JPH01208370A - Production of highly tough calcined silicon nitride compact - Google Patents
Production of highly tough calcined silicon nitride compactInfo
- Publication number
- JPH01208370A JPH01208370A JP63030059A JP3005988A JPH01208370A JP H01208370 A JPH01208370 A JP H01208370A JP 63030059 A JP63030059 A JP 63030059A JP 3005988 A JP3005988 A JP 3005988A JP H01208370 A JPH01208370 A JP H01208370A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- average particle
- dispersed particles
- powder
- particle diameter
- 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 abstract description 16
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000002245 particle Substances 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 14
- 150000001247 metal acetylides Chemical class 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 6
- 150000004767 nitrides Chemical class 0.000 claims abstract description 6
- 239000006104 solid solution Substances 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims description 17
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 7
- 238000001354 calcination Methods 0.000 abstract 3
- 238000000034 method Methods 0.000 description 13
- 239000000919 ceramic Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 229910005091 Si3N Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001272 pressureless sintering Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910026161 MgAl2O4 Inorganic materials 0.000 description 1
- 229910009043 WC-Co Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 229910052634 enstatite Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- 230000009466 transformation 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、靭性の高い窒化珪素焼結体の製法に関するも
ので、エンジニアリングセラミックスとして各種の機械
部品や自動車部品等に有用なものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for manufacturing a silicon nitride sintered body with high toughness, which is useful as engineering ceramics for various mechanical parts, automobile parts, etc.
セラミックスの本質的な性質である脆さを改善するため
の方法はこれまで幾つか提案されている。Several methods have been proposed to improve the brittleness, which is an essential property of ceramics.
板台化による方法は代表的なもので、ウィスカー、繊維
、粒子などの混合・分散による破壊靭性の向上がある。A typical method is to use a plate base, which improves fracture toughness by mixing and dispersing whiskers, fibers, particles, etc.
例えば、焦業協会発行、「特集セラミックスの強靭化に
挑む」セラミックスＶＯ１，２１Δｌ １９８６年７
月号に記されている。現在、窒化珪素焼結体の高靭化に
はウィスカー添加が最も有効と見ら几る。For example, published by Kogyo Association, "Special feature: Challenging the toughening of ceramics" Ceramics VO1, 21Δl, July 1986
It is written in the month issue. Currently, whisker addition is considered to be the most effective way to increase the toughness of silicon nitride sintered bodies.
しかしながら、昏合化による強靭化を行うには均一な分
散が要求される。特にウィスカー、繊維は分散が難しく
湿式ボールミル等で長時間混合しなければならないばか
りでなく、完全な均一分散は実質的に不可能に近いっま
た、スリップキャスト、射出成形等の成形方法も困難と
なる。さらには、ウィスカー、繊維を混入したもの全焼
結することは鰺しく、たとえホットプレス法であっても
理論密度近くにするのは容易ではない。However, uniform dispersion is required for toughening by coagulation. In particular, whiskers and fibers are difficult to disperse, requiring long-term mixing using a wet ball mill, etc., and completely uniform dispersion is virtually impossible, and molding methods such as slip casting and injection molding are also difficult. Become. Furthermore, it is difficult to completely sinter a material containing whiskers and fibers, and it is not easy to achieve a density close to the theoretical density even by hot pressing.
本発明は以上のような問題点上解決し、比較的容易に高
靭性の窒化珪素焼結体を得りうとするものである。The present invention aims to solve the above-mentioned problems and to relatively easily obtain a silicon nitride sintered body with high toughness.
すなわち、本発明は、平均粒径５ＰＬ以下の窒化珪素粉
末金主成分としＭｇＯｉ成分として含有してなる焼結助
剤’ｉ ＭｇＯ換算で０．２〜５容量係と平均粒径１・
５〜１０μ屏でかつ熱膨張係数６×１０−’／℃以上の
ｆｆａ族元素の窒化物、炭化物及びそれらの固溶体から
選ばｎ友少なくとも１種以上の分散粒子１〜５０容量係
と？含んでなる混合粉末を成形・焼結すること全特徴と
する高靭性窒化珪素焼結体の製法である。That is, the present invention provides a sintering aid made of silicon nitride powder having an average particle size of 5 PL or less as a main component of gold and containing as an MgOi component, with an average particle size of 1.
