JPH09315865A - Production of transparent yttrium oxide sintered compact - Google Patents
Production of transparent yttrium oxide sintered compactInfo
- Publication number
- JPH09315865A JPH09315865A JP8156142A JP15614296A JPH09315865A JP H09315865 A JPH09315865 A JP H09315865A JP 8156142 A JP8156142 A JP 8156142A JP 15614296 A JP15614296 A JP 15614296A JP H09315865 A JPH09315865 A JP H09315865A
- Authority
- JP
- Japan
- Prior art keywords
- yttrium
- yttrium oxide
- sintered body
- carbonate
- powder
- 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
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、レーザホスト材料,高
温用観察窓,放電灯用発光管等として使用される酸化イ
ットリウム透明焼結体を製造する方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a yttrium oxide transparent sintered body used as a laser host material, a high temperature observation window, an arc tube for a discharge lamp and the like.
【0002】[0002]
【従来の技術】酸化イットリウムは、結晶構造が立方晶
であり、複屈折がない。そのため、焼結体であっても、
不純物や気孔を除去することによって単結晶と同等の光
透過性を呈する材料が得られる。しかも、焼結体は、単
結晶よりも低い温度で合成できるため、経済性に優れ、
冷却時に2280℃の構造相転移点でクラックが発生す
る問題を回避することができる。酸化イットリウム透明
焼結体は、ホットプレスを用いて圧力7000psi,
温度1500℃の条件下で焼結させる方法,酸化トリウ
ム等の焼結助剤を添加して水素雰囲気中2000℃以上
で焼成する方法,焼結助剤を添加することなく水素雰囲
気中2200℃以上で焼成する方法等によって製造され
ている。2. Description of the Related Art Yttrium oxide has a cubic crystal structure and has no birefringence. Therefore, even if it is a sintered body,
By removing impurities and pores, a material exhibiting light transmittance equivalent to that of a single crystal can be obtained. Moreover, since the sintered body can be synthesized at a temperature lower than that of the single crystal, it is excellent in economic efficiency,
It is possible to avoid the problem that cracks occur at the structural phase transition point of 2280 ° C. during cooling. The yttrium oxide transparent sintered body was pressed using a hot press at a pressure of 7,000 psi,
A method of sintering at a temperature of 1500 ° C., a method of adding a sintering aid such as thorium oxide and firing at 2000 ° C. or higher in a hydrogen atmosphere, a temperature of 2200 ° C. or higher in a hydrogen atmosphere without adding a sintering aid It is manufactured by a method such as firing in.
【0003】しかし、ホットプレス法は、特別な装置を
必要とし、コスト負担が大きい。しかも、製品の大きさ
や形状に制約がある。焼結助剤を加えた通常焼結法で
は、酸化トリウムが放射性物質であること,10モル%
もの多量添加を必要としているので酸化イットリウム母
体の物性を変化させること,焼成温度が高温であること
等の欠点がある。また、焼結助剤を添加しない通常焼結
法では、焼成温度が更に高いため、多量のエネルギーを
消費し、焼結体の粒径が大きく成長して機械的強度が著
しく低下する欠点がある。However, the hot pressing method requires a special device and is costly. Moreover, there are restrictions on the size and shape of the product. In the normal sintering method with the addition of a sintering aid, thorium oxide is a radioactive substance, 10 mol%
Since it requires the addition of a large amount of substances, there are drawbacks such as changing the physical properties of the yttrium oxide matrix and the firing temperature being high. Further, in the normal sintering method in which the sintering aid is not added, since the firing temperature is higher, a large amount of energy is consumed, the grain size of the sintered body grows large, and the mechanical strength remarkably decreases. .
