JPS63291844A - Production of optical ceramics - Google Patents
Production of optical ceramicsInfo
- Publication number
- JPS63291844A JPS63291844A JP62127206A JP12720687A JPS63291844A JP S63291844 A JPS63291844 A JP S63291844A JP 62127206 A JP62127206 A JP 62127206A JP 12720687 A JP12720687 A JP 12720687A JP S63291844 A JPS63291844 A JP S63291844A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- strontium
- nb2o6
- ceramics
- barium
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 21
- 230000003287 optical effect Effects 0.000 title claims description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000000843 powder Substances 0.000 claims abstract description 49
- 229910052788 barium Inorganic materials 0.000 claims abstract description 27
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 20
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 239000010955 niobium Substances 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 12
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 11
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 11
- WOIHABYNKOEWFG-UHFFFAOYSA-N [Sr].[Ba] Chemical compound [Sr].[Ba] WOIHABYNKOEWFG-UHFFFAOYSA-N 0.000 claims description 10
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 150000002822 niobium compounds Chemical class 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 11
- 238000007731 hot pressing Methods 0.000 abstract description 7
- 229910019695 Nb2O6 Inorganic materials 0.000 abstract description 6
- 230000002776 aggregation Effects 0.000 abstract description 4
- 238000004220 aggregation Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 5
- LCGWNWAVPULFIF-UHFFFAOYSA-N strontium barium(2+) oxygen(2-) Chemical compound [O--].[O--].[Sr++].[Ba++] LCGWNWAVPULFIF-UHFFFAOYSA-N 0.000 description 5
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 4
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 4
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 4
- 238000001513 hot isostatic pressing Methods 0.000 description 4
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 230000001476 alcoholic effect Effects 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910000018 strontium carbonate Inorganic materials 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910000484 niobium oxide Inorganic materials 0.000 description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 150000003437 strontium Chemical class 0.000 description 2
- DKDQMLPMKQLBHQ-UHFFFAOYSA-N strontium;barium(2+);oxido(dioxo)niobium Chemical compound [Sr+2].[Ba+2].[O-][Nb](=O)=O.[O-][Nb](=O)=O.[O-][Nb](=O)=O.[O-][Nb](=O)=O DKDQMLPMKQLBHQ-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DSYGQOJJTJAWKY-UHFFFAOYSA-I [Nb+5].C(C)O.[Cl-].[Cl-].[Cl-].[Cl-].[Cl-] Chemical compound [Nb+5].C(C)O.[Cl-].[Cl-].[Cl-].[Cl-].[Cl-] DSYGQOJJTJAWKY-UHFFFAOYSA-I 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical class [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 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〕
本発明は光学セラミックス、より詳しくは、ニオブ酸ス
トロンチウムバリウム（Ｓｒ、Ｂａ）Ｎｂ、０．セラミ
ックスの製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to optical ceramics, more specifically, strontium barium niobate (Sr, Ba)Nb, 0.00% strontium barium niobate (Sr, Ba)Nb, 0.5% strontium barium niobate (Sr,Ba)Nb, strontium barium niobate, etc. The present invention relates to a method for manufacturing ceramics.
（Ｓｒ、Ｂａ）ＮｂｇＯｓセラミックスはその透光性と
電気光学特性とを有しており、偏光素子、光シャッタ、
画像記憶素子などの光学（オプト）セラミックスとして
広範囲の応用が期待されている。(Sr,Ba)NbgOs ceramics have translucency and electro-optic properties, and can be used as polarizing elements, optical shutters, etc.
It is expected to have a wide range of applications as optical (opto) ceramics such as image storage elements.
光学セラミックスとしての（Ｓｒ、Ｂａ）Ｎｂ、０．は
、代表的には、炭酸ストロンチウム粉末、炭酸バリウム
粉末および酸化ニオブ粉末を混合し、仮焼して得た原料
粉末をホットプレス（ＨＰ）や熱間等圧プレス（ＨＩＰ
）などで焼結することによって製造されている。(Sr, Ba)Nb as optical ceramics, 0. Typically, strontium carbonate powder, barium carbonate powder, and niobium oxide powder are mixed and the raw material powder obtained by calcining is heated by hot pressing (HP) or hot isostatic pressing (HIP).
