JPS60155571A - Manufacture of titanium carbonitride ceramic by normal baking process - Google Patents
Manufacture of titanium carbonitride ceramic by normal baking processInfo
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- JPS60155571A JPS60155571A JP59008430A JP843084A JPS60155571A JP S60155571 A JPS60155571 A JP S60155571A JP 59008430 A JP59008430 A JP 59008430A JP 843084 A JP843084 A JP 843084A JP S60155571 A JPS60155571 A JP S60155571A
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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) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
本発明は、炭窒化チタンとホウ化物との混合粉末から、
普通焼成によシ優れた機械的強度、硬度、じん性を有す
る高密度高強度焼結体を製造する方法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION The present invention comprises a mixed powder of titanium carbonitride and a boride.
The present invention relates to a method for producing a high-density, high-strength sintered body that has excellent mechanical strength, hardness, and toughness compared to ordinary firing.
炭窒化チタンは、一般に融点、硬度、じん性が高く、ま
た耐酸化性もよいため、耐摩耗性機械部品材料、切削工
具材料としての用途が期待されているが、炭窒化チタン
単味焼結体の抗折力は低く、もろいという欠点があり、
単味焼結体は工業的に利用されないでいる。またサーメ
ツト材の母材として炭窒化チタンは使われているが、結
合剤として添加するＮ１のため、炭窒化チタン系サーメ
ツト材は耐酸化性及び耐熱性に難点が生じる。Titanium carbonitride generally has a high melting point, hardness, toughness, and good oxidation resistance, so it is expected to be used as a material for wear-resistant mechanical parts and cutting tools. The body has a low transverse rupture strength and is brittle.
Plain sintered bodies are not used industrially. Furthermore, titanium carbonitride is used as a base material for cermet materials, but titanium carbonitride-based cermet materials suffer from difficulties in oxidation resistance and heat resistance due to the addition of N1 as a binder.
本発明者らは、このような従来法の欠点を改良するのを
目的として、先に炭窒化チタンと金属ホウ化物との混合
粉末をホットプレス法で焼結することによシ高密度、高
強度なセラミックスを得る方法を提案した（特願昭５７
−１２１７４８号）。In order to improve these drawbacks of the conventional method, the present inventors first sintered a mixed powder of titanium carbonitride and metal boride using a hot press method to create a high-density, high-density powder. Proposed a method to obtain strong ceramics (patent application 1983)
-121748).
しかしながら、ホットプレス法は、容易に高強度のセラ
ミックスが得られるという点では有利であるが、設備上
の関係で複雑な形状や大型のものを得ることが困難でち
るという問題を伴う。他方、普通焼成法を用いればこの
ような問題は解決されるが、空隙率が高くなるのを免れ
ないだめ、高強度のものとすることができない。However, although the hot pressing method is advantageous in that high-strength ceramics can be easily obtained, it is accompanied by the problem that it is difficult to obtain products with complex shapes or large sizes due to equipment constraints. On the other hand, if a normal firing method is used, this problem can be solved, but the porosity will increase, and high strength cannot be obtained.
本発明者らは、このような炭窒化チタン系セラミックス
が伴う種々の欠点を克服し、普通焼成法により高密度、
高強度のセラミックスを製造する方法を開発するために
、さらに研究を続けた結果、炭窒化チタン粉末に特定の
金属ホウ化物粉末を２種以上組み合わせて添加すれば、
ホットプレス法によらずに、比較的低い温度で焼成して
も高密度、高強度の強じんなセラミックスが得られるこ
とを見出し、この知見に基づいて本発明をなすに至った
。The present inventors have overcome the various drawbacks associated with such titanium carbonitride ceramics, and have achieved high density and
In order to develop a method for manufacturing high-strength ceramics, we continued our research and found that if a combination of two or more specific metal boride powders is added to titanium carbonitride powder,
It was discovered that a strong ceramic with high density and high strength can be obtained even if it is fired at a relatively low temperature without using the hot press method, and based on this knowledge, the present invention was accomplished.
すなわち、本発明は炭素と窒素とを１＝９ないし９：１
の原子比で含有する炭窒化チタン粉末に対し、ＴｉＢ２
． ＣｒＢ２ 、ＴａＢ２ 、 ＭｎＢ２ 、 ＭｏＢ
２ 、 ＶＢ２ 。That is, in the present invention, carbon and nitrogen are mixed in a ratio of 1=9 to 9:1.
For titanium carbonitride powder containing an atomic ratio of TiB2
．． CrB2, TaB2, MnB2, MoB
2, VB2.
