JPH0478596B2 - - Google Patents
Info
- Publication number
- JPH0478596B2 JPH0478596B2 JP32178388A JP32178388A JPH0478596B2 JP H0478596 B2 JPH0478596 B2 JP H0478596B2 JP 32178388 A JP32178388 A JP 32178388A JP 32178388 A JP32178388 A JP 32178388A JP H0478596 B2 JPH0478596 B2 JP H0478596B2
- Authority
- JP
- Japan
- Prior art keywords
- mol
- melt
- single crystal
- pbtio
- lead titanate
- 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.)
- Expired
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- 239000013078 crystal Substances 0.000 claims description 51
- 239000000155 melt Substances 0.000 claims description 17
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 11
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052810 boron oxide Inorganic materials 0.000 claims description 9
- 229910000464 lead oxide Inorganic materials 0.000 claims description 9
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- 239000013081 microcrystal Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 229910010413 TiO 2 Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 5
- 239000008710 crystal-8 Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000002050 diffraction method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007716 flux method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910008651 TiZr Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000000048 melt cooling Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、酸化ホウ素と酸化鉛と酸化チタン
とを融解した融液から種子結晶を引き上げること
によりチタン酸鉛の単結晶を得るチタン酸鉛単結
晶の製造方法に関するものである。[Detailed Description of the Invention] [Industrial Application Field] This invention relates to lead titanate, in which a single crystal of lead titanate is obtained by pulling up a seed crystal from a melt of boron oxide, lead oxide, and titanium oxide. This invention relates to a method for producing a single crystal.
PbTio3（チタン酸鉛）は128℃という高温で融
解するために有毒なPbo（酸化鉛）の蒸発が激し
く、融解した後直接単結晶を育成することが困難
なため、結晶育成温度を低くする工夫が必要とな
る。そのため、溶剤を用いたフラツクス法が多数
研究されている。
Because PbTio 3 (lead titanate) melts at a high temperature of 128℃, toxic Pbo (lead oxide) evaporates rapidly, making it difficult to grow a single crystal directly after melting, so the crystal growth temperature is lowered. Some ingenuity is required. Therefore, many flux methods using solvents have been studied.
また、本発明者は先にPbTio3の大型単結晶の
製造方法を提案した。この方法はPbTio3の構成
物質である過剰のPboを溶剤とした溶液引き上げ
法であり、Pboが88〜75.0モル％、TiO2（酸化チ
タン）が12〜25.0モル％の組成の混合融液１〜５
℃／ｈで徐冷しながら析出してくるPbTio3微結
晶を種子結晶に育成させながら0.2〜１mm／ｈの
引き上げ速度で引き上げて行く方法である。上記
の製造方法によると直径14×14×６mmの大きさで
7gの重さの大型単結晶を育成することができた。 Furthermore, the present inventor previously proposed a method for producing a large single crystal of PbTio 3 . This method is a solution pulling method using excess Pbo, which is a constituent of PbTio 3 , as a solvent, and a mixed melt 1 with a composition of 88 to 75.0 mol% Pbo and 12 to 25.0 mol% TiO 2 (titanium oxide) is used. ~5
This is a method in which the precipitated PbTio 3 microcrystals are grown into seed crystals while being slowly cooled at a rate of 0.2 to 1 mm/h while being pulled up at a pulling rate of 0.2 to 1 mm/h. According to the above manufacturing method, the size is 14 x 14 x 6 mm in diameter.
We were able to grow a large single crystal weighing 7g.
ところで、PboとB2O3（酸化ホウ素）を溶剤と
したフラツクス法では、15mm角、厚さ１mmぐらい
の大きさの単結晶の育成が可能であると報告され
ているにすぎない［Soviet Physics−
Crystallography vol.17、No.１ July−Aug.、
P.122〜125、1972］。さらに、これらの方法では、
単結晶を溶剤から分離するのに硝酸等の液に浸さ
なければならないという不都合な点があるという
問題点があつた。
By the way, it has only been reported that the flux method using Pbo and B 2 O 3 (boron oxide) as a solvent can grow a single crystal with a size of about 15 mm square and 1 mm thick [Soviet Physics −
Crystallography vol.17, No.1 July-Aug.
P.122-125, 1972]. Furthermore, these methods
There was a problem in that the single crystal had to be immersed in a liquid such as nitric acid to separate it from the solvent.
また、先に提案したPbTio3の大型単結晶の製
造方法では、単結晶の色が黄褐色をしており、光
学結晶として使用するためには十分ではないとい
う問題点があつた。 Furthermore, in the previously proposed method for producing large single crystals of PbTio 3 , there was a problem in that the single crystals were yellowish-brown in color and were not suitable for use as optical crystals.