Dispersed particles of at least one type selected from nitrides, carbides, and solid solutions of FFA group elements of nitrides, carbides, and solid solutions thereof of elements of the FFA group having a thermal expansion coefficient of 6 x 10-'/°C or more and having a thickness of 5 to 10 μm and a volume of 1 to 50? This is a method for producing a high-toughness silicon nitride sintered body, which is characterized by molding and sintering a mixed powder comprising the following:
以下、さらに詳しく本発明について説明する。The present invention will be explained in more detail below.
複合化による破壊靭性向上の主な機構として、クラック
・ディフレクション、マイクロクララ午ング、応力誘起
変態、ゾルアウトなどが鳥見られるが、本発明の方法に
おいては、クラック・デイフレクションとマイクロクラ
ラギングが重要である。クラック・デイフレクションは
、マトリックスと分散相の靭性や熱膨張率などの物性の
相違や両者の界面状態などが原因となってクラックが分
散粒子の同り？ジグザグに折れ曲って進むことに工りエ
ネルヤーが散逸するものである。を九、マイクロクラッ
キングも分散相とマトリックスの熱膨張率の差などによ
って分散粒子の周シに歪みが生じ、多数のクラックが発
生し、主クラック先端が微細クラックの生じた領域に進
むと、微細クラック同士が結合して成長したり、新しく
微細クラックが発生し定すしてこの領域の弾性率が低下
する。そのため、主クラック先端にかかる応力が減少す
るものである。The main mechanisms for improving fracture toughness through composite composition include crack deflection, microcracking, stress-induced transformation, and solve-out, but in the method of the present invention, crack deflection and microcracking are is important. Cracks and deflections are caused by differences in physical properties such as toughness and coefficient of thermal expansion between the matrix and dispersed phase, as well as by the state of the interface between the two. The energy of construction is dissipated by zigzagging and bending. 9. Microcracking also causes distortion in the circumference of the dispersed particles due to the difference in thermal expansion coefficient between the dispersed phase and the matrix, and many cracks are generated.When the tip of the main crack advances to the area where the microcracks have occurred, the microcracking occurs. Cracks may combine and grow, or new fine cracks may occur, resulting in a decrease in the elastic modulus of this region. Therefore, the stress applied to the tip of the main crack is reduced.
すなわち、本発明は、窒化珪素焼結体中に特定物性の■
ａ族元素の窒化物、炭化物及び／又はそれらの固溶体粒
子七遍度に分散させることに工り靭性の大幅な改善全可
能としたものである。That is, the present invention provides a silicon nitride sintered body with specific physical properties.
By uniformly dispersing the nitrides, carbides, and/or solid solution particles of group A elements, it is possible to significantly improve the mechanical toughness.
本発明で便用される窒化珪素Ｓｉ３Ｎ４粉末の平均粒径
は５μｍ以下であることを要し、５μｒｌＬ１に越えて
は靭性の改良は認められない。好ましい平均粒径は６−
以下特に１μｍ以下である。The average particle size of the silicon nitride Si3N4 powder conveniently used in the present invention is required to be 5 μm or less, and no improvement in toughness is observed if it exceeds 5 μrlL1. The preferred average particle size is 6-
In particular, the thickness is 1 μm or less.
焼結助剤としては、Ｍｇ０ｔ”成分として含有するもの
？ ＭｇＯ換算で０．２〜５容ｔ％に相当する量を存在
させる。０．２容量憾未漕では焼結効果は少なく、また
、５容量％を越えると強度が低下する。As a sintering aid, what is contained as a Mg0t component?Present in an amount equivalent to 0.2 to 5 volume t% in terms of MgO.If the volume is 0.2 volume, the sintering effect is small, and If it exceeds 5% by volume, the strength will decrease.
ＭｇＯ’ｉ成分として含有しない焼結助剤、例えばＡ１
□ｏ、 −Ｙ２Ｏ，系では高靭性化は達成できない。Sintering aids not included as MgO'i components, such as A1
High toughness cannot be achieved with the □o, -Y2O, system.