Ｎ１）Ｂ２ 、 ＨｆＢ２ 、 ＡｔＢ２ ｒ ＺｒＢ
２のニホウ化金属、Ｔｊ、Ｂ 、 ＣｒＢ 、 ＴａＢ
、 ＭｎＢ 、 ＭｏＢ 、 ＶＢ 、 ＮｂＢ 、
ＨｆＢ 。N1) B2, HfB2, AtB2 r ZrB
2 metal diborides, Tj, B, CrB, TaB
, MnB, MoB, VB, NbB,
HfB.
ＺｒＢの一ホウ化金属及びＷ２Ｂ６ ＋ ＭＯ２ＢＳの
五ニホウ化金属の中から選ばれた２種以上のホウ化金属
の粉末を全量に基づき５〜９５重量％の割合で添加した
混合粉末を圧粉体に成形したのち、普通焼成することを
特徴とする炭窒化チタン系セラミックスの製造方法を提
供するものである。A green compact is made of a mixed powder in which powders of two or more metal borides selected from metal monoboride of ZrB and metal pentaboride of W2B6 + MO2BS are added at a ratio of 5 to 95% by weight based on the total amount. The present invention provides a method for producing titanium carbonitride ceramics, which is characterized in that the titanium carbonitride ceramics are formed by molding and then normally fired.
本発明において原料主成分として用いられる炭窒化チタ
ンは、その組成中の炭素と窒素との原子比が１：９ない
し９：１の範囲内にあるもの、すなわち一般式
％式％
（式中のＸは０．１〜０．９の範囲内の数である）で表
わされるものである。The titanium carbonitride used as the main raw material component in the present invention has a composition in which the atomic ratio of carbon to nitrogen is within the range of 1:9 to 9:1, that is, the general formula % formula % (in the formula X is a number within the range of 0.1 to 0.9).
まだ、この炭窒化チタン粉末に添加されるホウ化金属粉
末としては、ＴｉＢ２ 、 ＣｒＢ２ 、 ＴａＢ２
。However, the metal boride powders added to the titanium carbonitride powder include TiB2, CrB2, and TaB2.
.
ＭｏＢ２ 、 ＶＢ２ 、 ＮｂＢ２ ＋ ＨｆＢ２Ｂ
、 ＡｔＢ２ 、 ＺｒＢ２のニホウ化金属、ＴｉＢ
ｒ ＣｒＢ 、 ＴａＢ 、 ＭｎＢ 、 ＭｏＢ
、 ＶＢ ＋ＮｂＢ 、 ＨｆＢ 、 ＺｒＢの一ホウ
化金属及びＷ２Ｂ５゜ＭＯ２Ｂ５の五ニホウ化金属の中
から選ばれた２種又はそれ以上の組合せが用いられる。MoB2, VB2, NbB2 + HfB2B
, AtB2, metal diboride of ZrB2, TiB
r CrB, TaB, MnB, MoB
, VB + NbB , HfB , metal monoboride of ZrB, and metal pentaboride of W2B5°MO2B5, or a combination of two or more thereof is used.
これらのホウ化金属粉末は、原料粉末全量に基づき５〜
９５重量％、好ましくは２０〜７０重量％の割合で添加
される。この量が５重量％未満、若しくは９５重量％よ
りも多くなると得られるセラミックスの強度が著しく低
下する。These metal boride powders are based on the total amount of raw material powder.
It is added in a proportion of 95% by weight, preferably 20-70% by weight. If this amount is less than 5% by weight or more than 95% by weight, the strength of the resulting ceramic will be significantly reduced.
特に良質のセラミックスは、前記のニホウ化金属の２種
以上、あるいは前記のニホウ化金属の１種以上と、前記
の一ホウ化金属及び五ニホウ化金属の中から選ばれた１
種以上との組合せを添加した場合、例えば全量当９２０
〜７０重量％のＴｌＢ２１Ｃ！ｒＢ２ 、 ＺｒＢ２の
中から選ばれた１種以上と、全量当り５０重量％以下の
ＴａＢ２ 、 ＶＢ２ 、 ＭｏＢ２ 、 Ｎ１）Ｂ２
ｒＭＯ２Ｂ５ ＋ Ｗ２Ｂ５の中から選ばれた１種以
上との組合せを添加した場合に得られる。Particularly high-quality ceramics include two or more of the above-mentioned metal diborides, or one or more of the above-mentioned metal diborides and one selected from the above-mentioned metal monoborides and metal pentaborides.
If a combination of seeds or more is added, for example, 920 per total amount
~70% by weight TlB21C! one or more selected from rB2, ZrB2, and 50% by weight or less of TaB2, VB2, MoB2, N1)B2 based on the total amount
It is obtained when a combination with one or more selected from rMO2B5 + W2B5 is added.