) is manufactured by sintering.
（Ｓｒ、 Ｂａ） ＮｂｚＯ，セラミックスの構成成分
の原料粉末の中で、炭酸ストロンチウム及び炭酸バリウ
ム原料粉末は極めて凝集し易い。この様な炭酸ストロン
チウム及び炭酸バリウム原料粉末を使用して乾式法で（
Ｓｒ、Ｂａ）ＮｂｚＯｂ原料粉末を作成しても平均粒径
は１〜２μｍ以上のものとなる。この程度の粒度の（Ｓ
ｒ、 Ｂａ） ＮｂｚＯｂ原料粉末を使用しても、高密
度且つ透光性が高く光学的に均一な（Ｓｒ＋ Ｂａ）
ＮｂｚＯｈセラミックスを得ることは難しい。(Sr, Ba) Among raw powders of NbzO and ceramic constituents, strontium carbonate and barium carbonate raw powders are extremely likely to aggregate. Using such raw material powders of strontium carbonate and barium carbonate, dry method (
Even if Sr, Ba)NbzOb raw material powder is prepared, the average particle size will be 1 to 2 μm or more. This level of particle size (S
r, Ba) Even if NbzOb raw material powder is used, high density, high translucency, and optically uniform (Sr + Ba)
NbzOh ceramics are difficult to obtain.
本発明は上記の（Ｓｒ、Ｂａ）ＮｂｔＯｂの乾式法によ
る合成における欠点を解消すべくなされたもので、その
目的は、分散性の良いサブミクロン級の変成酸化ストロ
ンチウム・バリウム原料粉末を作成し、該粉末を用いて
単なる乾式法によって易焼結性且つ高嵩密度の（Ｓｒ＋
Ｂａ） ＮｂｚＯｂ粉末を合成し、更にこの粉末を焼
結して高密度且つ透光性が高く光学的に均一な（Ｓｒ、
Ｂａ） Ｎｂ２Ｏ６セラミックスを製造する方法を提
供することにある。The present invention was made to solve the above-mentioned drawbacks in the dry synthesis of (Sr, Ba)NbtOb, and its purpose is to create a submicron-grade modified strontium/barium oxide raw material powder with good dispersibility, Using this powder, easily sinterable and high bulk density (Sr+
Ba) NbzOb powder is synthesized, and this powder is further sintered to produce a high-density, highly translucent, and optically uniform (Sr,
An object of the present invention is to provide a method for manufacturing Ba) Nb2O6 ceramics.
本発明者らは前記目的を達成すべく鋭意研究の結果、一
般式（Ｓｒ＋−、Ｂａ＋ｔ ）Ｎｂｚ０６． （０，２
＜ ｘ ＜ ０．８ ）で示めされる（ＳｒＢａ） Ｎ
ｂｚＯｉの乾式法による製造過程において、ニオブの適
量とストロンチウム及びバリウムとを含有する混合溶液
を作り、該混合溶液に加水分解反応を行わせることによ
って生成したゾルを乾燥後に、８００〜１４００℃で仮
焼すると、凝集の極めて少ないサブミクロン級の粉末（
変成酸化ストロンチウム・バリウム粉末）と成し得るこ
とが分った。これを原料とし、目的とする（ＳｒＢａ）
Ｎｂ、Ｏ６組成の残りのニオブ化合物を乾式法によって
混合すれば、サブミクロン級の粉末特性の優れた原料粉
末が容易に得られ、これを成形して焼結すると、ＨＰや
ＨＩＰなどの操作を省略しても極めて高密度且つ透光性
が高く光学的に均一な（ＳｒＢａ） ＮｂｚＯａセラミ
ックスが容易に得られることを究明し得た。これらの知
見に基いて本発明を完成した。As a result of intensive research to achieve the above object, the present inventors found that the general formula (Sr+-, Ba+t)Nbz06. (0,2
< x < 0.8 ) (SrBa) N
In the dry manufacturing process of bzOi, a mixed solution containing an appropriate amount of niobium, strontium, and barium is prepared, and the mixed solution is subjected to a hydrolysis reaction. After drying, the sol produced is temporarily heated at 800 to 1400°C. When baked, it becomes a submicron powder with very little agglomeration (
It has been found that this can be achieved with modified strontium/barium oxide powder). Use this as a raw material and use it as a purpose (SrBa)
If the remaining niobium compound with Nb and O6 compositions is mixed by a dry method, a raw material powder with excellent submicron powder properties can be easily obtained, and when this is molded and sintered, it can be easily processed by HP, HIP, etc. It has been found that even if this step is omitted, extremely high density, highly transparent, and optically uniform (SrBa)NbzOa ceramics can be easily obtained. The present invention was completed based on these findings.
