JPH0251970B2 - - Google Patents
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- JPH0251970B2 JPH0251970B2 JP56209024A JP20902481A JPH0251970B2 JP H0251970 B2 JPH0251970 B2 JP H0251970B2 JP 56209024 A JP56209024 A JP 56209024A JP 20902481 A JP20902481 A JP 20902481A JP H0251970 B2 JPH0251970 B2 JP H0251970B2
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- iron
- silicon nitride
- weight
- powder
- sintering
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Description
【発明の詳細な説明】
本発明は、耐摩耗性や耐熱強度の優れた窒化け
い素−鉄系複合材料の製造方法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a silicon nitride-iron composite material having excellent wear resistance and heat resistance strength.
従来、セラミツクス−金属系の複合材料には、
セラミツクス分散型合金として、Al2O3−Al系、
ThO2−Ni合金系などがあり、サーメツトとし
て、WC−Co系、WC−TiC−Co系、TiC−Ni
系、Cr3C2−Ni系、Al2O3−Cr系などがある。し
かしながら、窒化けい素−鉄系の複合材料は未た
実用化されていない。この理由は、窒化けい素と
鉄が焼結中に反応してしまい、窒化けい素質セラ
ミツクス相と鉄系金属相とが安定して存在しない
ためである。例えば、窒化けい素（Si3N4）粉末
と鉄（Fe）粉末とを混合したのち成形し、通常
の焼結治金の手法に従つて真空中で1150〜1250℃
の温度で加熱して焼結すると、Si3N4は消失して
しまい、所望の複合材料を得ることができない。
これは、従来焼結に用いられていた酸化および窒
化防止用の真空、不活性ガス、H2等の雰囲気中
において、Si3N4は約1100℃以上の温度で分解し
てしまうためである。 Conventionally, ceramic-metal composite materials have
As a ceramic dispersion type alloy, Al 2 O 3 -Al system,
There are ThO 2 -Ni alloys, and cermets include WC-Co, WC-TiC-Co, and TiC-Ni.
There are Cr 3 C 2 -Ni series, Al 2 O 3 -Cr series, etc. However, silicon nitride-iron composite materials have not yet been put to practical use. The reason for this is that silicon nitride and iron react during sintering, and the silicon nitride ceramic phase and iron-based metal phase do not stably exist. For example, silicon nitride (Si 3 N 4 ) powder and iron (Fe) powder are mixed, then molded, and heated at 1150 to 1250°C in vacuum according to the usual sintering metallurgy method.
When heated and sintered at a temperature of , Si 3 N 4 disappears, making it impossible to obtain the desired composite material.
This is because Si 3 N 4 decomposes at temperatures above about 1100°C in the vacuum, inert gas, H 2 , etc. atmosphere used to prevent oxidation and nitridation, which is conventionally used for sintering. .
他方、Si3N4粒子はFe系金属との濡れ性におい
て一般に酸化物よりもすぐれていることに着目
し、窒化けい素質セラミツクスと鉄または鉄合金
との複合材料を得ることを目的として種々の研究
を積重ねたところ、上記複合材料を開発するに至
つた。 On the other hand, focusing on the fact that Si 3 N 4 particles generally have better wettability with Fe-based metals than oxides, we have developed various materials with the aim of obtaining composite materials of silicon nitride ceramics and iron or iron alloys. After repeated research, they were able to develop the above composite material.
すなわち、本発明による窒化けい素−鉄系複合
材料の製造方法は、窒化けい素質セラミツクス粉
末0.1〜80重量％と、鉄または鉄合金粉末99.9〜
20重量％とを均一に混合したのち成形し、窒素分
圧が２×10-2〜3.8Torrの非酸化性雰囲気下で
1080〜1250℃の温度で焼結するようにしたことを
特徴としている。 That is, the method for producing a silicon nitride-iron composite material according to the present invention includes 0.1 to 80% by weight of silicon nitride ceramic powder and 99.9 to 99.9% by weight of iron or iron alloy powder.
After uniformly mixing with 20% by weight, it is molded under a non-oxidizing atmosphere with a nitrogen partial pressure of 2 x 10 -2 ~ 3.8 Torr.
