JPH04175265A - Colored light-transmitting yag sintered compact and production thereof - Google Patents
Colored light-transmitting yag sintered compact and production thereofInfo
- Publication number
- JPH04175265A JPH04175265A JP30161890A JP30161890A JPH04175265A JP H04175265 A JPH04175265 A JP H04175265A JP 30161890 A JP30161890 A JP 30161890A JP 30161890 A JP30161890 A JP 30161890A JP H04175265 A JPH04175265 A JP H04175265A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- sintered body
- coloring agent
- oxide
- sintered compact
- 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 abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 39
- 239000003086 colorant Substances 0.000 claims abstract description 21
- 238000002834 transmittance Methods 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 7
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 6
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 5
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims abstract description 5
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 3
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 229910003440 dysprosium oxide Inorganic materials 0.000 claims description 4
- 229910001940 europium oxide Inorganic materials 0.000 claims description 4
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims description 4
- OWCYYNSBGXMRQN-UHFFFAOYSA-N holmium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ho+3].[Ho+3] OWCYYNSBGXMRQN-UHFFFAOYSA-N 0.000 claims description 4
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims description 2
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 claims 2
- 239000011812 mixed powder Substances 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 8
- 239000002223 garnet Substances 0.000 abstract description 6
- 229910052691 Erbium Inorganic materials 0.000 abstract description 4
- 239000006104 solid solution Substances 0.000 abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract 2
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 239000002075 main ingredient Substances 0.000 abstract 1
- 238000005498 polishing Methods 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-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
- 239000011230 binding agent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 235000019646 color tone Nutrition 0.000 description 1
- 239000006103 coloring component Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000001747 exhibiting effect 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
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 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、透光性に優れ且つ鮮明に着色したＹＡＧ（イ
ツトリウム・アルミニウム・ガーネツト：ＹＡｌｏ）焼
結体及びその製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a YAG (yttrium aluminum garnet: YAlo) sintered body that has excellent translucency and is clearly colored, and a method for producing the same.
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、着色剤としてＣｒ Ｏ、Ｃ
ｏ Ｏ、ＭｎＯ等の無機顔料を添加することにより、桃
色、青色その他の色彩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 colorants such as CrO, C
o They were colored pink, blue, and other colors by adding inorganic pigments such as O and MnO.
しかし、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、母材であ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
色剤である第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
透光性を有する着色セラミックス焼結体が得られなかっ
た。However, in conventional colored alumina sintered bodies and colored zirconia sintered bodies, the crystal type of alumina and zirconia, which are the base materials, is not cubic, so scattering occurs at grain boundaries, and the second phase, which is a coloring agent, Colored ceramic sintered bodies with high light transmittance could not be obtained due to reasons such as scattering occurring at these grain boundaries due to the different crystal types of the base materials.
本発明はかかる従来の事情に鑑み、時計ケース等の装飾
部材用として充分に高い透光性を具えた着色セラミック
ス焼結体、及びその製造方法を提供することを目的とす
る。In view of the conventional circumstances, it is an object of the present invention to provide a colored ceramic sintered body having sufficiently high translucency for decorative members such as watch cases, and a method for manufacturing the same.
上記目的を達成するため、本発明が提供する着色透光性
セラミックス焼結体は、イツトリウム・アルミニウム・
ガーネツト （ＹＡＧ）を主成分トし、着色剤として０
．０５〜３７．５モル％のユウロピウム、ジスプロシウ
ム、又はホルミウムの酸化物を含有し、鏡面研磨した厚
さ１闘の試料での波長０．８μｍにおける直線透過率が
１０％以上であることを特徴とする着色透光性ＹＡＧ焼
結体である。In order to achieve the above object, the colored translucent ceramic sintered body provided by the present invention is made of yttrium, aluminum,
Contains garnet (YAG) as the main component and uses 0 as a coloring agent.
