JPS6374963A - Silicon nitride base sintered body for antiabrasive material - Google Patents
Silicon nitride base sintered body for antiabrasive materialInfo
- Publication number
- JPS6374963A JPS6374963A JP61218899A JP21889986A JPS6374963A JP S6374963 A JPS6374963 A JP S6374963A JP 61218899 A JP61218899 A JP 61218899A JP 21889986 A JP21889986 A JP 21889986A JP S6374963 A JPS6374963 A JP S6374963A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- silicon nitride
- pores
- toughness
- less
- 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 description 16
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims description 16
- 239000000463 material Substances 0.000 title claims description 13
- 239000011148 porous material Substances 0.000 claims description 22
- 238000005245 sintering Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- MOVRNJGDXREIBM-UHFFFAOYSA-N aid-1 Chemical compound O=C1NC(=O)C(C)=CN1C1OC(COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)CO)C(O)C1 MOVRNJGDXREIBM-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000007545 Vickers hardness test Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Abstract] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は軸受や各種メカニカルシール等に使用してすぐ
れた耐久性を示す耐摩耗材用窒化けい素質焼結体に関す
るものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a silicon nitride sintered body for wear-resistant materials that exhibits excellent durability when used in bearings, various mechanical seals, and the like.
窒化けい素質焼結体は、高強度、高耐食性、高硬度、軽
量等の特性を有し、各種構造用セラミックスとして注目
されている。また窒化けい素質焼結体は、寸法安定性、
耐摩耗性にもすぐれ、高温、腐食性雰囲気用あるいは高
負荷用の摺動部材としても期待されている。Silicon nitride sintered bodies have characteristics such as high strength, high corrosion resistance, high hardness, and light weight, and are attracting attention as ceramics for various structures. In addition, silicon nitride sintered bodies have excellent dimensional stability and
It also has excellent wear resistance and is expected to be used as a sliding member for use in high temperatures, corrosive atmospheres, and high loads.
しかし、突際に摺動部材として用いた場合、材料として
の信頼性が不充分で、必ずしも好ましい結果をもたらさ
ない場合が多い。例えば、軸受用のポール、ころ、レー
スとして使用すると、比較的短い寿命で破壊したシ、表
面のチッピング等が生じ、充分な特性が出ない。また他
の摺動部材として使用した場合にも、表面層のチッピン
グ等による摩耗量の増大が認められる。However, when used as a sliding member in the event of an accident, the reliability of the material as a material is insufficient and often the result is not always favorable. For example, when used as poles, rollers, or races for bearings, breakage occurs within a relatively short life span, chipping of the surface, etc. occurs, and sufficient characteristics are not achieved. Furthermore, when used as other sliding members, an increase in the amount of wear due to chipping of the surface layer is observed.
添加助剤、焼結条件等の検討で、より高強度、高靭性の
窒化けい素質焼結体′ｔ−得て、上記の問題を克服しよ
うとする試みがなされているが、その対策は必ずしも充
分とはいえない（特開昭５９−２６９’７４号、特開昭
５９−２１５８０号）。Attempts have been made to overcome the above-mentioned problems by obtaining silicon nitride sintered bodies with higher strength and toughness through examination of additives, sintering conditions, etc.; It cannot be said to be sufficient (Japanese Patent Application Laid-Open No. 59-269'74, JP-A No. 59-21580).
本発明は上記の来情に鑑みてなされたもので、耐摩耗材
用窒化けい素質焼結体、特に耐チッピング性、接触疲労
寿命にすぐれ、摺動部材として好適な鼠化けい素質焼結
体を提供し、もって従来の問題点を解決することを目的
とするものである。The present invention has been made in view of the above-mentioned circumstances, and provides a silicon nitride sintered body for wear-resistant materials, particularly a silicon nitride sintered body that has excellent chipping resistance and contact fatigue life and is suitable as a sliding member. The purpose of this project is to provide a solution to existing problems.
