JPS63319262A - Titanium nitride-based sintered body - Google Patents

Titanium nitride-based sintered body

Info

Publication number
JPS63319262A
JPS63319262A JP62154571A JP15457187A JPS63319262A JP S63319262 A JPS63319262 A JP S63319262A JP 62154571 A JP62154571 A JP 62154571A JP 15457187 A JP15457187 A JP 15457187A JP S63319262 A JPS63319262 A JP S63319262A
Authority
JP
Japan
Prior art keywords
oxide
sintered body
titanium nitride
oxides
particle size
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.)
Granted
Application number
JP62154571A
Other languages
Japanese (ja)
Other versions
JPH0753605B2 (en
Inventor
Tsunesuke Shioi
恒介 塩井
Yoshito Izumi
和泉 良人
Masayasu Yamaguchi
山口 雅靖
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.)
Onoda Cement Co Ltd
Original Assignee
Onoda Cement Co 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 Onoda Cement Co Ltd filed Critical Onoda Cement Co Ltd
Priority to JP62154571A priority Critical patent/JPH0753605B2/en
Publication of JPS63319262A publication Critical patent/JPS63319262A/en
Publication of JPH0753605B2 publication Critical patent/JPH0753605B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Abstract

PURPOSE:To obtain the titled sintered body having a lustrous fine gold color tone, superior hardness, scratch and corrosion resistances and heat conductivity by adding a prescribed amt. of one or more kinds of oxides selected among TiO2, Nb2O5, TaO, MoO3, WO3, Y2O3 and oxides of lanthanides to TiN as a principal component. CONSTITUTION:TiN powder of <=10mum particle size as a principal component is mixed with 0.5-10wt.% one or more kinds of oxides of <=5mum particle size selected among TiO2, niobium oxide, tantalum oxide, molybdenum oxide, tungsten oxide, yttrium oxide and oxides of lanthanides as sintering assistants. The mixture is press-molded and sintered at 1,600-1,850 deg.C for 30min-5hr in a nonoxidizing atmosphere of N2 or the like or in vacuum.

Description

【発明の詳細な説明】 「産業上の利用分野コ 本発明は黄金色の光沢を充分に有する窒化チタン質焼結
体に関する。
DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a titanium nitride sintered body having a sufficient golden luster.

[従来の技術・問題点コ 窒化チタン、窒化ジルコニウムなどの遷移金属窒化物は
緻密に焼結することにより美麗な黄金色を呈することが
知られており、装飾用部材等に使用することが期待され
ている。
[Conventional technology/problems] Transition metal nitrides such as titanium nitride and zirconium nitride are known to exhibit a beautiful golden color when densely sintered, and are expected to be used in decorative materials, etc. has been done.

しかしながら、窒化チタン、窒化ジルコニウム等は単独
では焼結が大変難しく、例えば窒化チタン粉末原料を単
味で焼結して焼結体を製造するには、ホットプレス装置
のような特別な装置を必要としたが、このような装置を
使用しても緻密焼結体を得ることは難しい。更に、ホッ
トプレス装置の保守や使用するカーボンモールド等型材
の寿命といった点などを考慮すると、経済的に極めて不
利であり実用的ではない。また、ホットプレス法では、
使用するカーボンモールド等型材から焼結体中に炭素が
含浸して焼結体表面に黒ずんだ「くすみ」を生じ、美麗
な黄金色を有する焼結体を得難く、更に、装飾用部材に
宿命的に要求されている複雑形状品の製造が至難である
等、ホットプレス法は装飾用セラミックス焼結体の製造
方法としては著しく不適であると言わざるを得ない。
However, it is very difficult to sinter titanium nitride, zirconium nitride, etc. alone, and special equipment such as a hot press is required to produce a sintered body by sintering titanium nitride powder raw materials alone. However, it is difficult to obtain a dense sintered body even using such equipment. Furthermore, considering the maintenance of the hot press equipment and the lifespan of the carbon mold and other molding materials used, this method is extremely disadvantageous economically and is not practical. In addition, in the hot press method,
Carbon is impregnated into the sintered body from the carbon molds and other mold materials used, causing a dark "dullness" on the surface of the sintered body, making it difficult to obtain a sintered body with a beautiful golden color, and furthermore, it is difficult to obtain a sintered body with a beautiful golden color. It must be said that the hot pressing method is extremely unsuitable as a method for manufacturing decorative ceramic sintered bodies, as it is extremely difficult to manufacture products with complex shapes as required by the industry.