本発明の要旨は、（ａ）ニオブ酸ストロンチウムバリウ
ム（（Ｓｒ、Ｂａ）Ｎｂ２Ｏ６〕を構成することになる
ニオブの適量とストロンチウムおよびバリウムとを含有
する混合溶液を作り、加水分解反応を行なってゾルを形
成し、乾燥後に８００〜１４００℃で仮焼する工程、（
ｂ）工程（ａ）で得られた仮焼物と、目的とするニオブ
酸ストロンチウムバリウムの組成の残部を成すニオブ化
合物とを混合し、８００〜１４００℃で仮焼する工程、
および（ｃ）工程（ｂ）で得られた仮焼粉末を成形し、
１１００〜１４００ ’Ｃで焼結してニオブ酸ストロン
チウムバリウム焼結体（セラミックス）を得る工程、か
らなることを特徴とする光学セラミックスの製造方法に
ある。The gist of the present invention is to (a) prepare a mixed solution containing an appropriate amount of niobium and strontium and barium constituting barium strontium niobate ((Sr, Ba)Nb2O6), and perform a hydrolysis reaction to form a sol. A process of forming and calcining at 800 to 1400°C after drying (
b) mixing the calcined product obtained in step (a) with a niobium compound forming the remainder of the composition of the target strontium barium niobate, and calcining at 800 to 1400°C;
and (c) molding the calcined powder obtained in step (b),
A method for producing optical ceramics, comprising the step of sintering at 1100 to 1400'C to obtain a strontium barium niobate sintered body (ceramics).
混合溶液は水溶液又はアルコール溶液であり、ストロン
チウム溶液、バリウム溶液およびニオブ溶液を混合する
のが好ましい。ストロンチウム溶液（水溶液又はアルコ
ール溶液）を作るために、塩化ストロンチウム、硝酸ス
トロンチウム、金属ストロンチウムなどが用いられる。The mixed solution is an aqueous solution or an alcoholic solution, and preferably a strontium solution, a barium solution and a niobium solution are mixed. Strontium chloride, strontium nitrate, strontium metal, etc. are used to make a strontium solution (aqueous or alcoholic).
金属ストロンチウムの場合には、酸の水溶液に溶解させ
ることができる。バリウム溶液（水溶液又はアルコール
溶液）を作るために、塩化バリウム、硝酸バリウム、金
属バリウムなどが用いられる。特に、金属バリウムは酸
の水溶液に溶解させることができる。In the case of metallic strontium, it can be dissolved in an aqueous solution of an acid. Barium chloride, barium nitrate, barium metal, etc. are used to make barium solutions (aqueous or alcoholic solutions). In particular, barium metal can be dissolved in an aqueous solution of an acid.
