JPS6287492A - Synthesis of star sapphire artificial crystal - Google Patents

Synthesis of star sapphire artificial crystal

Info

Publication number
JPS6287492A
JPS6287492A JP22738285A JP22738285A JPS6287492A JP S6287492 A JPS6287492 A JP S6287492A JP 22738285 A JP22738285 A JP 22738285A JP 22738285 A JP22738285 A JP 22738285A JP S6287492 A JPS6287492 A JP S6287492A
Authority
JP
Japan
Prior art keywords
crystal
star
hydrogen
star sapphire
sapphire
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
Application number
JP22738285A
Other languages
Japanese (ja)
Inventor
Haruo Haba
羽場 春夫
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Seiko Epson Corp
Original Assignee
Seiko Epson Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Seiko Epson Corp filed Critical Seiko Epson Corp
Priority to JP22738285A priority Critical patent/JPS6287492A/en
Publication of JPS6287492A publication Critical patent/JPS6287492A/en
Pending legal-status Critical Current

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  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

PURPOSE:To obtain a bright blue crystal containing rutile needlelike crystals finely distributed in the interior, by growing star sapphire in a reducing atmosphere, e.g. hydrogen or CO, etc., by a floating zone (FZ) method and heat- treating the resultant crystal in an oxidizing atmosphere after the growth. CONSTITUTION:A star sapphire crystal is grown in a reducing atmosphere consisting of hydrogen or carbon monoxide by using a floating zone (FZ) method. Since the reducing gas consisting of the hydrogen or carbon monoxide reduces iron oxide and titanium oxide which are raw materials for the star sapphire respectively into metallic iron and metallic titanium, a colorless transparent crystal is obtained. The resultant crystal is then placed in a furnace of an oxidizing atmosphere and heat-treated at 1,000-1,500 deg.C for about 10-50hr. The metallic iron and metallic titanium in the crystal are oxidized, ionized and uniformly colored to finely and densely grow rutile needlelike crystals at the same time and afford the aimed bright blue star sapphire without uneven color.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、スター・サファイア人工結晶の合成方法に関
する。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for synthesizing star sapphire artificial crystals.

〔発明の概要〕[Summary of the invention]

本発明はFz法でスター・サファイアを育ti14する
際において、還元雰囲気中で行^、育5X、後にそれら
を酸化雰囲気炉で熱処理することくより、スター・サフ
ァイア人工結晶を合成したものである。
The present invention synthesizes star sapphire artificial crystals by growing star sapphires using the Fz method in a reducing atmosphere, growing 5X, and then heat-treating them in an oxidizing atmosphere furnace. .

〔従来の技術〕[Conventional technology]

スター・サファイアとはブルー・サファイア中に内包物
として存在するルチルの針状結晶が、細かく密に発達し
た原石を山高にカポジョンカットしたとき、点光源に当
てて見ると、6榮の星彩線を現わす石のことである。
What is star sapphire? The rutile needle crystals that exist as inclusions in blue sapphire are finely and densely developed. When the raw stone is cut into a capojon at a mountain height, when viewed under a point light source, it shows six star colors. It is a stone that shows lines.

従来、このスター・サファイア人工結晶を合成すること
がyz法で試みられてきた。
Conventionally, attempts have been made to synthesize this star sapphire artificial crystal using the yz method.

〔発明が解決する問題点及び目的〕[Problems and objectives to be solved by the invention]

しかし、スター・サファイアの原料であるアルミナ、酸
化チタン、酸化鉄を溶融、固化することにより結晶を育
成するFZ法では、鉄イオンと、チタンイオンのアルミ
イオンとの置換しやすさの相違、溶融液中での鉄イオン
とチタンイオンの拡散速度の相違、育成雰囲気との鉄イ
オンとチタンイオンの反応速度の相違などのため、育成
されたスター・サファイアは、色むらが著しく、−に青
色を帯びた部分と透明な部分が混合路た場合においては
、ル、チルの針状結晶の分布も不均一になり、製品化す
ることが不可能であった。そこで本発明はこのような問
題点を解決するもので、その目的とするところは、色む
らがなく、ルチル針状結晶が細かく、密に発達したスタ
ー・サファイアに&成するところにある。
However, in the FZ method, which grows crystals by melting and solidifying alumina, titanium oxide, and iron oxide, which are the raw materials for star sapphire, there are differences in the ease with which iron ions and titanium ions can be replaced with aluminum ions, Due to the difference in the diffusion rate of iron ions and titanium ions in the liquid, and the difference in the reaction rate of iron ions and titanium ions with the growth atmosphere, the grown star sapphires have significant color unevenness, with a blue coloration. In the case where the colored part and the transparent part were mixed, the distribution of needle-like crystals of crystals became uneven, and it was impossible to commercialize the product. The present invention is intended to solve these problems, and its purpose is to form a star sapphire with no uneven color and fine, densely developed rutile needle crystals.

