JPH02145498A - Production of barium titanate single crystal - Google Patents
Production of barium titanate single crystalInfo
- Publication number
- JPH02145498A JPH02145498A JP29784488A JP29784488A JPH02145498A JP H02145498 A JPH02145498 A JP H02145498A JP 29784488 A JP29784488 A JP 29784488A JP 29784488 A JP29784488 A JP 29784488A JP H02145498 A JPH02145498 A JP H02145498A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- barium titanate
- raw material
- mixed
- oxide
- 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
- 239000013078 crystal Substances 0.000 title claims abstract description 25
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 24
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000010304 firing Methods 0.000 claims description 2
- 229910018663 Mn O Inorganic materials 0.000 claims 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract description 4
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- 230000000996 additive effect Effects 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract 1
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 abstract 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はチタン酸バリウム（ＢａＴｔＯ＋）単結晶の製
造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing a barium titanate (BaTtO+) single crystal.
チタン酸バリウムセラミックスは、誘電体材料や焦電体
材料として電子工業の分野で広く利用されている。Barium titanate ceramics are widely used in the electronic industry as dielectric materials and pyroelectric materials.
チタン酸バリウムセラミックスは、チタン酸バリウムの
微粉末を成形・焼結させて得られた多結晶体であるが、
セラミックスに比べて単結晶は結晶方位が一定方向にそ
ろっているため、一般に性能指数が高い。チタン酸バリ
ウムにおいても、セラミックスの形態で利用するよりも
単結晶の形態で利用した方が誘電率や焦電係数を高くす
ることができる。Barium titanate ceramics are polycrystalline materials obtained by molding and sintering fine barium titanate powder.
Compared to ceramics, single crystals generally have a higher figure of merit because their crystal orientation is aligned in a certain direction. Barium titanate also has a higher dielectric constant and pyroelectric coefficient when used in single crystal form than in ceramic form.
従来より知られているチタン酸バリウム単結晶の製造方
法としては、ＫＦ、 ＮａｚＣＯ３，ＫＣｌまたはＢａ
ＣＩ！、□などの溶剤を用いた溶液法がある。即ち、チ
タン酸バリウム原料に上記の溶剤を添加し、るつぼ内で
溶融した後、１〜２日間冷却してチタン酸バリウム単結
晶を育成させ、その後、同時に固化した溶剤を酸性溶液
などで溶解させて除去し、チタン酸バリウム単結晶を取
り出す方法である。Conventionally known methods for producing barium titanate single crystals include KF, NazCO3, KCl or Ba
CI! There are solution methods using solvents such as , □. That is, the above-mentioned solvent is added to the barium titanate raw material, melted in a crucible, cooled for 1 to 2 days to grow a barium titanate single crystal, and then, at the same time, the solidified solvent is dissolved in an acidic solution or the like. In this method, the barium titanate single crystal is extracted.
しかしながら、上述の製造方法の場合には、チタン酸バ
リウムセラミックスを製造する方法に比べて操作が複雑
で、長時間を必要とし、また得られた単結晶の品質も安
定させ難いため、工業的には利用されていない。However, in the case of the above-mentioned manufacturing method, compared to the method of manufacturing barium titanate ceramics, the operation is complicated and requires a long time, and the quality of the obtained single crystal is difficult to stabilize, so it is not suitable for industrial use. is not used.
そこで、本発明の目的は、工業的に利用可能なチタン酸
バリウム単結晶の製造方法を提供することにある。Therefore, an object of the present invention is to provide an industrially usable method for producing a barium titanate single crystal.