It is characterized by being sintered at a temperature of 1080 to 1250°C.
この場合、窒化けい素質セラミツクスが80重量
％超過でかつ鉄または鉄合金が20重量％未満であ
ると、結合相となるべき鉄系マトリツクスが不足
し、結合が不十分となるので望ましくない。ま
た、窒化けい素質セラミツクスが0.1重量％未満
でかつ鉄または鉄合金が99.9重量％超過である
と、窒化けい素質セラミツクスのもつ優れた耐摩
耗性ならびに耐熱性を活かすことができなくなる
ので望ましくない。 In this case, if the silicon nitride ceramic is more than 80% by weight and the iron or iron alloy is less than 20% by weight, the iron-based matrix to serve as the binding phase will be insufficient, resulting in insufficient bonding, which is undesirable. Furthermore, if the silicon nitride ceramic is less than 0.1% by weight and the iron or iron alloy is more than 99.9% by weight, it is not desirable because the excellent wear resistance and heat resistance of the silicon nitride ceramic cannot be utilized.
上記のうち、窒化けい素質セラミツクスとして
は、Si3N4単体のほか、Si3N4−MgO系、Si3N4
−Al2O3系、Si3N4−Y2O3系その他のSi3N4−酸
化物系のものなどが使用され、さらにはAl2O3を
焼結助剤としての含有量以上に高めて固溶させた
Si3N4−Al2O3系（Si−Al−Ｏ−Ｎ系）が使用さ
れ、そのほか、Si3N4−SiC、WC、Cr3C2等の
Si3N4−炭化物系や、Si3N4−BN、TiN、AlN等
のSi3N4−窒化物系が使用される。 Among the above, silicon nitride ceramics include Si 3 N 4 alone, Si 3 N 4 −MgO system, and Si 3 N 4
-Al 2 O 3 type, Si 3 N 4 - Y 2 O 3 type and other Si 3 N 4 - oxide type are used, and furthermore, the content of Al 2 O 3 as a sintering aid or more is used. It was raised to a solid solution.
Si 3 N 4 -Al 2 O 3 system (Si-Al-O-N system) is used, and in addition, Si 3 N 4 -SiC, WC, Cr 3 C 2 etc.
Si 3 N 4 -carbide systems and Si 3 N 4 -nitride systems such as Si 3 N 4 -BN, TiN, and AlN are used.
他方、鉄または鉄合金としては、Fe単体のほ
か、強靭鋼、耐食鋼あるいは耐熱鋼などの特殊鋼
さらにはFe−Cr系、Fe−Mo系、Fe−Cr−Ni系
などのFe基合金等が使用される。 On the other hand, iron or iron alloys include not only Fe alone, but also special steels such as strong steel, corrosion-resistant steel, and heat-resistant steel, and Fe-based alloys such as Fe-Cr series, Fe-Mo series, and Fe-Cr-Ni series. is used.
そして、複合材料を製造するに際して本発明に
おいては、上記のように窒化けい素質セラミツク
ス粉末0.1〜80重量％と、鉄または鉄合金粉末
99.9〜20重量％とを均一に混合したのち成形し、
窒素分圧が２×10-2〜3.8Torrの非酸化性雰囲気
下で1080〜1250℃の温度で焼結するようにしたこ
とを特徴としている。 In the present invention, when manufacturing a composite material, 0.1 to 80% by weight of silicon nitride ceramic powder and iron or iron alloy powder are used as described above.
After uniformly mixing 99.9 to 20% by weight, molding
It is characterized in that it is sintered at a temperature of 1080 to 1250°C in a non-oxidizing atmosphere with a nitrogen partial pressure of 2 x 10 -2 to 3.8 Torr.