〔間販点を解決するための手段〕[Means to solve intermittent sales points]

本発明は、IFZ法でスター・サファイアを育成する際
に、還元雰囲気である水素又は、一酸化炭素を用いて行
i、育成後にそれらを酸化雰囲気炉で熱処理することを
特徴とする。
The present invention is characterized in that when star sapphire is grown by the IFZ method, hydrogen or carbon monoxide is used as a reducing atmosphere, and after the growth, the star sapphire is heat-treated in an oxidizing atmosphere furnace.

〔作用〕[Effect]

本発明において、還元雰囲気は、水素及び一酸化炭素と
し、その濃度は、アルゴンガス中に10 ppm〜l 
O00p pmの間とする。
In the present invention, the reducing atmosphere is hydrogen and carbon monoxide, and the concentration thereof is 10 ppm to 1 in argon gas.
It is assumed to be between 000p and pm.

これらの還元ガスは、スター・サファイアの原料である
酸化鉄と酸化チタンをそれぞれ金属鉄と金属チタンに還
元するために使用するのである。
These reducing gases are used to reduce iron oxide and titanium oxide, the raw materials for star sapphire, to metallic iron and metallic titanium, respectively.

従って11’Z法で育成された結晶は、無色透明な結晶
である。そGらを酸化雰囲気炉で1000℃〜1500
℃でlO〜50時間程尻熱処哩をほどこす。
Therefore, the crystal grown by the 11'Z method is a colorless and transparent crystal. G and others in an oxidizing atmosphere furnace at 1000℃~1500℃
Heat treatment is performed at 10°C for about 50 hours.

これは、結晶中の金属鉄と金属チタンを酸化させて、イ
オン化することにより均一に着色させるためであり、ま
たルチルの針状結晶を細かく密に成長させるためである
。この酸化雰囲気中の熱処理により無色透明な結晶は、
内部にルチル針状結晶のよく発達した色むらのな匹鮮や
かな青色のスター・サファイアとなるのである。
This is to uniformly color the metal iron and metal titanium in the crystal by oxidizing and ionizing them, and also to grow fine and dense needle-shaped rutile crystals. This heat treatment in an oxidizing atmosphere produces colorless and transparent crystals.
The result is a bright blue star sapphire with a well-developed rutile needle crystal inside.

〔実施例〕〔Example〕

以下に本発明の詳細な説明する。 The present invention will be explained in detail below.

実施例1 原料であるアルミナ(AAgOs ) 90 wt%、
酸化鉄(′IPsxOs) 6 wt%、酸化チタ” 
(170g) 4 wt%を調合し、焼結したものを原
料棒とした。これを種結晶と共にF′z炉にセットした
後に、水素50ppmを含んだアルゴンガスを流しなが
ら、結晶を育成した。この得られた結晶を熱処理炉に入
れ、1200℃で20時間大気中(酸化雰囲気)で熱処
理した。
Example 1 Raw material alumina (AAgOs) 90 wt%,
Iron oxide ('IPsxOs) 6 wt%, titanium oxide”
(170g) 4 wt% was prepared and sintered to obtain a raw material rod. After setting this together with a seed crystal in an F'z furnace, crystals were grown while flowing argon gas containing 50 ppm of hydrogen. The obtained crystals were placed in a heat treatment furnace and heat treated at 1200° C. for 20 hours in the air (oxidizing atmosphere).

これによりルチル針状結晶が細かく密に分布した色むら
のなめスター・サファイアが製造された。
This produced unevenly colored star sapphires with fine, densely distributed rutile needles.

この結晶を山高にカポジョンカットしたところ、螢光灯
のような散乱光源下でさえも、明瞭な光の線条が6条現
われた。
When this crystal was cut into a capojon at a mountain height, six clear streaks of light appeared even under a scattered light source such as a fluorescent light.

Ij!施例2 原料としてアルミナ921ot% 、酸化鉄5 wt%
酸化チタン3 wt%を装置、混合し、焼結したものを
原料棒とした。これを種結晶と共にPZ炉にセットし、
一酸化炭素500ppmを含んだアルゴンガスを流しな
がら結晶の育成を行った。
Ij! Example 2 Raw materials: 921 ot% alumina, 5 wt% iron oxide
A raw material rod was obtained by mixing 3 wt% of titanium oxide in an apparatus and sintering it. Set this in a PZ furnace with a seed crystal,
Crystals were grown while flowing argon gas containing 500 ppm of carbon monoxide.

この得られた結晶を熱処理炉に入れ1300℃で30時
間大気中で熱処理したところ、ルチル針状結晶のよく発
達し、均一に着色したスター・サファイアが製造された
When the obtained crystals were placed in a heat treatment furnace and heat treated in the air at 1300° C. for 30 hours, a uniformly colored star sapphire with well-developed rutile needle crystals was produced.