この発明は、上記の問題点を解決するためにな
されたもので、種子結晶によつて望みの方向に大
型の黄色透明のPbTio3単結晶が製造できる方法
を得ることを目的とする。 The present invention was made to solve the above-mentioned problems, and aims to provide a method by which large, yellow transparent PbTio 3 single crystals can be produced in a desired direction using seed crystals.
この発明に係るチタン酸鉛単結晶の製造方法
は、酸化ホウ素と酸化鉛を配合してなる溶剤に酸
化チタンを溶剤に対する飽和濃度以上の割合、す
なわち三成分において酸化鉛が45〜85モル％、酸
化ホウ素が0.1〜45モル％、酸化チタンが１〜40
モル％の組成範囲で混合し、高温度に加熱して全
体を融解したのち、その融液を徐々に冷却するこ
とにより融液中に析出してくるチタン酸鉛微結晶
を融液に接触させた種子結晶上に結晶化させ、こ
れを育成させながら引き上げるものである。
The method for producing a lead titanate single crystal according to the present invention includes adding titanium oxide to a solvent containing boron oxide and lead oxide in a proportion equal to or higher than the saturation concentration of the solvent, that is, in the three components, lead oxide is 45 to 85 mol %, Boron oxide: 0.1 to 45 mol%, titanium oxide: 1 to 40 mol%
After mixing in a composition range of mol% and heating to high temperature to melt the whole, the melt is gradually cooled to bring the precipitated lead titanate microcrystals into contact with the melt. The method is to crystallize on seed crystals and pull them out while growing them.
また、チタン酸鉛の大型単結晶を得る組成範囲
として酸化鉛が45〜70モル％、酸化ホウ素が15〜
45モル％、酸化チタンが５〜20モル％にしたもの
である。 In addition, the composition range for obtaining large single crystals of lead titanate is 45 to 70 mol% lead oxide and 15 to 70 mol% boron oxide.
45 mol%, titanium oxide 5 to 20 mol%.
この発明においては、結晶育成終了後は
PbTio3単結晶を融液から離して室温まで徐冷し
ていくと、黄色透明の大型単結晶を単結晶と溶剤
の分離操作なしに直接得られる。
In this invention, after the crystal growth is completed,
When the PbTio 3 single crystal is separated from the melt and slowly cooled to room temperature, a large transparent yellow single crystal can be obtained directly without the need for separating the single crystal and the solvent.
また、Pbo、B2O3、TiO2の成分を小範囲に限
定することにより、さらに大型のPbTio3単結晶
が得られる。 Further, by limiting the components of Pbo, B 2 O 3 and TiO 2 to a small range, an even larger PbTio 3 single crystal can be obtained.
まず、この発明の原理について説明する。Pbo
とB2O3からなる溶剤にPboとTiO2が１対１の割
合からなる化合物PbTio3をこの溶剤に対して過
飽和濃度以上の割合で混合し、加熱融解する。そ
の後、この混合融液を徐々に冷却していくと過飽
和になつた分のPbTio3が結晶となつて析出して
くる。この過飽和になつて析出してくる微結晶を
同じPbTio3種子結晶上に析出せしめ、それを育
成させて引き上げる。
First, the principle of this invention will be explained. Pbo
PbTio 3, a compound consisting of Pbo and TiO 2 in a 1:1 ratio, is mixed with a solvent consisting of B 2 O 3 and B 2 O 3 at a ratio greater than the supersaturation concentration with respect to the solvent, and the mixture is heated and melted. Thereafter, when this mixed melt is gradually cooled, the supersaturated amount of PbTio 3 crystallizes and precipitates. The supersaturated microcrystals are deposited on the same PbTio 3 seed crystal, grown, and pulled up.
第１図はこの発明の原理を説明するためのPbo
−TiO2−B2O3系の相平衡図で、この図の黒い太
線で囲んだ部分Ａが、Pboが45〜85モル％、B2
O3が0.1〜45モル％、TiO2が１〜40モル％の組成
範囲であつて、上述した文献［Soviet Physics−
Crystallography］にも示されており、この発明
の成立領域でもある。そして、メツシユの部分Ｂ
がこの発明の最適の範囲を示すもので、Pboが45
〜70モル％、B2O3が15〜45モル％、TiO2が５〜
20モル％の組成範囲である。 Figure 1 shows Pbo to explain the principle of this invention.
In the phase equilibrium diagram of the -TiO 2 -B 2 O 3 system, the part A surrounded by the thick black line in this diagram is 45 to 85 mol% Pbo and B 2
The composition range is 0.1 to 45 mol% of O 3 and 1 to 40 mol% of TiO 2 , as described in the above-mentioned literature [Soviet Physics-
Crystallography], which is also the field in which this invention was made. And the mesh part B
indicates the optimum range of this invention, and Pbo is 45
~70 mol%, B2O3 15-45 mol%, TiO2 5~
The composition range is 20 mol%.
