JPH03153574A - High strength sialon-based sintered body - Google Patents
High strength sialon-based sintered bodyInfo
- Publication number
- JPH03153574A JPH03153574A JP1291247A JP29124789A JPH03153574A JP H03153574 A JPH03153574 A JP H03153574A JP 1291247 A JP1291247 A JP 1291247A JP 29124789 A JP29124789 A JP 29124789A JP H03153574 A JPH03153574 A JP H03153574A
- Authority
- JP
- Japan
- Prior art keywords
- sialon
- powder
- sintered body
- based sintered
- phase
- 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
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 239000011521 glass Substances 0.000 claims abstract description 6
- 239000013081 microcrystal Substances 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 3
- 239000010436 fluorite Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 abstract description 43
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 13
- 238000010438 heat treatment Methods 0.000 abstract description 8
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000470 constituent Substances 0.000 abstract 1
- 239000012299 nitrogen atmosphere Substances 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 16
- 239000001301 oxygen Substances 0.000 description 16
- 229910052760 oxygen Inorganic materials 0.000 description 16
- 238000005245 sintering Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、高温高強度、高硬度及び高靭性を有する各種
エンジニアリングセラミックスを製造するために有用な
高強度サイアロン基焼結体に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a high-strength sialon-based sintered body useful for producing various engineering ceramics having high temperature and high strength, high hardness, and high toughness.
（従来技術及びその問題点）
Ｙα−サイアロンは、α型窒化珪素のＳｉ位置にＡ！が
、Ｎ位置にＯが置換固溶すると同時に、Ｙが侵入固溶し
た物質であり、
式Ｙ、 （Ｓ ｉ、 Ａｌｌり 、ｔ （０，Ｎ） Ｉ
ｂ （Ｉ）（式中、Ｘは０＜ｘ≦２を満足する数である
。）で表される。このＹα−サイアロンは、高硬度、低
熱膨張率、優れた耐蝕性等のエンジニアリングセラミッ
クスとしての特性を有している。(Prior art and its problems) Yα-Sialon has A! at the Si position of α-type silicon nitride. is a substance in which O substitutes at the N position and at the same time Y enters into a solid solution, and has the formula Y, (S i, All , t (0, N) I
b (I) (wherein, X is a number satisfying 0<x≦2). This Yα-sialon has characteristics as an engineering ceramic, such as high hardness, low coefficient of thermal expansion, and excellent corrosion resistance.
しかし、Ｙα−サイアロン相単体の焼結体は、結晶形状
が粒状であるため、エンジニアリングセラミックスとし
ての強度、破壊靭性等の特性が充分ではない。そこで、
この欠点を改良するために、特開昭５８−１８５４８４
号公報には、Ｙα−サイアロン結晶と、β型窒化珪素の
Ｓｉ位置にＡ！が、Ｎ位置に０が置換固溶した
式Ｓ ｉ ａ−ｇＡ １ｘｏｚＮＩｌ−ｔ （Ｉ［
）（式中、２はＯ＜ｚ≦４．２を満足する数である。）
で表される針状のβ−サイアロン結晶とを複合化させた
サイアロン基焼結体が提案されている。However, since the sintered body of the single Yα-sialon phase has a granular crystal shape, it does not have sufficient properties such as strength and fracture toughness as an engineering ceramic. Therefore,
In order to improve this drawback, Japanese Patent Application Laid-Open No. 58-185484
The publication describes Yα-sialon crystal and A! at the Si position of β-type silicon nitride! is the formula Si a-gA 1xozNIl-t (I[
) (In the formula, 2 is a number that satisfies O<z≦4.2.)
A sialon-based sintered body has been proposed which is a composite of acicular β-sialon crystals represented by:
しかしながら、このサイアロン基焼結体の機械的特性も
実用上十分なものではない。However, the mechanical properties of this sialon-based sintered body are not sufficient for practical use.
（発明の目的）
本発明の目的は、前記問題点を解決し、高温強度及び靭
性の高い新規なサイアロン基焼結体を提供することであ
る。(Object of the Invention) An object of the present invention is to solve the above-mentioned problems and provide a novel sialon-based sintered body having high high-temperature strength and toughness.