発明者らは先に、摺動部材として要求される上記特性と
焼結体組織との関連性について冥験研究を重ねた結果、
焼結体中の空孔体積率が３％以下で、かつ５μｍ以上の
空孔の平均分布が５０個／ｍｍ３以下である窒化けい素
質焼結体は摺動部材としてすぐれた耐久性を発揮するこ
とを確認した（昭和６１年８月２６日付特許出願）。The inventors previously conducted extensive research into the relationship between the above characteristics required for sliding members and the structure of the sintered body, and found that
A silicon nitride sintered body with a pore volume ratio of 3% or less and an average distribution of pores of 5 μm or more of 50/mm3 or less exhibits excellent durability as a sliding member. (Patent application dated August 26, 1986).
発明者らは更に研究を重ねた結果、焼結体の靭性を６
ＭＰａ、／ｉ−以上とし、空孔Ｏ条件を、焼結体中の空
孔体積率が５５１以下、１０μｍ以上の空孔の平均分布
が１００個／霞３以下とすることで、摺動部材としてす
ぐれた耐久性を発揮し信頼性のある窒化けい素質焼結体
が得られることを確認した。As a result of further research, the inventors found that the toughness of the sintered body was 6.
MPa, /i- or more, and the pore O conditions are such that the pore volume fraction in the sintered body is 551 or less, and the average distribution of pores of 10 μm or more is 100/haze 3 or less. It was confirmed that a reliable silicon nitride sintered body with excellent durability could be obtained.
この焼結体を得るための焼結法としては、常圧、焼結、
加圧焼結、ナツトプレス、熱間静水圧プレス等の手段が
用いられ得るが、焼結体のち密化促進のためにホットプ
レス、熱間静水圧プレスが望ましく、かつ窒化けい素が
１分解しない温度域での焼結が望ましい。Sintering methods for obtaining this sintered body include normal pressure, sintering,
Pressure sintering, nut pressing, hot isostatic pressing, and other means may be used, but hot pressing and hot isostatic pressing are preferred in order to promote densification of the sintered body, and silicon nitride does not decompose even once. Sintering in a temperature range is desirable.
焼Ｍ助剤ト１．でハ、Ｍｇｏ、Ａｌ５Ｏｓ １ＭｇＡ４
０ａ ％Ｔｓ Ｏｓ 、Ｌａｗ Ｏｓ、Ｃｅｎｔ、Ｚｒ
Ｏｘ 、ＡＩＮ、 Ｔｉ、Ｎ。Baking M aid 1. Deha, Mgo, Al5Os 1MgA4
0a %Ts Os , Law Os, Cent, Zr
Ox, AIN, Ti, N.
ＺｒＮ％ＹＮ等が用いられ得る。ZrN%YN, etc. may be used.
窒化けい素質焼結体を摺動部材として用いる場合、破損
はチッピングの形態が多く、部材全体として空孔体積率
が低くてもチッピングの発生がしばしば起る。When a silicon nitride sintered body is used as a sliding member, damage often occurs in the form of chipping, and chipping often occurs even if the pore volume ratio of the member as a whole is low.
発明者らの実験によれば、空孔の大きさが５０μｍ以上
であると接触圧によってそのまわりにチッピングが容易
に発生する傾向があるが、５μｍ程度の空孔であっても
、複数の空孔が近接して存在した場合は局所的にチッピ
ングの発生がみられる。According to experiments conducted by the inventors, if the size of a hole is 50 μm or more, chipping tends to occur around it due to contact pressure, but even if the hole is about 5 μm, chipping tends to occur around it. If the holes are located close to each other, local chipping will occur.
しかして、空孔体積率を５％以下とするとともに１０μ
ｍ以上の空孔の平均分布を１００個／ｍｍ８以下とし、
かつ靭性を６ＭＦ〜量以上に設定することで、チッピン
グの発生もなく冥用上充分な耐久性と信頼性を有する摺
動部材として使用することができる。Therefore, the pore volume ratio is set to 5% or less and 10μ
The average distribution of pores of m or more is 100 pores/mm8 or less,
Moreover, by setting the toughness to 6 MF or more, it can be used as a sliding member having sufficient durability and reliability without causing chipping.