【0004】酸化イットリウムの焼結にこのような高
温,高圧等の特別な焼成条件が必要とされている主たる
原因は、使用する原料粉末が数μmの凝集粒子を形成し
ていることにある。このような大きな二次粒子が存在
し、粒度分布が広い粉末を用いる場合、成形した圧粉体
中に大きな空孔ができる。そして、その大きな空孔を除
去するため、高温高圧下での焼成が必要になる。従来よ
りも低温焼成で透明焼結体を製造しようとすると、一次
粒子が細かく凝集粒子のない特性の優れた粉末が必要で
あり、そのためには母塩の選択が重要になる。焼結体原
料用酸化イットリウム粉末の製造には、一般に母塩とし
て蓚酸塩が従来から使用されてきている。しかし、細か
な蓚酸塩沈澱物を得ることが困難であるため、仮焼後に
大きな形骸粒子が残り易く、結果として数μm程度の大
きな二次粒子が形成された。また、熱分解が発熱性反応
であるため、通常の仮焼法では温度を厳格に制御し、均
一な粉末を得ることが困難であった。このようなことか
ら、蓚酸塩を母塩にした方法では、特性の優れた粉末が
得られていない。The main reason why special firing conditions such as high temperature and high pressure are required for sintering yttrium oxide is that the raw material powder used forms agglomerated particles of several μm. When powders having such large secondary particles and a wide particle size distribution are used, large voids are formed in the molded green compact. Then, in order to remove the large pores, firing under high temperature and high pressure is required. In order to manufacture a transparent sintered body by firing at a lower temperature than before, it is necessary to use powder having fine primary particles and excellent characteristics without agglomerated particles, and for that purpose, the selection of the mother salt becomes important. In the production of yttrium oxide powder as a raw material for sintered bodies, oxalate has generally been used as a mother salt. However, since it is difficult to obtain a fine oxalate precipitate, large skeleton particles tend to remain after calcination, resulting in the formation of large secondary particles of about several μm. Further, since the thermal decomposition is an exothermic reaction, it is difficult to obtain a uniform powder by strictly controlling the temperature by the usual calcination method. For these reasons, powders having excellent characteristics have not been obtained by the method using oxalate as a mother salt.
【0005】[0005]
【発明が解決しようとする課題】そこで、易焼結性粉末
の合成に適した母塩が求められており、蓚酸塩以外の母
塩から易焼結性粉末を合成する方法が検討されている。
たとえば、アンモニアで中和し、水酸化物を沈澱させる
方法がある。この場合には、硝酸イオンや塩素イオン等
の母液の成分を取り込んだ水酸化物Y2 (OH)5 NO
3 やY2 (OH)5 Clが沈澱する。しかし、これら沈
澱物に含まれる陰イオンは、仮焼時に一次粒子の成長を
促進させたり、二次粒子を作る原因となる。そのため、
細かい均一な粉末が得られにくく、緻密な焼結体ができ
ても空孔が残り、ホットプレス法以外の方法で透明焼結
体を製造することが困難であった。Therefore, a mother salt suitable for synthesizing easily sinterable powder is required, and a method for synthesizing easily sinterable powder from a mother salt other than oxalate is being studied. .
For example, there is a method of neutralizing with ammonia to precipitate hydroxide. In this case, the hydroxide Y 2 (OH) 5 NO incorporating the components of the mother liquor such as nitrate ions and chlorine ions
3 and Y 2 (OH) 5 Cl precipitate. However, the anions contained in these precipitates cause the growth of primary particles during calcination or cause the formation of secondary particles. for that reason,
It was difficult to obtain a fine and uniform powder, and voids remained even if a dense sintered body was formed, making it difficult to manufacture a transparent sintered body by a method other than the hot pressing method.
