacture of high tenacity silicon nitride sintered body
JPS5891073A (en) * 1981-11-26 1983-05-30 旭硝子株式会社 Silicon nitride ceramics

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5860677A (en) * 1981-09-30 1983-04-11 日本特殊陶業株式会社 Manufacture of high tenacity silicon nitride sintered body
JPS5891073A (en) * 1981-11-26 1983-05-30 旭硝子株式会社 Silicon nitride ceramics

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63185864A (en) * 1986-09-05 1988-08-01 株式会社日立製作所 Composite ceramics and their manufacturing method
JPS63233077A (en) * 1986-11-14 1988-09-28 日立金属株式会社 Silicon nitride base composite sintered body

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