JPH04124061A - Production of colored transparent spinel-type sintered material - Google Patents
Production of colored transparent spinel-type sintered materialInfo
- Publication number
- JPH04124061A JPH04124061A JP2244825A JP24482590A JPH04124061A JP H04124061 A JPH04124061 A JP H04124061A JP 2244825 A JP2244825 A JP 2244825A JP 24482590 A JP24482590 A JP 24482590A JP H04124061 A JPH04124061 A JP H04124061A
- Authority
- JP
- Japan
- Prior art keywords
- spinel
- powder
- sintered body
- mno
- pressure
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000000463 material Substances 0.000 title abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 5
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 4
- 238000000465 moulding Methods 0.000 claims abstract description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 26
- 229910052596 spinel Inorganic materials 0.000 claims description 23
- 239000011029 spinel Substances 0.000 claims description 23
- 239000006103 coloring component Substances 0.000 claims description 11
- 239000011812 mixed powder Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000001272 pressureless sintering Methods 0.000 abstract description 3
- 239000011369 resultant mixture Substances 0.000 abstract 2
- 239000003086 colorant Substances 0.000 abstract 1
- 238000002834 transmittance Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、黄色系に着色し且つ透光性に優れたスピネル
焼結体の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for manufacturing a spinel sintered body that is colored yellowish and has excellent translucency.
近年、例えば時計ケース、ライターケース、ネクタイビ
ン等の装飾部材として、着色セラミックス焼結体が利用
されている。In recent years, colored ceramic sintered bodies have been used as decorative members for watch cases, lighter cases, tie bins, and the like.
従来の着色セラミックス焼結体は、特開昭６２−１２３
０５８号公報などに開示される如く殆どがアルミナ又は
ジルコニアを主成分とし、着色成分としてＯｒ Ｏ、（
！ｏ Ｏ、ＭｎＯ等の無機顔料を添加することにより、
桃色、青色その他の色影に着色したものであった。Conventional colored ceramic sintered bodies are disclosed in Japanese Patent Application Laid-Open No. 123-1983.
As disclosed in Publication No. 058, most of them contain alumina or zirconia as a main component, and contain Or O, (
! o By adding inorganic pigments such as O, MnO, etc.
They were colored pink, blue, and other shades.
しかし、かかる従来の着色アルミナ焼結体や着色ジルコ
ニア焼結体では、母材となるアルミナやジルコニアの結
晶型が立方晶でないため結晶粒界で散乱を受けること、
及び着色成分である第２相と母材の結晶型が異なるため
これらの粒界においても散乱を受けること等の理由によ
り、高い透光性を有するものを得ることが困難であった
。However, in such conventional colored alumina sintered bodies and colored zirconia sintered bodies, the crystal type of the alumina and zirconia used as the base material is not cubic, so they are subject to scattering at grain boundaries.
Furthermore, it has been difficult to obtain a material with high light transmittance because the crystal types of the second phase, which is a coloring component, and the base material are different, and scattering occurs even at these grain boundaries.
（発明が解決しようとするｉ！１ｌｆ）本発明はかかる
従来の事情に鑑み、時計ケース等の装飾部材用として黄
色系に着色し且つ充分に高い透光性を具えた着色透光性
セラミックス焼結体の製造方法を提供することを目的と
する。(i!1lf to be solved by the invention) In view of the above-mentioned conventional circumstances, the present invention provides a colored translucent ceramic sintered material which is colored yellowish and has sufficiently high translucency for decorative members such as watch cases. The object of the present invention is to provide a method for producing a compact.
上記目的を達成するため、本発明による着色透光性セラ
ミックス焼結体はスピネルを母材とすることとし、その
製造方法は純度９９．９％以上及び比表面積（ＢＥＴ値
）５ｍ’／ｇ以上のスピネル粉末に、着色成分として酸
化マンガン又は加熱により酸化マンガンとなる無機塩若
しくはアルコキシドを酸化マンガンに換算して１０〜５
０００ ｐｐｍ添加混合し、その混合粉末を加圧成形し
た後、１５００〜１８００ Ｃの温度で常圧焼結するこ
とを特徴とする。In order to achieve the above object, the colored translucent ceramic sintered body according to the present invention uses spinel as a base material, and its manufacturing method has a purity of 99.9% or more and a specific surface area (BET value) of 5 m'/g or more. of spinel powder, manganese oxide or an inorganic salt or alkoxide that becomes manganese oxide by heating as a coloring component is 10 to 5 in terms of manganese oxide.
000 ppm is added and mixed, the mixed powder is pressure molded, and then pressureless sintered at a temperature of 1500 to 1800 C.