．． 05 to 37.5 mol% of europium, dysprosium, or holmium oxide, and the in-line transmittance at a wavelength of 0.8 μm in a mirror-polished sample with a thickness of 1 mm is 10% or more. It is a colored translucent YAG sintered body.
又、本発明による着色透光性ＹＡＧ焼結体の製造方法は
、純度９９．９％以上及び比表面積（ＢＥＴ値） ５
ｍ７８以上のＹ２Ｏ３粉末とＡ１０ 粉末に、着色剤と
してユウロピウム、ジスプロシウム、又はホルミウムの
酸化物又は加熱によりこれら酸化物となる無機塩若しく
はアルコキシドを各酸化物に換算して０．０５〜３７．
５モル％添加混合し、混合粉末を１２００〜１５００ｒ
の温度で仮焼し、得られた粉末をＱ、 ５ ｔ ＯｎＡ
ｍ２以上の圧力で加圧成形した後、１６００〜１８５０
Ｃの温度で焼結することを特徴とする０
上記方法により得られたＹＡＧ焼結体の直線透過率を更
に向上させたい場合には、１６００〜１８５０Ｃの温度
及び５００ψｍ２以上の圧力でＨＩＰ処理することが出
来る。Further, the method for producing a colored translucent YAG sintered body according to the present invention has a purity of 99.9% or more and a specific surface area (BET value) of 5.
m78 or more Y2O3 powder and A10 powder, as a coloring agent, an oxide of europium, dysprosium, or holmium, or an inorganic salt or alkoxide that becomes these oxides by heating is added in a range of 0.05 to 37.
Add 5 mol% and mix, mix powder at 1200~1500r
The powder obtained by calcining at a temperature of Q, 5 t OnA
After pressure molding with a pressure of m2 or more, 1600-1850
If it is desired to further improve the in-line transmittance of the YAG sintered body obtained by the above method, HIP treatment is performed at a temperature of 1600 to 1850C and a pressure of 500ψm2 or more. I can do it.
本発明においては、結晶型が立方＆（ガーネット構造）
であるＹＡＧ（ＹＡＩＯ）を焼結体の母材とするので、
結晶粒界での散乱が少なく、微密に焼結することにより
可視から赤外の領域で極めて高い透光性が得られる。し
かも、着色剤としてＫｒ、Ｄｙ又はＨＯの酸化物を所定
量添加することにより鮮明に着色出来るうえ、これら酸
化物が母材のＹＡＧに固溶して焼結体の組成が
Ｙ Ｌｎ ＡＩ Ｏ（Ｌｎ＝Ｅｒ、 Ｄｙ又はＨＯｌ
ｏ、００１３３−ＸＸ５１２
≦Ｘ〈３）であるガーネット構造の単一相となるので、
着色剤との粒界における散乱もない。In the present invention, the crystal type is cubic & (garnet structure).
Since YAG (YAIO) is used as the base material of the sintered body,
There is little scattering at grain boundaries, and by finely sintering, extremely high light transmittance can be obtained in the visible to infrared range. Furthermore, by adding a predetermined amount of Kr, Dy, or HO oxide as a coloring agent, it is possible to vividly color the product, and these oxides are dissolved in the YAG base material, so that the composition of the sintered body becomes Y Ln AI O ( Ln=Er, Dy or HOl
o, 00133-XX512 ≦X<3) as it becomes a single phase with a garnet structure,
There is no scattering at grain boundaries with the colorant.