この結晶の断面iFtPMA法で定置分析した。その結
果より鉄イオンとチタンイオンがほぼ均一に分布してお
り、また、ルチル(”#O*)の針状結晶が六角柱面に
千行に分布しており、柱面の両対面に垂直な3方向に並
び、互iに120°に交差してよく発達していることが
わかった。
A cross section of this crystal was analyzed in situ using the iFtPMA method. The results show that iron ions and titanium ions are almost uniformly distributed, and that needle-like crystals of rutile (#O*) are distributed in 1,000 rows on the hexagonal prismatic surface, and are perpendicular to both sides of the cylindrical surface. They were found to be well developed, lining up in three directions and intersecting each other at 120°.

この組織に垂直な方向にカポジョンカットしたところ中
心に明るく6条の星彩線が現われた。
When a capojon was cut in a direction perpendicular to this tissue, six bright star lines appeared in the center.

〔発明の効果〕〔Effect of the invention〕

以上述べたように、FZ法でスター・サファイアを育成
する際に、還元雰囲気である水素又は、一酸化炭素を用
いて行い、育成後にそれらを酸化雰囲気炉で熱処理する
ことにより、内部にルチルの針状結晶が細かく密に分布
した色むらのない鮮やかな青色のスター・サファイアが
合成することができる。
As mentioned above, when growing star sapphires using the FZ method, it is done using a reducing atmosphere of hydrogen or carbon monoxide, and after the growth, they are heat-treated in an oxidizing atmosphere furnace to create rutile inside. It is possible to synthesize bright blue star sapphires with fine, densely distributed needle-like crystals.

以   上that's all

Claims (1)

【特許請求の範囲】[Claims] FZ法でスター・サファイアを育成する際に、還元雰囲
気である水素又は、一酸化炭素を用いて行い、育成後に
それらを酸化雰囲気炉で熱処理することを特徴とするス
ター・サファイア人工結晶の合成方法。
A method for synthesizing star sapphire artificial crystals, which is characterized in that star sapphires are grown by the FZ method using a reducing atmosphere of hydrogen or carbon monoxide, and after the growth, they are heat-treated in an oxidizing atmosphere furnace. .
JP22738285A 1985-10-11 1985-10-11 Synthesis of star sapphire artificial crystal Pending JPS6287492A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP22738285A JPS6287492A (en) 1985-10-11 1985-10-11 Synthesis of star sapphire artificial crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP22738285A JPS6287492A (en) 1985-10-11 1985-10-11 Synthesis of star sapphire artificial crystal

Publications (1)

Publication Number Publication Date
JPS6287492A true JPS6287492A (en) 1987-04-21

Family

ID=16859935

Family Applications (1)

Application Number Title Priority Date Filing Date
JP22738285A Pending JPS6287492A (en) 1985-10-11 1985-10-11 Synthesis of star sapphire artificial crystal

Country Status (1)

Country Link
JP (1) JPS6287492A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100699048B1 (en) 2004-12-10 2007-03-23 서울시립대학교 산학협력단 Heat treatment method for blue sapphire
KR100856109B1 (en) 2007-04-05 2008-09-02 한국원자력연구원 Method for manufacturing the color controlled sappire
WO2009151160A1 (en) * 2008-06-12 2009-12-17 Korea Atomic Energy Research Institute Method for manufacturing the color controlled sappire
WO2011001905A1 (en) * 2009-07-03 2011-01-06 昭和電工株式会社 Method for producing sapphire single crystal, and sapphire single crystal obtained by the method
US11288633B2 (en) 2010-04-02 2022-03-29 Vivint, Inc. Door to door sales management tool
US11537993B2 (en) 2010-04-02 2022-12-27 Vivint, Inc. Gathering and display of sales data for an identified residence via a graphical user interface (GUI) of a mobile software application executing on a wireless mobile computer device

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100699048B1 (en) 2004-12-10 2007-03-23 서울시립대학교 산학협력단 Heat treatment method for blue sapphire
KR100856109B1 (en) 2007-04-05 2008-09-02 한국원자력연구원 Method for manufacturing the color controlled sappire
WO2009151160A1 (en) * 2008-06-12 2009-12-17 Korea Atomic Energy Research Institute Method for manufacturing the color controlled sappire
US8778463B2 (en) 2008-06-12 2014-07-15 Jae-Won Park Method for manufacturing the color controlled sapphire
WO2011001905A1 (en) * 2009-07-03 2011-01-06 昭和電工株式会社 Method for producing sapphire single crystal, and sapphire single crystal obtained by the method
US11288633B2 (en) 2010-04-02 2022-03-29 Vivint, Inc. Door to door sales management tool
US11537993B2 (en) 2010-04-02 2022-12-27 Vivint, Inc. Gathering and display of sales data for an identified residence via a graphical user interface (GUI) of a mobile software application executing on a wireless mobile computer device
US11537992B2 (en) 2010-04-02 2022-12-27 Vivint, Inc. Sales route planning using an interactive electronic map displayed on a graphical user interface (GUI) of a mobile software application executing on a wireless mobile computer device

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