【0006】尿素やトリクロロ酢酸を用いた均一沈澱法
では、均一な球状沈澱物が生成する。しかし、この球状
沈澱物を仮焼すると、球状の形骸が残り、一次粒子が密
に凝集した集合体の二次粒子になる。このような粉末粒
子を焼結すると、形骸の中での一次粒子の焼結後に二次
粒子相互の焼結が進行し、焼結が不均一になる。その結
果、二次粒子間の空孔が最後まで残存し、透明焼結体を
合成することが困難であった。また、炭酸塩を母塩に使
用した焼結体については、Ceramic Bulle
tin 45(1966)1051に報告されている
が、母塩の合成条件を制御したものでないため、粒子内
に空孔が残った焼結体しか得られていない。このように
従来使用されている母塩からは、一次粒子径が小さく、
凝集粒子のない易焼結性,均一性を備えた原料粉末を合
成することが困難であった。そのため、透明焼結体の製
造に高温・高圧等の特別な焼成条件を採用せざるをえな
かった。本発明は、このような問題を解消すべく案出さ
れたものであり、特定条件下で合成・熟成した炭酸イッ
トリウムを易焼結性粉末の母塩として使用することによ
り、従来よりも低温の通常焼結法を採用でき、微構造が
均一な酸化イットリウム透明焼結体を得ることを目的と
する。The uniform precipitation method using urea or trichloroacetic acid produces a uniform spherical precipitate. However, when this spherical precipitate is calcined, spherical particles remain, and the primary particles become secondary particles of an aggregate in which the primary particles are densely aggregated. When such powder particles are sintered, sintering of the secondary particles progresses after sintering of the primary particles in the skeleton, resulting in non-uniform sintering. As a result, the voids between the secondary particles remained until the end, and it was difficult to synthesize the transparent sintered body. Regarding the sintered body using carbonate as a mother salt, Ceramic Bullet
Tin 45 (1966) 1051 has been reported, but since the conditions for synthesizing the mother salt are not controlled, only a sintered body in which pores remain in the particles is obtained. Thus, from the conventionally used mother salt, the primary particle size is small,
It was difficult to synthesize a raw material powder that is easy to sinter and has no agglomerates. Therefore, special firing conditions such as high temperature and high pressure have to be adopted for the production of the transparent sintered body. The present invention has been devised to solve such a problem, and by using yttrium carbonate synthesized and aged under a specific condition as a mother salt of an easily sinterable powder, a temperature lower than that of a conventional one can be obtained. The purpose of the present invention is to obtain a yttrium oxide transparent sintered body which can adopt a usual sintering method and has a uniform microstructure.
【0007】[0007]
【課題を解決するための手段】本発明の製造方法は、そ
の目的を達成するため、イットリウムの酸性塩水溶液を
炭酸含有塩基性塩水溶液でpH4以上で且つ板状結晶が
生成する値以下に中和して炭酸イットリウムを沈澱さ
せ、次いで50℃以下の温度範囲で撹拌しながら10時
間以上熟成した後、炭酸イットリウムを仮焼して酸化イ
ットリウム粉末とし、該酸化イットリウム粉末を焼成す
ることを特徴とする。熟成後の炭酸イットリウムは、7
00〜1300℃の温度で仮焼することが好ましい。In order to achieve the object of the present invention, in order to achieve the object, the aqueous solution of yttrium acidic salt is adjusted to pH 4 or more with a carbonate-containing basic salt aqueous solution and to a value not more than a value at which plate crystals are formed. And yttrium carbonate to be precipitated, followed by aging for 10 hours or more with stirring in a temperature range of 50 ° C. or lower, and then yttrium carbonate is calcined into yttrium oxide powder, and the yttrium oxide powder is calcined. To do. Yttrium carbonate after aging is 7
It is preferable to perform calcination at a temperature of 00 to 1300 ° C.
【0008】[0008]
【作用】本発明者等は、一次粒子が細かく凝集粒子のな
い焼結用粉末について種々調査・研究した。その結果、
特定条件化で合成,熟成された炭酸イットリウムから得
られた酸化イットリウム粉末が好適であることを見い出
した。すなわち、pH調整によって沈澱させた炭酸イッ
トリウムを適正な条件下で熟成した後、炭酸イットリウ
ムを仮焼して酸化イットリウム粉末にする。この酸化イ
ットリウム粉末を使用すると、従来よりも600〜80
0℃も低い温度での通常焼結法によって焼結助剤を加え
ることなく酸化イットリウム透明焼結体が製造できる。
本発明の酸化イットリウム透明焼結体の製造方法は、生
成条件を制御した炭酸イットリウムを母塩として使用す
る方法である。この炭酸イットリウムは、凝集のない易
焼結性粉末の母塩に求められる(1)仮焼時の凝集粒子
生成の原因となる副生成物が残留しないこと,(2)仮
焼後に形骸が残らないような微細な形状であること等の
要件を満足する。そのため、炭酸イットリウムを仮焼す
ることにより易焼結性の酸化イットリウム粉末が得ら
れ、従来よりも低温での通常焼結法によって酸化イット
リウム透明焼結体が製造できる。The present inventors conducted various investigations and researches on sintering powder having fine primary particles and no agglomerated particles. as a result,
It has been found that yttrium oxide powder obtained from yttrium carbonate synthesized and aged under specific conditions is suitable. That is, yttrium carbonate precipitated by adjusting pH is aged under appropriate conditions, and then yttrium carbonate is calcined to obtain yttrium oxide powder. When this yttrium oxide powder is used, it is 600-80
A yttrium oxide transparent sintered body can be produced without adding a sintering aid by a normal sintering method at a temperature as low as 0 ° C.
The method for producing a yttrium oxide transparent sintered body of the present invention is a method in which yttrium carbonate whose production conditions are controlled is used as a mother salt. This yttrium carbonate is required for the mother salt of the easily sinterable powder without aggregation (1) no by-products that cause the formation of aggregated particles during calcination remain, and (2) skeleton remains after calcination. Satisfies requirements such as a fine shape that does not exist. Therefore, yttrium carbonate powder is calcined to obtain easily sinterable yttrium oxide powder, and the yttrium oxide transparent sintered body can be manufactured by a normal sintering method at a lower temperature than conventional ones.
【0009】[0009]
【実施の形態】炭酸イットリウムの合成には、先ずイッ
トリウムの酸性塩水溶液を炭酸を含む塩基性塩水溶液で
pH4〜8に中和して非晶質の沈澱物を生成する。この
とき、pHが4より低いと沈澱物が生成しない。逆にp
Hが高いと、板状結晶が生成する領域に入り好ましくな
い。pHの上限は、温度によって変化し、20℃ではp
H=7,50℃ではpH=8である。板状結晶は、ミク
ロンサイズの大きな結晶であるため、仮焼後の粉末は形
骸が残った難焼結性粉末となる。その結果、製造された
焼結体は、空孔が残存した低密度のものとなる。原料の
イットリウムの酸性塩としては、塩化物,硝酸塩,硫酸
塩,酢酸塩等の水溶性無機酸塩又は有機酸塩のうち、1
種又は2種以上が使用される。炭酸を含む塩基性塩に
は、炭酸アンモニウム,炭酸ナトリウム,炭酸カリウム
又はそれらの炭酸水素塩等の水溶性炭酸塩の1種又は2
種以上が使用される。BEST MODE FOR CARRYING OUT THE INVENTION In the synthesis of yttrium carbonate, first, an acidic salt aqueous solution of yttrium is neutralized with a basic salt aqueous solution containing carbonic acid to pH 4 to 8 to form an amorphous precipitate. At this time, if the pH is lower than 4, no precipitate is formed. Conversely p
When H is high, it enters the region where plate crystals are generated, which is not preferable. The upper limit of pH changes with temperature, and at 20 ° C,
At H = 7 and 50 ° C., pH = 8. Since the plate-like crystal is a large crystal of micron size, the powder after calcination is a hardly sinterable powder in which a skeleton remains. As a result, the produced sintered body has a low density with voids remaining. As the acid salt of yttrium as a raw material, one of water-soluble inorganic acid salts or organic acid salts such as chlorides, nitrates, sulfates and acetates can be used.
Species or two or more are used. The basic salt containing carbonic acid includes one or two of water-soluble carbonates such as ammonium carbonate, sodium carbonate, potassium carbonate or hydrogen carbonates thereof.
More than one seed is used.
【0010】沈澱を生成した後、適正な条件下で沈澱物
を熟成することが易焼結性粉末を得る上で重要な役割を
果たす。すなわち、初めに生成した沈澱物は非晶質であ
るため、仮焼時に悪影響を及ぼす副生成物を吸蔵し易
い。残留する副生成物は、仮焼後の粉末に不均一性をも
たらす原因となり、透明な焼結体を得ることを困難にす
る。これに対し、熟成すると、非晶質の沈澱物が結晶質
の炭酸イットリウムに変化するので、熟成中の結晶化過
程で、吸蔵されている副生成物が放出される。そのた
め、熟成された炭酸イットリウムを仮焼すると、透明焼
結体の製造に適した凝集のない紛末が得られる。After forming the precipitate, aging the precipitate under appropriate conditions plays an important role in obtaining a sinterable powder. That is, since the precipitate formed initially is amorphous, it is easy to occlude by-products that adversely affect calcining. The residual by-product causes non-uniformity in the powder after calcination, making it difficult to obtain a transparent sintered body. On the other hand, upon aging, the amorphous precipitate changes to crystalline yttrium carbonate, so that the occluded by-product is released during the crystallization process during aging. Therefore, when the aged yttrium carbonate is calcined, agglomerate-free powder suitable for producing a transparent sintered body can be obtained.
【0011】熟成は、50℃以下の温度で行うことが好
ましい。熟成温度が50℃を超えると、結晶性が高く、
大きなサイズの炭酸イットリウム結晶子が生成される。
そのため、仮焼後に形骸粒子が残り、粒径の揃った均一
な粉末が得られない。熟成時間は熟成温度が高いほど短
くできるが、好ましくは10時間以上,より好ましくは
1日以上の時間をかけて熟成される。熟成が不十分であ
ると、非晶質の塩基性沈澱物が残留する。非晶質沈澱物
は、仮焼時に悪影響を及ぼす副生成物を吸蔵し易く、仮
焼後の粉末に不均一性をもたらす原因となり、焼結体の
透光性を低下させる。炭酸イットリウム結晶子の大きさ
や組成は、1日以上熟成しても変化しないので、長時間
の熟成には実質上制約がない。Aging is preferably carried out at a temperature of 50 ° C. or lower. When the aging temperature exceeds 50 ° C, the crystallinity is high,
Large size yttrium carbonate crystallites are produced.
Therefore, skeleton particles remain after calcination, and a uniform powder having a uniform particle size cannot be obtained. The aging time can be shortened as the aging temperature increases, but the aging time is preferably 10 hours or longer, more preferably 1 day or longer. Insufficient aging leaves an amorphous basic precipitate. Amorphous precipitates are likely to occlude by-products that have an adverse effect during calcination, causing non-uniformity in the powder after calcination, and reducing the translucency of the sintered body. Since the size and composition of the yttrium carbonate crystallites do not change even after aging for 1 day or longer, there is virtually no restriction on aging for a long time.
【0012】このようにして得られた炭酸イットリウム
を仮焼すると、一次粒子径が0.01〜0.2μmと微
細で、凝集粒子のない酸化イットリウム粉末が得られ
る。仮焼温度は、700〜1300℃が好ましい。70
0℃より低い温度で仮焼すると、粉末に未分解物が残留
し、焼結が不均一に進む原因となる。また、粒子サイズ
が細かく、充填性が悪い。その結果、緻密で透明な焼結
体が得られない。他方、1300℃を超える高温で仮焼
すると、一次粒子,二次粒子の成長が著しく、不均一な
粉末となる。この場合も、焼結性が低下し、緻密で透明
な焼結体が得られない。この酸化イットリウム粉末を成
形し、1500℃以上の温度で焼成すると、透明な焼結
体が得られる。本発明の方法によるとき、従来よりもか
なり低温の通常焼結法で、添加剤を加えることなく酸化
イットリウム透明焼結体が得られる。When the yttrium carbonate thus obtained is calcined, yttrium oxide powder having a primary particle size of 0.01 to 0.2 μm and no agglomerated particles is obtained. The calcination temperature is preferably 700 to 1300 ° C. 70
If calcined at a temperature lower than 0 ° C., undecomposed matter remains in the powder, which causes uneven sintering. In addition, the particle size is fine and the filling property is poor. As a result, a dense and transparent sintered body cannot be obtained. On the other hand, when calcined at a temperature higher than 1300 ° C., primary particles and secondary particles grow remarkably, and the powder becomes non-uniform. Also in this case, the sinterability is lowered, and a dense and transparent sintered body cannot be obtained. When this yttrium oxide powder is molded and fired at a temperature of 1500 ° C. or higher, a transparent sintered body is obtained. According to the method of the present invention, the yttrium oxide transparent sintered body can be obtained by the ordinary sintering method at a temperature much lower than that of the conventional method, without adding an additive.
【0013】[0013]
実施例1:0.5モル/lの硝酸イットリウム水溶液5
0mlに2.5モル/lの炭酸水素アンモニウム水溶液
20mlを滴下し、pH4.5に調整することにより沈
澱物を生成させた。沈澱物を含むスラリー水溶液を室温
で撹拌しながら、2日間熟成した。その結果、長さ0.
1μm,直径0.02μmの微細な炭酸イットリウムの
針状結晶が得られた。この針状結晶を濾過,洗浄,乾燥
した後、酸素雰囲気中1000℃で4時間仮焼し、酸化
イットリウム粉末を得た。酸化イットリウム粉末は、平
均粒径が0.07μmであった。この酸化イットリウム
粉末を2トン/cm2 の静水圧下で圧粉成形した後、真
空中1600℃で1時間焼成した。得られた焼結体は、
焼結密度がほぼ理論密度に等しい緻密度構造であり、高
い透明度を示した。また、焼結体は、粒径が約5μmと
比較的細かく均一な微構造を示した。比較のため、同じ
条件で生成した沈澱物を熟成することなく、仮焼した。
このときの沈澱物は非晶質で大きさが約0.1μmの無
定形のものであり、仮焼後の粉末は均一性に問題があっ
た。そのため、1700℃で焼成して得られた焼結体
は、相対密度が99%と緻密性に問題はないが、不透明
であった。Example 1: 0.5 mol / l yttrium nitrate aqueous solution 5
20 ml of a 2.5 mol / l ammonium hydrogen carbonate aqueous solution was added dropwise to 0 ml, and the pH was adjusted to 4.5 to form a precipitate. The slurry aqueous solution containing the precipitate was aged for 2 days while stirring at room temperature. As a result, the length 0.
Fine yttrium carbonate needle crystals having a diameter of 1 μm and a diameter of 0.02 μm were obtained. The needle crystals were filtered, washed and dried, and then calcined in an oxygen atmosphere at 1000 ° C. for 4 hours to obtain yttrium oxide powder. The yttrium oxide powder had an average particle size of 0.07 μm. The yttrium oxide powder was compacted under a hydrostatic pressure of 2 ton / cm 2 and then calcined in vacuum at 1600 ° C. for 1 hour. The obtained sintered body is
It had a dense structure with a sintered density almost equal to the theoretical density and showed high transparency. The sintered body had a relatively fine and uniform microstructure with a particle size of about 5 μm. For comparison, the precipitate formed under the same conditions was calcined without aging.
The precipitate at this time was amorphous and had an amorphous size of about 0.1 μm, and the powder after calcination had a problem in uniformity. Therefore, the sintered body obtained by firing at 1700 ° C. was opaque although the relative density was 99% and there was no problem in denseness.
