JPH0818908B2 - Raw material for Bernoulli method single crystal Alumina powder - Google Patents
Raw material for Bernoulli method single crystal Alumina powderInfo
- Publication number
- JPH0818908B2 JPH0818908B2 JP61256600A JP25660086A JPH0818908B2 JP H0818908 B2 JPH0818908 B2 JP H0818908B2 JP 61256600 A JP61256600 A JP 61256600A JP 25660086 A JP25660086 A JP 25660086A JP H0818908 B2 JPH0818908 B2 JP H0818908B2
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- alumina powder
- raw material
- alumina
- bernoulli method
- 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 - Lifetime
Links
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 32
- 239000013078 crystal Substances 0.000 title claims description 27
- 238000000034 method Methods 0.000 title claims description 23
- 239000000843 powder Substances 0.000 title claims description 20
- 239000002994 raw material Substances 0.000 title claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 3
- 239000010936 titanium Substances 0.000 description 13
- 239000012535 impurity Substances 0.000 description 8
- 235000011124 aluminium ammonium sulphate Nutrition 0.000 description 4
- LCQXXBOSCBRNNT-UHFFFAOYSA-K ammonium aluminium sulfate Chemical compound [NH4+].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O LCQXXBOSCBRNNT-UHFFFAOYSA-K 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】 〈産業上の利用分野〉 本発明はベルヌーイ法による単結晶製造用原料アルミ
ナ粉末（以下単にベルヌーイ法単結晶用原料アルミナ粉
末と称する。）に関するものである。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a raw material alumina powder for producing a single crystal by the Bernoulli method (hereinafter simply referred to as a raw material alumina powder for a Bernoulli method single crystal).
〈従来の技術〉 ベルヌーイ法単結晶用原料アルミナ粉末には従来、精
製したアンモニウム明ばんを焼成して得られるγ−アル
ミナが主として用いられている。<Prior Art> γ-alumina obtained by firing purified ammonium alum has been mainly used as a raw material alumina powder for Bernoulli method single crystal.
このアルミナはNa,Si,Fe,Mg等の不純物を通常数10ppm
含有しており、これを原料アルミナとして適用した場合
には該不純物が結晶育成時に結晶の配列を乱し、アルミ
ナ単結晶ブール中に気泡がとり込まれる問題があった。This alumina usually contains impurities such as Na, Si, Fe, Mg, etc. of several 10 ppm.
When it is contained as a raw material alumina, there is a problem that the impurities disturb the crystal arrangement during crystal growth, and bubbles are taken into the alumina single crystal boule.
このような不都合を解決するため原料アルミナ粉末を
精製し、不純物濃度を下げて使用する方法、例えばアン
モニウム明ばんの再結晶を繰返して不純物を除いたアル
ミニウム粉末を原料として用いる方法が採用されている
が、この場合には気泡は減少するものの得られるアルミ
ナ単結晶ブールにＣ面が顕著に現われ、ブールが四角柱
となる現象が生じる為、主として円柱状単結晶が製品形
状として要求される現工程においては、四角柱から円柱
状への研削コストが増大すると伴に製品の収率を大巾に
低下させるという不都合を有する。In order to solve such inconvenience, a method of purifying the raw material alumina powder and using it by reducing the impurity concentration, for example, a method of using aluminum powder from which impurities have been removed by repeating recrystallization of ammonium alum as a raw material is adopted. However, in this case, although the number of bubbles is reduced, the C-plane appears remarkably in the obtained alumina single crystal boule, and the phenomenon that the boule becomes a square pillar occurs. Therefore, a cylindrical single crystal is mainly required as a product shape in the present process. In the above, there is a disadvantage that the yield of the product is drastically reduced as the grinding cost from the square pole to the cylinder increases.
〈発明が解決しようとする問題点〉 かかる事情下に鑑み本発明者等はベルヌーイ法による
透明アルミナ単結晶の製造に於いて、気泡、着色がな
く、かつＣ面の発現が抑制された円柱状単結晶を得る事
を目的とし鋭意検討した結果、原料アルミナ中の不純物
およびその量を特定化する場合には上記目的を全て満足
し得る事を見出し、本発明を完成するに至った。<Problems to be Solved by the Invention> In view of such circumstances, the present inventors have, in the production of a transparent alumina single crystal by the Bernoulli method, a columnar shape having no bubbles or coloring and suppressing the development of the C plane. As a result of extensive studies aimed at obtaining a single crystal, it was found that all of the above objects can be satisfied when the impurities in the raw material alumina and the amount thereof are specified, and the present invention has been completed.