これらの原料粉末はいずれも平均粒径２μ以下、好まし
くは１μ以下の粉末として用いるのがよい。All of these raw material powders are preferably used as powders with an average particle size of 2 μm or less, preferably 1 μm or less.
本発明方法においては、このような原料粉末混合物を普
通焼成法によシ焼結するが、これは例えば原料粉末混合
物を金型に入れ、５００〜５０００〜／ｄ程度の圧力を
加えて圧粉体とし、次いでラバープレスでさらに５００
〜１．０．０００％／ｃＪ程度の圧力を加えたのち、真
空中、あるいは水素ガス、窒素ガス、アルゴンガスなど
の非酸化性雰囲気中において１５００〜２０００℃、好
ましくは１７００〜１９００℃の温度で３０〜３００分
間焼成することによって行うことができる。この場合、
金型における冷間圧縮工程は所望に応じ省略することも
できるし、また泥しよう法により圧粉体を形成させるこ
ともできる。さらにまた、上記のようにして得だ焼成体
をＨ工Ｐ法を用いてち密化することもできる。In the method of the present invention, such a raw material powder mixture is sintered by a normal sintering method, which involves, for example, placing the raw material powder mixture in a mold and applying a pressure of about 500 to 5000 m/d to compact the powder. body and then rubber press for another 500
After applying a pressure of ~1.0.000%/cJ, the temperature is 1500 to 2000°C, preferably 1700 to 1900°C in vacuum or in a non-oxidizing atmosphere such as hydrogen gas, nitrogen gas, or argon gas. This can be done by baking for 30 to 300 minutes. in this case,
The cold compression step in the mold can be omitted if desired, and the green compact can also be formed by a slurry method. Furthermore, the obtained fired body as described above can also be densified using the H-P method.
本発明の材料は、低い温度で、高強度、高硬度、強靭性
かつ高密度な焼結体であシ、切削工具、耐摩耗性機械部
品としても使用することができる。The material of the present invention can also be used as a sintered body having high strength, high hardness, toughness and high density at low temperatures, cutting tools, and wear-resistant mechanical parts.
又、この材料中のホウ化金属は、周期率表のＩＶ ｂ族
化合物を含む環境中では潤滑性に富むＭ−（ＩＶｌ））
２化合物表面層を形成し、一層すぐれた摺動性能を付与
できる。In addition, the metal boride in this material has a high lubricity in an environment containing Group IVb compounds of the periodic table (M-(IVl)).
By forming a two-compound surface layer, even better sliding performance can be imparted.
次に実施例によシ本発明をさらに詳細に説明する。Next, the present invention will be explained in more detail with reference to Examples.
実施例１
炭素と窒素の原子比が１：１の炭窒化チタンＴ１Ｃｏ、
５１”ｌｏ、ｓ の粉末（平均粒径１μ）に、全量当り
３０重量％に相当するＴ ｉ Ｂ ２粉末（平均粒径２
μ）と、第１表に示した量のＴａＢ２粉末（平均粒径２
μ）を加え、十分に混合し、この混合粉末を１０００
Ｋ９ ／ｃｎｆで冷間圧縮後、３０００に７／ｃｒｌで
ラバープレスして圧粉体を形成させる。この圧粉体を真
空焼結炉に入れ、１７００℃で９０分間加熱焼成する。Example 1 Titanium carbonitride T1Co with an atomic ratio of carbon and nitrogen of 1:1,
51" lo,s powder (average particle size 1 μ), T i B 2 powder (average particle size 2
μ) and the amount of TaB2 powder (average particle size 2
μ), mix thoroughly, and add this mixed powder to 1000
After cold compression at K9/cnf, a green compact is formed by rubber pressing at 3000/7/crl. This green compact is placed in a vacuum sintering furnace and fired at 1700° C. for 90 minutes.
このようにして得た焼結体の特性を第１表に示す。The properties of the sintered body thus obtained are shown in Table 1.
第１表
実施例１で用いた炭窒化チタンＴ Ｉ Ｃｏ 、 ｓ
Ｎ ｏ、 ｓ の粉末（平均粒径１μ）に全量当り３０
重量％のＴｉＢ２粉末（平均粒径２μ）及び全量描シ１
重量％のＴａＢ２粉末（平均粒径２μ）を加え、実施例
１と同様にして圧粉体を形成させたのち、真空焼結炉中
、異なった温度で９０分間加熱焼成する。Table 1 Titanium carbonitride T I Co , s used in Example 1
30 per total amount of N o,s powder (average particle size 1μ)
Weight% TiB2 powder (average particle size 2μ) and total amount drawn 1
After adding % by weight of TaB2 powder (average particle size 2 μm) and forming a green compact in the same manner as in Example 1, it is heated and fired for 90 minutes at different temperatures in a vacuum sintering furnace.