従って、本発明の着色透光性ＹＡＧ焼結体は、Ｅｒ、Ｄ
ｙ又はＨｏの酸化物に応じて着色すると同時に、銅面研
磨した厚さ１龍の試料での波長０．８μｍ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。尚、着
色剤によりＹＡＧ焼結体が呈する色彩は、酸化ユウロピ
ウム（Ｅｒ Ｏ）で桃色系、酸化ジスプロシウム（Ｄ７
ｏ ）で黄緑色系及び酸化ホルミウム（Ｈｏ Ｏ）で
だいだい色糸であり、それぞれの色調は各酸化物の添加
量によりフントロール出来る。Therefore, the colored translucent YAG sintered body of the present invention has Er, D
It is colored according to the oxide of y or Ho, and at the same time exhibits excellent light transmittance with a linear transmittance of 10% or more at a wavelength of 0.8 μm in a sample with a thickness of 1 dragon with polished copper surface. The color that the YAG sintered body exhibits due to the colorant is pinkish for europium oxide (ErO), pinkish for dysprosium oxide (D7), and pinkish for dysprosium oxide (D7).
The threads are yellow-green in color and orange in color with holmium oxide (HoO), and the color tones can be adjusted depending on the amount of each oxide added.
本発明方法において、着色透光性ＹＡＧ焼結体の母材原
料として用いるＹ２Ｏ３粉末及びＡＩ ２Ｏ３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、これらの粉末は
一次粒子の粒径が約０．３μｍ以下、即ち比表面積がＢ
ＥＴ値で５ ｒｒｌ／ｇ以上、好ましくは１０ ｒｒｌ
／（＜以上であることが、微密な焼結体を得るために必
要である。このように高純度で且つ微細なＹ２Ｏ３粉末
及びＡＩ０ 粉末としては、アルコキシドの加水分解又
は共沈法等により製造した粉末が好適である。In the method of the present invention, the Y2O3 powder and AI2O3 powder used as the base material raw materials for the colored translucent YAG sintered body are:
99. to prevent coloring or deterioration of translucency due to impurities.
Use one with a purity of 9% or higher. In addition, these powders have a primary particle size of about 0.3 μm or less, that is, a specific surface area of B.
ET value of 5 rrl/g or more, preferably 10 rrl
/(< is necessary in order to obtain a fine sintered body. In this way, high purity and fine Y2O3 powder and AI0 powder can be obtained by hydrolysis of alkoxide or co-precipitation method, etc. Preference is given to manufactured powders.
着色剤として添加されるＥｒ、Ｄｙ又はＨＯの酸化物の
粉末は、安定した発色を得るため９９％以上のものが好
ましく、又色むらが無いよう均一分散させるため粒径０
．３μｍ以下とすることが好ましい。又加熱により上記
各酸化物となる無機塩若しくはアルコキシドを用いるこ
ともできる。着色剤の添加量を上記各酸化物に換算して
０．０５〜３７．５モル％の範囲とするのは、０．０５
モル％未満では着色が不充分となり、３７．５モル％を
超えると第２相の析出により粒界での散乱が急増し、十
分な透光性が得られなくなるからである。The powder of Er, Dy or HO oxide added as a coloring agent is preferably 99% or more in order to obtain stable color development, and the particle size is 0 to ensure uniform dispersion without color unevenness.
．． The thickness is preferably 3 μm or less. Furthermore, inorganic salts or alkoxides that become each of the above oxides upon heating can also be used. The amount of the coloring agent to be added is in the range of 0.05 to 37.5 mol% in terms of each of the above oxides.
If it is less than 37.5 mol %, coloring will be insufficient, and if it exceeds 37.5 mol %, scattering at grain boundaries will rapidly increase due to precipitation of the second phase, making it impossible to obtain sufficient light transmittance.