上記目的を達成するために、本発明のチタン酸バリウム
単結晶の製造方法は、チタン酸バリウム”原料１００モ
ルに対し、ＭｇＯ＋ ＭｎＯ，ＮｉＯ＋ Ｃ０ＪｉＦｅ
ｚ０３． Ｃｒ２Ｏ３又はＺｎＯのうち少なくとも１種
類をその合計量が０．２５〜１．５モルになるように添
加し混合する工程と、該混合された原料を圧密体に成形
する工程と、該圧密体を焼成する工程とを含むものであ
る。In order to achieve the above object, the method for producing a barium titanate single crystal of the present invention is based on a method for producing a barium titanate single crystal of MgO+ MnO, NiO+ C0JiFe for 100 mol of barium titanate raw material.
z03. A step of adding and mixing at least one kind of Cr2O3 or ZnO in a total amount of 0.25 to 1.5 moles, a step of forming the mixed raw material into a compacted body, and a step of forming the compacted body. This includes a step of firing.
即ち、チタン酸バリウム原料に微量の添加物を加えるこ
とにより、従来のセラミックスと同様の製造方法によっ
て単結晶を得ることができる。添加物の量を０．２５〜
１．５モルの範囲に限定１した理由は、添加量がこの範
囲外になると、圧密体を焼成しても育成される単結晶が
微細であり、セラミックスと同様となるからである。That is, by adding a small amount of additives to the barium titanate raw material, a single crystal can be obtained by the same manufacturing method as conventional ceramics. Adjust the amount of additives from 0.25 to
The reason for limiting the amount to 1.5 mol is that if the amount added is outside this range, even if the compact is fired, the single crystal grown will be fine and similar to ceramics.
（実施例〕
、本発明にか、かるチタン酸バリウム単結晶の具体的製
造方法を説明する。(Example) A specific method for producing a barium titanate single crystal according to the present invention will be described.
まず、純度９９．９５％以上のＢａＣＯ３およびＴｉＯ
２をＢａＴｉＯ３となるように調合し、ＢａＴｉ０＋原
料１００モルに対して、ＭｇＯ＋ ＭｎＯ＋ Ｎｉｐ、
ＣＯ２Ｏ３，Ｆｅ、０３． Ｃｒ２Ｏ３又はＺｎＯの
うち少なくとも１種類をその合計量が０．２５〜１．５
モルになるように、純度９９．５％以上の酸化物、炭酸
塩又は塩化物の形で添加し、メノウボールを用いたポリ
ポットミル中で混合した後、１１００°Ｃで３時間仮焼
した。得られた仮焼粉を２５００ｋｇｆ／ｃｍ２の圧力
で成形し、直径１０ｍｍ、厚さ１■の大きさの圧密体を
得た。この圧密体をＳｉＣを発熱体とする電気炉中で１
４００〜１４５０°Ｃで焼成した。なお、昇温速度及び
降温速度は５０〜５００°Ｃ／ｈの範囲に設定した。そ
して、得られた焼成物を反射顕微鏡で観察し、結晶の大
きさを測定した。First, BaCO3 and TiO with a purity of 99.95% or more
2 to become BaTiO3, and for 100 mol of BaTi0+ raw material, MgO+ MnO+ Nip,
CO2O3,Fe,03. The total amount of at least one of Cr2O3 or ZnO is 0.25 to 1.5
The mixture was added in the form of an oxide, carbonate, or chloride with a purity of 99.5% or more so as to have a molar amount, mixed in a polypot mill using an agate ball, and then calcined at 1100°C for 3 hours. The obtained calcined powder was molded at a pressure of 2500 kgf/cm2 to obtain a compacted body with a diameter of 10 mm and a thickness of 1 square inch. This compacted body was placed in an electric furnace using SiC as a heating element.
It was fired at 400-1450°C. Note that the temperature increase rate and temperature decrease rate were set in the range of 50 to 500°C/h. Then, the obtained fired product was observed with a reflection microscope, and the size of the crystals was measured.