〔冥験例１〕
窒化けい素質焼結体の空孔の分布、靭性と圧砕荷重の関
係をみるため、空孔体積率の異る試料について圧砕試験
（Ｊ工Ｓ Ｂ ｌ！５０１．２個の球状試料に荷重
をかけて破壊荷重を測定するもの）を行なった。[Experience Example 1] In order to examine the relationship between pore distribution, toughness, and crushing load in silicon nitride sintered bodies, crushing tests were conducted on samples with different pore volume ratios (J Engineering S B l!501.2 pieces) The fracture load was measured by applying a load to a spherical sample.
空孔の分布は、自動研摩盤で鏡面研磨後、ダイヤモンド
ペーストでパフ研磨し九試料を用い、１００倍以上の光
学顕微鏡写真の実面積換算で１■８以上の部分での平均
！１にとった。The distribution of pores was determined by mirror-polishing with an automatic polishing machine, then puff-polishing with diamond paste, using 9 samples.The average of the areas of 1*8 or more in terms of the actual area of optical micrographs taken at a magnification of 100 times or more! I took it to 1.
靭性ｆ！は、鏡面研磨された試料表面に荷重２゜１９（
３０秒負荷）でビッカース圧こんを打ち、第２図に示す
ように圧こんの長さ２ａおよび発生したクラックの長さ
ｌを光学粛微鏡で２００倍以上の倍率で観察し測定する
。そして各試料につき測定値を次の２式に代入し、計算
値の小さい方を靭性値（ＫＸｃ ）とし、少くとも５点
以上の圧こんについて平均値をとった。Toughness f! is a load of 2°19 (
A Vickers indentation is made under a load of 30 seconds), and the length 2a of the indentation and the length l of the generated crack are observed and measured with an optical microscope at a magnification of 200 times or more, as shown in FIG. Then, the measured values for each sample were substituted into the following two equations, the smaller of the calculated values was taken as the toughness value (KXc), and the average value was taken for at least five indentations.
ＫＩｃ−０，０１８（Ｔ） Ｔｉｐ （−４−）−”
’ −ａ４
Ｋｒａ−０，２０３ＨＪＴ″（４閂）−” ’（Ｈ：硬
さ 、 Ｅ：ヤング率）
第１図に示すように、空孔量と圧砕荷重との間には相関
が認められ、圧砕荷重は空孔量が大きい程、高くなる傾
向を有する。しかしながら、バラツキ幅は可成シ大きい
。特に焼結助剤、焼結条件を変化させると相関度は著し
く悪くなる。KIc-0,018(T) Tip (-4-)-”
' -a4 Kra-0,203HJT'' (4 bars) -'' (H: hardness, E: Young's modulus) As shown in Figure 1, there is a correlation between the amount of pores and the crushing load. The crushing load tends to increase as the amount of pores increases. However, the variation width is quite large. In particular, when the sintering aid and sintering conditions are changed, the correlation becomes significantly worse.
そこで試料の靭性についてみると、図中、点線上ＶＣ靭
性値（ＫＩＯ） ６ ＭＰａ、／”； がある。こレ
ヨ勺、１０μｍ以上の空孔が１００個／１１１１２以下
で、靭、性値が６ＭＰａ、／’；ｉ 以上にすれば圧
砕荷重が充分く高く、寿命の長いもの（図中Ｏ印）が得
られることがわかる。このことは、空孔量および分布を
制御することにより接触疲労てよるチッピングの発生起
点数が減少し、かつ靭性を６ＭＰａ、／”’；ｉ 以
上とすることでチッピングの成長が抑制され、また母材
強度自体も高くなることによるものと認められた。Therefore, looking at the toughness of the sample, the VC toughness value (KIO) shown on the dotted line in the figure is 6 MPa, /''. This specimen has 100 pores/11112 or less with a diameter of 10 μm or more, and the toughness and toughness values are It can be seen that if the crushing load is set to 6 MPa, /'; It was recognized that this is due to the fact that the number of starting points for chipping due to mechanical strength is reduced, the growth of chipping is suppressed by setting the toughness to 6 MPa, /'';i or more, and the strength of the base material itself is increased.