そこで、高密度焼結体を得るために、窒化チタン原料粉
末、窒化ジルコニウム原料粉末にFe、Co、Cr、N
i等の低融点金属を添加して焼結することがなされてい
る。この方法を用いると、比較的低い焼結温度で緻密な
焼結体が得られるが、高度な研摩によってもくずんだ光
沢面か残り、充分な光沢を有した研摩面が得られ難く、
また、焼結体中に存在する金属成分の腐食が進行し、例
えば海水、汗、酸性雨等のため、変色するなどして装飾
用部材として好適な色調が損なわれるという問題があっ
た。
Therefore, in order to obtain a high-density sintered body, titanium nitride raw material powder and zirconium nitride raw material powder were mixed with Fe, Co, Cr, and N.
Sintering is carried out by adding a low melting point metal such as i. When this method is used, a dense sintered body can be obtained at a relatively low sintering temperature, but even after high-level polishing, a glossy surface remains, making it difficult to obtain a polished surface with sufficient gloss.
In addition, there is a problem in that the metal components present in the sintered body undergo corrosion and change in color due to seawater, sweat, acid rain, etc., and the color tone suitable for use as a decorative member is lost.

本発明の目的は充分な光沢を有する美麗な黄金色を呈し
、高硬度で耐食性に優れた窒化チタン質焼結体を得るこ
とにある。
An object of the present invention is to obtain a titanium nitride sintered body that exhibits a beautiful golden color with sufficient luster, is highly hard, and has excellent corrosion resistance.

[問題点を解決するための手段] 本発明者らは上記問題点に鑑み、鋭意研究を進めた結果
、窒化チタン原料粉末に焼結助剤として種々の酸化物粉
末を特定の割合で添加し、成形後、ポットプレス法に依
らず焼結したところ、充分に緻密で、しかも美麗な黄金
色を呈する窒化チタン質焼結体が得られることを見出し
、本発明を完成するに至った。
[Means for Solving the Problems] In view of the above problems, the inventors of the present invention have carried out intensive research and have found that various oxide powders are added as sintering aids to titanium nitride raw material powder in specific proportions. After molding, the inventors discovered that a titanium nitride sintered body that was sufficiently dense and had a beautiful golden color could be obtained by sintering it without relying on the pot press method, leading to the completion of the present invention.

即ち、本発明は窒化チタンを主成分とし、酸化チタン、
酸化ニオブ、酸化タンタル、酸化モリブデン、酸化タン
グステン、酸化イツトリウム及びランタニド系希土類元
素の酸化物からなる群から選択された1種または2種以
上を0.5〜10重量%含有させたことを特徴とする窒
化チタン質焼結体を提供するにある。
That is, the present invention has titanium nitride as the main component, titanium oxide,
It is characterized by containing 0.5 to 10% by weight of one or more selected from the group consisting of niobium oxide, tantalum oxide, molybdenum oxide, tungsten oxide, yttrium oxide, and oxides of lanthanide rare earth elements. The purpose of the present invention is to provide a titanium nitride sintered body.

[作 用] 本発明の窒化チタン質焼結体は窒化チタン原料粉末に、
酸化チタン、酸化ニオブ、酸化タンタル、酸化モリブデ
ン、酸化タングステン、酸化イツトリウム、ランタニド
系希土類元素の酸化物から選ばれる1種または2種以上
の酸化物焼結助剤を添加して焼結することにより得られ
るが、これらの酸化物焼結助剤の添加量は0.5〜10
重量%、好ましくは3〜7重量%の範囲内である。添加
量が0.5重量%未満では充分に緻密な焼結体が得られ
ず、また、硬度も低く、充分な光沢を有する研摩面も得
られない。また、添加量が10重量%を超えると、光沢
を有する緻密焼結体を得ることができるが、鮮やかな黄
金色が得られず、また、硬度も低くなるために好ましく
ない。
[Function] The titanium nitride sintered body of the present invention has titanium nitride raw material powder,
By adding and sintering one or more oxide sintering aids selected from titanium oxide, niobium oxide, tantalum oxide, molybdenum oxide, tungsten oxide, yttrium oxide, and oxides of lanthanide rare earth elements. However, the amount of these oxide sintering aids added is 0.5 to 10
% by weight, preferably within the range of 3-7% by weight. If the amount added is less than 0.5% by weight, a sufficiently dense sintered body cannot be obtained, the hardness is low, and a polished surface with sufficient gloss cannot be obtained. Moreover, if the amount added exceeds 10% by weight, a dense sintered body with gloss can be obtained, but a bright golden color cannot be obtained and the hardness also becomes low, which is not preferable.