〈問題点を解決するための手段〉 すなわち本発明は、Na,Si,FeおよびMgの金属或はこれ
らの金属の化合物をNa,Si,FeおよびMg原子として各々20
ppm以下、Ti金属または該金属の化合物をTi原子として1
0〜50ppm含有することを特徴とするベルヌーイ法単結晶
用原料アルミナ粉末を提供するにある。<Means for Solving Problems> That is, the present invention provides a metal of Na, Si, Fe and Mg or a compound of these metals as Na, Si, Fe and Mg atoms, each of which is 20
ppm or less, Ti metal or compound of the metal as Ti atom 1
It is intended to provide a raw material alumina powder for Bernoulli method single crystal, which is characterized by containing 0 to 50 ppm.
以下本発明を更に詳細に説明する。 The present invention will be described in more detail below.
本発明のアルミナ粉末は該アルミナ粉末中にNa,Si,Fe
およびMgの金属或はこれらの金属の化合物がNa,Si,Feお
よびMg原子として各々約20ppm以下、好ましくは約15ppm
以下、Ti金属または該金属の化合物をTi原子として約10
〜約50ppm好ましくは約15〜約40ppm含有することを必須
とする。The alumina powder of the present invention contains Na, Si, Fe in the alumina powder.
And Mg metal or compounds of these metals as Na, Si, Fe and Mg atoms are each about 20 ppm or less, preferably about 15 ppm.
Hereinafter, a Ti metal or a compound of the metal is used as a Ti atom in an amount of about
To about 50 ppm, preferably about 15 to about 40 ppm is essential.
Na,Si,Fe,Mgが上記範囲を越える場合には得られる単
結晶に気泡が発生するので好ましくない。If Na, Si, Fe, or Mg exceeds the above range, bubbles are generated in the obtained single crystal, which is not preferable.
またTi量が上記範囲未満の場合にはＣ面の発現を抑え
るのに十分でなく、他方上記範囲を越える場合には、単
結晶に着色が発生するので好ましくない。On the other hand, when the Ti content is less than the above range, it is not sufficient to suppress the development of the C plane, while when it exceeds the above range, the single crystal is colored, which is not preferable.
原料アルミナ粉末の粒径はベルヌーイ法単結晶製造時
に溶融し得る程度であれば、特に限定されないが、通常
一次粒子径で約１μｍ以下、より好ましくは約0.5μｍ
以下がよい。The particle size of the raw material alumina powder is not particularly limited as long as it can be melted at the time of producing Bernoulli method single crystal, but the primary particle size is usually about 1 μm or less, and more preferably about 0.5 μm.
The following is good.
このようなベルヌーイ法単結晶用原料アルミナ粉末の
製造方法としては有機アルミニウム溶液にTi塩を添加
し、加水分解後、必要に応じて乾燥し、焼成する方法、
アンモニウム明礬にTi塩を添加しこれを熱分解する方
法、或はバイヤー法により得られたアルミナを精製し
たアルミナ粉末、有機アルミニウムの加水分解法やアン
モニウム明礬熱分解法により得られたアルミナ粉末に金
属チタン或はチタン含有物を振動ミルやボールミル等の
乾式混合装置でチタンが均一に分散するよう混合する方
法、更にはアルミナスラリー中にTi塩を添加し、湿式
混合した後、通常の加熱乾燥或はスプレードライ法等に
より乾燥する方法等が挙げられる。As a method for producing such a raw material alumina powder for Bernoulli method single crystal, a Ti salt is added to an organoaluminum solution, after hydrolysis, a method of drying and baking if necessary,
Aluminium powder obtained by adding Ti salt to ammonium alum and thermally decomposing it, or alumina obtained by the Bayer method, or alumina powder obtained by hydrolysis of organic aluminum or ammonium alum thermal decomposition. A method in which titanium or a titanium-containing material is mixed by a dry mixing device such as a vibration mill or a ball mill so that titanium is uniformly dispersed. Further, a Ti salt is added to an alumina slurry and wet-mixed, followed by ordinary heat drying or Examples of the method include a method of drying by a spray drying method or the like.
得られたアルミナ粉末の結晶形態も、通常ベルヌーイ
法単結晶原料用アルミナ粉末として公知の形態であれば
よく、水酸化アルミニウムからσ，δ，θ，γ等の遷移
アルミナ、更にはα−アルミナ迄のいずれの形態であっ
てもよい。The crystal morphology of the obtained alumina powder may be any of those generally known as alumina powder for Bernoulli method single crystal raw materials, from aluminum hydroxide to transition alumina such as σ, δ, θ, γ, and further α-alumina. Either form may be used.
〈発明の効果〉 このように本発明の特定の不純物を有するアルミナ粉
末を通常のベルヌーイ法単結晶の原料用アルミナ粉末と
して用いる場合には得られる単結晶に気泡、着色がな
く、かつＣ面の発現が抑制された円柱状単結晶を得る事
を可能ならしめるもので、研削コストの低減ならびに製
品の収率向上に寄与しその工業的価値は頗る大なるもの
である。<Effects of the Invention> As described above, when the alumina powder having the specific impurities of the present invention is used as the alumina powder as a raw material for a normal Bernoulli method single crystal, the obtained single crystal is free from bubbles and coloring, and has a C-plane It makes it possible to obtain a cylindrical single crystal whose expression is suppressed, which contributes to reduction of grinding cost and improvement of product yield, and its industrial value is extremely great.
〈実施例〉 以下、実施例により本発明を説明するが、本発明はか
かる実施例により制限されるものではない。<Examples> Hereinafter, the present invention will be described with reference to examples, but the present invention is not limited to the examples.
尚、実施例に於いて有効断面積は、得られた単結晶ブ
ール断面積に対しての、該ブールより得られる最大径の
円柱の断面積の割合を百分率で示したものである。In the examples, the effective cross-sectional area is the percentage of the cross-sectional area of the cylinder having the maximum diameter obtained from the boule with respect to the obtained single-crystal boule cross-sectional area.
実施例１〜４ アルミニウムイソプロポキシドを加水分解した後焼成
して得られた不純物としてNa2ppm,Si2ppm,Fe1ppm及びMg
1ppmを含有するγ−Al2O3とアルミナに対してTiとして
第１表に示す量のTi（SO4）２水溶液を混合し、スラリ
ー状とした後、スプレードライヤーで乾燥した。Examples 1 to 4 Na2ppm, Si2ppm, Fe1ppm and Mg as impurities obtained by hydrolyzing aluminum isopropoxide and then calcining
Γ-Al 2 O 3 containing 1 ppm and alumina were mixed with Ti (SO 4 ) 2 aqueous solution in an amount shown in Table 1 to form a slurry, which was then dried with a spray dryer.
この様にして得られたアルミナ粉末をベルヌーイ法単
結晶製造装置で結晶成長させ、得られたブールの気泡、
円柱として切出せる有効断面積及び色を測定した。Alumina powder obtained in this manner was subjected to crystal growth with a Bernoulli method single crystal manufacturing apparatus, and obtained boulle bubbles,
The effective area and color that can be cut out as a cylinder were measured.
その結果を第１表に示す。 The results are shown in Table 1.
比較例１ 第２表に示す不純物を含有するγ−Al2O3を、アルミ
ナに対してTiとして第２表に示す量のTi（SO4）２水溶
液を混合しスラリー状とした後、スプレードライヤーで
乾燥した。Comparative Example 1 γ-Al 2 O 3 containing impurities shown in Table 2 was mixed with alumina in an amount of Ti (SO 4 ) 2 aqueous solution shown in Table 2 to form a slurry, and then sprayed. It was dried with a dryer.
このようにして得られたアルミナ粉末をベルヌーイ法
単結晶製造装置で結晶成長させ、得られたブールの気
泡、円柱として切出せる有効断面積及び色を測定した。The alumina powder thus obtained was crystal-grown by a Bernoulli method single crystal manufacturing apparatus, and the bubbles of the obtained boule, the effective area that can be cut out as a cylinder, and the color were measured.
その結果を第２表に示す。 The results are shown in Table 2.
Claims (2)
化合物をNa,Si,FeおよびMg原子として各々20ppm以下、T
i金属または該金属の化合物をTi原子として10〜50ppm含
有することを特徴とするベルヌーイ法単結晶用原料アル
ミナ粉末。1. A metal of Na, Si, Fe and Mg or a compound of these metals is contained as Na, Si, Fe and Mg atoms in an amount of 20 ppm or less and T, respectively.
A raw material alumina powder for Bernoulli method single crystal, which contains 10 to 50 ppm of a metal or a compound of the metal as a Ti atom.
〜40ppm含有することを特徴とする特許請求の範囲第１
項記載のベルヌーイ法単結晶用原料アルミナ粉末。2. A Ti metal or a compound of the metal as Ti is 15
Claim 1 characterized by containing ~ 40ppm
A raw material alumina powder for Bernoulli method single crystal according to the item.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61256600A JPH0818908B2 (en) | 1986-10-27 | 1986-10-27 | Raw material for Bernoulli method single crystal Alumina powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61256600A JPH0818908B2 (en) | 1986-10-27 | 1986-10-27 | Raw material for Bernoulli method single crystal Alumina powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63112498A JPS63112498A (en) | 1988-05-17 |
| JPH0818908B2 true JPH0818908B2 (en) | 1996-02-28 |
Family
ID=17294883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61256600A Expired - Lifetime JPH0818908B2 (en) | 1986-10-27 | 1986-10-27 | Raw material for Bernoulli method single crystal Alumina powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0818908B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4844429B2 (en) * | 2007-02-26 | 2011-12-28 | 日立化成工業株式会社 | Method for producing sapphire single crystal |
| TW201130156A (en) * | 2009-11-26 | 2011-09-01 | Showa Denko Kk | Sapphire single crystal for producing sapphire single crystal substrate for LED, sapphire single crystal substrate for LED, light-eliciting element, and method for preparing the same |
-
1986
- 1986-10-27 JP JP61256600A patent/JPH0818908B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63112498A (en) | 1988-05-17 |
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