【0014】沈澱物の生成及び熟成温度を70℃とし、
同様に炭酸イットリウムを沈澱させた。得られた沈澱物
は、長さ3μm,直径0.2μmの大きな針状結晶であ
った。この沈澱物を仮焼して得た酸化イットリウム粉末
には形骸粒子が残った。そのため、1700℃で焼成し
たところ、得られた焼結体の相対密度は95%であっ
た。また、滴下する炭酸水素アンモニウム水溶液の量を
50mlにすると、溶液のpHが約7.5で、辺の長さ
が3μmの大きな板状結晶の沈澱物が生成した。仮焼後
の酸化イットリウム粉末には形骸粒子が残った。これを
1700℃で焼成したところ、得られた焼結体の相対密
度は94%であった。他方、市販の炭酸イットリウムを
1100℃で仮焼して得た粉末を1700℃で焼成した
場合には、得られた焼結体の相対密度は92%であっ
た。The formation and aging temperature of the precipitate was 70 ° C.,
Similarly, yttrium carbonate was precipitated. The obtained precipitate was large needle-like crystals with a length of 3 μm and a diameter of 0.2 μm. Formed particles remained in the yttrium oxide powder obtained by calcining this precipitate. Therefore, when fired at 1700 ° C., the relative density of the obtained sintered body was 95%. Further, when the amount of the ammonium hydrogen carbonate aqueous solution added dropwise was 50 ml, a large plate-like crystal precipitate having a pH of the solution of about 7.5 and a side length of 3 μm was formed. Shaped particles remained in the yttrium oxide powder after calcination. When this was fired at 1700 ° C., the relative density of the obtained sintered body was 94%. On the other hand, when the powder obtained by calcining commercially available yttrium carbonate at 1100 ° C. was fired at 1700 ° C., the relative density of the obtained sintered body was 92%.
【0015】実施例2:0.6モル/lの塩化イットリ
ウム水溶液50mlに1.5モル/lの炭酸アンモニウ
ム水溶液20mlを滴下してpH5に調整し、炭酸イッ
トリウムを沈澱させた。沈澱物を室温で撹拌下2日間熟
成し、針状結晶を得た。これを濾過,洗浄,乾燥した
後、酸素雰囲気中1100℃で4時間仮焼し、酸化イッ
トリウム粉末を得た。この酸化イットリウム粉末を2ト
ン/cm2 の静水圧下で圧粉成形した後、真空中160
0℃で1時間焼成した。得られた焼結体は、密度がほぼ
理論密度に等しく、緻密で透明な焼結体であった。Example 2: 20 ml of a 1.5 mol / l ammonium carbonate aqueous solution was added dropwise to 50 ml of a 0.6 mol / l yttrium chloride aqueous solution to adjust the pH to 5 to precipitate yttrium carbonate. The precipitate was aged at room temperature for 2 days with stirring to obtain needle crystals. This was filtered, washed and dried, and then calcined in an oxygen atmosphere at 1100 ° C. for 4 hours to obtain yttrium oxide powder. This yttrium oxide powder was compacted under a hydrostatic pressure of 2 ton / cm 2 and then compacted in vacuum 160
It was baked at 0 ° C. for 1 hour. The obtained sintered body had a density almost equal to the theoretical density and was a dense and transparent sintered body.
【0016】実施例3:0.2モル/lの硝酸イットリ
ウム水溶液200mlに1モル/lの炭酸水素ナトリウ
ム水溶液80mlを滴下してpH5に調整し、炭酸イッ
トリウムを沈澱させた。沈澱物を室温で撹拌下2日間熟
成し、針状結晶を得た。これを濾過,洗浄,乾燥した
後、酸素雰囲気中1000℃で4時間仮焼し、酸化イッ
トリウム粉末を得た。この酸化イットリウム粉末を2ト
ン/cm2 の静水圧下で圧粉成形した後、真空中160
0℃で1時間焼成した。得られた焼結体は、密度がほぼ
理論密度に等しく、緻密で透明な焼結体であった。Example 3: 80 ml of a 1 mol / l sodium hydrogencarbonate aqueous solution was added dropwise to 200 ml of a 0.2 mol / l yttrium nitrate aqueous solution to adjust the pH to 5 to precipitate yttrium carbonate. The precipitate was aged at room temperature for 2 days with stirring to obtain needle crystals. This was filtered, washed, and dried, and then calcined in an oxygen atmosphere at 1000 ° C. for 4 hours to obtain yttrium oxide powder. This yttrium oxide powder was compacted under a hydrostatic pressure of 2 ton / cm 2 and then compacted in vacuum 160
It was baked at 0 ° C. for 1 hour. The obtained sintered body had a density almost equal to the theoretical density and was a dense and transparent sintered body.