本発明で使用される焼結助剤の具体例としては、ＭｇＯ
、ＭｇＡｌ２Ｏ４、Ｍｇ８１０． 、ＭｇＳｉＯ３、Ｍ
ｇ（ＯＨ） ２、Ｍｇ（ＮＯｓ）ａ、Ｍｇ５Ｏ，、コー
ディエライト等から選ばれ九１種又は２種以上である。Specific examples of sintering aids used in the present invention include MgO
, MgAl2O4, Mg810. , MgSiO3, M
91 types or 2 or more types selected from g(OH)2, Mg(NOs)a, Mg5O, cordierite, etc.
なお、本発明においては、Ａｌ２Ｏ３、Ｙ２Ｏ３、ＣＯ
Ａ１ｇ０４ 、ＺｒＯ２，８１０２等の他の焼結助剤と
併用することによって焼結性等全向上させることができ
、その割合は０．２〜５容量チ程度である。In addition, in the present invention, Al2O3, Y2O3, CO
By using it in combination with other sintering aids such as A1g04, ZrO2, 8102, etc., the sinterability and other properties can be completely improved, and the ratio is about 0.2 to 5 by volume.
高靭性化のための分散粒子は種々検討し窺結果、平均粒
径が１．５〜１０μｍでかつ熱膨張係数が６Ｘ １０−
６７’Ｃ以上の■ａ族元素の窒化物、炭化物及びそれら
の固溶体から選ばれ７’ｅ１ｍ以上の無機粉末が良好で
あることを見い出した。具体的な化合物としては、Ｔｉ
Ｎ ＸＴｉＣ、ＺｒＮ ＸＺｒＣ、ＨｆＨ。We investigated various types of dispersed particles to improve toughness and found that the average particle size was 1.5 to 10 μm and the coefficient of thermal expansion was 6X 10-
It has been found that inorganic powders selected from nitrides, carbides, and solid solutions of group (III) elements of 67'C or higher and 7'e1m or higher are good. As a specific compound, Ti
NXTiC, ZrNXZrC, HfH.
ＨｆＣ、ＴｉＣ０５Ｎ Ｏ，５環上あげることができる
。特にＴｉＮは最も良好な靭性化を示し友。Examples include HfC, TiC05N O, 5-ring. In particular, TiN shows the best toughness.
分散粒子の平均粒径が１．５μｍ未満又は１０μｍケこ
えては高靭性化は期待できない。また、熱膨張係数が６
Ｘ １０−６ ／°Ｏ未滴の粒子であっても同様に期
待できず、さらには、本発明に係る熱膨張係数を有して
も上記し九以外の化合物、例えば■ａ族元素の金属、硼
化物、酸化物等であっては高靭性化？達成することがで
きない。望ましい熱膨張係数は８ Ｘ １０−’ ／’
Ｃ以上である。分散粒子の含有量は、Ｓｉ３Ｎ、粉末、
焼結助剤及び分散粒子からなる混合粉末中１〜５０容量
係である。１容量係未満では靭性の向上は認めらルす、
また、５０容量％七こえては強度等の物性が低下する。If the average particle diameter of the dispersed particles is less than 1.5 μm or more than 10 μm, high toughness cannot be expected. Also, the coefficient of thermal expansion is 6
The same cannot be expected even if the particle is a droplet of , borides, oxides, etc. to increase toughness? cannot be achieved. Desired coefficient of thermal expansion is 8 x 10-'/'
C or higher. The content of the dispersed particles is Si3N, powder,
The volume ratio is 1 to 50 in a mixed powder consisting of a sintering aid and dispersed particles. No improvement in toughness is observed below 1 volume ratio.
Moreover, if the content exceeds 50% by volume, physical properties such as strength will deteriorate.
Ｓｉ３Ｎ、粉末、焼結助剤、Ｃｒ３Ｃ２粉末の混合は、
ボールミル等の混合＋Ｍ’を用い、湿式あるいは乾式で
行われる。成形・焼結方法とは、一般に、常圧焼結、ホ
ットプレス、ＨＩＰ焼結があるが、特に限定されるもの
ではなく、分散粒子の種類と用途に工って選択される。The mixture of Si3N, powder, sintering aid, and Cr3C2 powder is
Mixing is carried out wet or dry using a ball mill or the like +M'. The molding/sintering method generally includes pressureless sintering, hot pressing, and HIP sintering, but is not particularly limited and is selected depending on the type and purpose of the dispersed particles.
例えば、ＴｉＮについては常圧焼結で高い焼結密度が得
られるが、焼結性の悪いものはホットプレス法が採用さ
れる。For example, for TiN, a high sintered density can be obtained by pressureless sintering, but if the sintering property is poor, the hot pressing method is adopted.