この場合、焼結雰囲気中の窒素分圧の制御は、
窒化けい素質セラミツクス相と鉄系金属相とを安
定して存在させるための必須要件である。すなわ
ち、焼結雰囲気中の窒素分圧が２×10-2Torrよ
りも小さすぎると、Si3N4の分解傾向が強すぎる
ので望ましくなく、他方、窒素分圧が3.8Torr
（3.8mmHgに相当）よりも大きすぎるとFeおよび
Fe合金が強く窒化してしまい、複合材料の特性
を劣化させてしまうので望ましくない。 In this case, the control of nitrogen partial pressure in the sintering atmosphere is
This is an essential requirement for stably existing the silicon nitride ceramic phase and the iron-based metal phase. That is, if the nitrogen partial pressure in the sintering atmosphere is too small than 2×10 -2 Torr, the tendency of Si 3 N 4 to decompose is too strong, which is undesirable.
(equivalent to 3.8mmHg)
This is undesirable because the Fe alloy is strongly nitrided, deteriorating the properties of the composite material.
また、焼結温度が1080℃よりも低すぎると焼結
が不十分であり、1250℃よりも高すぎるとSi3N4
の分解傾向が強くなるため好ましくない。そし
て、より好ましい焼結温度範囲は1150〜1200℃で
ある。 Also, if the sintering temperature is too low than 1080℃, sintering will be insufficient, and if the sintering temperature is too high than 1250℃, Si 3 N 4
This is not preferable because the tendency of decomposition becomes stronger. A more preferable sintering temperature range is 1150 to 1200°C.
さらに、窒化けい素質セラミツクス粉末と鉄ま
たは鉄合金粉末とを混合するに際し、適宜な成形
用バインダーや焼結助剤などを混合することも場
合によつては望ましい。 Furthermore, when mixing the silicon nitride ceramic powder and the iron or iron alloy powder, it may be desirable in some cases to mix an appropriate molding binder, sintering aid, etc.
実施例 １
平均粒径2μのSi3N4粉末５重量％と、−
250meshのSUS304L粉末95重量％とをポリエチ
レン製のボールミル容器中に入れ、ｎ−ヘキサン
中で湿式混合した。このｎ−ヘキサンを飛散させ
た後直径50mmの成形空間を有する金型内に移し、
5ton／cm2の圧力で成形した。この成形体の密度は
5.8ｇ／cm3であつた。次いでこの成形体を真空炉
内に入れ、1170℃×30分の加熱を行つたのち炉冷
し、この間雰囲気中の窒素分圧が0.1Torrとなる
ように制御しながら焼結した。この結果、密度
6.8ｇ／cm3（理論密度比87％）の焼結体を得た。
次いで、この焼結体を切断してミクロ組織を観察
したところ、ステンレス鋼のマトリツクス中に
Si3N4粒子が均一に分散している良好な複合組織
を呈していた。Example 1 5% by weight of Si 3 N 4 powder with an average particle size of 2μ and -
95% by weight of 250 mesh SUS304L powder was placed in a polyethylene ball mill container and wet mixed in n-hexane. After scattering this n-hexane, it was transferred into a mold having a molding space of 50 mm in diameter.
It was molded at a pressure of 5 tons/cm 2 . The density of this compact is
It was 5.8 g/cm 3 . Next, this molded body was placed in a vacuum furnace, heated at 1170° C. for 30 minutes, and then cooled in the furnace. During this time, sintering was performed while controlling the nitrogen partial pressure in the atmosphere to be 0.1 Torr. As a result, the density
A sintered body of 6.8 g/cm 3 (theoretical density ratio 87%) was obtained.
Next, when we cut this sintered body and observed its microstructure, we found that
It exhibited a good composite structure in which Si 3 N 4 particles were uniformly dispersed.
比較例 １
実施例１と同様にして得た成形体を５×
10-3Torrの真空中において1170℃の温度で焼結
し、得られた焼結体を切断してミクロ組織を観察
したところ、Si3N4相の存在は認められず、Fe合
金マトリツクス中のSi量が約３％（母材中のSi量
0.9％）に増加していた。Comparative Example 1 A molded body obtained in the same manner as in Example 1 was
Sintering was carried out at a temperature of 1170°C in a vacuum of 10 -3 Torr, and when the obtained sintered body was cut and the microstructure was observed, the presence of Si 3 N 4 phase was not observed, and the presence of Si 3 N 4 phase was not observed. The amount of Si in the base material is approximately 3% (the amount of Si in the base material
0.9%).