このようにして得た焼結体の特性を第２表に示す。The properties of the sintered body thus obtained are shown in Table 2.
第２表
実施例３
実施例１で用いた炭窒化チタンＴｉ０ｏ、５Ｎｏ、ｓ
の粉末（平均粒径１μ）に全量当９３０重量％に相当す
るＴｉＢ２粉末（平均粒径ｌμ）と、第３表に示した量
のＴ ａ Ｂ ２粉末（平均粒径１μ）を加え、十分に
混合し、これを実施例１と同様の条件で圧粉体とし、次
いで焼成する。Table 2 Example 3 Titanium carbonitride used in Example 1 Ti0o, 5No, s
powder (average particle size 1μ), add TiB2 powder (average particle size 1μ) equivalent to 930% by weight based on the total amount and the amount of TaB2 powder (average particle size 1μ) shown in Table 3, and add enough This is made into a powder compact under the same conditions as in Example 1, and then fired.
このようにして得た焼結体の特性を第３表に示す。Table 3 shows the properties of the sintered body thus obtained.
第３表
実施例４
それぞれ異なった炭素と窒素の原子比をもつ１重々の炭
窒化チタンの粉末（平均粒径１μ）と、全量当り６０重
量％に相当するＴｉＢ２の粉末（平均粒径１μ）と、全
量当り０．５重量％に相当するＴ ａ Ｂ ２の粉末（
平均粒径１μ）とを混合し、これを実施例１と同様の条
件で圧粉体とし、次いで１８００℃において焼結する。Table 3 Example 4 One layer of titanium carbonitride powder (average particle size 1μ) with different atomic ratios of carbon and nitrogen, and TiB2 powder (average particle size 1μ) corresponding to 60% by weight based on the total amount and T a B 2 powder corresponding to 0.5% by weight based on the total amount (
(average particle size: 1 μm), this is made into a powder compact under the same conditions as in Example 1, and then sintered at 1800°C.
このようにして得た焼結体の特性を第４表に示す・ い
４ 。The properties of the sintered body thus obtained are shown in Table 4.
実施例５
実施例１で用いた炭窒化チタンＴｉＣ（，５Ｎ（，５の
粉末（平均粒径１μ）に対し、全量当り３０重量％に相
当する量のＴｉＢ２の粉末（平均粒径ｌμ）と、全量描
シ１重量％に相当する量の各種ホウ化金属を添加し、実
施例１と同様の条件を用いて圧粉体とし、これを焼成す
る。Example 5 To the powder of titanium carbonitride TiC(,5N(,5) (average particle size 1μ) used in Example 1, an amount of TiB2 powder (average particle size 1 μ) corresponding to 30% by weight based on the total amount was added. , various metal borides were added in an amount equivalent to 1% by weight of the total amount, and a compact was prepared using the same conditions as in Example 1, which was then fired.
このようにして得た焼結体の抗折力を第５表に示す。Table 5 shows the transverse rupture strengths of the sintered bodies thus obtained.
第５表
実施例６
１重量％の量で添加するホウ化金属として、ＴａＢ、
ＶＢ又はＮｂＢを用い、アルゴン雰囲気中１７００℃で
１２０分間焼成すること以外は全〈実施例５と同様にし
て焼結体を製造する。Table 5 Example 6 As the metal boride added in an amount of 1% by weight, TaB,
A sintered body is produced in the same manner as in Example 5 except that VB or NbB is used and the sintered body is fired at 1700° C. for 120 minutes in an argon atmosphere.
このようにして得た焼結体はいずれも８０〜／実施例７
実施例１で用いた炭窒化チタンＴｌＣｏ、５Ｎｏ、５
の粉末（平均粒径１μ）に対し種々のホウ化金属の組合
せを添加し、実施例１と同様にして圧粉体に成形し、こ
れを水素雰囲気中、１７００℃で１２０分焼成する。The sintered bodies thus obtained were all 80~/Example 7 Titanium carbonitride TlCo, 5No, 5 used in Example 1
Combinations of various metal borides were added to the powder (average particle size: 1 μm), formed into a green compact in the same manner as in Example 1, and baked at 1700° C. for 120 minutes in a hydrogen atmosphere.
このようにして得た抗折力を第６表に示す。The transverse rupture strengths thus obtained are shown in Table 6.