破壊靭性値に工。の測定法には種々あるが、本発明では
ＩＭ （Ｉｎｄｅｎｔａｉｏｎ Ｍｉｃｒｏ ｆｒａｃ
ｔｕｒｅ ）法を採用する。これは、７昭和５９年度通
商産業省工業技術院委託ファインセラミックスの標醜化
に関する調査研究報告書昭和６０年６月ファインセラミ
ックス協会”に記載されている測定法であ夛、試料の鏡
面研磨、圧子圧入、クラック長さ測定、経験式を用い−
ｆｃＫ工。の算出の４つの過程からなる。Modified fracture toughness value. Although there are various methods for measuring , the present invention uses IM (Indentation Micro frac).
ture) method. This is a measurement method described in the 1985 Ministry of International Trade and Industry Agency of Industrial Science and Technology Commissioned Investigation Research Report on Fine Ceramics Defacement (June 1986) by the Fine Ceramics Association. Using press fitting, crack length measurement, and empirical formula -
fcK engineering. It consists of four processes of calculation.
すなわち、表面研磨し九試料にぎツカース圧子全圧入す
る。装置はビッカースやヌープ硬度計を用いる。試料に
発生し几クラックの長さ七光学顕微鏡あるいはＳ−を用
いて測定するものである。That is, the surface is polished and nine samples are fully pressed into the indenter. The device used is Vickers or Knoop hardness tester. The length of the cracks that occur in the sample is measured using an optical microscope or S-.
Ｋ工。全算出する経験式は数多くあるが、本発明では次
式を用いた。K engineering. Although there are many empirical formulas for total calculation, the following formula is used in the present invention.
（Ｋ工（Ｈ＜６／！！ＬＡ） （ＨＡ＄）’ ＝ Ｏ−
１２９（ｃ／ａ） ＡＥ・・・ヤング率、Ｈ・・・硬度
、ａ・・・圧痕長さ、Ｃ・・・亀裂長さ、φ＝６、荷重
は２０ゆ、荷重印加時間１５秒間
各種セラミックスの破壊靭性１１ｉＫ工。（ＭＰａ−ｍ
Ａ ）は、一般に、Ｓｉ３Ｎ、 ４〜６．８１Ｃ’ ３
〜５、Ａ１２０３６〜５、部分安定化＆ｒＣ）ａ（ＰＳ
Ｚ） ７〜１０、ガラス０．７５、ＷＣ−Ｃｏ合金１２
〜１６、アルミ合金６４と２われている。本発明によれ
ば、これｔ常圧焼結に１夛７以上にすることができるも
のである。(K engineering (H<6/!!LA) (HA$)' = O-
129 (c/a) AE... Young's modulus, H... hardness, a... indentation length, C... crack length, φ=6, load is 20 mm, load application time is 15 seconds, various Fracture toughness of ceramics is 11iK. (MPa-m
A) is generally Si3N, 4-6.81C'3
~5, A12036~5, Partially Stabilized &rC) a(PS
Z) 7-10, glass 0.75, WC-Co alloy 12
~16, aluminum alloy 64 and 2. According to the present invention, the pressureless sintering process can be performed in 1 to 7 times or more.
以下、実施例ｔあげてさらに具体的に本発明全説明する
。Hereinafter, the present invention will be fully explained in more detail with reference to Example t.
実施例１
表−１に示す種々の容量チの焼結助剤Ｍｇｏ、ＭｇＡｌ
２Ｏ４、Ａｌ２Ｏ３、Ｙ２Ｏ３及び分散粒子として平均
粒径４．Ｏｔｔｍ、熱膨張係数９．５ ｘ １０−リ／
’Ｑ （Ｄ ＴｉＮ粉末１５容ｉｎ’を平均粒径０．
６μ扉の５１３Ｎ４粉末（′ｌ！気化学工業社製ＳＮ
−ＧＤ ６）に混合して全体全１００容量チの混合粉末
上調製し九〇これを１７５０°Ｃ，６時間、Ｎ２９に９
／ｃＩｒ？−の常圧焼結法により８１３Ｎ、焼結体を得
、破壊靭性値に工。？測定した。その結果を表−１に示
す。Example 1 Sintering aids Mgo, MgAl with various capacities shown in Table-1
2O4, Al2O3, Y2O3 and dispersed particles with an average particle size of 4. Ottm, coefficient of thermal expansion 9.5 x 10-li/
'Q (D) 15 volumes of TiN powder with an average particle size of 0.