上記方法により得られたスピネル焼結体の直線透過率を
更に向上させたい場合には、１５００〜１８ＯＯＣの温
度及び５００ ｋｇ７Ｅ、ｍ”以上の圧力でＨＩＰ処理
することが出来る。If it is desired to further improve the in-line transmittance of the spinel sintered body obtained by the above method, HIP treatment can be performed at a temperature of 1500 to 18 OOC and a pressure of 500 kg7E, m'' or more.
本発明方法においては、焼結体の母材としてスピネル（
ＭｇＡ／ Ｏ）を用いるので、結晶型が立方晶であるた
め結晶粒界での光散乱が少なく、緻密に焼結することに
より極めて高い透光性を示す焼結体が得られる。しかも
、着色成分として所定量の酸化マンガンを含有させるこ
とによって、鮮明で美しい黄色系の色彩に着色出来る。In the method of the present invention, spinel (
Since MgA/O) is used, the crystal type is cubic, so there is little light scattering at grain boundaries, and by dense sintering, a sintered body exhibiting extremely high translucency can be obtained. Moreover, by containing a predetermined amount of manganese oxide as a coloring component, it can be colored in a clear and beautiful yellowish color.
尚、黄色系の色調は、着色成分である酸化マンガンの添
加量によりフントロールすることができる。The yellow color tone can be controlled by adjusting the amount of manganese oxide, which is a coloring component.
従って、本発明方法で得られる着色透光性スピネル焼結
体は、黄色系に着色していると同時に、鏡面研磨した厚
さ２ｍの試料での波長０．６μｍにおける直線透過率が
１０％以上という優れた透光性を示す。Therefore, the colored translucent spinel sintered body obtained by the method of the present invention is yellowish in color and at the same time has a linear transmittance of 10% or more at a wavelength of 0.6 μm in a mirror-polished 2 m thick sample. It exhibits excellent translucency.
本発明方法において用いるスピネル粉末は、不純物によ
る着色或いは透光性の低下を防ぐため９９．９％以上の
純度のものを使用する。又、スピネル粉末は一次粒子の
粒径が約０．３μｍ以下、即ち比表面積がＥＥＴ値で５
ｍ２／ｇ以上、好ましくは１０ ＷＸ／ｇ以上であるこ
とが、緻密な焼結体を得る為に必要である。このように
高純度で且つ微細なスピネル粉末としては、アルコキシ
ドの加水分解又は共沈法などにより製造した粉末が好適
である。The spinel powder used in the method of the present invention has a purity of 99.9% or more in order to prevent coloration or reduction in translucency due to impurities. In addition, spinel powder has a primary particle size of about 0.3 μm or less, that is, a specific surface area of 5 in terms of EET value.
m2/g or more, preferably 10 WX/g or more is necessary in order to obtain a dense sintered body. As such a highly pure and fine spinel powder, a powder produced by an alkoxide hydrolysis or coprecipitation method is suitable.
着色成分として添加される酸化マンガンの粉末は、安定
した発色を得るため９９％以上の純度のものが好ましく
、又色むらが無いよう均一分散させるため平均粒径０．
３μｍ以下とすることが好ましい。尚、加熱により酸化
マンガンとなる無機塩若しくはアルコキシドを用いるこ
とも出来る。The manganese oxide powder added as a coloring component preferably has a purity of 99% or higher in order to obtain stable color development, and has an average particle size of 0.000000000000000000000000000000000000000000000000000000000.0.0.0.0.0.0.0.
The thickness is preferably 3 μm or less. Incidentally, an inorganic salt or alkoxide which becomes manganese oxide upon heating can also be used.
かかる着色成分の添加量は酸化マンガンに換算して１０
〜５０００ ｐｐｍの範囲であり、１０ ｐｐｍ未満で
は着色が不充分となり、５０００ ｐｐｍを超えると着
色成分元素による吸収係数の増加により充分な透光性が
得られなくなる。The amount of the coloring component added is 10 in terms of manganese oxide.
-5000 ppm; if it is less than 10 ppm, the coloring will be insufficient, and if it exceeds 5000 ppm, the absorption coefficient will increase due to the coloring component elements, making it impossible to obtain sufficient translucency.
