JPH01242467A - Production of high-density sintered body of silicon nitride - Google Patents
Production of high-density sintered body of silicon nitrideInfo
- Publication number
- JPH01242467A JPH01242467A JP63068274A JP6827488A JPH01242467A JP H01242467 A JPH01242467 A JP H01242467A JP 63068274 A JP63068274 A JP 63068274A JP 6827488 A JP6827488 A JP 6827488A JP H01242467 A JPH01242467 A JP H01242467A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- sintered body
- molding
- wear resistance
- hot isostatic
- 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 27
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000011521 glass Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 230000002706 hydrostatic effect Effects 0.000 claims 1
- 238000003825 pressing Methods 0.000 claims 1
- 238000001513 hot isostatic pressing Methods 0.000 abstract description 9
- 239000002775 capsule Substances 0.000 abstract description 6
- 238000000465 moulding Methods 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract 2
- 238000005245 sintering Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- FXNGWBDIVIGISM-UHFFFAOYSA-N methylidynechromium Chemical compound [Cr]#[C] FXNGWBDIVIGISM-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
- C04B35/593—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by pressure sintering
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はベアリングやローラ等の摺動部材に好適に使用
される高密度窒化ケイ素焼結体の製造方法に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for manufacturing a high-density silicon nitride sintered body suitably used for sliding members such as bearings and rollers.
（従来の技術）
従来、摺動部材等の耐摩耗材料としては、高炭素クロム
鋼等の金属材料のほか、セラミック材料特に窒化ケイ素
焼結体が使用されている。その一例として、本願人は特
開昭６２−６５９７８号公報において、Ｍｇ＋ Ｓｒ＋
ＣｅおよびＡＩ！、の所定量を焼結助剤とした窒化ケ
イ素粉末を窒素雰囲気あるいは不活性雰囲気で焼成して
機械的強度等の良好な窒化ケイ素焼結体を得る製造法を
開示している。(Prior Art) Conventionally, as wear-resistant materials for sliding members and the like, in addition to metal materials such as high carbon chromium steel, ceramic materials, particularly silicon nitride sintered bodies, have been used. As an example, in Japanese Patent Application Laid-Open No. 62-65978, the applicant describes
Ce and AI! , as a sintering aid, is fired in a nitrogen atmosphere or an inert atmosphere to obtain a silicon nitride sintered body having good mechanical strength.
（発明が解決しよとする課題）
しかしながら、金属材料はもとより上述した窒化ケイ素
焼結体にあっても近年要望の高い高耐摩耗性は達成し難
く、さらに高耐摩耗性の材料の開発が望まれていた。(Problem to be solved by the invention) However, it is difficult to achieve the high wear resistance that has been in high demand in recent years, not only with metal materials but also with the silicon nitride sintered bodies mentioned above, and it is difficult to develop materials with even higher wear resistance. It was wanted.
本発明の目的は上述した課題を解決して、近年要望の高
い高耐摩耗性を達成でき、ベアリング、ローラ等の摺動
部材として好適に使用可能な高密度窒化ケイ素焼結体の
製造方法を提供しようとするものである。The purpose of the present invention is to solve the above-mentioned problems and provide a method for manufacturing a high-density silicon nitride sintered body that can achieve the high wear resistance that has been highly demanded in recent years and can be suitably used as sliding members such as bearings and rollers. This is what we are trying to provide.
（課題を解決するための手段）
本発明の高密度窒化ケイ素焼結体の製造方法は、ＭｇＯ
０，１〜３重量％、Ｓｒ０ ０．１〜３重量％、ＣｅＯ
。(Means for Solving the Problems) The method for producing a high-density silicon nitride sintered body of the present invention includes MgO
0.1-3% by weight, Sr0 0.1-3% by weight, CeO
.
０．３〜５重量％であって、これらの合計を１．５〜７
．５重量％含み残部が窒化ケイ素原料粉末よりなる調整
原料を成形し、次いで成形体にガラス被覆を施して熱間
静水圧プレスすることを特徴とするものである。0.3 to 5% by weight, the total of these being 1.5 to 7%
．． The method is characterized in that a prepared raw material containing 5% by weight and the remainder consisting of silicon nitride raw material powder is molded, and then the molded body is coated with glass and subjected to hot isostatic pressing.