6μ door 513N4 powder ('l! SN manufactured by Ki Kagaku Kogyo Co., Ltd.
-GD 6) to prepare a total of 100 volumes of mixed powder.
/cIr? - A sintered body of 813N was obtained by the pressureless sintering method, and the fracture toughness value was improved. ? It was measured. The results are shown in Table-1.
表−１
（注）実験屑２〜７．９及び１１は本発明例、実験／ｒ
６１．８及び１０は比較例である。なお、実験屑１は硬
度不足にエリＫＩＣ”測定することはできなかった。Table-1 (Note) Experimental scraps 2 to 7.9 and 11 are examples of the present invention, experiment/r
61.8 and 10 are comparative examples. It should be noted that it was not possible to measure EriKIC'' for Experimental Scrap 1 due to insufficient hardness.
実施例２
表−１の実験腐９において、ＴｉＮ粉末を種々の割合と
じＳｉ３Ｎ、粉末に置きかえて使用したこと以外は同様
の条件で焼結体を作製し破壊靭性ｔＫＩＣ’勿測定した
。その結果全表−２に示す。Example 2 Sintered bodies were produced under the same conditions as in Experiment 9 in Table 1, except that TiN powder was replaced with Si3N powder in various proportions, and the fracture toughness tKIC' was measured. The results are shown in Table 2.
表−２
（注）実験／１６１３〜１９は本発明例、実験層１２及
び２０は比較例である。Table 2 (Note) Experiments/1613 to 19 are examples of the present invention, and experimental layers 12 and 20 are comparative examples.
実施例３
表−１の実験層９において、Ｓｉ３Ｎ、粉末とＴｉＮ粉
末の平均粒径を表−３に示すぶつに変えたこと以外は同
機の条件で焼結体を作製し破壊靭性、１に工。とＪＩＳ
Ｒ１６０１の常温曲げ強度を測定した。Example 3 A sintered body was produced under the same conditions as in the same machine except that in experimental layer 9 of Table 1, the average particle diameters of Si3N powder and TiN powder were changed to those shown in Table 3, and the fracture toughness was 1. Engineering. and JIS
The room temperature bending strength of R1601 was measured.
それらの結果を表−６に示す。The results are shown in Table-6.
以下余白
表−３
（注）実験／ｌ６２ｉ〜２４．２７〜３０は本発明例、
実験Ａ２５．２６及び６１は比較例である。Margin Table-3 (Note) Experiment/l62i~24.27~30 are examples of the present invention,
Experiments A25, 26 and 61 are comparative examples.
実施例４
表−１の実験／１６９において、平均粒径４．０μｍの
ＴｉＮ粉末のかわシに表−４に示す種々の分散粒子？用
い、かつ、１６５０℃、２時間、３００ｋｇ／Ｃ！ＩＬ
２の条件でホットプレス焼結し丸こと以外は同様の条件
で焼結体を作製し破壊靭性値に工。を測定した。その結
果を表−４に示す。Example 4 In the experiment/169 shown in Table 1, various dispersed particles shown in Table 4 were added to TiN powder with an average particle size of 4.0 μm. and 1650℃, 2 hours, 300kg/C! IL
A sintered body was produced under the same conditions except for hot press sintering under the conditions of 2, and the fracture toughness was determined. was measured. The results are shown in Table 4.
以下余白
表−４
（注）実験層６２〜６８は本発明例、実験／１ｆｉ３９
〜４２は比較例である。Margin Table-4 (Note) Experimental layers 62 to 68 are examples of the present invention, Experiment/1fi39
-42 are comparative examples.
以上の実施例から次のことがわかる。The following can be seen from the above examples.
（１）実施例１からＭｇＯｉ成分として含有してなる焼
結助剤の添加量は、１容量チ以上５容量係が適切である
。中でも、ＭｇＡ１□０４＋Ａ】２０３系が最も高いＫ
ＩＣｋ示した。Ａｌ２Ｏ３＋Ｙ２Ｏ３系は最も低い値全
示し九がＭｌｇＯｉ加えることによりＫＩＣは向上した
。(1) From Example 1, the appropriate amount of the sintering aid contained as the MgOi component is 1 to 5 by volume. Among them, the MgA1□04+A]203 series has the highest K
ICk was shown. The Al2O3+Y2O3 system showed the lowest value in all cases, but the KIC was improved by adding MlgOi.