〔実験例２〕
各種窒化けい素質焼結体を添加助剤、焼結方法、条件を
変化させて作製し、その摺動特性を、（ａ）Ｊ工Ｓ
Ｂ １５０１に準じ表面を残留応力が残らないように
研磨した約１０ｇＩｍφの球状試料を用いた圧砕試験、
（１））鏡面研磨した板材を用い相手材約１０■φの鋼
球で荷重２００神の回転試験（ｌｌｉｌ波動試験）の２
種類の方法で評価した。[Experimental Example 2] Various types of silicon nitride sintered bodies were prepared by changing additives, sintering methods, and conditions, and their sliding properties were evaluated by (a) J Engineering S
Crushing test using a spherical sample of approximately 10 g Imφ whose surface was polished so that no residual stress remained according to B 1501,
(1)) 2 of the rotation test (llil wave test) using a mirror-polished plate material and a steel ball of approximately 10 mm diameter under a load of 200 cm.
It was evaluated using different methods.
（１） 平均粒径０．７ ｐ ｍ ＯＳ ｉ３Ｎ ４
粉末にＹ２Ｏ２、ＭｇＡ ｌ倉０４を各・９５ｗｔ％添
加し、エタノール中で混合後、乾燥、解砕して原料粉末
とした。(1) Average particle size 0.7 pm OS i3N 4
95 wt% each of Y2O2 and MgAl 04 were added to the powder, mixed in ethanol, dried and crushed to obtain a raw material powder.
ボー１ｖおよび平板を金型プレスにより成形した後、１
５００〜１７００°Ｃ％ｌＯ気圧ＯＮ雪中で焼結した。After forming the bow 1v and the flat plate with a mold press, 1
Sintering was carried out in snow at 500-1700°C and %lO atmospheric pressure ON.
その一部を更に各種パッド材中に埋め込んで１５００〜
ｌ ” ＯＯ”０％２００気圧、で熱間静圧プレス（Ｈ
工Ｐ）を行なった。焼結後、真球度を出すとともに表面
の残留応力をなくすためＳｉＣ砥粒で研磨した。結果を
第１表に示す。なおすべての試料の空孔体−積率Ｉｒ！
、５％以下である。A part of it is further embedded in various pad materials for 1,500~
l ” OO” 0% 200 atm, hot isostatic press (H
Engineering P) was carried out. After sintering, it was polished with SiC abrasive grains to achieve sphericity and eliminate residual stress on the surface. The results are shown in Table 1. In addition, the pore volume fraction Ir of all samples!
, 5% or less.
本発明のものは比較材に比べ圧砕荷重が高く、回転試験
の寿命も長い。なお、比較材Ａｇｏ〜ユ５は空孔数が多
く、ＫＩｃが低い。The material of the present invention has a higher crushing load and a longer rotation test life than the comparative materials. Note that the comparative materials Ago to Yu5 have a large number of pores and a low KIc.
（２）第２表に示す焼結助剤１に添加した各種組成の混
合粉末を粒径０．６μｍ以下のＳｉｓ Ｎ４粉末を用い
て湿式混合で準備し、ボールおよび平板を金型プレスで
成形し各種条件でホットプレス（ＨＰ）した。焼結後、
ＳｉＯ砥粒で研磨して試験に供した。すべての試料は充
分にち密化しておシ、空孔体積率は５％以下であった。(2) Mixed powders of various compositions added to sintering aid 1 shown in Table 2 were prepared by wet mixing using Sis N4 powder with a particle size of 0.6 μm or less, and balls and flat plates were formed using a mold press. and hot pressed (HP) under various conditions. After sintering,
It was polished with SiO abrasive grains and used for testing. All samples were sufficiently densified and the pore volume fraction was less than 5%.