第２図はこの発明を実施するためのPbTio3単
結晶の製造装置の構成図である。なお、この製造
装置は有毒のPbo蒸気を製造者から隔離するため
の結晶育成観察窓付の容器に入つている。第２図
において、１は水冷シヤフト、２は白金シヤフ
ト、３は保温材、４は高周波加熱コイル、５は熱
電対、６はるつぼ支持物、７は種子結晶、８は
PbTio3単結晶、９は出発原料、１０は白金るつ
ぼである。 FIG. 2 is a block diagram of a PbTio 3 single crystal production apparatus for carrying out the present invention. This production equipment is housed in a container with a crystal growth observation window to isolate toxic Pbo vapor from the manufacturer. In Fig. 2, 1 is a water cooling shaft, 2 is a platinum shaft, 3 is a heat insulating material, 4 is a high frequency heating coil, 5 is a thermocouple, 6 is a crucible support, 7 is a seed crystal, and 8 is a
PbTio 3 single crystal, 9 is a starting material, and 10 is a platinum crucible.
〔実施例 １〕
次にこの発明によるチタン酸鉛単結晶の製造方
法について説明する。[Example 1] Next, a method for producing a lead titanate single crystal according to the present invention will be described.
出発原料９は、一例としてPboを55モル％、
TiO2を15モル％、B2O3を30モル％の組成に混合
し（第１図のＰ点）、第２図に示す口径55mm、高
さ40mmの発熱体を兼ねた白金るつぼ１０に入れ、
高周波加熱コイル４による誘導加熱方式により〜
900℃まで加熱して融解させた後、PbTio3単結晶
からなる種子結晶７を融液表面に接触させる。融
液を徐々に降温させると、融液中で最も温度の低
い種子結晶７と接触している融液の界面に
PbTio3微結晶が少しずつ析出してきて種子結晶
７上に結晶化する。このようにして成長した
PbTio3単結晶８を融液から徐々に引き上げる。
すなわち、融液を降温しながら、育成された単結
晶引き上げを同時に行つていくのである。 As an example, starting material 9 contains 55 mol% of Pbo,
A mixture of 15 mol% TiO 2 and 30 mol% B 2 O 3 (point P in Figure 1) was placed in a platinum crucible 10 with a diameter of 55 mm and a height of 40 mm, which also served as a heating element, as shown in Figure 2. Get in,
By induction heating method using high frequency heating coil 4~
After heating to 900° C. to melt, a seed crystal 7 made of a PbTio 3 single crystal is brought into contact with the surface of the melt. When the temperature of the melt is gradually lowered, the temperature increases at the interface of the melt that is in contact with the seed crystal 7, which has the lowest temperature in the melt.
PbTio 3 microcrystals precipitate little by little and crystallize on the seed crystal 7. This is how I grew up
Gradually pull up the PbTio 3 single crystal 8 from the melt.
That is, while cooling the melt, the grown single crystal is simultaneously pulled.
この時の製造条件としては、PbTio3単結晶８
の引き上げ速度は0.2〜１mm／ｈ、融液降温速度
１〜５℃／ｈ、結晶回転数30〜50rpm、雰囲気は
空気中である。また、PbTio3単結晶８の育成を
完了するまでに要する時間は、30×28×７mmの大
きさで約13gの黄色透明のPbTio3単結晶８が28時
間で得られた。 The manufacturing conditions at this time were PbTio 3 single crystal 8
The pulling rate is 0.2 to 1 mm/h, the melt cooling rate is 1 to 5° C./h, the crystal rotation speed is 30 to 50 rpm, and the atmosphere is air. Further, the time required to complete the growth of the PbTio 3 single crystal 8 was 28 hours, with a size of 30 x 28 x 7 mm and a weight of about 13 g of transparent yellow PbTio 3 single crystal 8.
〔実施例 ２〕
Pboを50モル％、TiO2を1.25モル％、ZrO2を
7.1モル％、B2O341.65モル％の組成に混合し、実
施例１の方法と同様の操作により同様の経過を経
て５×５×８mmの白色透明の板状単結晶が集合し
たPb（TiZr）O3単結晶が育成された。[Example 2] 50 mol% Pbo, 1.25 mol% TiO2 , ZrO2
7.1 mol% of B 2 O 3 and 41.65 mol% of Pb ( TiZr)O 3 single crystals were grown.
上述のようにPbTio3単結晶の製造方法におい
て何らかの異種元素を少量混合した時に、
PbTio3固溶体単結晶の析出条件が本質的に変わ
らない場合は、上述と全く同一の方法、条件によ
つて異種元素を混合したPbTio3固溶体単結晶を
製造することも可能である。 As mentioned above, when a small amount of some kind of different element is mixed in the manufacturing method of PbTio 3 single crystal,
If the precipitation conditions for the PbTio 3 solid solution single crystal remain essentially the same, it is also possible to produce a PbTio 3 solid solution single crystal containing a mixture of different elements using exactly the same method and conditions as described above.
以上説明したようにこの発明は、酸化ホウ素と
酸化鉛を配合してなる溶剤にチタン酸鉛を溶剤に
対する飽和濃度以上の割合で混合し、高温度に加
熱して全体を融解したのち、その融液を徐々に冷
却することにより融液中に析出してくるチタン酸
鉛微結晶を融液に接触させた種子結晶上に結晶化
させ、これを育成させながら引き上げるようにし
たので、黄色透明の大型の単結晶で種子結晶によ
り望みの方向に成長したが固化した融剤の除去操
作なしに得られるという利点を有する。
As explained above, the present invention involves mixing lead titanate in a solvent containing boron oxide and lead oxide at a ratio exceeding the saturation concentration of the solvent, heating the mixture to a high temperature to melt the whole, and then melting the mixture. By gradually cooling the liquid, the lead titanate microcrystals that precipitate in the melt are crystallized on seed crystals that are in contact with the melt, and are pulled up while growing, resulting in a transparent yellow color. It has the advantage that a large single crystal can be grown in a desired direction using seed crystals without removing the solidified flux.
また、チタン酸鉛の大型単結晶を得る組成範囲
として酸化鉛が45〜70モル％、酸化ホウ素が15〜
45モル％、酸化チタンが５〜20モル％にしたもの
は、さらに大型PbTio3単結晶を得ることができ
る利点を有する。 In addition, the composition range for obtaining large single crystals of lead titanate is 45 to 70 mol% lead oxide and 15 to 70 mol% boron oxide.
45 mol % and 5 to 20 mol % of titanium oxide has the advantage that even larger PbTio 3 single crystals can be obtained.
第１図はこの発明の原理を説明するためのPbo
−TiO2−B2O3系の相平衡図、第２図はこの発明
を実施するためのPbTio3単結晶の製造装置の構
成図である。
図中、１は水冷シヤフト、２は白金シヤフト、
３は保温材、４は高周波加熱コイル、５は熱電
対、６はるつぼ支持物、７は種子結晶、８は
PbTio3単結晶、９は出発原料、１０は白金るつ
ぼである。
Figure 1 shows Pbo to explain the principle of this invention.
-TiO 2 -B 2 O 3 system phase equilibrium diagram, FIG. 2 is a block diagram of a PbTio 3 single crystal manufacturing apparatus for carrying out the present invention. In the figure, 1 is a water-cooled shaft, 2 is a platinum shaft,
3 is a heat insulator, 4 is a high-frequency heating coil, 5 is a thermocouple, 6 is a crucible support, 7 is a seed crystal, 8 is a
PbTio 3 single crystal, 9 is a starting material, and 10 is a platinum crucible.
Claims (1)
タン酸鉛を前記溶剤に対する飽和濃度以上の割合
で混合し、高温度に加熱して全体を融解したの
ち、その融液を徐々に冷却することにより前記融
液中に析出してくるチタン酸鉛微結晶を融液に接
触させた種子結晶上に結晶化させ、これを育成さ
せながら引き上げることを特徴とするチタン酸鉛
単結晶の製造方法。 ２ チタン酸鉛の大型単結晶を得る組成範囲とし
て酸化鉛が45〜70モル％、酸化ホウ素が15〜45モ
ル％、酸化チタンが５〜20モル％にした請求項１
記載のチタン酸鉛単結晶の製造方法。[Scope of Claims] 1. Lead titanate is mixed in a solvent containing boron oxide and lead oxide at a ratio equal to or higher than the saturation concentration of the solvent, heated to a high temperature to melt the whole, and then the melt is obtained. Lead titanate microcrystals precipitated in the melt by gradually cooling the melt are crystallized on seed crystals in contact with the melt, and the lead titanate is pulled up while growing. Method for producing single crystals. 2. Claim 1: The composition range for obtaining a large single crystal of lead titanate is 45 to 70 mol% of lead oxide, 15 to 45 mol% of boron oxide, and 5 to 20 mol% of titanium oxide.
The method for producing the lead titanate single crystal described above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32178388A JPH02167894A (en) | 1988-12-20 | 1988-12-20 | Production of single crystal of lead titanate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32178388A JPH02167894A (en) | 1988-12-20 | 1988-12-20 | Production of single crystal of lead titanate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02167894A JPH02167894A (en) | 1990-06-28 |
| JPH0478596B2 true JPH0478596B2 (en) | 1992-12-11 |
Family
ID=18136377
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32178388A Granted JPH02167894A (en) | 1988-12-20 | 1988-12-20 | Production of single crystal of lead titanate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02167894A (en) |
-
1988
- 1988-12-20 JP JP32178388A patent/JPH02167894A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02167894A (en) | 1990-06-28 |
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