比較例 ２
実施例１と同様にして得た成形体を窒素分圧10
〜50Torrの非酸化性雰囲気中で1170℃の温度で
焼結したところ、焼結体中にSi3N4相はほぼ完全
に残留していたものの、その他に針状のCr窒化
物が全体に生成していた。このCr窒化物の生成
はFe合金マトリツクス中のCr量を低下させ、耐
酸化性を劣化させるため、耐熱焼結体としては不
適当なものとなる。Comparative Example 2 A molded body obtained in the same manner as in Example 1 was heated to a nitrogen partial pressure of 10
When sintered at a temperature of 1170℃ in a non-oxidizing atmosphere of ~50Torr, the Si 3 N 4 phase remained almost completely in the sintered body, but in addition, needle-shaped Cr nitrides were found throughout the sintered body. It was generating. The formation of this Cr nitride reduces the amount of Cr in the Fe alloy matrix and deteriorates the oxidation resistance, making it unsuitable as a heat-resistant sintered body.
実施例 ２
葡均粒径2μのSi3N4粉末５重量％と、平均粒径
0.5μのAl2O3粉末２重量％と、−250meshの
SUS304L粉末93重量％とをポリエチレン製のボ
ールミル容器中に入れ、ｎ−ヘキサン中で湿式混
合した。このｎ−ヘキサンを飛散させた後直径50
mmの成形空間を有する金型内に移し、5ton／cm2の
圧力で成形した。次いでこの成形体を真空炉内に
入れ、1170℃×30分の加熱を行つたのち炉冷し、
この間雰囲気中の窒素分圧が0.1Torrとなるよう
に制御しながら焼結した。そして、得られた焼結
体を切断してミクロ組織を観察したところ、
Si3N4粒子およびAl2O3粒子が共にFe合金マトリ
ツクス中で均一に分散している良好な焼結体を得
ることができた。Example 2 5% by weight of Si 3 N 4 powder with an average particle size of 2μ and an average particle size of
2 wt% of 0.5μ Al 2 O 3 powder and −250mesh
93% by weight of SUS304L powder was placed in a polyethylene ball mill container and wet mixed in n-hexane. After scattering this n-hexane, the diameter is 50 mm.
It was transferred into a mold having a molding space of mm and molded at a pressure of 5 ton/cm 2 . Next, this molded body was placed in a vacuum furnace, heated at 1170°C for 30 minutes, and then cooled in the furnace.
During this time, sintering was performed while controlling the nitrogen partial pressure in the atmosphere to be 0.1 Torr. Then, when the obtained sintered body was cut and the microstructure was observed,
A good sintered body in which both Si 3 N 4 particles and Al 2 O 3 particles were uniformly dispersed in the Fe alloy matrix could be obtained.
実施例 ３
平均粒径2μのSi3N4粉末10重量％と、−
250meshのインコロイ800合金（32％Ni−20％Cr
−0.3％Cu−Fe）粉末90重量％とをボールミルを
用いてｎ−ヘキサン中で湿式混合し、このｎ−ヘ
キサンを飛散させた後金型内に移し、5ton／cm2の
圧力で成形した。この成形体の密度は5.1ｇ／cm3
であつた。次いで、Ar：N2＝99.1（体積比）の混
合ガスにより炉内を約100Torrに保持した真空炉
内に装入し、1200℃×１時間保持の条件で焼結を
行つた。得られた焼結体の密度は6.8ｇ／cm3（理
論密度比91％）であり、その組織を観察したとこ
ろ、Fe合金マトリツクス中にSi3N4粒子が均一に
分散している良好な組織を呈していた。Example 3 10% by weight of Si 3 N 4 powder with an average particle size of 2μ and -
250mesh Incoloy 800 alloy (32% Ni-20% Cr
-0.3%Cu-Fe) powder was wet mixed in n-hexane using a ball mill, and after scattering the n-hexane, it was transferred into a mold and molded at a pressure of 5ton/ cm2 . . The density of this molded body is 5.1g/cm 3
It was hot. Next, the material was placed in a vacuum furnace maintained at approximately 100 Torr with a mixed gas of Ar:N 2 =99.1 (volume ratio), and sintered at 1200° C. for 1 hour. The density of the obtained sintered body was 6.8 g/cm 3 (91% of the theoretical density ratio), and its structure was observed to be good, with Si 3 N 4 particles uniformly dispersed in the Fe alloy matrix. It showed organization.
