JPS5997527A - Manufacture of high purity alumina particle - Google Patents
Manufacture of high purity alumina particleInfo
- Publication number
- JPS5997527A JPS5997527A JP57205088A JP20508882A JPS5997527A JP S5997527 A JPS5997527 A JP S5997527A JP 57205088 A JP57205088 A JP 57205088A JP 20508882 A JP20508882 A JP 20508882A JP S5997527 A JPS5997527 A JP S5997527A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- purity alumina
- alumina
- high purity
- purity
- 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002245 particle Substances 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 22
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 3
- 239000007858 starting material Substances 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract description 2
- 238000011109 contamination Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 235000011124 aluminium ammonium sulphate Nutrition 0.000 description 2
- -1 aluminum alkoxide Chemical class 0.000 description 2
- 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 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000007751 thermal spraying Methods 0.000 description 2
- 244000105975 Antidesma platyphyllum Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 235000009424 haa Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は高純度アルミナ粒子の製造方法に関し、更に詳
細には流動性に優れた高純度アルミナ粒子の製造方法に
関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing high-purity alumina particles, and more particularly to a method for producing high-purity alumina particles with excellent fluidity.
従来、アンモニウムミョウバンの熱分解法やアルミニウ
ムの水中放電法、アルミニウムアルコキサイドの熱分解
法等多くの高純度アルミナ粉末の製造方法が知られてい
るが、これらの方法により得られた高純度アルミナ粉末
は極めて流動性か悪く、サファイア等の単結晶製造分野
では使用し難いとされていた。Conventionally, many methods for producing high-purity alumina powder are known, such as the pyrolysis method of ammonium alum, the underwater discharge method of aluminum, and the pyrolysis method of aluminum alkoxide. The powder had extremely poor fluidity and was considered difficult to use in the field of producing single crystals such as sapphire.
このため該粉末をいったんプレス成形し、その後位結成
は溶融し、さらに粉砕粒状化して使用したり、又は該粉
末をスプレィドライ法でいったん顆粒化した後焼結して
粒状原料とする方法等の手段が取られて来た。For this reason, the powder may be press-molded, then melted, and then pulverized into granules for use, or the powder may be granulated by a spray drying method and then sintered to form a granular raw material. Measures have been taken.
しかしながらこれらの粒状化方法はプロセスが繁雑であ
るばかりか成形、焼成、粉砕等の作業過程で鉄分、硅素
分、ソーダ分等の不純物の混入を招きやすいという欠点
を有する。However, these granulation methods have the drawback that not only are the processes complicated, but also impurities such as iron, silicon, and soda are likely to be mixed in during operations such as molding, firing, and pulverization.
かかる事情下に鑑み本発明者らは、原料として使用する
高純度アルミナ粉末を何等汚染することなくかつ、流動
性のすぐれた高純度アルミナ粒を得るべく鋭意検討を行
なった結果、特定の条件下に高純度アルミナ粉末を処理
する場合には流動性は勿論のこと、得られる高純度アル
ミナ粒は出′発原料アルミナよりも史に純度が向上する
ことを見い出し、本発明を完成するに至った。In view of these circumstances, the inventors of the present invention conducted intensive studies to obtain high-purity alumina grains with excellent fluidity without contaminating the high-purity alumina powder used as a raw material. The inventors discovered that when high-purity alumina powder is processed, not only the fluidity but also the purity of the resulting high-purity alumina grains is improved compared to the starting material alumina, leading to the completion of the present invention. .
すなわち本発明は酸素過剰の高温火炎中に同純度アルミ
ナ粉末を投入し、該粉末表面を溶除I或は半溶融するこ
とを特徴とする高純度アルミナ粒子の製造方法、この際
好ましくは高温火炎中に投入する原料粉末として高純度
アルミナ100重量部に塩酸0.1〜1重量部を添加し
た原料粉末を用い、上記方法により該粉末の表面を溶融
或は半溶融することによる高純度アルミナ粒子の製造方
法を提供する蚤こある。That is, the present invention provides a method for producing high-purity alumina particles, which is characterized by introducing alumina powder of the same purity into a high-temperature flame with excess oxygen, and melting or semi-melting the powder surface. High-purity alumina particles are obtained by melting or semi-melting the surface of the powder using the method described above, using a raw material powder containing 100 parts by weight of high-purity alumina and 0.1 to 1 part by weight of hydrochloric acid as the raw material powder to be introduced. There is a flea company that provides a manufacturing method.
以下、本発明方法を更に詳細に説明する。The method of the present invention will be explained in more detail below.
本発明方法1こ適用するアルミナ粉は通常純度約99.
8%以上、好ましく99.9%以上、平均粒径0.1〜
50μm程度の高純度アルミナであり、その製法として
はアンモニウムミョウバンの熱分解法やアルミニウムの
水中放電法、アルミニウムアルコキサイドの熱分解法、
バイヤー法等の公知方法によれはよい。The alumina powder used in Method 1 of the present invention usually has a purity of about 99.
8% or more, preferably 99.9% or more, average particle size 0.1-
It is a high-purity alumina with a diameter of about 50 μm, and its manufacturing methods include ammonium alum thermal decomposition method, aluminum underwater discharge method, aluminum alkoxide thermal decomposition method,
A known method such as the Bayer method may be used.