測定の結果、ＭｇＯ＋ ＭｎＯ，Ｎｌ０１． ＣＯ２０
３１ＦｅＪｉ＋Ｃｒ、０３又はＺｎＯのうち少なくとも
１種類を合計量０．２５〜１．５モル添加した場合、に
は、１ｍ＋ｙ３以上の大きさの単結晶が再現性よく育成
され、最大のものは圧密体焼成物の全ての部分が１つの
単結晶（約５０ｍｍ’ ）となった。一方、上述の酸化
物の添加量が０．２５〜１．５モルの範囲から外れると
、圧密体焼成物は１．ｍｍ３未満の単結晶粒子の集合体
からなるセラミックスとなった。As a result of the measurement, MgO+ MnO, Nl01. CO20
When a total amount of 0.25 to 1.5 mol of at least one of 31FeJi+Cr, 03, or ZnO is added, single crystals with a size of 1 m+y3 or more are grown with good reproducibility, and the largest one is sintered as a compact. All parts of the object became one single crystal (approximately 50 mm'). On the other hand, if the amount of the above-mentioned oxide added is out of the range of 0.25 to 1.5 moles, the fired compacted product will be 1.5 to 1.5 moles. The result was a ceramic consisting of an aggregate of single-crystal particles of less than mm3.
以上の説明で明らかなように、本発明によればチタン酸
バリウム原料１００モルに対し、ＭｇＯ，ＭｎＯ。As is clear from the above description, according to the present invention, MgO and MnO are used for 100 moles of barium titanate raw material.
Ｎｉｐ、 Ｃｏ２Ｏ３，ＦｅｚＯ３，Ｃｒ２Ｏ２又はＺ
ｎＯのうち少なくとも１種類をその合計量が０．２５〜
１．５モルになるように添加し、添加された原料を圧密
体に成形した後、焼成することにより単結晶を製造する
ようにしたので、セラミックスと同様の製造方法によっ
て単結晶を得ることができる。つまり、従来の溶液法に
比べて操作が簡単で、短時間に製造でき、しかも得られ
た単結晶の品質を安定させやすいため、工業的に利用可
能性の高い製造方法を実現できる。Nip, Co2O3, FezO3, Cr2O2 or Z
The total amount of at least one type of nO is 0.25~
Since the added raw material was added to a concentration of 1.5 mol and formed into a compact and then fired to produce a single crystal, it was possible to obtain a single crystal using the same manufacturing method as ceramics. can. In other words, compared to the conventional solution method, the operation is simpler, the production can be completed in a shorter time, and the quality of the obtained single crystal is more easily stabilized, making it possible to realize a production method with high industrial applicability.
Claims (1)
Ｏ、ＮｉＯ、Ｃｏ＿２Ｏ＿３、Ｆｅ＿２Ｏ＿３、Ｃｒ＿
２Ｏ＿３又はＺｎＯのうち少なくとも１種類をその合計
量が０．２５〜１．５モルになるように添加し混合する
工程と、該混合された原料を圧密体に成形する工程と、
該圧密体を焼成する工程とを含むチタン酸バリウム単結
晶の製造方法。For 100 mol of barium titanate raw material, MgO, Mn
O, NiO, Co_2O_3, Fe_2O_3, Cr_
A step of adding and mixing at least one type of 2O_3 or ZnO so that the total amount is 0.25 to 1.5 mol, and a step of forming the mixed raw material into a compacted body,
A method for producing a barium titanate single crystal, comprising the step of firing the compacted body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29784488A JPH02145498A (en) | 1988-11-25 | 1988-11-25 | Production of barium titanate single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29784488A JPH02145498A (en) | 1988-11-25 | 1988-11-25 | Production of barium titanate single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02145498A true JPH02145498A (en) | 1990-06-04 |
Family
ID=17851882
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29784488A Pending JPH02145498A (en) | 1988-11-25 | 1988-11-25 | Production of barium titanate single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02145498A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0536999A3 (en) * | 1991-10-08 | 1994-03-02 | Fujikura Ltd |
-
1988
- 1988-11-25 JP JP29784488A patent/JPH02145498A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0536999A3 (en) * | 1991-10-08 | 1994-03-02 | Fujikura Ltd | |
| US5366583A (en) * | 1991-10-08 | 1994-11-22 | Fujikura Ltd. | Process for preparing barium titanate single crystals |
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