（発明の要旨）
本発明によれば、蛍石型結晶構造のＹｔＨｆｚＯ７の微
結晶、ｉｎ記式（１）で表されるＹα〜サイアロンの結
晶、前記式（Ｕ）で表されるβ−サイアロンの結晶及び
Ｙを含むガラス相からなる高強度サイアロン基焼結体が
提供される。(Summary of the Invention) According to the present invention, microcrystals of YtHfzO7 having a fluorite crystal structure, crystals of Yα-sialon represented by the in formula (1), and β-sialon represented by the formula (U) A high-strength sialon-based sintered body consisting of a glass phase containing crystals and Y is provided.
（発明の詳細な説明）
本発明のサイアロン基焼結体における各相の含有割合は
、通常以下に示す範囲である。(Detailed Description of the Invention) The content ratio of each phase in the sialon-based sintered body of the present invention is usually within the range shown below.
１ ＜ Ｙ ｚ Ｈｆ ｚ Ｏ７の微結晶相 く２０重
量％５＜Ｙα−サイアロンの結晶相〈５０重全量３０く
β−サイアロンの結晶相 〈９０重量％ｉ＜ｙを含むガ
ラス相 〈１０重量％Ｙ２Ｈｆ２Ｏ７の微結晶相
の割合が前記範囲を外れると、得られるサイアロン基焼
結体の機械的強度が低下するので好ましくない。1 < Y z Hf z Microcrystalline phase of O7 20% by weight 5 < Y If the proportion of the microcrystalline phase of Y2Hf2O7 is outside the above range, the mechanical strength of the obtained sialon-based sintered body will decrease, which is not preferable.
また、本発明のサイアロン基焼結体において、Ｙα−サ
イアロンの結晶の長径が０．０５〜１０μｍ、β−サイ
アロンの結晶の長径が１〜１００μｍであることが好ま
しい。Further, in the sialon-based sintered body of the present invention, it is preferable that the major axis of the Yα-sialon crystal is 0.05 to 10 μm, and the major axis of the β-sialon crystal is 1 to 100 μm.
本発明のサイアロン基焼結体中には、Ｙα−サイアロン
とα−窒化珪素との反応によって生成すると考えられる
、β−サイアロンの結晶、Ｙを含むガラス相及び粒界で
結晶化した蛍石型結晶構造のＹ２Ｈｆ２Ｏ７の微粒結晶
が、原料のＹα−サイアロンの組成より式ＣＩ）のＸが
若干低いＹα−サイアロンの結晶と共に存在する。The sialon-based sintered body of the present invention contains β-sialon crystals, a glass phase containing Y, and a fluorite type crystallized at grain boundaries, which are thought to be produced by the reaction between Yα-sialon and α-silicon nitride. Fine grain crystals having a crystal structure of Y2Hf2O7 exist together with crystals of Yα-sialon having a slightly lower X of formula CI) than the composition of the raw material Yα-sialon.
この様なＹｚＨｆ、ｏ、の微粒結晶により粒界相（Ｙｚ
ＨｆｇｏｔとＹを含むガラス相）の強度特性が向上し、
また焼結体中には組成、結晶形及び熱膨張率の異なる４
種類の相が存在し、焼結後に焼結体中に微小歪に基づく
微小クランクが発生することにより、得られるサイアロ
ン基焼結体の破壊靭性等の機械的特性が向上するもとの
考えられる。Such fine crystals of YzHf, o form a grain boundary phase (Yz
The strength properties of the glass phase (containing Hfgot and Y) are improved,
In addition, there are four types of sintered bodies with different compositions, crystal shapes, and coefficients of thermal expansion.
It is thought that the presence of different types of phases and the generation of microcranks based on microstrains in the sintered body after sintering improve the mechanical properties such as fracture toughness of the resulting sialon-based sintered body. .