本発明方法では、Ｙ２Ｏ３粉末及びＡＩ ２Ｏ３粉末と
着色剤粉末を前記ＹＬｎＡ１０ の組成となるよ３−
Ｘ Ｘ ５ ＋２うに配合して混合後
、１２００〜１５００ ｒで仮焼することにより反応さ
せ、着色剤である各Ｅｒ、Ｄｙ又はＨａの酸化物の固溶
したＹＡＧ粉末を予め生成させる。次に、この粉末を加
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、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０．５ ｔ ｏｎ
Ａｍ”以上の圧力で成形する。焼結は真空中又は水素ガ
ス若しくはＨｅ等の不活性ガスの常圧雰囲気中で行なう
ことが好ましく、焼結温度は１６００〜１８５０Ｃ，好
ましくは１７００〜１８００ Ｃである。焼結温度が１
６００Ｃ未満では焼結が不充分のため鮮明な発色も充分
な透光性も得られず、１８５０ Ｕを超えると着色成分
の蒸発や液相又は第２相の発生を引き起こし、組成比の
ずれが生じて透光性が著しく低下する。In the method of the present invention, Y2O3 powder, AI2O3 powder, and colorant powder are mixed to have the composition of YLnA10.
X Next, this powder is compacted by pressure molding, subjected to binder removal treatment if necessary, and then sintered. It is preferable that the molded body has a relative density ratio of 55% or more, and for that purpose, 0.5 ton on
Sintering is preferably carried out in a vacuum or in a normal pressure atmosphere of an inert gas such as hydrogen gas or He, and the sintering temperature is 1600 to 1850 C, preferably 1700 to 1800 C. Yes, the sintering temperature is 1
If it is less than 600C, sintering will be insufficient and neither clear color development nor sufficient transparency will be obtained, and if it exceeds 1850U, the coloring component will evaporate and a liquid phase or second phase will occur, resulting in a deviation in the composition ratio. This results in a significant decrease in translucency.
又、焼結時間は０．５〜２４時間、好ましくは３〜９時
間とする。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ＹＡＧ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出来る。By subjecting the YAG 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.
ＨＩＰ処理の温度は１６００〜１８５０ｒ、好ましくは
１７５０〜１８３０Ｃであり、圧力は５００ ｋｇＡｍ
２以上、好ましくは１．５ ｔＯｎＡｍ２以上である。The temperature of HIP treatment is 1600-1850r, preferably 1750-1830C, and the pressure is 500 kgAm
2 or more, preferably 1.5 tOnAm2 or more.
ＨＩＰ処理の温度が１６００ Ｃ未満又は圧力が５００
に９／Ａｍ２未満では緻密化が進行せず、従って直線透
過率の改善がみられない。又、ＨＩＰ処理の温度が１８
５Ｏｒを超えると蒸発、液相又は第２相の発生により組
成比がずれ、透光性が著しく低下する。尚、ＨＩＰ処理
の圧力媒体はＡｒ等の不活性ガス、又は酸素ガス、若し
くはこれらの混合ガスが好ましい。The temperature of HIP treatment is less than 1600 C or the pressure is 500 C.
If the ratio is less than 9/Am2, densification does not proceed, and therefore no improvement in in-line transmittance is observed. Also, the temperature of HIP treatment is 18
When it exceeds 5 Or, the composition ratio shifts due to evaporation, the generation of a liquid phase or a second phase, and the light transmittance is significantly reduced. Note that the pressure medium for the HIP process is preferably an inert gas such as Ar, oxygen gas, or a mixed gas thereof.
！ｌｊ」
純度９９．９％、比表面積１５．１ ｍＪ／ｇ （Ｂ
Ｅ Ｔ値）の高純度ＡＩ ２Ｏ３粉末、純度９９．９％
、比表面積９．４ ＷＶｇ （Ｂ Ｅ Ｔ値）の高純度
Ｙ２Ｏ３粉末に、着色剤として１モル％のＥｒ ２Ｏ３
粉末を添加し、アルミナボールでボールミル混合し、乾
燥した後、１４００ Ｃで仮焼することによりＥｒ Ｏ
を匪溶したＹＡＧ粉末を得た。次に、この粉末を粉砕し
２．０ｔｏｎΔｍ２の圧力でＣ工Ｐ成形した後、成形体
をＨｅガスの常圧雰囲気中において温度１７５０ ｒで
６時間焼結し、理論密度比９９．２％で薄桃色を呈する
半透明のＹＡＧ焼結体を得た。! lj'' purity 99.9%, specific surface area 15.1 mJ/g (B
High purity AI 2O3 powder with ET value), purity 99.9%
, high-purity Y2O3 powder with a specific surface area of 9.4 WVg (BET value), and 1 mol% of Er2O3 as a coloring agent.