第６表
実施例８
実施例１と同じ炭窒化チタンＴｌＣ０，５Ｎｏ、５ の
粉末（平均粒径１μ）に対し、全量当９８０重量％に相
当する量のＴ ａ Ｂ ２の粉末（平均粒径１μ）と全
量当９１重量％に相当する量のｖＢ２粉末（平均粒径１
μ）を添加し、実施例１と同じ方法で圧粉体としたのち
、真空焼結炉中に入れ１８００℃で９０分間焼成する。Table 6 Example 8 Titanium carbonitride TlC0,5No.5 powder (average particle size 1μ), which is the same as in Example 1, was added with T a B 2 powder (average particle size 1 μ) and an amount of vB2 powder (average particle size 1 μ) corresponding to 91% by weight based on the total amount
μ) was added to form a green compact in the same manner as in Example 1, and then placed in a vacuum sintering furnace and fired at 1800° C. for 90 minutes.
このようにして抗折力９０に９／−の焼結体を得た。In this way, a sintered body with a transverse rupture strength of 90 to 9/- was obtained.
特許出願人 工業技術院長 外１名 復代理人 阿 形 明Patent applicant: Director of the Agency of Industrial Science and Technology and 1 other person Sub-Agent Akira Agata
Claims (1)
する炭窒化チタン粉末に対し、Ｔ Ｉ Ｂ ２ ＋Ｃｒ
Ｂ２ 、−ＴａＢ２ 、 ＭｎＢ２ 、 ＭｏＢ２ ＋
ＶＢ２ ＋ ’ＮｂＢ２１ＨｆＢ２ 、 ＡｔＢ２
、 ＺｒＢ２のニホウ化金属、ＴｉＢ。 ＣｒＢ 、 ＴａＢ 、 ＭｎＢ 、 ＭｏＢ 、 Ｖ
Ｂ 、 ＮｂＢ 、 ＨｆＢ 、 ＺｒＢの一ホウ化金
属及びＷ２Ｂ６１ ＭＯ２Ｂ５の五ニホウ化金属の中か
ら選ばれた２種以上のホウ化金属の粉末を全量に基づき
５〜９５重量％の割合で添加した混合粉末を圧粉体に成
形したのち、普通焼成することを特徴とする炭窒化チタ
ン系セラミックスの製造方法。[Claims] 1. For titanium carbonitride powder containing carbon and nitrogen at an atomic ratio of 1=9 to 9:1, T I B 2 +Cr
B2 , -TaB2 , MnB2 , MoB2 +
VB2 + 'NbB21HfB2, AtB2
, metal diboride of ZrB2, TiB. CrB, TaB, MnB, MoB, V
A mixture in which powders of two or more metal borides selected from metal monoborides of B, NbB, HfB, and ZrB and metal pentaborides of W2B61 MO2B5 are added at a ratio of 5 to 95% by weight based on the total amount. A method for producing titanium carbonitride ceramics, which comprises forming powder into a green compact and then firing it normally.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59008430A JPS60155571A (en) | 1984-01-23 | 1984-01-23 | Manufacture of titanium carbonitride ceramic by normal baking process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59008430A JPS60155571A (en) | 1984-01-23 | 1984-01-23 | Manufacture of titanium carbonitride ceramic by normal baking process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60155571A true JPS60155571A (en) | 1985-08-15 |
| JPS6353150B2 JPS6353150B2 (en) | 1988-10-21 |
Family
ID=11692903
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59008430A Granted JPS60155571A (en) | 1984-01-23 | 1984-01-23 | Manufacture of titanium carbonitride ceramic by normal baking process |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60155571A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4910171A (en) * | 1987-03-26 | 1990-03-20 | Agency Of Industrial Science And Technology | Titanium hafnium carbide-boride metal based ceramic sintered body |
| US5036028A (en) * | 1988-05-03 | 1991-07-30 | Agency Of Industrial Science And Technology | High density metal boride-based ceramic sintered body |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5918349A (en) * | 1982-07-20 | 1984-01-30 | 松下精工株式会社 | Heat pump system separation type air conditioner |
-
1984
- 1984-01-23 JP JP59008430A patent/JPS60155571A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5918349A (en) * | 1982-07-20 | 1984-01-30 | 松下精工株式会社 | Heat pump system separation type air conditioner |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4910171A (en) * | 1987-03-26 | 1990-03-20 | Agency Of Industrial Science And Technology | Titanium hafnium carbide-boride metal based ceramic sintered body |
| US5036028A (en) * | 1988-05-03 | 1991-07-30 | Agency Of Industrial Science And Technology | High density metal boride-based ceramic sintered body |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6353150B2 (en) | 1988-10-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |