JPS6350384A - Manufacture of coated zro2 ceramics - Google Patents

Manufacture of coated zro2 ceramics

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Publication number
JPS6350384A
JPS6350384A JP61193702A JP19370286A JPS6350384A JP S6350384 A JPS6350384 A JP S6350384A JP 61193702 A JP61193702 A JP 61193702A JP 19370286 A JP19370286 A JP 19370286A JP S6350384 A JPS6350384 A JP S6350384A
Authority
JP
Japan
Prior art keywords
ceramics
zro
coating layer
coated
manufacture
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
Application number
JP61193702A
Other languages
Japanese (ja)
Inventor
良二 井上
久雄 原
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Proterial Ltd
Original Assignee
Hitachi Metals Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hitachi Metals Ltd filed Critical Hitachi Metals Ltd
Priority to JP61193702A priority Critical patent/JPS6350384A/en
Publication of JPS6350384A publication Critical patent/JPS6350384A/en
Pending legal-status Critical Current

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  • Compositions Of Oxide Ceramics (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、表面に硬質被覆層を有するZ r Oz系セ
ラミックスの製造方法に関し、刃物、ダイス、射出成形
工具、バルブ、ポンプ部品等の耐摩用工具、あるいは時
計ケース、ネクタイビン等の装飾部品に用いられて有効
な被覆ZrO,系セラミックスの製造方法に関する。
Detailed Description of the Invention [Industrial Application Field] The present invention relates to a method for manufacturing ZrOz ceramics having a hard coating layer on the surface, and to improve the wear resistance of cutlery, dies, injection molding tools, valves, pump parts, etc. The present invention relates to a method for producing coated ZrO-based ceramics that are effective for use in decorative parts such as tools, watch cases, and tie bins.

〔従来の技術〕[Conventional technology]

ZrO,系セラミックスの中には、強靭性に優れたもの
があり、特にy2o、を添加した場合に高強度、MgO
又はCeO□を添加した場合に高靭性が得られ、刃物や
ダイス等の工具に応用が検討されている。
Some ZrO-based ceramics have excellent toughness, and especially when y2o is added, they have high strength and MgO
Alternatively, high toughness can be obtained by adding CeO□, and its application to tools such as knives and dies is being considered.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

従来、刃物やダイス等の耐摩耗性を要求される分野にお
いては、超硬合金が主として用いられており、一方Zr
O,系セラミックスは、超硬合金に比べ硬さが低いため
耐摩耗性が劣るという問題点を有していた。本願発明は
以上の問題点に着目してなされたもので、耐摩耗性の向
上を図ったZrO2系セラミックスの製造方法の提供を
目的とする。
Conventionally, cemented carbide has been mainly used in fields that require wear resistance such as blades and dies, while Zr
O,-based ceramics have a problem of inferior wear resistance because of their lower hardness than cemented carbide. The present invention was made in view of the above problems, and aims to provide a method for manufacturing ZrO2 ceramics with improved wear resistance.

〔問題点を解決するための手段〕[Means for solving problems]

本願発明は、Y、03、MgO1Cab2等の安定化剤
を含有したZ r O2系セラミツクスの表面にTi、
Zr、Hf、V、Nbの窒化物、炭化物および炭窒化物
の1種又は2種以上の被膜層を形成するにあたり、前記
ZrO2系セラミックスを窒化性ガス、炭化性ガスの1
種又は2種以上の分圧が合計で1×10−4〜9 X 
1O−1torrの雰囲気中、400〜700℃で10
分間保持して被膜層を形成した後、1000〜1600
℃の温度範囲で加熱処理することを特徴とする被覆Zr
O,系セラミックスの製造方法である。
In the present invention, Ti, Ti,
In forming a coating layer of one or more of nitrides, carbides, and carbonitrides of Zr, Hf, V, and Nb, the ZrO2-based ceramics are exposed to one of a nitriding gas and a carbonizing gas.
The total partial pressure of the species or two or more species is 1 x 10-4 to 9
10 at 400-700℃ in an atmosphere of 1O-1torr
After holding for a minute to form a film layer,
Coated Zr characterized by heat treatment in the temperature range of °C
This is a method for producing O, series ceramics.

〔作用〕[Effect]

本願発明によると母材のZrO□系セラミックス表面に
TiN、TiC等の窒化物、炭化物が密着性良く被覆さ
れるものであるが、これは蒸着中にTiの一部がZrO
,と反応してTie、などを形成し、これと蒸着物質で
あるT iN 、 T x C等が強固に結合するため
ではないかと推定する。
According to the present invention, the surface of the ZrO□ base ceramic is coated with nitrides and carbides such as TiN and TiC with good adhesion.
It is presumed that this is because Tie, etc. are formed by reacting with Tie, etc., and this is strongly bonded to the vapor deposited substances such as TiN, TxC, etc.

とくに、蒸着の前段階であるいは蒸着時にN2、NH,
などの窒化性ガスやCH4,C,H,などの炭化性ガス
あるいはこれらの混合ガス雰囲気中で温度400〜70
0℃1時間10分間〜3時間保持すれば、密着性の良い
被覆が形成される。この場合反応性ガスは合計の分圧が
I X 10−’  torr未満では、効果が実質的
に現われず、一方、9 X 10゛1torrを越える
と反応膜がポーラスになって逆に密着性が低下するので
、 I X 10−’ 〜9 X 10−’ torr
となるように流量調整を行なう。
In particular, N2, NH,
at a temperature of 400 to 70°C in an atmosphere of nitriding gases such as nitriding gases, carbonizing gases such as CH4, C, H, or mixed gases thereof.
If the temperature is maintained at 0° C. for 1 hour and 10 minutes to 3 hours, a coating with good adhesion will be formed. In this case, if the total partial pressure of the reactive gas is less than I x 10-' torr, there will be virtually no effect, whereas if it exceeds 9 x 10-1 torr, the reaction film will become porous and the adhesion will be impaired. Since I X 10-' ~ 9 X 10-' torr
Adjust the flow rate so that

本願発明では以上のようにして被覆層を形成した後、1
000〜1600℃の温度範囲で加熱処理することによ
り、母材であるZrO,系セラミックスとTiN、Ti
C等の被覆層との密着力が向上することを見い出した点
に大きな特徴を有する。この理由は、被覆層が分解しな
い雰囲気中で加熱処理すると、被覆層中の成分であるT
i、Zr、Hf等が母材中に拡散し、密着力の大きい被
覆層が形成されるためである。しかし、大気中のような
02分圧の高い雰囲気中では、被覆層の窒化物、炭化物
が酸化、分解されやすく還元雰囲気中で熱処理すること
が好ましい。
In the present invention, after forming the coating layer as described above, 1
By heat treatment in the temperature range of 000 to 1600°C, the base material ZrO-based ceramics and TiN and Ti
A major feature is that it has been found that the adhesion with a coating layer such as C is improved. The reason for this is that when the coating layer is heat-treated in an atmosphere that does not decompose, T, which is a component in the coating layer,
This is because i, Zr, Hf, etc. diffuse into the base material, forming a coating layer with high adhesion. However, in an atmosphere with a high O2 partial pressure such as the atmosphere, the nitrides and carbides of the coating layer are likely to be oxidized and decomposed, and it is preferable to perform the heat treatment in a reducing atmosphere.

なお、第1表にZrO□、A1□o3を含有するZrO
,系セラミックスおよび被覆層となる物質の硬さく H
v )、熱膨張率を示す。木表より母材としては熱膨張
率が被覆物質と近似することからA1□O1を含有する
ZrO,系セラミックスが望ましいことがわかる。
In addition, Table 1 shows ZrO containing ZrO□, A1□o3
, hardness of ceramics and coating layer material H
v) indicates the coefficient of thermal expansion. From the wood surface, it can be seen that ZrO-based ceramics containing A1□O1 are preferable as the base material because the coefficient of thermal expansion is similar to that of the coating material.

第  1  表 〔実施例〕 AlzOi 20wt%残部Y、O,を3nlo1%含
有したZrO□からなるZrO,系セラミックスにホロ
ーカソード方式のイオンブレーティングによりTiNの
被覆処理を行なった。条件は、温度600℃、N3分圧
: 4 X 10−’ torrで保持時間を1時間と
した。
Table 1 [Example] ZrO-based ceramics consisting of ZrO□ containing 20 wt% AlzOi and 3 nlo 1% Y, O, balance was coated with TiN by hollow cathode ion blating. The conditions were a temperature of 600°C, a N3 partial pressure of 4 x 10-' torr, and a holding time of 1 hour.

さらに被覆処理した後、N21stmの雰囲気中で熱処
理した試験片を作成した。
After further coating treatment, a test piece was prepared which was heat treated in an atmosphere of N21stm.