Er O
YAG powder was obtained. Next, this powder was crushed and subjected to C/P molding at a pressure of 2.0 ton Δm2, and then the molded body was sintered at a temperature of 1750 r for 6 hours in a normal pressure atmosphere of He gas, and the theoretical density ratio was 99.2%. A translucent YAG sintered body exhibiting a light pink color was obtained.
このＹＡＧ焼結体の両面を鏡面研磨加工して厚さ１ｍｍ
とした試料は、滑らかで深みのある薄桃色に着色し且つ
透光性を示し、可視光領域での直線透過率を分光光度計
で測定したところ、波長０．８μｍで１２％であった。Both sides of this YAG sintered body are mirror polished to a thickness of 1 mm.
The sample was colored a smooth, deep pale pink color and exhibited translucency, and the linear transmittance in the visible light region was measured with a spectrophotometer and was 12% at a wavelength of 0.8 μm.
実施例２
上記実施例１と同一条件で製造した薄桃色半透明のＹＡ
Ｇ焼結体をＨＩＰ装置に入れ、Ａｒガスを用いて１７５
０ Ｕの温度及び２０００ψｍ２の圧力で３時間のＨＩ
Ｐ処理を行ない、理論密度比９９．８％の薄桃色で透明
なＹＡＧ焼結体を得た。Example 2 Light pink translucent YA produced under the same conditions as Example 1 above
The G sintered body was placed in a HIP device and heated to 175% using Ar gas.
HI for 3 hours at a temperature of 0 U and a pressure of 2000 ψm2
P treatment was performed to obtain a pale pink transparent YAG sintered body with a theoretical density ratio of 99.8%.
このＹＡＧ焼結体の両面を鏡面研磨加工して厚さ１ｍｍ
とした試料は、透明感を有し滑らかで深みのある薄桃色
に着色しており、可視光領域での直線透過率は波長０．
８μｍで５８％であった。Both sides of this YAG sintered body are mirror polished to a thickness of 1 mm.
The sample was transparent, smooth, and colored a deep light pink color, and the linear transmittance in the visible light region was at a wavelength of 0.
It was 58% at 8 μm.
実施例３
実施例１と同じＡＩ ２Ｏ３粉末とＹ２Ｏ３粉末に、着
色剤としてＫｒ２０．換算で１モル％のＥｒ（Ｎｏ、）
８を添加して超音波混合し、乾燥した後、１４００１：
’で仮焼することによりＥｒ Ｏを固溶したＹＡＧ粉末
を得た。次に、この粉末を粉砕し２．０ ｔｏｎ／／Ｃ
ｍ”の圧力でＯＩＰ成形した後、成形体をＨｅガスの常
圧雰囲気中において温度１７５０ ｒで６時間焼結し、
理論密度比９９．３％で薄桃色を呈する半透明のＹＡＧ
焼結体を得た。Example 3 In addition to the same AI 2O3 powder and Y2O3 powder as in Example 1, Kr20. Converted to 1 mol% Er(No,)
After adding 8, ultrasonic mixing, and drying, 14001:
YAG powder in which Er 2 O was dissolved in solid solution was obtained by calcination at '. Next, this powder was pulverized to 2.0 ton//C
After OIP molding at a pressure of 50 m'', the molded body was sintered at a temperature of 1750 r for 6 hours in a normal pressure atmosphere of He gas,
Translucent YAG with a pale pink color at a theoretical density ratio of 99.3%
A sintered body was obtained.
このＹＡＧ焼結体の両面を鏡面研磨加工して厚さ１闘と
した試料は、滑らかで深みのある薄桃色に着色し且つ透
光性を示し、可視光領域での直線透過率を分光光度計で
測定したところ、波長０．８μｍで１５％であった。This YAG sintered body was mirror-polished on both sides to a thickness of 1 mm, and was colored a smooth, deep pale pink color and exhibited translucency. When measured with a meter, it was 15% at a wavelength of 0.8 μm.
実施例４
上記実施例３と同一条件で製造した薄桃色半透明のＹＡ
Ｇ焼結体をＨＩＰ装置に入れ、Ａｒガスを用いて１７５
０ Ｃの温度及び２０００ ｋｑＡｍ’の圧力で３時間
のＨＩＰ処理を行ない、薄桃色で透明なＹＡＧ焼結体を
得た。Example 4 Light pink translucent YA produced under the same conditions as Example 3 above.
The G sintered body was placed in a HIP device and heated to 175% using Ar gas.
HIP treatment was performed for 3 hours at a temperature of 0 C and a pressure of 2000 kqAm' to obtain a pale pink and transparent YAG sintered body.
このＹＡＧ焼結体の両面を鏡面研磨加工して厚さＩＷｍ
とした試料は、透明感を有し滑らかで深みのある薄桃色
に着色しており、可視光領域での直線透過率は波長Ｑ、
３ ／ｊｍで６０％であった。Both sides of this YAG sintered body are mirror polished to a thickness of IWm.
The sample was transparent, smooth, and colored a deep pale pink, and the linear transmittance in the visible light region was at wavelength Q,
3/jm was 60%.
実施例５
純度９９．９％、比表面積１５．１袷’ｇ（ＢｚＴ値）
の高純度ＡＩ ２Ｏ３粉末、純度９９．９％、比表面積
９．４ｒｒｌ／ｇ （Ｂ Ｅ Ｔ値）の高純度Ｙ２Ｏ
３粉末に、着色剤として１モル％のＤｙ○ 粉末を添加
し、アルミナボールでボールミル混合し、乾燥した後、
１４００Ｃで仮焼することによりＤｙ Ｏを固溶したＹ
ＡＧ粉末を得た。次に、この粉末を粉砕し２． Ｏｔ
ｏ ｎ７ｃｍ”の圧力でＣ工Ｐ成形した後、成形体をＨ
ｅガスの常圧雰囲気中において温度１７００ Ｃで６時
間焼結し、理論密度比９９．２％で半透明のＹＡＧ焼結
体を得た。更に、この焼結体をＨＩＰ装置に入れ、Ａｒ
ガスを用いて１７５０ ｃの温度及び２０００ ｋｇ／
Ｃｍ”の圧力で３時間のＨＩＰ処理を行なった。Example 5 Purity 99.9%, specific surface area 15.1 g (BzT value)
High purity AI 2O3 powder, high purity Y2O with a purity of 99.9% and a specific surface area of 9.4rrl/g (BET value)
1 mol% of Dy○ powder was added as a coloring agent to the 3 powder, mixed in a ball mill with an alumina ball, and after drying,
Y containing DyO as a solid solution by calcining at 1400C
AG powder was obtained. Next, crush this powder and 2. Ot
After C/P molding at a pressure of 7 cm, the molded body was
Sintering was carried out at a temperature of 1700 C for 6 hours in an e-gas normal pressure atmosphere to obtain a translucent YAG sintered body with a theoretical density ratio of 99.2%. Furthermore, this sintered body was placed in a HIP device and Ar
using gas at a temperature of 1750 c and 2000 kg/
HIP treatment was carried out for 3 hours at a pressure of 1.5 cm.