本発明の窒化チタン質焼結体を製造するための窒化チタ
ン原料粉末の粒度は10μm以下であれば特に限定され
るものではないが、5μm以下の粒度をもつ窒化チタン
原料粉末を使用することが好ましい。また、酸化物焼結
助剤の粒度はいずれの酸化物でも5μm以下であれば良
く、好ましくは2ノ1m以下が良い。
The particle size of the titanium nitride raw material powder for producing the titanium nitride sintered body of the present invention is not particularly limited as long as it is 10 μm or less, but it is possible to use titanium nitride raw material powder with a particle size of 5 μm or less. preferable. Further, the particle size of the oxide sintering aid may be 5 μm or less for any oxide, preferably 2 μm or less.

上述の割合で窒化チタン原料粉末に酸化物焼結助剤を添
加した混合物を加圧成形し、窒素、アルゴン等の非酸化
性雰囲気あるいは真空中で1600〜1850℃の温度
で焼結することにより美麗な黄金色を有する窒化チタン
質焼結体を容易に得ることができる。また、焼結時間は
焼結温度等にもよるが、通常30分〜5時間である。
By press-molding a mixture of titanium nitride raw material powder and adding an oxide sintering aid in the above ratio, and sintering it at a temperature of 1600 to 1850°C in a non-oxidizing atmosphere such as nitrogen or argon or in vacuum. A titanium nitride sintered body having a beautiful golden color can be easily obtained. Further, the sintering time depends on the sintering temperature, etc., but is usually 30 minutes to 5 hours.

[実 施 例] 丸順健 平均粒径1.3μmの窒化チタン原料粉末に、平均粒径
0.05〜1,0μmの以下の第1表に記載する各種酸
化物焼結助剤を配合し、次にエタノールを加えて湿式ボ
ールミル中で21時間混合した。
[Example] Various oxide sintering aids listed in Table 1 below with an average particle size of 0.05 to 1.0 μm were blended into titanium nitride raw material powder with an average particle size of 1.3 μm, Next, ethanol was added and mixed in a wet ball mill for 21 hours.

得られた混合粉末からエタノールを蒸発乾燥後、2トン
/cm2の圧力で加圧成形し、1500〜1850℃の
温度で、窒素ガス1気圧の条件で雰囲気焼成を2時間行
なった。
After evaporating and drying the ethanol from the obtained mixed powder, the powder was press-molded at a pressure of 2 tons/cm 2 and fired in an atmosphere of 1 atm of nitrogen gas at a temperature of 1500 to 1850° C. for 2 hours.

このようにして得られた窒化チタン質焼結体を鏡面研摩
し、色調、耐食性、ビッカース硬度(llv)、焼結体
密度及び耐食性を試験しな。得られた結果を第1表に記
載する。
The titanium nitride sintered body thus obtained was mirror-polished and tested for color tone, corrosion resistance, Vickers hardness (llv), sintered body density, and corrosion resistance. The results obtained are listed in Table 1.

ここで、焼結体密度はアルキメデス法により測定し、理
論密度に対する相対値として示す。また、耐食性試験は
鏡面研摩を施した試料を海水中に浸漬して変色を観察し
た。第1表中、耐食性試験結果に示す○印は変色が全く
認められない状態を示し、X印は変色が認められたこと
を示す。
Here, the sintered body density is measured by the Archimedes method and is shown as a relative value to the theoretical density. In addition, a corrosion resistance test was performed by immersing a mirror-polished sample in seawater and observing discoloration. In Table 1, the mark ○ shown in the corrosion resistance test results indicates that no discoloration was observed, and the mark X indicates that discoloration was observed.

第1表に記載するように、実験番号1及び2(比較例〉
は焼結不良のため、低密度の多孔質体であり、鏡面研摩
を施しても鏡面は得られず、また、硬度も低かった。実
験番号23(比較例)は焼結助剤としてCo及びNiを
使用したものであり、研摩面に光沢か乏しく、耐食性試
験の結果、その研摩面は著しく損なわれた。また、実験
番号6及び7(比較例)は酸化物焼結助剤を本発明範囲
外の量で添加したものであり、研摩面の色調に難点があ
り、また、硬度も低い。
As described in Table 1, Experiment No. 1 and 2 (Comparative Example)
Due to poor sintering, it was a porous body with low density, a mirror surface could not be obtained even after mirror polishing, and the hardness was also low. Experiment No. 23 (comparative example) used Co and Ni as sintering aids, and the polished surface had poor gloss, and as a result of the corrosion resistance test, the polished surface was significantly damaged. Further, in Experiment Nos. 6 and 7 (comparative examples), the oxide sintering aid was added in an amount outside the range of the present invention, and the polished surface had a poor color tone and low hardness.