本発明方法では、スピネル粉末と着色成分の粉末を混合
し、混合粉末を加圧成形して緻密化し、必要に応じて脱
バインダー処理を行なった後、常圧焼結する。成形体は
相対密度比５５％以上とすることが好ましく、そのため
には１．ＯｔＱｎ／ｃｍ”以上の圧力で成形する。成形
体の焼結は常圧焼結とし、真空中又は水素ガス若しくは
Ｈｅ等の不活性ガスの雰囲気中で行なうことが好ましい
。焼結温度は１５００〜１８００Ｃ，好ましくは１６０
０〜１７００ｔｌｌｌ’であり、焼結温度が１５００
Ｃ未満では焼結不充分のため鮮明な発色も充分な透光性
も得られず、１８００Ｃを超えると着色成分の蒸発やス
ピネルの組成比のズレが生じやすくなる。又、焼結時間
は０．５〜２４時間、好ましくは３〜９時間とする。In the method of the present invention, spinel powder and coloring component powder are mixed, the mixed powder is compacted by pressure molding, and after performing binder removal treatment if necessary, pressureless sintering is performed. It is preferable that the molded body has a relative density ratio of 55% or more, and for this purpose 1. Sintering of the molded body is carried out under normal pressure, preferably in a vacuum or in an atmosphere of an inert gas such as hydrogen gas or He. The sintering temperature is 1500 ~ 1800C, preferably 160
0 to 1700 tlll', and the sintering temperature is 1500 tlll'.
If it is less than 1,800 C, sintering is insufficient and neither clear color development nor sufficient translucency can be obtained, and if it exceeds 1,800 C, evaporation of the coloring component and deviation in the composition ratio of the spinel tend to occur. Further, the sintering time is 0.5 to 24 hours, preferably 3 to 9 hours.
上記焼結により得られたスピネル焼結体をＨＩＰ処理す
ることによって、焼結体の緻密化が更に進行し、直線透
過率を一層向上させることができる。ＨＩＰ処理の温度
が１５００ Ｃ未満又は圧力が５００ψ♂未満では緻密
化が充分に進行せず、従って直線透過率の改讐がみられ
ない。又、ＨＩＰ処理の温度が１８００ Ｃを超えると
、炉内雰囲気の影響を受けて焼結体が変色する。尚、Ｈ
ＩＰ処理の圧力媒体はＡｒ等の不活性ガス、窒素ガス又
は酸素ガス、若しくはこれらの混合ガスが好ましい。By subjecting the spinel sintered body obtained by the above sintering to HIP treatment, the sintered body is further densified and the in-line transmittance can be further improved. If the temperature of the HIP treatment is less than 1500 C or the pressure is less than 500 ψ♂, densification will not proceed sufficiently, and therefore no improvement in in-line transmittance will be observed. Furthermore, if the temperature of the HIP treatment exceeds 1800 C, the sintered body will discolor due to the influence of the furnace atmosphere. In addition, H
The pressure medium for the IP treatment is preferably an inert gas such as Ar, nitrogen gas, oxygen gas, or a mixed gas thereof.
実施例１
純度９９．９％以上、比表面積１４．５ ＷＶｇ （Ｂ
Ｅ Ｔ値）の高純度スピネル粉末に、着色成分として
５００ｐ１ｍの酸化マンガン粉末（平均粒径０．４μＩ
！Ｉ）を添加してボールミル混合し、乾燥した後２．Ｏ
ｔｏｎ／ｃｍ”の圧力でＣ工Ｐ成形した。この成形体を
Ｈｅガスの常圧雰囲気中において１７００ｒで６時間焼
結し、理論密度比９９．２％で黄色を呈する半透明のス
ピネル焼結体を得た。Example 1 Purity 99.9% or more, specific surface area 14.5 WVg (B
500p1m manganese oxide powder (average particle size 0.4μI) as a coloring component to high-purity spinel powder with a
! After adding I), mixing in a ball mill, and drying, 2. O
C-P molded at a pressure of 1000 ton/cm". This molded product was sintered at 1700 r for 6 hours in a normal pressure atmosphere of He gas, resulting in a semi-transparent spinel sintered material with a yellow color at a theoretical density ratio of 99.2%. I got a body.
この焼結体を厚さ’１ｍに鏡面研磨加工したところ、滑
らかで深みのある黄色に着色し且つ透光性を有していた
。この厚さ２１１＠の鏡面加工した試料の可視光領域で
の直線透過率を測定したところ、波長０．６μｍで１１
％であった。When this sintered body was mirror-polished to a thickness of 1 m, it was smooth, colored a deep yellow, and had translucency. When we measured the linear transmittance in the visible light region of this mirror-finished sample with a thickness of 211@, it was found to be 11 at a wavelength of 0.6 μm.
%Met.
実施例２
酸化マンガン粉末の代りにＭｎ２ に換算して５００ｐ
ｐｍの硝酸マンガン粉末を用いて超音波混合した以外は
、実施例１と同一条件により常圧焼結し、理論密度比９
９．３％で黄色を呈する半透明のスピネル焼結体を得た
。Example 2 500p converted to Mn2 instead of manganese oxide powder
Pressureless sintering was performed under the same conditions as in Example 1, except that pm manganese nitrate powder was used for ultrasonic mixing, and the theoretical density ratio was 9.