本発明のサイアロン基焼結体を製造する方法としては、
前記構造の焼結体が得られれば、どのような方法を用い
てもよい。The method for producing the sialon-based sintered body of the present invention includes:
Any method may be used as long as a sintered body having the above structure can be obtained.
以下に、本発明のサイアロン基焼結体を製造する方法の
一例を示す。An example of a method for manufacturing the sialon-based sintered body of the present invention is shown below.
本発明のサイアロン基焼結体は、前記式（１）で表され
るＹα−サイアロンを主たる相とし、かつ式（１）で規
定される理論酸素量に対して８重量％以下の過剰酸素を
含有するＹα−サイアロン粉末５０重量％以下、酸化ハ
フニウム粉末１５重量％以下、及び残部がα−窒化珪素
粉末からなる原料粉末を、最高温度１６００〜２１００
°Ｃの範囲に加熱、焼結することにより得られる。The sialon-based sintered body of the present invention has Yα-sialon represented by the formula (1) as a main phase, and contains 8% by weight or less of excess oxygen with respect to the theoretical oxygen amount defined by the formula (1). The raw material powder containing 50% by weight or less of Yα-sialon powder, 15% by weight or less of hafnium oxide powder, and the balance consisting of α-silicon nitride powder is heated to a maximum temperature of 1600 to 2100.
It is obtained by heating and sintering in the range of °C.
Ｙα−サイアロン粉末としては、式（１）で表されるＹ
α−サイアロンを主たる相とする粉末であればいかなる
粉末でも良いが、本出願人が先に提案した特開昭６２−
２２３００９号の発明に従って調製した粉末が好適であ
る。この提案の方法は、
（ａ）非晶質窒化珪素粉末、
（ｂ）金属アルミニウム又は窒化アルミニウム、（ｃ）
Ｙα−サイアロンの格子間に侵入型固溶するＹの酸化物
を生成する金属塩類、及び必要に応じて、
（ｄ）アルミニウム又は珪素の酸素含有化合物を所望の
Ｙα−サイアロン組成になるように混合し、混合物を窒
素含有雰囲気下で１３００〜１９００°Ｃの範囲の温度
に加熱することにより、Ｙα−サイアロン粉末を製造す
る方法である。この方法で得られるＹα−サイアロン粉
末は、−成粒子の大きさが０．２〜２μｍの微細かつ均
一粒度の粉末であって、遊離炭素及び金属不純物を殆ど
含有しないので、気孔及び異常粒成長のない焼結体を与
えることができる。As Yα-sialon powder, Y expressed by formula (1)
Any powder may be used as long as it has α-sialon as its main phase.
Powders prepared according to the invention of No. 223009 are preferred. This proposed method consists of (a) amorphous silicon nitride powder, (b) metallic aluminum or aluminum nitride, (c)
A metal salt that forms an oxide of Y that forms an interstitial solid solution between the lattices of Yα-sialon, and (d) an oxygen-containing compound of aluminum or silicon, if necessary, is mixed to obtain a desired Yα-sialon composition. This is a method for producing Yα-sialon powder by heating the mixture to a temperature in the range of 1300 to 1900°C under a nitrogen-containing atmosphere. The Yα-sialon powder obtained by this method is a fine and uniform powder with a particle size of 0.2 to 2 μm, and contains almost no free carbon and metal impurities, so it does not have pores or abnormal grain growth. It is possible to provide a sintered body without
Ｙα−サイアロン粉末の焼結性を高めると同時に高強度
のサイアロン基焼結体を得るためには、焼結原料のＹα
−サイアロン粉末が式ＣＩ）で規定される理論酸素量に
対して８重量％以下の過剰酸素を含有していることが必
要である。In order to improve the sinterability of the Yα-sialon powder and at the same time obtain a high-strength sialon-based sintered body, it is necessary to increase the sintering raw material Yα.
- It is necessary that the Sialon powder contains not more than 8% by weight of excess oxygen relative to the theoretical oxygen amount defined by formula CI).
Ｙα−サイアロン粉末に過剰の酸素を含有させる方法と
しては、例えば、Ｙα−サイアロン粉末の調製段階で非
晶質窒化珪素に珪素、アルミニウム又はイツトリウムの
酸素含有化合物を過剰量添加する方法、Ｙα−サイアロ
ン粉末を酸素含有雰囲気中で加熱する方法が採用される
。後者の一例としては、Ｙα−サイアロン粉末を酸素含
有雰囲気中で８００〜１２００°Ｃの範囲の温度に加熱
して、理論量より過剰の酸素をＹα−サイアロン粉末に
含有させる方法が挙げられる。加熱時間は通常０．５〜
５時間である。この処理は、例えばＹαサイアロン粉末
を保持板上に薄く乗せて酸素含有雰囲気中に放置する方
法、α−サイアロン粉末を酸素含有雰囲気中で流動化さ
せる方法によって行うことができる。Examples of methods for containing excess oxygen in the Yα-sialon powder include a method of adding an excessive amount of an oxygen-containing compound of silicon, aluminum, or yttrium to amorphous silicon nitride in the preparation stage of the Yα-sialon powder; A method is employed in which the powder is heated in an oxygen-containing atmosphere. An example of the latter is a method in which Yα-sialon powder is heated to a temperature in the range of 800 to 1200° C. in an oxygen-containing atmosphere to cause the Yα-sialon powder to contain oxygen in excess of the stoichiometric amount. Heating time is usually 0.5~
It is 5 hours. This treatment can be carried out, for example, by placing Yα-sialon powder thinly on a holding plate and leaving it in an oxygen-containing atmosphere, or by fluidizing α-sialon powder in an oxygen-containing atmosphere.
過剰酸素量は８重量％以下、好ましくは１〜６．５重量
％、特に好ましくは２〜４重量％である。The amount of excess oxygen is 8% by weight or less, preferably 1 to 6.5% by weight, particularly preferably 2 to 4% by weight.
過剰酸素量が過度に多いと焼結体中に融点の低い相が多
く残留し、高温での機械的特性が損なわれるようになる
。If the amount of excess oxygen is too large, many phases with a low melting point remain in the sintered body, which impairs the mechanical properties at high temperatures.
α−窒化珪素粉末としては、焼結性の面で１μｍ以下の
粒径を有していることが好ましく、さらに得られる焼結
体の高温での強度、耐蝕性、耐酸化性を損なう不純物の
含有量が１重量％以下であることが好ましい。The α-silicon nitride powder preferably has a particle size of 1 μm or less in terms of sinterability, and further contains impurities that impair the strength, corrosion resistance, and oxidation resistance of the resulting sintered body at high temperatures. It is preferable that the content is 1% by weight or less.
Ｙα−サイアロン粉末、α−窒化珪素粉末、及び酸化ハ
フニウム粉末の混合物中のα−窒化珪素粉末の配合割合
は３０重量％以上、好ましくは５０〜９０重量％、さら
に好ましくは６０〜８０重量％である。上記範囲内にお
いて窒化珪素粉末の配合割合を高めるに従って生成サイ
アロン基焼結体中のβ−サイアロン相の割合が増大する
。α−窒化珪素粉末の配合割合が９０重量％を超えると
、混合物の焼結性が低下し焼結体の緻密化が進行しなく
なる。また、必要に応じて、１０重量％以下の酸化イツ
トリウム粉末を添加することもできる。The blending ratio of α-silicon nitride powder in the mixture of Yα-sialon powder, α-silicon nitride powder, and hafnium oxide powder is 30% by weight or more, preferably 50 to 90% by weight, and more preferably 60 to 80% by weight. be. Within the above range, as the blending ratio of silicon nitride powder increases, the ratio of the β-sialon phase in the produced sialon-based sintered body increases. When the blending ratio of the α-silicon nitride powder exceeds 90% by weight, the sinterability of the mixture decreases and the densification of the sintered body does not proceed. Further, if necessary, 10% by weight or less of yttrium oxide powder can be added.