このＹＡＧ焼結体の両面を鏡面研磨加工して厚さ１闘と
した試料は、透明感があり滑らかで深みのある薄黄緑色
に着色しており、この試料の可視光領域での直線透過率
を分光光度計で測定したところ、波長０．８μｍで４８
％であった。This YAG sintered body was mirror-polished on both sides to a thickness of 1 mm, and was transparent, smooth, and colored a deep pale yellow-green.The straight line transmission of this sample in the visible light range When the rate was measured with a spectrophotometer, it was 48 at a wavelength of 0.8 μm.
%Met.
実施例６
純度９９．９％、比表面積１５．１ダｇ（ＢＥＴ値）の
高純度ＡＩ ２Ｏ３粉末、純度９９．９％、比表面積９
．４ｔｒＶｇ（Ｂ Ｋ Ｔ値）の高純度Ｙ２Ｏ３粉末に
、着色剤として１モル％のＨｏ ２Ｏ３粉末を添加し、
アルミナボールでボールミル混合し、乾燥した後、１４
００Ｃで仮焼することによりＨｐ Ｏを固溶したＹＡＧ
粉末を得た。次に、この粉末を粉砕し２． Ｏｔ ｏ
ｎ７ｃｍ２の圧力でＣ工Ｐ成形した後、成形体をＨｅガ
スの常圧雰囲気中において温度１７００ Ｃで６時間焼
結し、理論密度比９９．０％で半透明のＹＡＧ焼結体を
得た。更に、この焼結体をＨＩＰ装置に入れ、Ａｒガス
を用いて１７５０ｔ？の温度及び２０００ ｋｇＡｍの
圧力で３時間のＨＩＰ処理を行った。Example 6 High purity AI 2O3 powder with a purity of 99.9% and a specific surface area of 15.1 dag (BET value), a purity of 99.9% and a specific surface area of 9
．． 1 mol% Ho 2 O 3 powder was added as a coloring agent to high purity Y 2 O 3 powder of 4 trVg (B K T value),
After mixing in a ball mill with an alumina ball and drying, 14
YAG with Hp O dissolved in it by calcining at 00C
A powder was obtained. Next, crush this powder and 2. Oto o
After C/P molding at a pressure of n7 cm2, the molded body was sintered at a temperature of 1700 C for 6 hours in a normal pressure He gas atmosphere to obtain a translucent YAG sintered body with a theoretical density ratio of 99.0%. . Furthermore, this sintered body was placed in a HIP device and heated to 1750 tons using Ar gas. HIP treatment was performed for 3 hours at a temperature of 2000 kgAm and a pressure of 2000 kgAm.
このＹＡＧ焼結体の両面を波面研磨加工して厚さ１朋と
した試料は、透明感があり滑らかで深みのある薄だいだ
い色に着色しており、この試料の可視光領域での直線透
過率を分光光度計で測定したところ、波長０．８μｍで
５６％であった。This YAG sintered body was wave-polished on both sides to a thickness of 1 mm, and was transparent, smooth, and colored a deep pale orange.The straight line transmission of this sample in the visible light range The rate was measured with a spectrophotometer and was 56% at a wavelength of 0.8 μm.
本発明によれば、ＹＡＧを母材とするガーネット構造の
単一相からなり、各種の色彩に着色すると同時に透光性
にも優れた着色透光性ＹＡＧ焼結体を提供することが出
来る。According to the present invention, it is possible to provide a colored translucent YAG sintered body that is made of a single phase with a garnet structure using YAG as a base material, and is colored in various colors and has excellent translucency.
この着色透光性ＹＡＧ焼結体は、時計ケース等の装飾部
材として特に有用である。This colored translucent YAG sintered body is particularly useful as a decorative member for watch cases and the like.