実施例 ４
平均粒径2μのSi3N4粉末70重量％と、−
250meshのSUS410L粉末30重量％とをボールミ
ルを用いてｎ−ヘキサン中で湿式混合し、このｎ
−ヘキサンを飛散させた後金型内に移動し、金型
予備成形→ラバープレス成形によつて密度2.2
ｇ／cm3の直径20mm×長さ15mmの成形体を得た。次
に、窒素分圧を1.0Torrに保持した真空炉中に上
記成形体を入れ、1150℃×２時間の焼結を行つて
密度4.1ｇ／cm3の焼結体を得た。その後、焼結体
の組織観察を行つたところ、焼結体中のほとんど
のSi3N4粒子がSUS410Lの結合層を伴なつた均一
な組織を有していた。Example 4 70% by weight of Si 3 N 4 powder with an average particle size of 2μ and -
Wet-mix 30% by weight of 250mesh SUS410L powder in n-hexane using a ball mill.
- After scattering hexane, move into the mold, mold preforming → rubber press molding to a density of 2.2
A molded article having a diameter of 20 mm and a length of 15 mm was obtained. Next, the molded body was placed in a vacuum furnace with a nitrogen partial pressure of 1.0 Torr, and sintered at 1150° C. for 2 hours to obtain a sintered body with a density of 4.1 g/cm 3 . Thereafter, when the structure of the sintered body was observed, it was found that most of the Si 3 N 4 particles in the sintered body had a uniform structure with a bonding layer of SUS410L.
以上詳述したように、本発明によれば、従来実
用化されなかつた窒化けい素−鉄系複合材料を得
ることができ、耐摩耗性や耐熱強度が要求される
例えば各種燃焼装置、燃焼機関、工具、原子力機
器等の部品の素材として活用することが可能であ
るという非常にすぐれた効果を有する。 As described in detail above, according to the present invention, it is possible to obtain a silicon nitride-iron composite material that has not been put to practical use in the past, and for various combustion devices and combustion engines that require wear resistance and heat resistance strength. It has a very good effect that it can be used as a material for parts of tools, nuclear equipment, etc.
Claims (1)
％と、鉄または鉄合金粉末99.9〜20重量％とを均
一に混合したのち成形し、窒素分圧が２×10-2〜
3.8Torrの非酸化性雰囲気下で1080〜1250℃の温
度で焼結することを特徴とする窒化けい素−鉄系
複合材料の製造方法。1. 0.1 to 80% by weight of silicon nitride ceramic powder and 99.9 to 20% by weight of iron or iron alloy powder are uniformly mixed and then molded to a nitrogen partial pressure of 2×10 -2 to
A method for producing a silicon nitride-iron composite material, characterized by sintering at a temperature of 1080 to 1250°C in a non-oxidizing atmosphere of 3.8 Torr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20902481A JPS58110656A (en) | 1981-12-25 | 1981-12-25 | Composite material and its manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20902481A JPS58110656A (en) | 1981-12-25 | 1981-12-25 | Composite material and its manufacture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58110656A JPS58110656A (en) | 1983-07-01 |
| JPH0251970B2 true JPH0251970B2 (en) | 1990-11-09 |
Family
ID=16565999
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20902481A Granted JPS58110656A (en) | 1981-12-25 | 1981-12-25 | Composite material and its manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58110656A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4918196B2 (en) * | 2001-08-31 | 2012-04-18 | 大塚化学株式会社 | Method for producing metal composite composition |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS592732B2 (en) * | 1977-01-14 | 1984-01-20 | 住友電気工業株式会社 | Sintered alloy friction material |
| JPS5937735B2 (en) * | 1977-10-18 | 1984-09-11 | 住友電気工業株式会社 | Wear-resistant sintered alloy |
-
1981
- 1981-12-25 JP JP20902481A patent/JPS58110656A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58110656A (en) | 1983-07-01 |
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