Ｙα−サイアロン粉末、α−窒化珪素粉末、及び酸化ハ
フニウム粉末の混合方法については特に制限はなく、そ
れ自体公知の方法、例えば、両者を乾式混合する方法、
不活性液体中で両者を湿式混合した後不活性液体を除去
する方法等を適宜採用することができる。混合装置とし
てはＶ型混合機、ボールミル等が便利に使用される。There are no particular restrictions on the method of mixing Yα-sialon powder, α-silicon nitride powder, and hafnium oxide powder, and methods known per se, such as a method of dry mixing the two,
A method of wet-mixing both in an inert liquid and then removing the inert liquid can be appropriately adopted. As a mixing device, a V-type mixer, a ball mill, etc. are conveniently used.
混合粉末の加熱焼結は、例えば、混合粉末をそのまま乾
式あるいは湿式で所定の形状に成形し、湿式で成形した
場合は乾燥処理を行った後に、常圧又は加圧した窒素含
有非酸化性ガス雰囲気下で焼結する方法、原料粉末を所
定の形状のダイスに充填し、ホットプレスする方法等を
採用することができる。また上記方法で得られた焼結体
をさらに熱間静水圧プレスすることにより、焼結体の物
理的特性を一層高めることもできる。For heating and sintering of mixed powder, for example, the mixed powder is directly shaped into a predetermined shape using a dry or wet method, and if it is formed using a wet method, it is dried and then heated with a nitrogen-containing non-oxidizing gas under normal pressure or pressurized. A method of sintering in an atmosphere, a method of filling a die of a predetermined shape with raw material powder and hot pressing, etc. can be adopted. Moreover, by further subjecting the sintered body obtained by the above method to hot isostatic pressing, the physical properties of the sintered body can be further improved.
常圧又は雰囲気加圧焼結に先立つ混合粉末の成形は公知
の方法、例えばラバープレス法、−軸成形法、鋳込成形
法、射出成形法、爆発圧縮成形法等によって行うことが
できる。Molding of the mixed powder prior to normal pressure or atmospheric pressure sintering can be performed by a known method, such as a rubber press method, a -axial molding method, a cast molding method, an injection molding method, an explosive compression molding method, and the like.
焼結温度は通常１６００〜２１００°Ｃであり、焼結時
間は通常０．５〜１０時間である。焼結温度が過度に低
いと焼結が進行せず、また焼結温度が過度に高いと焼結
体に熱分解による組成変化が生じるようになる。The sintering temperature is usually 1600 to 2100°C, and the sintering time is usually 0.5 to 10 hours. If the sintering temperature is too low, sintering will not proceed, and if the sintering temperature is too high, a compositional change will occur in the sintered body due to thermal decomposition.
（発明の効果）
本発明で得られるサイアロン基焼結体は、従来のサイア
ロン基焼結体に比較して、高温強度、破壊靭性等の機械
的特性が向上しているので、信顛性の高い構造材料、特
にガスタービン部品、切削チップ、ロール、ダイス、ノ
ズル等の耐摩耗、耐熱材料として好適に使用することが
できる。(Effects of the Invention) The sialon-based sintered body obtained by the present invention has improved mechanical properties such as high temperature strength and fracture toughness compared to conventional sialon-based sintered bodies, so it has improved reliability. It can be suitably used as a highly structural material, especially as a wear-resistant and heat-resistant material for gas turbine parts, cutting chips, rolls, dies, nozzles, etc.
（実施例） 以下に実施例及び比較例を示す。(Example) Examples and comparative examples are shown below.
実施例１〜５及び比較例１
非晶質窒化珪素粉末５００ ｇ、ＹｔＯｘ粉末６２ｇ及
び金属Ａｌ粉末６５．７ ｇを窒素ガス雰囲気下に振動
ミルで１時間混合した。混合粉末をカーボン製ルツボに
充填して抵抗加熱式高温炉にセットし、窒素ガス雰囲気
下、室温から１２００°Ｃ迄を１時間、１２００°Ｃか
ら１４００’Ｃ迄を４時間、さらに１４００″Ｃから１
６００ ’Ｃ迄を２時間の昇温スケジュールで加熱する
ことにより結晶化させ、Ｙα−サイアロン粉末を得た。Examples 1 to 5 and Comparative Example 1 500 g of amorphous silicon nitride powder, 62 g of YtOx powder, and 65.7 g of metal Al powder were mixed for 1 hour in a vibration mill under a nitrogen gas atmosphere. The mixed powder was filled into a carbon crucible, set in a resistance heating high temperature furnace, and heated under a nitrogen gas atmosphere from room temperature to 1200°C for 1 hour, from 1200°C to 1400'C for 4 hours, and then at 1400'C. from 1
It was crystallized by heating up to 600'C on a 2 hour heating schedule to obtain Yα-Sialon powder.