そして、ニオブ溶液は、代表的には塩化ニオブをアルコ
ールに溶解させるが、酸化ニオブをアルカリ溶液ないし
ＨＦの水溶液に溶解させ、あるいは、金属ニオブを酸の
水溶液に溶解させるなどによっても作れる。これら溶液
を別々に調製するのが望ましいが、同一の溶媒に各化合
物を溶解させて調製してもよい。The niobium solution is typically made by dissolving niobium chloride in alcohol, but it can also be made by dissolving niobium oxide in an alkaline solution or an aqueous HF solution, or dissolving niobium metal in an aqueous acid solution. Although it is desirable to prepare these solutions separately, they may also be prepared by dissolving each compound in the same solvent.
混合溶液には、目的とするニオブ酸ストロンチウムバリ
ウムの組成（Ｓｒ＋−ｘＢａｘ ）ＮｂｚＯｂに対応す
る所定の割合のストロンチウムとバリウムが、適量のニ
オブと共に含有されている。このニオブの量は最終的に
得られる酸化ストロンチウムバリウム粉末の凝集を抑制
し得る範囲が好ましい。The mixed solution contains strontium and barium in a predetermined ratio corresponding to the target composition of barium strontium niobate (Sr+-xBax)NbzOb, along with an appropriate amount of niobium. The amount of niobium is preferably within a range that can suppress agglomeration of the finally obtained strontium barium oxide powder.
加水分解反応は加熱状態で行なわせ、得られたゾルはろ
過および洗浄によって回収される。The hydrolysis reaction is carried out under heating, and the resulting sol is recovered by filtration and washing.
得られたゾルの乾燥物の仮焼温度は、８００〜１４００
℃である。８００℃より低いと凝集が顕著に起り、１４
００℃を超えると粒子が粗大化する傾向がある。仮焼は
大気雰囲気中で行なうことができる。The calcination temperature of the dried sol obtained is 800 to 1400.
It is ℃. At temperatures lower than 800°C, significant aggregation occurs;
When the temperature exceeds 00°C, particles tend to become coarse. Calcination can be carried out in an air atmosphere.
この様にして得られたものに、ニオブの不足分を加えて
混合する。The amount of niobium missing is added to the mixture thus obtained and mixed.
これら混合物の仮焼温度は、ストロンチウムとバリウム
の含有の比率により異なるが、固相反応がほぼまたは完
全に完了する最低温度以上で、顕著な粒子成長が生じな
い最裔温度範囲内であることが必要であり、８００〜１
４００℃の範囲がよい。この仮焼も大気雰囲気中で行な
うことができる。The calcination temperature of these mixtures varies depending on the content ratio of strontium and barium, but it should be at least the minimum temperature at which the solid phase reaction is almost or completely completed, and within the ultimate temperature range at which no significant particle growth occurs. necessary, 800-1
A temperature range of 400°C is preferable. This calcination can also be carried out in an air atmosphere.
この様にして得られた粉末を成形する。焼結温度は前記
の混合物の仮焼温度と同様にストロンチウムとバリウム
の含有の比率によって異なるが、一般に１１００〜１４
００℃の範囲である。１１００℃より低いと焼結が不十
分で高密度が得られず、１４００℃を超えると粒子が粗
大化したり、あるいは構成成分の揮発が起る。焼結酸素
ガス雰囲気下で行なう。The powder thus obtained is molded. The sintering temperature varies depending on the content ratio of strontium and barium as well as the calcination temperature of the mixture described above, but is generally 1100 to 14
It is in the range of 00°C. If it is lower than 1100°C, sintering will be insufficient and high density will not be obtained, and if it exceeds 1400°C, the particles will become coarse or the constituent components will volatilize. Sintering is performed under an oxygen gas atmosphere.
焼結方法は、従来法におけるようにＨＰやＨＩＰである
必要はなく、単純な焼結法によって光学セラミックスと
して優れた特性を有するニオブ酸ストロンチウムバリウ
ム焼結体くセラミックス）を得ることができる。The sintering method does not need to be HP or HIP as in conventional methods, and a strontium barium niobate sintered body (ceramics) having excellent properties as an optical ceramic can be obtained by a simple sintering method.