実験番号3〜5及び8〜22は本発明例であり、いずれ
の窒化チタン質焼結体も充分な光沢を有する美麗な黄金
色を呈し且つ硬度、耐食性に優れているものであった。
Experiment numbers 3 to 5 and 8 to 22 are examples of the present invention, and all titanium nitride sintered bodies had a beautiful golden color with sufficient luster and were excellent in hardness and corrosion resistance.

[発明の効果] 窒化チタン原料粉末に上述のような酸化物焼結助剤を添
加することにより、ホットプレスのような経済的に不利
な特殊装置を用いることなく優れた性質を有する窒化チ
タン質焼結体を得ることができる。
[Effect of the invention] By adding the above-mentioned oxide sintering aid to the titanium nitride raw material powder, titanium nitride material with excellent properties can be produced without using economically disadvantageous special equipment such as a hot press. A sintered body can be obtained.

8一 本発明の窒化チタン質焼結体は光沢に富んだ美麗な色調
を有し、且つ高硬度で耐スクラッチ性に優れていること
から、アクセサリ−1時計用外装部品、食器等の装飾用
部材に利用することができる。また、美麗な色調に加え
、耐食性に優れていることから、化粧タイル等の建設用
部材や衛生陶器、釣り具などにも利用可能である。更に
、高硬度であることに加え、窒化チタン本来の性質とし
て熱伝導性に優れることから、ローラー、メカニカルシ
ール等の耐摩耗摺動部材としての利用も期待される。
81 The titanium nitride sintered body of the present invention has a beautiful color tone rich in gloss, and has high hardness and excellent scratch resistance. It can be used for parts. In addition to its beautiful color tone, it also has excellent corrosion resistance, so it can be used for construction materials such as decorative tiles, sanitary ware, fishing equipment, etc. Furthermore, in addition to its high hardness, titanium nitride has excellent thermal conductivity as an inherent property, so it is expected to be used as wear-resistant sliding members such as rollers and mechanical seals.

Claims (1)

【特許請求の範囲】[Claims] 窒化チタンを主成分とし、酸化チタン、酸化ニオブ、酸
化タンタル、酸化モリブデン、酸化タングステン、酸化
イットリウム及びランタニド系希土類元素の酸化物から
なる群から選択された1種または2種以上を0.5〜1
0重量%含有させたことを特徴とする窒化チタン質焼結
体。
The main component is titanium nitride, and 0.5 to 10% of one or more selected from the group consisting of titanium oxide, niobium oxide, tantalum oxide, molybdenum oxide, tungsten oxide, yttrium oxide, and oxides of lanthanide rare earth elements. 1
A titanium nitride sintered body containing 0% by weight.
JP62154571A 1987-06-23 1987-06-23 Method for manufacturing titanium nitride sintered body Expired - Lifetime JPH0753605B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62154571A JPH0753605B2 (en) 1987-06-23 1987-06-23 Method for manufacturing titanium nitride sintered body

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62154571A JPH0753605B2 (en) 1987-06-23 1987-06-23 Method for manufacturing titanium nitride sintered body

Publications (2)

Publication Number Publication Date
JPS63319262A true JPS63319262A (en) 1988-12-27
JPH0753605B2 JPH0753605B2 (en) 1995-06-07

Family

ID=15587140

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62154571A Expired - Lifetime JPH0753605B2 (en) 1987-06-23 1987-06-23 Method for manufacturing titanium nitride sintered body

Country Status (1)

Country Link
JP (1) JPH0753605B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009119481A1 (en) * 2008-03-24 2009-10-01 京セラ株式会社 Ceramic for decorative part and decorative part comprising the same
JP2010129440A (en) * 2008-11-28 2010-06-10 National Institute Of Advanced Industrial Science & Technology Three-component system electrode material particles for lithium battery or hybrid capacitor, and their manufacturing method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60255673A (en) * 1984-01-31 1985-12-17 三菱マテリアル株式会社 Manufacture of titanium oxynitride sintered body

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60255673A (en) * 1984-01-31 1985-12-17 三菱マテリアル株式会社 Manufacture of titanium oxynitride sintered body

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009119481A1 (en) * 2008-03-24 2009-10-01 京セラ株式会社 Ceramic for decorative part and decorative part comprising the same
JP2010129440A (en) * 2008-11-28 2010-06-10 National Institute Of Advanced Industrial Science & Technology Three-component system electrode material particles for lithium battery or hybrid capacitor, and their manufacturing method

Also Published As

Publication number Publication date
JPH0753605B2 (en) 1995-06-07

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