Claims (3)
Ｇ）を主成分とし、着色剤として０．０５〜３７．５モ
ル％のユウロピウム、ジスプロシウム又はホルミウムの
酸化物を含有し、鏡面研磨した厚さ１ｍｍの試料での波
長０．８μｍにおける直線透過率が１０％以上であるこ
とを特徴とする着色透光性ＹＡＧ焼結体。(1) Yttrium aluminum garnet (YA
Linear transmittance at a wavelength of 0.8 μm for a mirror-polished 1 mm thick sample containing G) as the main component and 0.05 to 37.5 mol% of europium, dysprosium, or holmium oxide as a coloring agent. A colored translucent YAG sintered body, characterized in that: 10% or more.
ｍ＾３／ｇ以上のＹ＿２Ｏ＿３粉末とＡｌ＿２Ｏ＿３粉
末に、着色剤としてユウロピウム、ジスプロシウム又は
ホルミウムの酸化物又は加熱によりこれら酸化物となる
無機塩若しくはアルコキシドを各酸化物に換算して０．
０５〜３７．５モル％添加混合し、混合粉末を１２００
〜１５００℃の温度で仮焼し、得られた粉末を０．５ｔ
ｏｎ／ｃｍ＾２以上の圧力で加圧成形した後、１６００
〜１８５０℃の温度で焼結することを特徴とする着色透
光性ＹＡＧ焼結体の製造方法。(2) Purity 99.9% or more and specific surface area (BET value) 5
m^3/g or more of Y_2O_3 powder and Al_2O_3 powder, and as a coloring agent, an oxide of europium, dysprosium, or holmium, or an inorganic salt or alkoxide that becomes these oxides by heating is added to each oxide.
Add 05 to 37.5 mol% and mix to make the mixed powder 1200
Calcinate at a temperature of ~1500°C, and 0.5t of the resulting powder
After pressure molding at a pressure of on/cm^2 or more, 1600
A method for producing a colored translucent YAG sintered body, characterized by sintering at a temperature of ~1850°C.
００〜１８５０℃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Ｙ
ＡＧ焼結体の製造方法。(3) The sintered body obtained according to claim (2) is further added to 16
Colored translucent Y characterized by HIP treatment at a temperature of 00 to 1850°C and a pressure of 500 kg/cm^2 or more
Method for manufacturing AG sintered body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30161890A JPH04175265A (en) | 1990-11-07 | 1990-11-07 | Colored light-transmitting yag sintered compact and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30161890A JPH04175265A (en) | 1990-11-07 | 1990-11-07 | Colored light-transmitting yag sintered compact and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04175265A true JPH04175265A (en) | 1992-06-23 |
Family
ID=17899115
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30161890A Pending JPH04175265A (en) | 1990-11-07 | 1990-11-07 | Colored light-transmitting yag sintered compact and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04175265A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100517271B1 (en) * | 1996-07-29 | 2005-09-28 | 니치아 카가쿠 고교 가부시키가이샤 | Light emitting device and display device |
| KR100537349B1 (en) * | 1996-06-26 | 2006-02-28 | 오스람 게젤샤프트 미트 베쉬랭크터 하프퉁 | Light-emitting semiconductor component with luminescence conversion element |
| JP2009084060A (en) * | 2007-09-27 | 2009-04-23 | Covalent Materials Corp | Translucent oxidized yttrium aluminum garnet sintered compact and its producing method |
-
1990
- 1990-11-07 JP JP30161890A patent/JPH04175265A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100537349B1 (en) * | 1996-06-26 | 2006-02-28 | 오스람 게젤샤프트 미트 베쉬랭크터 하프퉁 | Light-emitting semiconductor component with luminescence conversion element |
| US9196800B2 (en) | 1996-06-26 | 2015-11-24 | Osram Gmbh | Light-radiating semiconductor component with a luminescence conversion element |
| KR100517271B1 (en) * | 1996-07-29 | 2005-09-28 | 니치아 카가쿠 고교 가부시키가이샤 | Light emitting device and display device |
| JP2009084060A (en) * | 2007-09-27 | 2009-04-23 | Covalent Materials Corp | Translucent oxidized yttrium aluminum garnet sintered compact and its producing method |
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