（２）実施例２から分散粒子が１容量チ以上５０容量チ
以下で７．０〜９＊６ＭＰａ−ｍ／ｉのＫＩＣが得られ
る。(2) From Example 2, a KIC of 7.0 to 9*6 MPa-m/i can be obtained when the dispersed particles are 1 to 50 volumes.
（３）実施例６にはＳｉ３Ｎ、粉末と分散粒子の平均粒
径の影響が示されてお’）、Ｓ’３Ｎ４は５．０μｍ以
下、分散粒子は１．５μｍ以上１０μｍ以下で７．０〜
９．２ＭＰａ−ｍ／ｌのにＩＣが得られる。(3) Example 6 shows the influence of the average particle size of Si3N, powder and dispersed particles. ~
An IC of 9.2 MPa-m/l is obtained.
（４）実施例４では熱膨張係数が破壊靭性値に与える影
響が調べられており、ｌＶａ族の炭化物、窒化物及びそ
れらの固溶体であって熱膨張係数が６、ＯＸ １ ｏ−
６７１以上のものにおいて初めて７、ＯＭｐａ−ｍＡ以
上の高い靭性１！’ｔ”達成することができる。(4) In Example 4, the influence of the coefficient of thermal expansion on the fracture toughness value was investigated.
High toughness of 7, OMpa-mA or higher for the first time in 671 or higher! 't' can be achieved.
本発明の方法によれば、簡単に高靭性の窒化珪素焼結体
全製造することができる。According to the method of the present invention, a highly tough silicon nitride sintered body can be easily manufactured.
特許出願人 電気化学工業株式会社Patent applicant Denki Kagaku Kogyo Co., Ltd.
Claims (1)
ＭｇＯを成分として含有してなる焼結助剤をＭｇＯ換算
で０．２〜５容量％と平均粒径１．５〜１０μｍでかつ
熱膨張係数６×１０＾−＾６／℃以上のIVａ族元素の窒
化物、炭化物及びそれらの固溶体から選ばれた少なくと
も１種以上の分散粒子１〜５０容量％とを含んでなる混
合粉末を成形・焼結することを特徴とする高靭性窒化珪
素焼結体の製法。(1) A sintering aid mainly composed of silicon nitride powder with an average particle size of 5 μm or less and containing MgO as a component with an average particle size of 1.5 to 10 μm and 0.2 to 5 volume % in terms of MgO, and A mixed powder containing 1 to 50% by volume of at least one type of dispersed particles selected from nitrides, carbides, and solid solutions of group IVa elements having a thermal expansion coefficient of 6 x 10^-^6/°C or more. A method for producing a high-toughness silicon nitride sintered body, which is characterized by forming and sintering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63030059A JPH0653610B2 (en) | 1988-02-13 | 1988-02-13 | Manufacturing method of high toughness silicon nitride sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63030059A JPH0653610B2 (en) | 1988-02-13 | 1988-02-13 | Manufacturing method of high toughness silicon nitride sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01208370A true JPH01208370A (en) | 1989-08-22 |
| JPH0653610B2 JPH0653610B2 (en) | 1994-07-20 |
Family
ID=12293256
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63030059A Expired - Lifetime JPH0653610B2 (en) | 1988-02-13 | 1988-02-13 | Manufacturing method of high toughness silicon nitride sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0653610B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0649824A3 (en) * | 1993-10-25 | 1996-04-10 | Toshiba Kk | Silicon nitride-based sinters. |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59207880A (en) * | 1983-05-13 | 1984-11-26 | 工業技術院長 | Manufacture of silicon nitride sintered body |
-
1988
- 1988-02-13 JP JP63030059A patent/JPH0653610B2/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59207880A (en) * | 1983-05-13 | 1984-11-26 | 工業技術院長 | Manufacture of silicon nitride sintered body |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0649824A3 (en) * | 1993-10-25 | 1996-04-10 | Toshiba Kk | Silicon nitride-based sinters. |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0653610B2 (en) | 1994-07-20 |
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