JPH0283264A - Production of silicon nitride ceramics and ceramics ball for ball mill used for the same production - Google Patents
Production of silicon nitride ceramics and ceramics ball for ball mill used for the same productionInfo
- Publication number
- JPH0283264A JPH0283264A JP63233721A JP23372188A JPH0283264A JP H0283264 A JPH0283264 A JP H0283264A JP 63233721 A JP63233721 A JP 63233721A JP 23372188 A JP23372188 A JP 23372188A JP H0283264 A JPH0283264 A JP H0283264A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- powder
- ball mill
- ball
- ceramics
- 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
Links
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 29
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000000919 ceramic Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 10
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract 4
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 12
- 239000000203 mixture Substances 0.000 abstract description 5
- 229910052593 corundum Inorganic materials 0.000 abstract 3
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 3
- 238000000034 method Methods 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔概 要〕
窒化珪素（ＳｉＪｎ）セラミックス、より詳しくは、窒
化珪素セラミックスの製造方法での原料粉末混合に関し
、
好ましくない材料の混入をなくし、かつ従来ボールミル
混合を改善して、窒化珪素セラミックスの特性を向上さ
せることを目的とし、
窒化珪素粉末と、焼結助剤粉末との混合工程を有する窒
化珪素セラミックスの製造方法において、少なくともア
ルミナおよびイツトリアからなる緻密性の低いボールミ
ル用セラミックスボールを用いて混合工程をボールミル
で行うように構成する。[Detailed Description of the Invention] [Summary] Regarding the mixing of raw material powder in the manufacturing method of silicon nitride (SiJn) ceramics, more specifically, silicon nitride ceramics, the present invention eliminates the mixing of undesirable materials and improves the conventional ball mill mixing. In order to improve the properties of silicon nitride ceramics, a method for producing silicon nitride ceramics that includes a step of mixing silicon nitride powder and sintering aid powder is used. The mixing process is performed in a ball mill using ceramic balls.
本発明は、窒化珪素（ＳｉＪｔ）セラミックス、より詳
しくは、窒化珪素セラミックスの製造方法での原料粉末
混合に関する。The present invention relates to silicon nitride (SiJt) ceramics, and more particularly to raw material powder mixing in a method for manufacturing silicon nitride ceramics.
窒化珪素セラミックスは高温・高強度のエンジニアリン
グセラミックスとして研究開発が進み実用化が図られて
いる。窒化珪素は高温まで安定で強度低下が少ないが、
このことは逆に難焼結性であることを意味して緻密焼結
は難しい。緻密な焼結体を得るためにかつ常圧焼結を可
能にするために、焼結助剤〔例えば、アルミナ（Ａｅ
ｇｏｓ）−イツトリア（ＭｇＯ３））の添加がなされて
いる。このような焼結助剤の粉末を窒化珪素粉末と均一
に混合させる必要があり、そのために、通常、湿式のボ
ールミルにて長時間混合を行っている。Silicon nitride ceramics are being researched and developed as high-temperature, high-strength engineering ceramics and are being put into practical use. Silicon nitride is stable up to high temperatures and has little strength loss, but
On the contrary, this means that it is difficult to sinter, and dense sintering is difficult. In order to obtain a dense sintered body and to enable pressureless sintering, sintering aids such as alumina (Ae
gos)-yttoria (MgO3)). It is necessary to uniformly mix the sintering aid powder with the silicon nitride powder, and for this purpose, mixing is usually performed for a long time using a wet ball mill.
従来のボールミルにて使用するボールは、超硬合金製、
あるいはアルミナもしくはジルコニア等のセラミック製
である。これは、ボールミル用ボールは混合と同時に粉
砕を行うので、一般に硬い材料が用いられているわけで
ある。しかしながら、長時間のボールミル混合を行うと
、ボールの摩耗によるわずかな混入は避けられない。ボ
ール材料によっては、そのわずかな混入が得られる焼結
体の特性を大きく劣化させることがある。The balls used in conventional ball mills are made of cemented carbide,
Alternatively, it is made of ceramic such as alumina or zirconia. This is because balls for ball mills perform mixing and pulverization at the same time, so generally hard materials are used. However, when ball mill mixing is performed for a long time, slight contamination due to ball wear is unavoidable. Depending on the ball material, even a small amount of ball material may significantly deteriorate the properties of the obtained sintered body.
本発明の目的は、好ましくない材料の混入をなくし、か
つ従来ボールミル混合を改善して、窒化珪素セラミック
スの特性を向上させることである。It is an object of the present invention to improve the properties of silicon nitride ceramics by eliminating undesirable material contamination and improving conventional ball milling.