第２表に示すように、本発明のものは圧砕荷重、回転試
験の寿命に高い値を示し、摺動特性にすぐれていること
がわかる。比較例はいずれも空孔数が多すぎ、＆８は靭
性も不足する。As shown in Table 2, the products of the present invention show high values for crushing load and rotation test life, and are found to have excellent sliding properties. All of the comparative examples have too many pores, and &8 also lacks toughness.
以上より明かなように、本発明の窒化けい素質焼結体は
耐摩耗材、特に摺動部材としてすぐれた耐久性を発揮す
るものである。As is clear from the above, the silicon nitride sintered body of the present invention exhibits excellent durability as a wear-resistant material, especially as a sliding member.
第１図は、セラミック焼結体の空孔量と圧砕荷重の関係
についての実験結果を示す図、第２図は焼結体表面の庄
こんおよび発生クラックの模式図である。
第１図FIG. 1 is a diagram showing experimental results regarding the relationship between the amount of pores in a ceramic sintered body and crushing load, and FIG. 2 is a schematic diagram of cracks and generated cracks on the surface of the sintered body. Figure 1
Claims (1)
％以下で、１０μｍ以上の空孔の平均分布が１００個／
ｍｍ＾２以下であり、かつ焼結体の靭性値が６ＭＰａ√
ｍ以上であることを特徴とする耐摩耗材用窒化けい素質
焼結体。The main component is silicon nitride, and the pore volume ratio in the sintered body is 5.
% or less, and the average distribution of pores of 10 μm or more is 100/
mm^2 or less, and the toughness value of the sintered body is 6MPa√
A silicon nitride sintered body for use in wear-resistant materials, characterized in that it has a diameter of at least m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61218899A JPS6374963A (en) | 1986-09-16 | 1986-09-16 | Silicon nitride base sintered body for antiabrasive material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61218899A JPS6374963A (en) | 1986-09-16 | 1986-09-16 | Silicon nitride base sintered body for antiabrasive material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6374963A true JPS6374963A (en) | 1988-04-05 |
Family
ID=16727053
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61218899A Pending JPS6374963A (en) | 1986-09-16 | 1986-09-16 | Silicon nitride base sintered body for antiabrasive material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6374963A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02120057A (en) * | 1988-10-31 | 1990-05-08 | Toshiba Corp | Thermal head |
| DE3938644A1 (en) * | 1988-11-21 | 1990-05-23 | Ngk Spark Plug Co | Sintered body of silicon nitride used in roller bearings - nitride particles are elongated with specific width and length dimensions to improve fracture strength |
| US5395807A (en) * | 1992-07-08 | 1995-03-07 | The Carborundum Company | Process for making silicon carbide with controlled porosity |
-
1986
- 1986-09-16 JP JP61218899A patent/JPS6374963A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02120057A (en) * | 1988-10-31 | 1990-05-08 | Toshiba Corp | Thermal head |
| DE3938644A1 (en) * | 1988-11-21 | 1990-05-23 | Ngk Spark Plug Co | Sintered body of silicon nitride used in roller bearings - nitride particles are elongated with specific width and length dimensions to improve fracture strength |
| JPH02141474A (en) * | 1988-11-21 | 1990-05-30 | Ngk Spark Plug Co Ltd | Silicon nitride-based sintered body for bearing |
| US5395807A (en) * | 1992-07-08 | 1995-03-07 | The Carborundum Company | Process for making silicon carbide with controlled porosity |
| US5589428A (en) * | 1992-07-08 | 1996-12-31 | The Carborundum Company | Silicon carbide with controlled porosity |
| US5635430A (en) * | 1992-07-08 | 1997-06-03 | The Carborundum Company | Intermediate for producing porous silicon carbide |
| US5834387A (en) * | 1992-07-08 | 1998-11-10 | The Carborundum Company | Ceramic comprising silicon carbide with controlled porosity |
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