得られたＹα−サイアロン粉末の特性を以下に示す。The properties of the obtained Yα-sialon powder are shown below.
理論組成 Ｙｏ、 ５ｓｉｖ、 ｙｓＡｌｚ、 ｚｓＯ
ｏ、 ？ＳＮＩ Ｓ、 ｚｓ比表面積 ２．５ボ／ｇ
粒子形状 等軸結晶
生成相 α相２９０％
生成物組成（ｗｔχ）
Ｙニア、２ Ｓｉ：４４．２ Ａｌ：９．８ ０：
４．９ Ｎ：３３．９過剰酸素量 ２．９重量％
上記Ｙα−サイアロン粉末、α−窒化珪素粉末（宇部興
産■製５Ｎ−ＥＩＯ；比表面積：１１ボ／ｇ、酸素含有
量：１．３ｗｔ％）、及び酸化ハフニウム粉末（ヘルマ
ン・シー・スタルク■製）を第１表に示す割合で、媒体
としてエタノールを用い４８時間湿式ボールミリングし
た後、８０°Ｃで真空乾燥した。得られた原料粉末４０
ｇを表面が窒化硼素で被覆された内径１００印の黒鉛製
ダイスに充填し、ホットプレス焼結装置にセットした後
、２５０ ｋｇ／ｃｉの加圧下に室温から１７５０°Ｃ
まで２００°Ｃ／時で昇温し、同温度に１時間保持した
。Theoretical composition Yo, 5siv, ysAlz, zsO
o, ? SNI S, zs specific surface area 2.5bo/g Particle shape Equiaxed crystallization phase α phase 290% Product composition (wtχ) Ynia, 2 Si: 44.2 Al: 9.8 0:
4.9 N: 33.9 Excess oxygen amount 2.9% by weight The above Yα-sialon powder, α-silicon nitride powder (5N-EIO manufactured by Ube Industries, Ltd.; specific surface area: 11 bo/g, oxygen content: 1. 3 wt %) and hafnium oxide powder (manufactured by Hermann C. Starck ■) in the proportions shown in Table 1 were wet ball milled for 48 hours using ethanol as a medium, and then vacuum dried at 80°C. Obtained raw material powder 40
After filling a graphite die with an inner diameter of 100 marks and whose surface is coated with boron nitride and setting it in a hot press sintering device, the die was heated from room temperature to 1750°C under a pressure of 250 kg/ci.
The temperature was raised at a rate of 200°C/hour until the temperature reached 200°C, and the temperature was maintained at the same temperature for 1 hour.
作製した焼結体から３Ｘ４Ｘ５０ｍｍのテストピース５
０本を切り出し、これを外スパン３０Ｍ１１、内スパン
１０＋ｍａの４点曲げ強度試験を行い（室温及び１４０
０℃）強度及びワイブル係数を求めた。Test piece 5 of 3X4X50mm from the produced sintered body
0 was cut out and subjected to a 4-point bending strength test with an outer span of 30M11 and an inner span of 10+ma (at room temperature and at 140mA).
(0°C) strength and Weibull coefficient were determined.
また、５ＥＰＢ法によりＫＩＣを測定した。結果を第１
表に示す。Further, KIC was measured by the 5EPB method. Results first
Shown in the table.