【0017】[0017]
【発明の効果】以上に説明したように、本発明において
は、酸性塩水溶液からpH調整によって沈澱させた炭酸
イットリウムを熟成して針状結晶とし、この針状結晶を
仮焼して酸化イットリウム粉末を得ている。この酸化イ
ットリウム粉末は、従来よりも焼結温度が600〜80
0℃低い通常焼結法で理論密度まで焼結でき、粒径が小
さく均一な微構造をもつ透明度の高い焼結体に製造され
る。通常焼結法が採用できるためエネルギーが節減さ
れ、特別な加熱炉を必要としないので製造コストを下げ
ることができる。また、従来法で使用されている蓚酸や
トリウム等の毒物,危険物を使用することなく酸化イッ
トリウムが合成されるため、安全面や環境面においても
問題のない製造法となる。As described above, in the present invention, yttrium carbonate precipitated from an acidic salt aqueous solution by pH adjustment is aged to obtain needle crystals, and the needle crystals are calcined to obtain yttrium oxide powder. Is getting This yttrium oxide powder has a sintering temperature of 600 to 80 as compared with the conventional one.
It can be sintered to a theoretical density by a normal sintering method at 0 ° C., and is manufactured into a highly transparent sintered body having a small grain size and a uniform microstructure. Since the usual sintering method can be adopted, energy can be saved and a special heating furnace is not required, so that the manufacturing cost can be reduced. Further, since yttrium oxide is synthesized without using poisonous substances such as oxalic acid and thorium, which are used in the conventional method, and dangerous substances, the manufacturing method has no problem in terms of safety and environment.
Claims (2)
塩基性塩水溶液でpH4以上で且つ板状結晶が生成する
値以下に中和して炭酸イットリウムを沈澱させ、次いで
50℃以下の温度範囲で撹拌しながら10時間以上熟成
した後、炭酸イットリウムを仮焼して酸化イットリウム
粉末とし、該酸化イットリウム粉末を焼成することを特
徴とする酸化イットリウム透明焼結体の製造方法。1. A yttrium acidic salt aqueous solution is neutralized with a carbonate-containing basic salt aqueous solution to a pH of 4 or more and below a value at which plate crystals are formed to precipitate yttrium carbonate, and then stirred at a temperature range of 50 ° C. or less. A method for producing a transparent yttrium oxide sintered body, which comprises aging the yttrium carbonate for 10 hours or more, calcining the yttrium carbonate to obtain yttrium oxide powder, and firing the yttrium oxide powder.
ムを700〜1300℃で仮焼して酸化イットリウムに
する酸化イットリウム透明焼結体の製造方法。2. A method for producing a yttrium oxide transparent sintered body, which comprises calcining yttrium carbonate after aging at 700 to 1300 ° C. to obtain yttrium oxide.
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JP8156142A JP2843909B2 (en) | 1996-05-27 | 1996-05-27 | Method for producing yttrium oxide transparent sintered body |
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JP8156142A JP2843909B2 (en) | 1996-05-27 | 1996-05-27 | Method for producing yttrium oxide transparent sintered body |
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JPH09315865A true JPH09315865A (en) | 1997-12-09 |
JP2843909B2 JP2843909B2 (en) | 1999-01-06 |
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