（作 用）
上述した構成において、所定組成および所定量の焼結助
剤の合計量を少なくした窒化ケイ素粉末の成形体に対し
て、ガラスカプセルを使用した熱間静水圧プレスを行う
ことにより、最大のクラックの幅が１０μｍ以下の高密
度で高耐摩耗性の窒化ケイ素焼結体を得ることができる
。すなわち、組成の限定とガラスカプセルを利用した熱
間静水圧プレスとの相乗効果により、本発明の高密度で
高耐摩耗性の窒化ケイ素焼結体を得ることができる。(Function) In the above-mentioned configuration, by performing hot isostatic pressing using a glass capsule on a molded body of silicon nitride powder with a predetermined composition and a predetermined amount of reduced total amount of sintering aid, A high-density, highly wear-resistant silicon nitride sintered body with a maximum crack width of 10 μm or less can be obtained. That is, the synergistic effect of compositional limitation and hot isostatic pressing using glass capsules makes it possible to obtain the high-density, highly wear-resistant silicon nitride sintered body of the present invention.
ここで、ＭｇＯを０．１〜３重量％、ＳｒＯを０．１〜
３重量％、ＣｅＯ□を０．３〜５重量％と限定する理由
は、ＭｇＯおよびＳｒＯの所定量の添加は窒化ケイ素中
に微量存在する５ｉＯｚと反応してＳｒＯ−ＭｇＯ−５
ｉｎ２系の結晶または液相を作るとともに、一部は窒化
ケイ素中に固溶して固溶体を作り、この両者の働きがα
相からβ相への転移と同時に起きるため緻密化を促進す
るとともに窒化ケイ素粒子は強固に結合するものである
。また、Ｃｅ０ｚはＳｒ０．ＭｇＯなどと共存した場合
、窒化ケイ素粒子の界面に均一に分布してＳｒ０．Ｍｇ
Ｏ及びＳｉＯ□と結合して高融点の液相又は結晶を作り
、窒化ケイ素の緻密化に効果が大である。Here, MgO is 0.1 to 3% by weight and SrO is 0.1 to 3% by weight.
The reason for limiting CeO□ to 0.3 to 5% by weight is that the addition of a predetermined amount of MgO and SrO reacts with 5iOz present in a trace amount in silicon nitride, forming SrO-MgO-5.
In2-based crystals or liquid phase are formed, and some of them are dissolved in silicon nitride to form a solid solution, and the functions of both are α
Since this occurs simultaneously with the transition from the phase to the β phase, densification is promoted and the silicon nitride particles are strongly bonded. Moreover, Ce0z is Sr0. When coexisting with MgO etc., Sr0. Mg
It combines with O and SiO□ to form a high melting point liquid phase or crystal, and is highly effective in densifying silicon nitride.
さらに、焼結助剤の合計を１．５〜７．５重量％と限定
するのは、１．５重量％に満たないと緻密化はするもの
の曲げ強度が低下するとともに、７．５重量％を越える
と曲げ強度は大であるが焼結体中に粗大な気孔が残留す
るためである。Furthermore, the reason why the total amount of sintering aids is limited to 1.5 to 7.5% by weight is that if it is less than 1.5% by weight, densification will occur but the bending strength will decrease, and 7.5% by weight This is because, although the bending strength is high when the sintered body exceeds this, coarse pores remain in the sintered body.
また、ガラス被覆による熱間静水圧プレスは従来から公
知の技術を使用でき、例えば特公昭５９−３５８７０号
公報あるいは特開昭５５−８９４０５号公報で開示され
た技術を利用できる。Further, for hot isostatic pressing using glass coating, conventionally known techniques can be used, for example, techniques disclosed in Japanese Patent Publication No. 59-35870 or Japanese Patent Application Laid-open No. 55-89405 can be used.
（実施例）
本発明の窒化ケイ素焼結体を作るには、まず所定量のＭ
ｇ０．Ｓｒ０．Ｃｅ０．を焼結助剤として含む所定の窒
化ケイ素混合粉末を準備する。次に、混合粉末を金型を
利用したプレス成形、射出成形等の従来公知の方法で成
形する。最後に、得られた成形体に対してガラスカプセ
ル等を使用してガラスを被覆した後、熱間静水圧プレス
を実施することにより、本発明の窒化ケイ素焼結体を得
ている。(Example) To make the silicon nitride sintered body of the present invention, first, a predetermined amount of M
g0. Sr0. Ce0. A predetermined silicon nitride mixed powder containing as a sintering aid is prepared. Next, the mixed powder is molded by a conventionally known method such as press molding using a mold or injection molding. Finally, the obtained molded body is coated with glass using a glass capsule or the like, and then subjected to hot isostatic pressing to obtain the silicon nitride sintered body of the present invention.
以下、実際の例について説明する。An actual example will be explained below.
