JPS632914B2 - - Google Patents
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- Publication number
- JPS632914B2 JPS632914B2 JP58180625A JP18062583A JPS632914B2 JP S632914 B2 JPS632914 B2 JP S632914B2 JP 58180625 A JP58180625 A JP 58180625A JP 18062583 A JP18062583 A JP 18062583A JP S632914 B2 JPS632914 B2 JP S632914B2
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- sintered body
- conductivity
- powder
- 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.)
- Expired
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- 239000000843 powder Substances 0.000 claims description 25
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 23
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 23
- 238000005245 sintering Methods 0.000 claims description 12
- 238000009760 electrical discharge machining Methods 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 229910052745 lead Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims 2
- 239000002245 particle Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910012949 LiV2O4 Inorganic materials 0.000 description 1
- 229910003114 SrVO Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002482 conductive additive Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Description
(イ) 技術分野
この発明は導電性を有する窒化けい素
（Si3N4）焼結体の特性の改良に係り、詳しくの
べると、窒化けい素粉末に焼結助剤と導電性付与
剤の両者の働らきを兼ね備えた酸化物粉末を添加
して焼結を行なつて得られる焼結体の粒界層すべ
てに導電性を付与させ、これによつて焼結体全体
の導電率を改善するものであり、これを0.05〜40
体積％の酸化物粉末の添加によつて発揮させた窒
化けい素焼結体およびその製造法に関するもので
ある。
(ロ) 技術背景
従来、窒化けい素焼結体は酸化物を焼結助剤と
し、非酸化性雰囲気中で焼結することによつて、
窒化けい素相とガラス相の２相からなる焼結体と
して得られている。そのため電気絶縁体となつて
いるのである。
しかしてこのような電気絶縁性の焼結体に導電
性の物質を添加することによつて導電率を向上
し、放電加工を行なうといつた報告がなされてい
る。例えば大工試ニユース（工業技術院、大阪工
業技術試験所の刊行物）26(11)1982、および特願昭
56−118239号である。
前者はSiCウイスカーの添加、後者はIVa、
Va、VIa族炭化物、窒化物等の添加によつて放
電加工に必要な導電率を確保するものである。
ところが、前者は焼結体の強度が低く、従来の
焼結体に比べて機械的強度面の改良が必要であ
り、また放電加工肌が劣る点に問題を有してい
た。後者は、導電率に分布が起りやすく、放電加
工性の均一性を得がたい点に問題があつた。
(ハ) 発明の開示
本発明者らは上記のうち特に後者の原因につい
て種々検討を行なつた結果、102Ω-1cm-1以上の
導電率を有する酸化物、なかでもABO3、AB2O4
（ＡおよびＢは後述する元素である）あるいは
ReO3の酸化物の１種または２種以上を窒化けい
素粉末とともに用いることにより、均一な導電性
が得られるとともに、導電性添加物の量を従来よ
り減少させ得ることを見出し、この発明に至つた
ものである。
即ち、この発明は窒化けい素焼結体を得るに当
り、窒化けい素粉末の焼結助剤として、従来用い
られている絶縁体であるMgO、Al2O3、Y2O3な
どの酸化物ではなく、導電性を有し、しかも窒化
けい素粉末の焼結助剤としての働きをする酸化物
を加えたことを特徴とし、これによつて上記した
効果を得るものである。
詳しくのべると、この発明は102Ω-1cm-1以上
の導電率を有するABO3、AB2O4（Ａ、Ｂは夫々
異なる元素を示す）あるいはReO3からなる酸化
物の１種または２種以上を0.05〜40体積％窒化け
い素粉末に添加して焼結した窒化けい素焼結体お
よびその製造法を提供するものである。
この発明において窒化けい素粉末に添加する酸
化物のうちABO3、AB2O4におけるＡおよびＢの
元素としては、ＡはLa、Ca、Sr、Lu、Ba、Cu、
Li、NaがまたＢとしてはTi、Cr、Fe、Co、Ni、
Ru、Zr、Pb、Ｖ、Ｗ、Re、Mo、Nbなどがよ
く、これらの１種または２種以上の酸化物を用い
る場合に効果が最も大きい。この酸化物の窒化け
い素粉末に対する添加量としては、0.05体積％未
満では添加効果が非常に小さく、また40体積％を
超えると窒化けい素が本来有している高硬度、高
強度の特性が低下するため好ましくなく、従つて
0.05〜40体積％の範囲が適当である。
しかして特にこの発明の窒化けい素焼結体の用
途として高温、高強度を必要とする場合には酸化
物の添加量を10体積％以下とすることにより焼結
体強度を損なうことなく、十分な導電率を得るこ
とができる。
さらに焼結体の導電率として10-2Ω-1cm-1を有
するものは放電加工が可能である。
この発明の焼結体を得るに使用する原料粉末と
して1μ以上の窒化けい素粉末、酸化物粉末を使
用した場合は、焼結体強度が低く、さらに1μ以
下の微粒の窒化けい素粉末、導電性酸化物粉末を
使用すれば、添加量を減少させても安定した導電
性を得た。すなわち導電性粉末は焼結体中の0.05
体積％まで添加量を減少させても放電加工が安定
して可能であることが認められた。
また焼結法としては、常圧、非酸化性雰囲気ガ
ス圧、ホツトプレス、HIP焼結のいずれの方法で
も可能である。
上述のようにこの発明は窒化けい素粉末に焼結
助剤を兼ねる導電性粉末としての酸化物粉末を加
え、非酸化性雰囲気下にて焼結することによつて
高温強度、耐酸化性にすぐれ、放電加工によつて
安価に複雑形状品を得るものである。
以下実施例により詳細に説明する。
実施例 １
平均粒径0.5μのSi3N4粉末に第１表に示すよう
な種々の容積比でReO3（平均粒径0.5μ）を焼結助
剤および導電性付与剤として添加し、混合後1700
℃×60分、400Kg／cm2の条件で加圧焼結して
Si3N4焼結体を得た。
そしてこれら焼結体の導電率、抗折力を測定し
たところ第１表に示す結果を得た。
(a) Technical field The present invention relates to improving the characteristics of a conductive silicon nitride (Si 3 N 4 ) sintered body. Adding oxide powder that has both functions and performing sintering imparts conductivity to all grain boundary layers of the sintered body, thereby improving the conductivity of the entire sintered body. 0.05~40
The present invention relates to a silicon nitride sintered body that exhibits its properties by adding oxide powder in a volume percent manner, and a method for producing the same. (b) Technical background Conventionally, silicon nitride sintered bodies are produced by sintering in a non-oxidizing atmosphere using an oxide as a sintering aid.
It is obtained as a sintered body consisting of two phases: a silicon nitride phase and a glass phase. Therefore, it is an electrical insulator. However, it has been reported that by adding a conductive substance to such an electrically insulating sintered body, the conductivity can be improved and electrical discharge machining can be performed. For example, Carpentry Examination News (a publication of the Agency of Industrial Science and Technology, Osaka Institute of Technology) 26(11) 1982, and
No. 56-118239. The former is the addition of SiC whiskers, the latter is IVa,
By adding Va, group VIa carbides, nitrides, etc., the conductivity required for electrical discharge machining is ensured. However, the former has problems in that the strength of the sintered body is low, requires improvement in mechanical strength compared to conventional sintered bodies, and has poor electrical discharge machining surface. The latter has a problem in that it tends to have a distribution of electrical conductivity, making it difficult to obtain uniform electrical discharge machinability. (C) Disclosure of the Invention The present inventors have conducted various studies on the latter cause among the above, and have found that oxides having a conductivity of 10 2 Ω -1 cm -1 or more, especially ABO 3 and AB 2 o 4
(A and B are elements described later) or
It has been discovered that by using one or more ReO 3 oxides together with silicon nitride powder, uniform conductivity can be obtained and the amount of conductive additives can be reduced compared to the conventional one. It has been reached. That is, in obtaining a silicon nitride sintered body, the present invention uses oxides such as MgO, Al 2 O 3 and Y 2 O 3 , which are insulators conventionally used, as a sintering aid for silicon nitride powder. Instead, it is characterized by the addition of an oxide that has conductivity and acts as a sintering aid for the silicon nitride powder, thereby achieving the above-mentioned effects. More specifically, this invention uses one or more oxides consisting of ABO 3 , AB 2 O 4 (A and B each represent a different element) or ReO 3 having a conductivity of 10 2 Ω -1 cm -1 or more. The present invention provides a silicon nitride sintered body obtained by adding 0.05 to 40% by volume of two or more types of silicon nitride powder to sintered silicon nitride powder, and a method for producing the same. In this invention, among the oxides added to silicon nitride powder, the elements A and B in ABO 3 and AB 2 O 4 include La, Ca, Sr, Lu, Ba, Cu,
Li, Na and B are Ti, Cr, Fe, Co, Ni,
Ru, Zr, Pb, V, W, Re, Mo, Nb, etc. are preferable, and the effect is greatest when one or more of these oxides are used. As for the amount of this oxide added to silicon nitride powder, if it is less than 0.05% by volume, the effect of adding it will be very small, and if it exceeds 40% by volume, the high hardness and high strength characteristics that silicon nitride originally has will be lost. undesirable as it reduces
A range of 0.05 to 40% by volume is suitable. However, especially when high temperature and high strength are required for the use of the silicon nitride sintered body of the present invention, by setting the amount of oxide added to 10% by volume or less, sufficient strength can be obtained without impairing the strength of the sintered body. Electrical conductivity can be obtained. Furthermore, a sintered body having an electrical conductivity of 10 -2 Ω -1 cm -1 can be subjected to electrical discharge machining. If silicon nitride powder or oxide powder with a particle size of 1μ or more is used as the raw material powder to obtain the sintered body of this invention, the strength of the sintered body will be low, and if silicon nitride powder with a particle size of 1μ or less or a conductive By using the oxide powder, stable conductivity was obtained even if the amount added was reduced. In other words, the conductive powder is 0.05% in the sintered body.
It was found that electric discharge machining can be performed stably even when the amount added is reduced to % by volume. Further, as the sintering method, any of normal pressure, non-oxidizing atmosphere gas pressure, hot press, and HIP sintering can be used. As mentioned above, this invention improves high-temperature strength and oxidation resistance by adding oxide powder as a conductive powder that also serves as a sintering aid to silicon nitride powder and sintering it in a non-oxidizing atmosphere. Excellent, complex-shaped products can be obtained at low cost by electrical discharge machining. This will be explained in detail below using examples. Example 1 ReO 3 (average particle size 0.5μ) was added as a sintering aid and conductivity imparting agent at various volume ratios as shown in Table 1 to Si 3 N 4 powder with an average particle size of 0.5μ, 1700 after mixing
Pressure sintered at 400Kg/ cm2 for 60 minutes at ℃
A Si 3 N 4 sintered body was obtained. When the electrical conductivity and transverse rupture strength of these sintered bodies were measured, the results shown in Table 1 were obtained.
【表】
実施例 ２
実施例１で用いたReO3に代えて、SrVO3およ
びLiV2O4を用いた以外は実施例１と同様にして
Si3N4焼結体を得た。そしてこれら焼結体の導電
率、抗折力を測定したところ、第２表に示す結果
を得た。[Table] Example 2 The same procedure as in Example 1 was carried out except that SrVO 3 and LiV 2 O 4 were used in place of ReO 3 used in Example 1.
A Si 3 N 4 sintered body was obtained. When the electrical conductivity and transverse rupture strength of these sintered bodies were measured, the results shown in Table 2 were obtained.
【表】
実施例 ３
実施例１に示した第１表のNo.３の組成における
ReO3粉末の粒径を第３表のようにかえて、実施
例１と同様の条件で焼結体を作成し、導電率およ
び抗折力を測定した結果、第３表の通りであつ
た。[Table] Example 3 In the composition No. 3 of Table 1 shown in Example 1
A sintered body was prepared under the same conditions as in Example 1 by changing the particle size of the ReO 3 powder as shown in Table 3, and the conductivity and transverse rupture strength were measured, and the results were as shown in Table 3. .
【表】
実施例 ４
実施例１に示した第１表のNo.３の組成における
Si3N4粉末の粒径を第４表のようにかえて、実施
例１と同様の条件で焼結体を作成し、導電率およ
び抗折力を測定したところ第４表の結果を得た。[Table] Example 4 In the composition No. 3 of Table 1 shown in Example 1
A sintered body was prepared under the same conditions as in Example 1 by changing the particle size of the Si 3 N 4 powder as shown in Table 4, and the conductivity and transverse rupture strength were measured, and the results shown in Table 4 were obtained. Ta.
【表】
実施例 ５
95体積％のSi3N4粉末（平均粒径0.5μ）に第５
表に示す各種酸化物（平均粒径0.5μ）を５体積％
添加し、混合後1850℃×60分、20atmN2ガス雰
囲気下で焼結を行つた。
得られた焼結体の導電率および抗折力を測定し
たところ第５表の結果を得た。[Table] Example 5 95% by volume of Si 3 N 4 powder (average particle size 0.5μ)
5% by volume of various oxides shown in the table (average particle size 0.5μ)
After addition and mixing, sintering was performed at 1850°C for 60 minutes in a 20 atmN 2 gas atmosphere. When the electrical conductivity and transverse rupture strength of the obtained sintered body were measured, the results shown in Table 5 were obtained.
【表】【table】
Claims (1)
を有するABO3、AB2O4（但し、ＡはLa、Ca、
Sr、Lu、Ba、Cu、Liであり、ＢはTi、Cr、Fe、
Co、Ni、Ru、Ir、Pb、Ｖ、Ｗ、Re、Mo、Nb
を表わす）あるいはReO3からなる酸化物の１種
または２種以上を0.05〜40体積％含有してなる窒
化けい素焼結体。 ２ 導電率が10-2Ω-1cm-1以上を有し、放電加工
が可能であることを特徴とする特許請求の範囲第
１項記載の窒化けい素焼結体。 ３ 窒化けい素粉末に102Ω-1cm-1以上の導電率
を有するABO3、AB2O4（但し、ＡはLa、Ca、
Sr、Lu、Ba、Cu、Li、であり、ＢはTi、Cr、
Fe、Co、Ni、Ru、Ir、Pb、Ｖ、Ｗ、Re、Mo、
Nbを表わす）あるいはReO3からなる酸化物の１
種または２種以上を0.05〜40体積％含有する1μ以
下の微粉末を非酸化性雰囲気中で焼結することを
特徴とする窒化けい素焼結体の製造法。[Claims] 1 ABO 3 , AB 2 O 4 having a conductivity of 10 2 Ω -1 cm -1 or more in silicon nitride powder (where A is La, Ca,
Sr, Lu, Ba, Cu, Li, B is Ti, Cr, Fe,
Co, Ni, Ru, Ir, Pb, V, W, Re, Mo, Nb
A silicon nitride sintered body containing 0.05 to 40% by volume of one or more oxides consisting of ReO 3 ) or ReO 3 . 2. The silicon nitride sintered body according to claim 1, which has an electrical conductivity of 10 -2 Ω -1 cm -1 or more and can be subjected to electrical discharge machining. 3 ABO 3 , AB 2 O 4 having a conductivity of 10 2 Ω -1 cm -1 or more in silicon nitride powder (A is La, Ca,
Sr, Lu, Ba, Cu, Li, and B is Ti, Cr,
Fe, Co, Ni, Ru, Ir, Pb, V, W, Re, Mo,
Nb) or an oxide consisting of ReO 3
1. A method for producing a silicon nitride sintered body, which comprises sintering a fine powder of 1 μm or less containing a species or two or more species in an amount of 0.05 to 40% by volume in a non-oxidizing atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58180625A JPS6077173A (en) | 1983-09-30 | 1983-09-30 | Silicon nitride sintered body and manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58180625A JPS6077173A (en) | 1983-09-30 | 1983-09-30 | Silicon nitride sintered body and manufacture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6077173A JPS6077173A (en) | 1985-05-01 |
| JPS632914B2 true JPS632914B2 (en) | 1988-01-21 |
Family
ID=16086472
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58180625A Granted JPS6077173A (en) | 1983-09-30 | 1983-09-30 | Silicon nitride sintered body and manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6077173A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0692270B2 (en) * | 1985-08-15 | 1994-11-16 | 株式会社日立製作所 | Silicon nitride sintered body |
| DE102012207802A1 (en) * | 2012-05-10 | 2013-11-28 | Schaeffler Technologies AG & Co. KG | Silicon nitride ceramics and process for their preparation |
-
1983
- 1983-09-30 JP JP58180625A patent/JPS6077173A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6077173A (en) | 1985-05-01 |
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