実施例６〜１３及び比較例２
実施例１〜５で使用したＹα−サイアロン粉末、α−窒
化珪素粉末及び酸化ハフニウム粉末を第２表に示す割合
で、媒体としてエタノールを用い４８時間湿式ボールミ
リングした後、８０℃で真空乾燥した。Examples 6 to 13 and Comparative Example 2 The Yα-sialon powder, α-silicon nitride powder, and hafnium oxide powder used in Examples 1 to 5 were wet ball milled for 48 hours using ethanol as a medium in the proportions shown in Table 2. After that, it was vacuum dried at 80°C.
粉末混合物を、断面が５０Ｘ８０ｒＭ１角の金型を用い
て予備成形した後、圧力１．５ｔｏｎ／ｄでラバープレ
スした。得られた成形品を電気炉を用いて、第２表に記
載の温度−雰囲気ガス圧力条件下に昇温し、同温度に２
時間保持して、常圧焼結又は雰囲気加圧焼結を行った。The powder mixture was preformed using a mold with a cross section of 50 x 80 rM, and then rubber pressed at a pressure of 1.5 ton/d. The obtained molded product was heated in an electric furnace under the temperature and atmospheric gas pressure conditions listed in Table 2, and then heated to the same temperature for 2 hours.
Pressureless sintering or atmospheric pressure sintering was performed by holding for a certain time.
得られた焼結体の特性を実施例１と同様にして測定した
。結果を第２表に示す。The properties of the obtained sintered body were measured in the same manner as in Example 1. The results are shown in Table 2.
Claims (1)
Ｙ＿ｘ（Ｓｉ，Ａｌ）＿１＿２（Ｏ，Ｎ）＿１＿６（式
中、ｘは０＜ｘ≦２を満足する数である。）で表される
Ｙα−サイアロンの結晶、 式Ｓｉ＿６＿−＿ｚＡｌ＿ｚＯ＿２Ｎ＿８＿−＿ｚ（式
中、ｚは０＜ｚ≦４．２を満足する数である。）で表さ
れるβ−サイアロンの結晶及びＹを含むガラス相からな
る高強度サイアロン基焼結体。[Claims] Microcrystals of Y_2Hf_2O_7 with a fluorite crystal structure, formula Y_x(Si,Al)_1_2(O,N)_1_6 (where x is a number satisfying 0<x≦2.) Yα-Sialon crystal represented by the formula Si_6_-_zAl_zO_2N_8_-_z (wherein, z is a number satisfying 0<z≦4.2); A high-strength sialon-based sintered body consisting of a glass phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1291247A JPH03153574A (en) | 1989-11-10 | 1989-11-10 | High strength sialon-based sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1291247A JPH03153574A (en) | 1989-11-10 | 1989-11-10 | High strength sialon-based sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03153574A true JPH03153574A (en) | 1991-07-01 |
| JPH0559074B2 JPH0559074B2 (en) | 1993-08-30 |
Family
ID=17766391
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1291247A Granted JPH03153574A (en) | 1989-11-10 | 1989-11-10 | High strength sialon-based sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03153574A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005298299A (en) * | 2004-04-14 | 2005-10-27 | Kurosaki Harima Corp | Silicon nitride-based disk |
| WO2008068283A2 (en) * | 2006-12-06 | 2008-06-12 | Ceramtec Ag | Material based on sialons |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101654964B1 (en) * | 2013-04-11 | 2016-09-08 | 배건택 | Portable treatment machine of periodontitis |
-
1989
- 1989-11-10 JP JP1291247A patent/JPH03153574A/en active Granted
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005298299A (en) * | 2004-04-14 | 2005-10-27 | Kurosaki Harima Corp | Silicon nitride-based disk |
| WO2008068283A2 (en) * | 2006-12-06 | 2008-06-12 | Ceramtec Ag | Material based on sialons |
| WO2008068283A3 (en) * | 2006-12-06 | 2008-09-12 | Ceramtec Ag | MATERIAL BASED ON SiAlONS |
| US9637417B2 (en) | 2006-12-06 | 2017-05-02 | Ceramtec Gmbh | Material based on SiAlONs |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0559074B2 (en) | 1993-08-30 |
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