実詣貫
９０％以上がα相からなる窒化ケイ素粉末に、第１表に
示す所定量のＳｒ０．Ｍｇ０．ＣｅＯ□を焼結助剤とし
て混合した粉末を金型プレスして直径８０ｍｍ、肉厚１
５ｍｍの円筒状の成形体を得た。得られた成形体をガラ
スカプセルに真空下で封入し、第１表に示す条件で熱間
静水圧プレスを実施して、本発明、比較例および従来例
の窒化ケイ素焼結体を得た。A predetermined amount of Sr0. Mg0. The powder mixed with CeO□ as a sintering aid was pressed into a mold with a diameter of 80 mm and a wall thickness of 1.
A 5 mm cylindrical molded body was obtained. The obtained molded bodies were sealed in a glass capsule under vacuum, and hot isostatic pressing was performed under the conditions shown in Table 1 to obtain silicon nitride sintered bodies of the present invention, comparative examples, and conventional examples.
得られた本発明、比較例および従来例の窒化ケイ素焼結
体を、転がり耐久試験装置にて回転数１２０゜ｒｐｍ
、接触応力６００ ｋｇｆ／ｃｍ” 、ボール数３個、
潤滑スピンドル油で転がり疲れ寿命を測定した。また、
これらの焼結体からＪＩＳ Ｒ−１６０１に記載の４点
曲げ法で強度を測定するとともに、研摩面の任意の部位
ｌＸ２ｍｍを４００倍の光学顕微鏡で調査して最大気孔
径を求めた。結果を第１表に示す。The obtained silicon nitride sintered bodies of the present invention, comparative examples, and conventional examples were tested at a rotation speed of 120° rpm in a rolling durability tester.
, contact stress 600 kgf/cm”, number of balls: 3,
Rolling fatigue life was measured using lubricating spindle oil. Also,
The strength of these sintered bodies was measured by the four-point bending method described in JIS R-1601, and the maximum pore diameter was determined by examining an arbitrary part of the polished surface measuring 1 x 2 mm using an optical microscope with a magnification of 400 times. The results are shown in Table 1.
第 １ 表
第１表の結果から、比較例、従来例と比べて本発明の焼
結体は最大気孔径も小さく、数倍の耐久性があるととも
に４点曲げ強さも十分であることがわかる。Table 1 From the results in Table 1, it can be seen that the sintered body of the present invention has a smaller maximum pore diameter, several times the durability, and sufficient four-point bending strength than the comparative and conventional examples. .
（発明の効果）
以上の説明から明らかなように、本発明の高密度窒化ケ
イ素焼結体によれば、限定した組成の成形体をガラスカ
プセルを利用した熱間静水圧プレスすることにより、従
来品に比べて数倍の耐摩耗性を達成することができ、ベ
アリング、ローラ等の摺動部材や耐摩耗材として好適に
使用できる。(Effects of the Invention) As is clear from the above explanation, according to the high-density silicon nitride sintered body of the present invention, by hot isostatic pressing a molded body of a limited composition using a glass capsule, it is possible to It can achieve several times the wear resistance compared to conventional products, and can be suitably used as sliding members such as bearings and rollers, and as wear-resistant materials.
特許出願人 日本碍子株式会社Patent applicant: Nippon Insulator Co., Ltd.
Claims (1)
、ＣｅＯ＿２０．３〜５重量％であって、これらの合計
を１．５〜７．５重量％含み残部が窒化ケイ素原料粉末
よりなる調整原料を成形し、次いで成形体にガラス被覆
を施して熱間静水圧プレスすることを特徴とする高密度
窒化ケイ素焼結体の製造方法。1. MgO0.1-3% by weight, SrO0.1-3% by weight
, CeO_20.3 to 5% by weight, the total of these being 1.5 to 7.5% by weight and the balance being silicon nitride raw material powder, and then the molded body was coated with glass and heated. 1. A method for producing a high-density silicon nitride sintered body, the method comprising hydrostatic pressing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63068274A JPH01242467A (en) | 1988-03-24 | 1988-03-24 | Production of high-density sintered body of silicon nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63068274A JPH01242467A (en) | 1988-03-24 | 1988-03-24 | Production of high-density sintered body of silicon nitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01242467A true JPH01242467A (en) | 1989-09-27 |
Family
ID=13369014
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63068274A Pending JPH01242467A (en) | 1988-03-24 | 1988-03-24 | Production of high-density sintered body of silicon nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01242467A (en) |
-
1988
- 1988-03-24 JP JP63068274A patent/JPH01242467A/en active Pending
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