以下、本発明に係る実施例および比較例によって本発明
の詳細な説明する。Hereinafter, the present invention will be explained in detail using Examples and Comparative Examples according to the present invention.
１施■
硝酸ストロンチウム水溶液（０，７５ｍｏｌ／ ｌ ？
ａ度）１００ｃｃおよび硝酸バリウム水溶液（０，２５
ｍｏｌ／ １． ？３度）ＬＯＯｃｃと、塩化ニオブエ
タノール溶ｔＦＬ （０、４０ｍｏ １／ ｔｉ ？１
度）３００ｃｃとを混合した。この混合溶液を１００℃
で１００時間保持することによって加水分解反応を行い
、Ｓｒ”・Ｂａ”及びＮｂ”を含むゾルを得た。これを
ろ過、洗浄、乾燥した後、１０００℃で４時間仮焼して
、（Ｓｒｏ、 ？５Ｂａｏ、 ｚｓ）Ｎｂ＋、 ｇｏｓ
粉末を作成した。この粉末は、サブミクロン級の粒子で
あった。1 ■ Strontium nitrate aqueous solution (0.75 mol/l?
a degree) 100 cc and barium nitrate aqueous solution (0.25
mol/1. ? 3 degrees) LOOcc and niobium chloride ethanol solution tFL (0, 40mo 1/ti?1
degree) and 300cc were mixed. This mixed solution was heated to 100°C.
A hydrolysis reaction was carried out by holding the sol for 100 hours to obtain a sol containing Sr'', Ba'' and Nb''. After filtering, washing and drying this, it was calcined at 1000°C for 4 hours to form (Sr , ?5Bao, zs)Nb+, gos
A powder was created. This powder had submicron particles.
この得られた粉末１３７．７７ｇと市販のＮｂｚＯｓ粉
末５３．１６４ｇとをボールミルで一昼夜混合した後、
１１００℃で４時間仮焼して、（Ｓｒｏ、 ｔｓＢａｏ
、 ｚｓ）Ｎｂｚ０６粉末を得た。この平均粒径は０．
５３μｍであった。After mixing 137.77 g of the obtained powder and 53.164 g of commercially available NbzOs powder in a ball mill overnight,
Calcined at 1100℃ for 4 hours, (Sro, tsBao
, zs) Nbz06 powder was obtained. This average particle size is 0.
It was 53 μm.
この粉末を１ｔｏｎ／ａａで成形したタブレットを、酸
素ガス雰囲気下、１３５０℃で４時間焼結した。得られ
た（Ｓｒｏ、 ｔｓＢａｏ、 ｚｓ）ＮｂｚＯａセラミ
ックスの密度は、５．３２ｇ／−で理論密度に極めて近
い値であつた。また透光率は、厚さ０．２Ｈの試料で５
０ｏｎ−の波長で、６８％であった。A tablet formed by molding this powder at 1 ton/aa was sintered at 1350° C. for 4 hours in an oxygen gas atmosphere. The density of the obtained (Sro, tsBao, zs)NbzOa ceramics was 5.32 g/-, which was extremely close to the theoretical density. In addition, the light transmittance is 5 for a sample with a thickness of 0.2H.
At a wavelength of 0on-, it was 68%.
北較皿
市販の、５ｒＣ０３粉末、ＢａＣ０１粉末およびＮｂｇ
Ｏｓ粉末を、（Ｓｒｏ、 ｔｓＢａｏ、 ｚｓ）Ｎｂｚ
Ｏｂの組成になる様に配合し、ボールミルで一昼夜混合
した後、１１００℃で４時間仮焼した。この仮焼粉末を
１ｔｏｎ／−で成形したタブレフトを、酸素ガス雰囲気
下、１３５０℃で４時間焼結した。得られた焼結体（セ
ラミックス）の密度は、５．０８ｇ／ｃｄであった。5rC03 powder, BaC01 powder and Nbg commercially available from Hokkaidara
Os powder, (Sro, tsBao, zs)Nbz
After mixing in a ball mill all day and night, the mixture was calcined at 1100° C. for 4 hours. A table left formed by molding this calcined powder at 1 ton/- was sintered at 1350° C. for 4 hours in an oxygen gas atmosphere. The density of the obtained sintered body (ceramics) was 5.08 g/cd.
また透光率は、厚さ０．２ ｙｎの試料で５０Ｏｒ＋＋
＋＋の波長で１７％であった。In addition, the light transmittance is 50 Or++ for a sample with a thickness of 0.2 yn.
It was 17% at ++ wavelength.
尚、仮焼して得られた粉末は、大きな凝集体から成り、
平均粒径は特定できなかった。In addition, the powder obtained by calcining consists of large aggregates,
The average particle size could not be determined.
本発明の方法によると、加水分解を利用した湿式法によ
る（Ｓｒ、Ｂａ） Ｎｂｚｏ＆の構成成分のニオブを含
む酸化ストロンチウムバリウム粉末（変成酸化ストロン
チウムバリウム粉末）は、二次粒子の極めて少ないサブ
ミクロン粒子となし得、これを使用することによって、
以後単なる乾式法によって、容易にサブミクロン級の（
Ｓｒ＋ Ｂａ） ＮｂｇＯｉ原料粉末が得られ、更にこ
れを原料として透光性が良く高密度の（Ｓｒ、Ｂａ）Ｎ
ｂｚＯａセラミックスが得られる、という優れた効果が
奏せられる。そのほか次のような効果も奏される。According to the method of the present invention, strontium barium oxide powder (modified strontium barium oxide powder) containing niobium, which is a component of (Sr, Ba) Nbzo&, produced by a wet method using hydrolysis, has submicron particles with extremely few secondary particles. By using this,
After that, by a simple dry method, it was easy to obtain submicron (
Sr+Ba)NbgOi raw material powder is obtained, and this is further used as a raw material to produce (Sr,Ba)N with good translucency and high density.
The excellent effect of obtaining bzOa ceramics can be achieved. In addition, the following effects are also produced.
（１）仮焼によって得られる変成酸化ストロンチウム・
バリウム粉末が十分分散されたものが得られるため、仮
焼物の粉砕工程を特に必要としないで、原料粉末として
供給し得られる。(1) Modified strontium oxide obtained by calcination.
Since a sufficiently dispersed barium powder is obtained, the calcined product can be supplied as a raw material powder without the need for a particular pulverizing process.
（２）該仮焼変成酸化ストロンチウムバリウム粉末から
乾式法で得られる（ＳｒＢａ）ＮｂｚＯｉ粉末も単分散
状態で得られ、従って粉砕工程を除いても十分易焼結性
且つ高密度の特性を有する。(2) The (SrBa)NbzOi powder obtained from the calcined modified strontium barium oxide powder by a dry method is also obtained in a monodisperse state, and therefore has characteristics of sufficiently easy sinterability and high density even without the pulverization step.
（３）極めて高密度且つ光学的高均一性を要求される光
学エレクトロニクス用（Ｓｒ、 Ｂａ） ＮｂｇＯａセ
ラミックスをＨＰやＨＩＰなどの操作を省略して単なる
固相焼結によって、理論密度に極めて近い高密度且つ光
学的高均一・高透光率で得ることができる。(3) For optical electronics applications that require extremely high density and high optical uniformity (Sr, Ba) NbgOa ceramics can be produced with high density extremely close to the theoretical density by simple solid phase sintering without operations such as HP or HIP. It can be obtained with high density, high optical uniformity, and high light transmittance.
（４）優れた粉末特性を有する変成、酸化ストロンチウ
ムバリウム粉末を大量生産することによって、任意の組
成の（Ｓｒ、Ｂａ）ＮｂｚＯａを極めて安価に供給し得
る。(4) By mass producing modified strontium barium oxide powder with excellent powder properties, (Sr,Ba)NbzOa of any composition can be supplied at extremely low cost.
Claims (1)
Ｂａ）Ｎｂ＿２Ｏ＿６〕を構成することになるニオブの
適量とストロンチウムおよびバリウムとを含有する混合
溶液を作り、加水分解反応を行なってゾルを形成し、乾
燥後に８００〜１４００℃で仮焼する工程、（ｂ）工程
（ａ）で得られた仮焼物と、目的とするニオブ酸ストロ
ンチウムバリウムの組成の残部を成すニオブ化合物とを
混合し、８００〜１４００℃で仮焼する工程、および （ｃ）工程（ｂ）で得られた仮焼粉末を成形し、１１０
０〜１４００℃で焼結してニオブ酸ストロンチウムバリ
ウム焼結体を得る工程、からなることを特徴とする光学
セラミックスの製造方法。[Claims] 1. (a) Strontium barium niobate [(Sr,
A step of preparing a mixed solution containing an appropriate amount of niobium, strontium and barium, which will constitute niobium (Ba)Nb_2O_6], performing a hydrolysis reaction to form a sol, and calcining it at 800 to 1400°C after drying. b) A step of mixing the calcined product obtained in step (a) and a niobium compound forming the remainder of the composition of the target strontium barium niobate, and calcining at 800 to 1400 ° C., and (c) step ( The calcined powder obtained in b) was molded and heated to 110
A method for producing optical ceramics, comprising the step of sintering at 0 to 1400°C to obtain a strontium barium niobate sintered body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62127206A JPS63291844A (en) | 1987-05-26 | 1987-05-26 | Production of optical ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62127206A JPS63291844A (en) | 1987-05-26 | 1987-05-26 | Production of optical ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63291844A true JPS63291844A (en) | 1988-11-29 |
Family
ID=14954347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62127206A Pending JPS63291844A (en) | 1987-05-26 | 1987-05-26 | Production of optical ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63291844A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7674738B2 (en) | 2006-05-31 | 2010-03-09 | Murata Manufacturing Co., Ltd. | Translucent ceramic and electro-optical component |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS538606A (en) * | 1976-07-14 | 1978-01-26 | Tokyo Shibaura Electric Co | Light permeable ceramic materials |
| JPS5510449A (en) * | 1978-07-07 | 1980-01-24 | Nippon Electric Co | Oxide permittivity material |
| JPS6153114A (en) * | 1984-08-18 | 1986-03-17 | Natl Inst For Res In Inorg Mater | Production of powdery raw material of easily sintering perovskite solid solution |
| JPS61186219A (en) * | 1985-02-13 | 1986-08-19 | Natl Inst For Res In Inorg Mater | Production of lead-containing fine powder |
| JPS61186223A (en) * | 1985-02-13 | 1986-08-19 | Natl Inst For Res In Inorg Mater | Production of fine powder of dielectric material |
-
1987
- 1987-05-26 JP JP62127206A patent/JPS63291844A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS538606A (en) * | 1976-07-14 | 1978-01-26 | Tokyo Shibaura Electric Co | Light permeable ceramic materials |
| JPS5510449A (en) * | 1978-07-07 | 1980-01-24 | Nippon Electric Co | Oxide permittivity material |
| JPS6153114A (en) * | 1984-08-18 | 1986-03-17 | Natl Inst For Res In Inorg Mater | Production of powdery raw material of easily sintering perovskite solid solution |
| JPS61186219A (en) * | 1985-02-13 | 1986-08-19 | Natl Inst For Res In Inorg Mater | Production of lead-containing fine powder |
| JPS61186223A (en) * | 1985-02-13 | 1986-08-19 | Natl Inst For Res In Inorg Mater | Production of fine powder of dielectric material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7674738B2 (en) | 2006-05-31 | 2010-03-09 | Murata Manufacturing Co., Ltd. | Translucent ceramic and electro-optical component |
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