A translucent spinel sintered body exhibiting yellow color was obtained at 9.3%.
この焼結体を厚さ２謔に鏡面研磨加工したところ、滑ら
かで深みのある黄色に着色し且つ透光性を有し、この厚
さ２鴎の試料の直線透過率は波長０．６μｍで１３％で
あった。When this sintered body was mirror-polished to a thickness of 2 mm, it was colored a smooth, deep yellow color and had translucency.The in-line transmittance of this 2 mm thick sample was at a wavelength of 0.6 μm. It was 13%.
実施例３
上記実施例１と同一条件で製造した黄色半透明のスピネ
ル焼結体をＨＩＰ装置に入れ、Ａｒガスを用いて１７０
０ｒの温度及び２０００ψ♂の圧力で３時間のＨＩＰ処
理を行なった。Example 3 A yellow semi-transparent spinel sintered body manufactured under the same conditions as in Example 1 above was placed in a HIP device and heated at 170° C. using Ar gas.
HIP treatment was performed for 3 hours at a temperature of 0 r and a pressure of 2000 ψ♂.
得られたスピネル焼結体は黄色を呈し、透明であった。The obtained spinel sintered body was yellow and transparent.
この焼結体を厚さ２１１＠に鏡面研磨加工すると、滑ら
かで深みのある黄色に着色しており、この厚さ２鴎の試
料の可視光領域での直線透過率は波長０．６μｍで２４
％であった。When this sintered body was mirror-polished to a thickness of 211@, it was colored a smooth and deep yellow, and the linear transmittance in the visible light region of this 2-thick sample was 24 at a wavelength of 0.6 μm.
%Met.
本発明によれば、立方晶のスピネルを母材とすることに
よって、透光性に優れ、且つ黄色系に着色した着色透光
性スピネル焼結体を提供することが出来る。According to the present invention, by using cubic spinel as a base material, it is possible to provide a colored translucent spinel sintered body that has excellent translucency and is colored yellowish.
この着色透光性スピネル焼結体は、黄色系に着色し且つ
透明であるから、時計ケース等の装飾部材として特に有
用である。Since this colored translucent spinel sintered body is yellowish in color and transparent, it is particularly useful as decorative members for watch cases and the like.
出願人 住友電気工業株式会社Applicant: Sumitomo Electric Industries, Ltd.
Claims (2)
ｍ＾２／ｇ以上のスピネル粉末に、着色成分として酸化
マンガン又は加熱により酸化マンガンとなる無機塩若し
くはアルコキシドを酸化マンガンに換算して１０〜５０
００ｐｐｍ添加混合し、その混合粉末を加圧成形した後
、１５００〜１８００℃の温度で常圧焼結することを特
徴とする着色透光性スピネル焼結体の製造方法。(1) Purity 99.9% or more and specific surface area (BET value) 5
m^2/g or more of spinel powder, as a coloring component, manganese oxide or an inorganic salt or alkoxide that becomes manganese oxide when heated is 10 to 50 in terms of manganese oxide.
A method for producing a colored translucent spinel sintered body, which comprises adding and mixing 00 ppm of the mixed powder, press-molding the mixed powder, and then sintering it under normal pressure at a temperature of 1500 to 1800°C.
００〜１８００℃の温度及び５００ｋｇ／ｃｍ＾２以上
の圧力でＨＩＰ処理することを特徴とする着色透光性ス
ピネル焼結体の製造方法。(2) The sintered body obtained according to claim (1) is further added to 15
A method for producing a colored translucent spinel sintered body, characterized by performing HIP treatment at a temperature of 00 to 1800°C and a pressure of 500 kg/cm^2 or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2244825A JPH04124061A (en) | 1990-09-14 | 1990-09-14 | Production of colored transparent spinel-type sintered material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2244825A JPH04124061A (en) | 1990-09-14 | 1990-09-14 | Production of colored transparent spinel-type sintered material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04124061A true JPH04124061A (en) | 1992-04-24 |
Family
ID=17124515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2244825A Pending JPH04124061A (en) | 1990-09-14 | 1990-09-14 | Production of colored transparent spinel-type sintered material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04124061A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9624136B2 (en) | 2014-07-01 | 2017-04-18 | Corning Incorporated | Transparent spinel article and tape cast methods for making |
-
1990
- 1990-09-14 JP JP2244825A patent/JPH04124061A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9624136B2 (en) | 2014-07-01 | 2017-04-18 | Corning Incorporated | Transparent spinel article and tape cast methods for making |
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