そして、耐摩耗性の評価は大端式の摩耗テストで行なっ
た。条件はリング材を5US304、摺速度0.74m
/s、最終荷重2.1kg、摺動距離600 mで比摩
耗量を測定することにより評価した。その結果を第2表
に示すが、本発明にかかるN003.4の被覆ZrO,
系セラミックスは良好な耐摩耗性を改良することがわか
る。
The wear resistance was evaluated using a large end type wear test. Conditions are ring material 5US304, sliding speed 0.74m
/s, a final load of 2.1 kg, and a sliding distance of 600 m. The evaluation was made by measuring the specific wear amount. The results are shown in Table 2, and the coating ZrO of N003.4 according to the present invention,
It can be seen that the ceramics have good improved wear resistance.

なお、本実施例では、ZrO2−20%Al2O,セラ
ミックスを母材とし、TiNを被覆した例について説明
したが、本願発明はこれに限定されるものでないことは
言うまでもない。
In this embodiment, an example in which ZrO2-20% Al2O and ceramics are used as the base material and TiN is coated is explained, but it goes without saying that the present invention is not limited to this.

第2表 ※:O印は本発明 X印は比較例 〔発明の効果〕 以上説明のごとく、本発明によるとZrO,系セラミッ
クスの耐摩耗性を向上させることが可能となり、刃物、
ダイス等の工具へ適用した場合に耐久性が向上し、また
本発明被覆ZrO,系セラミックスは、表面光沢を有し
装飾品としても使用可能であり、工業上有益である。
Table 2 *: O indicates the present invention;
Durability is improved when applied to tools such as dies, and the coated ZrO ceramics of the present invention have a glossy surface and can be used as decorative items, making them industrially useful.

Claims (1)

【特許請求の範囲】 1 Y_2O_3、MgO、CeO_2等の安定化剤を
含有したZrO_2系セラミックスの表面にTi、Zr
、Hf、V、Nbの窒化物、炭化物および炭窒化物の1
種又は2種以上の被覆層を形成するにあたり、前記Zr
O_2系セラミックスを窒化性ガス、炭化性ガスの1種
又は2種以上の分圧が合計で1×10^−^4〜9×1
0^−^1torrの雰囲気中、400〜700℃で1
0分間〜3時間保持して被覆層を形成した後、1000
〜1600℃の温度範囲で加熱処理することを特徴とす
る被覆ZrO_2系セラミックスの製造方法。 2 ZrO_2系セラミックスがAl_2O_35〜6
0wt%を含有する特許請求の範囲第1項記載の被覆Z
rO_2系セラミックスの製造方法。
[Claims] 1 Ti, Zr on the surface of ZrO_2 ceramics containing stabilizers such as Y_2O_3, MgO, CeO_2, etc.
, Hf, V, Nb nitrides, carbides and carbonitrides 1
In forming the seed or two or more types of coating layer, the Zr
The partial pressure of one or more types of nitriding gas and carbonizing gas is 1×10^-^4 to 9×1 in O_2 series ceramics.
1 at 400-700℃ in an atmosphere of 0^-^1 torr
After forming a coating layer by holding for 0 minutes to 3 hours,
A method for producing coated ZrO_2 ceramics, characterized by heat treatment in a temperature range of ~1600°C. 2 ZrO_2 ceramics are Al_2O_35~6
The coating Z according to claim 1 containing 0 wt%
Method for manufacturing rO_2 ceramics.
JP61193702A 1986-08-19 1986-08-19 Manufacture of coated zro2 ceramics Pending JPS6350384A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP61193702A JPS6350384A (en) 1986-08-19 1986-08-19 Manufacture of coated zro2 ceramics

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61193702A JPS6350384A (en) 1986-08-19 1986-08-19 Manufacture of coated zro2 ceramics

Publications (1)

Publication Number Publication Date
JPS6350384A true JPS6350384A (en) 1988-03-03

Family

ID=16312360

Family Applications (1)

Application Number Title Priority Date Filing Date
JP61193702A Pending JPS6350384A (en) 1986-08-19 1986-08-19 Manufacture of coated zro2 ceramics

Country Status (1)

Country Link
JP (1) JPS6350384A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01197360A (en) * 1988-02-03 1989-08-09 Sumitomo Electric Ind Ltd Zirconia-based golden spike and production thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01197360A (en) * 1988-02-03 1989-08-09 Sumitomo Electric Ind Ltd Zirconia-based golden spike and production thereof

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