上述した目的が、窒化珪素粉末と、焼結助剤粉末との混
合工程を有する窒化珪素セラミックスの製造方法におい
て、少なくともアルミナおよびイツトリアからなる緻密
性の低いボールミル用セラミックスボールを用いて混合
工程をボールミルで行うことを特徴とする窒化珪素セラ
ミックスの製造方法によって達成される。The above-mentioned purpose is to perform the mixing step in a ball mill using low-density ball mill ceramic balls made of at least alumina and yttoria in a method for manufacturing silicon nitride ceramics that includes a mixing step of silicon nitride powder and sintering aid powder. This is achieved by a method for manufacturing silicon nitride ceramics characterized by carrying out the following steps.
ボールミルに用いボールを焼結助剤材料であるアルミナ
およびイントリアで作るので、ボールの摩耗によって混
入してもそれは微細であって窒化珪素粉末中に均一に分
散される。また、好ましくない材料をボール材料に用い
ていないので、当然そのような材料の混入はない。Since the balls used in the ball mill are made of alumina and intoria, which are sintering aid materials, even if they are mixed in due to wear of the balls, they are fine and uniformly dispersed in the silicon nitride powder. Furthermore, since undesirable materials are not used in the ball material, there is naturally no contamination of such materials.
ボールミル用ボールをアルミナおよびイツトリアで作る
わけであるが、焼結性に悪影響を及ぼさないマグネシア
（ＭｇＯ） 、窒化珪素などの物質を含有させて作るこ
ともできる。Balls for ball mills are made of alumina and ittria, but they can also be made by containing substances such as magnesia (MgO) and silicon nitride that do not adversely affect sinterability.
ボールミル用ボールはセラミックス（焼結体）であり、
その相対密度が６５〜９５％、好ましくは、７０〜９０
％であり、気孔率が４０〜５％、好ましくは、３５〜１
０％である。このように緻密性が低い焼結体とするのは
、相対密度が６５％より低いと、ボールミルの際、摩耗
が早すぎ、また、かけ、われが生じてしまう。また、緻
密性が高すぎると、効果的な摩耗・混入が行なわれない
。The balls for ball mills are ceramics (sintered bodies).
Its relative density is 65-95%, preferably 70-90%
%, and the porosity is 40-5%, preferably 35-1
It is 0%. The reason why the sintered body has such low density is that if the relative density is lower than 65%, it will wear out too quickly during ball milling, and will also suffer from chipping and cracking. Furthermore, if the density is too high, effective abrasion and mixing will not occur.
以下、本発明の実施例および比較例によって本発明の詳
細な説明する。Hereinafter, the present invention will be explained in detail with reference to Examples and Comparative Examples.
実施例
まず、市販のアルミナ（＾／ｌ ２０：ｌ）粉末および
イツトリア（Ｙｚ（ｈ）粉末を重量比で４対６の割合で
ボールミルに装入し十分に混合した。このボールミルで
は市販のアルミナ（Ａ ｌ ２０３）のボールを用いた
。Example First, commercially available alumina (^/l 20:l) powder and ittria (Yz(h) powder were charged into a ball mill at a weight ratio of 4:6 and thoroughly mixed. (A 1 203) ball was used.
混合物を乾燥した後で、金型ブレスで直径２１の球状成
形体にした。この成形体を大気中で１４００℃にて１時
間加熱して焼結させた。得られた球状焼結体（ボール）
はその相対密度が９０％で、気孔率は１５％であった。After drying the mixture, it was molded into spheres with a diameter of 21 mm using a mold press. This molded body was sintered by heating at 1400° C. for 1 hour in the air. Obtained spherical sintered body (ball)
Its relative density was 90% and its porosity was 15%.
窒化珪素粉末と、３．０重量％のアルミナ粉末と、４、
０ 重量％のイツトリア粉末とをボールミルに装入し、
上述のボールを用いて２４時間混合した。silicon nitride powder, 3.0% by weight alumina powder, 4.
0% by weight of ittria powder was charged into a ball mill,
Mixed for 24 hours using the bowl described above.
この混合物を乾燥した後で、通常の方法により成形し、
１００気圧のＮ２中で１８００℃にて５時間加熱して加
圧焼結し、ＪＩＳ−Ｒ１６０１に準じた４点曲げ試験片
（５０本）を作製した。これら窒化珪素セラミックス試
験片を曲げ試験してその結果を第１表に示す。After drying this mixture, it is shaped by the usual method,
Pressure sintering was performed by heating at 1800° C. for 5 hours in N2 at 100 atmospheres to produce 4-point bending test pieces (50 pieces) according to JIS-R1601. These silicon nitride ceramic test pieces were subjected to bending tests and the results are shown in Table 1.
比較例
実施例と同じに窒化珪素粉末と、３．０重量％のアルミ
ナと、４．０重量％のイツトリアとをボールミルに装入
し、市販のアルミナボール（直径ｌ’、５ｃｍ）を用い
て２４時間混合した。そして、実施例と同じに乾燥、成
形、焼結して曲げ試験片（５０本）を作製した。これら
試験片の曲げ試験結果を第１表に示す。Comparative Example Same as in Example, silicon nitride powder, 3.0% by weight of alumina, and 4.0% by weight of ittria were charged into a ball mill, and a commercially available alumina ball (diameter l', 5 cm) was used. Mixed for 24 hours. Then, bending test pieces (50 pieces) were prepared by drying, molding, and sintering in the same manner as in the example. The bending test results of these test pieces are shown in Table 1.
第 表 ができる。No. table Can be done.
第１表かられかるように、比較例の窒化珪素セラミック
スよりも本発明の製造方法に係る窒化珪素セラミ・ノク
スのほうが曲げ強さおよびワイブル係数が大きい。ワイ
ブル係数が大きいほど材料強度面での均質性が良いこと
を意味する。なお、ボールミルは湿式でも乾式でもよい
。As can be seen from Table 1, the silicon nitride ceramic NOX according to the manufacturing method of the present invention has higher bending strength and Weibull coefficient than the silicon nitride ceramic of the comparative example. The larger the Weibull coefficient, the better the homogeneity in terms of material strength. Note that the ball mill may be a wet type or a dry type.
Claims (2)
ールミル混合に用いられるセラミックスボールであって
、少なくともアルミナおよびイットリアからなる緻密性
の低いボールミル用セラミックスボール。1. A ceramic ball used for ball mill mixing of raw material powder in the manufacturing process of silicon nitride ceramics, which is a low-density ceramic ball for a ball mill made of at least alumina and yttria.
る窒化珪素セラミックスの製造方法において、前記混合
を請求項１記載のボールミル用セラミックスボールを用
いたボールミルで行うことを特徴とする窒化珪素セラミ
ックスの製造方法。2. A method for producing silicon nitride ceramics comprising a step of mixing silicon nitride powder and sintering aid powder, characterized in that the mixing is carried out in a ball mill using the ceramic ball for a ball mill according to claim 1. manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63233721A JPH0283264A (en) | 1988-09-20 | 1988-09-20 | Production of silicon nitride ceramics and ceramics ball for ball mill used for the same production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63233721A JPH0283264A (en) | 1988-09-20 | 1988-09-20 | Production of silicon nitride ceramics and ceramics ball for ball mill used for the same production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0283264A true JPH0283264A (en) | 1990-03-23 |
Family
ID=16959521
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63233721A Pending JPH0283264A (en) | 1988-09-20 | 1988-09-20 | Production of silicon nitride ceramics and ceramics ball for ball mill used for the same production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0283264A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206082A (en) * | 2011-03-03 | 2011-10-05 | 北方民族大学 | Method for preparing submicron silicon nitride |
| CN106810265A (en) * | 2015-11-27 | 2017-06-09 | 衡阳凯新特种材料科技有限公司 | A kind of preparation method of silicon nitride protecting tube |
| CN113135762A (en) * | 2021-05-13 | 2021-07-20 | 中材高新氮化物陶瓷有限公司 | Large-size silicon nitride ceramic ball and preparation method thereof |
| CN113999017A (en) * | 2021-11-10 | 2022-02-01 | 衡阳凯新特种材料科技有限公司 | Ceramic composition, silicon nitride ceramic material, preparation method thereof and ceramic product |
-
1988
- 1988-09-20 JP JP63233721A patent/JPH0283264A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206082A (en) * | 2011-03-03 | 2011-10-05 | 北方民族大学 | Method for preparing submicron silicon nitride |
| CN106810265A (en) * | 2015-11-27 | 2017-06-09 | 衡阳凯新特种材料科技有限公司 | A kind of preparation method of silicon nitride protecting tube |
| CN113135762A (en) * | 2021-05-13 | 2021-07-20 | 中材高新氮化物陶瓷有限公司 | Large-size silicon nitride ceramic ball and preparation method thereof |
| CN113135762B (en) * | 2021-05-13 | 2022-03-08 | 中材高新氮化物陶瓷有限公司 | Large-size silicon nitride ceramic ball and preparation method thereof |
| CN113999017A (en) * | 2021-11-10 | 2022-02-01 | 衡阳凯新特种材料科技有限公司 | Ceramic composition, silicon nitride ceramic material, preparation method thereof and ceramic product |
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