次いで本発明方法に実施に当っては高純度アルミナ粉末
原料を可燃性ガス、例えば水素、プロパン、アセチレン
等を原料とする火炎発生装置内に供給し、火炎中で該原
料粉末表面を溶融或は半溶岬;するが、この際処理は必
ず酸素過剰の状態下に処理しなけれはならない。Next, when carrying out the method of the present invention, a high-purity alumina powder raw material is supplied into a flame generator using a flammable gas such as hydrogen, propane, acetylene, etc., and the surface of the raw material powder is melted or heated in the flame. Half-melted cape: However, in this case, the treatment must be carried out under conditions of excess oxygen.
火炎発生装置内の酸素濃度を可燃性ガスを完全に燃焼せ
しめ得る童以上存在せしめない場合1こはアルミナ粒子
中に可燃性ガスの熱分解1こよって生じた炭素が取り込
まれ、原料アルミナの純度低fを招いたり、或はアルミ
ナの結晶欠陥多発の原因となって、遷移アルミナの生成
が著しくなり、主としてα−アルミナが要望される前記
のごとき単結晶製造分野の原材料としては使用できない
こととなるので適さない。If the oxygen concentration in the flame generator is not higher than that which can completely burn the flammable gas, the carbon generated by the thermal decomposition of the combustible gas will be incorporated into the alumina particles, and the purity of the raw material alumina will be reduced. This results in a low f value or a frequent occurrence of crystal defects in alumina, resulting in significant formation of transitional alumina, making it impossible to use it as a raw material in the above-mentioned single-crystal manufacturing field where α-alumina is primarily desired. Therefore, it is not suitable.
又酸素過剰の高温火炎中にて処理される原料制純度アル
ミナ粉末としては所要の純度を有する高純度アルミナ粉
末単味でもよいが、高純度アルミナ粉末100車を部当
り0.1〜1屯遺部の塩酸を予め添加したものを原料粉
末として火炎中fこ投入処理する場合には原料粉本中の
不純物が処理前よりも減少し、更に高純度化されるとと
も(こ遷移アルミナの生成率も低下するので好抜しい態
様である、アルミナ粉末に対する塩酸の添加量が0.1
%未7.7この場合(こは添加効果が顕著ではなく、他
方1直鍛%を越える場合にはそれに見合う添加効果の発
現がな(、むしろ発生する塩素ガス1こより装置材料が
腐食されるので好ましくない。The raw material-based purity alumina powder to be treated in a high-temperature flame with excess oxygen may be a single high-purity alumina powder having the required purity; When raw material powder to which 100% hydrochloric acid has been added in advance is thrown into a flame, the impurities in the raw material powder are reduced compared to before the treatment, and the purity is further increased (this is due to the formation of transition alumina). The amount of hydrochloric acid added to the alumina powder is 0.1, which is a preferred embodiment because the ratio also decreases.
% not 7.7 In this case, the effect of the addition is not significant; on the other hand, if it exceeds 1%, the corresponding addition effect will not appear (in fact, the equipment material will be corroded by one chlorine gas generated). So I don't like it.
本発明方法において原料高純度アルミナ粉末に塩酸を添
加すること1こより何故遷移アルミナの生成が低いのか
詳らかではないが、高純度化1こついてはアルミナ中l
こ含有される鉄、シリカ、゛ノーズ等が塩酸と共存し、
2000℃以上の温度で高温加熱されること(こより揮
発性塩化物を形成し、蒸発除去されるものと推測される
。Although it is not clear why the production of transition alumina is lower due to the addition of hydrochloric acid to the raw material high purity alumina powder in the method of the present invention,
Iron, silica, nose, etc. contained in this coexist with hydrochloric acid,
It is assumed that volatile chlorides are formed and removed by evaporation due to high temperature heating at a temperature of 2000° C. or higher.
以上計述した本発明方法にょJl、は(・ハめてr11
単な方法で純度低下がなく、遷移アルミナ晶への転移を
少なくして流動性の優れた高純度アルミナを得ることを
可能としたものであり、その工業的価値は頗を大なるも
のである。The method of the present invention as described above is (・Hame r11
This method makes it possible to obtain high-purity alumina with excellent fluidity by reducing the transition to transitional alumina crystals without reducing the purity, and its industrial value is enormous. .
以下本発明方法を実施例シこより気蚤こ詳細に説明する
。The method of the present invention will be explained in more detail below with reference to Examples.
実施例
ミョウバン法Vこより合成した篩純度α−アルミテ粉末
(平均粒径1oμill 、純度99、95 ?6 )
を粉末供給手段を介してプロパン−酸素火炎中Iこ投入
した。溶射条件はプロパンl On? / 11. ?
+f素60yy//h、殿料アルミナ粉末投入M 10
kQ / llとした。Example Sieve purity α-almite powder synthesized by alum method V (average particle size 1oμill, purity 99, 95-6)
was introduced into a propane-oxygen flame via a powder feed means. Thermal spraying conditions are propane l On? / 11. ?
+f element 60yy//h, alumina powder input M 10
kQ/ll.
(粉末キャリアガス、酸素1 m” / b )溶1寸
されたアルミナ粉末は中空のステンレスパイフ(100
yw×1000**e )ヲaaシた後水中に捕集した
。(Powder carrier gas, oxygen 1 m”/b) The melted alumina powder was placed in a hollow stainless steel pipe (100 m”/b).
yw×1000**e) was collected in water after washing.
取得されたアルミナ粒子はX線的Iこ90%以上かα−
アルミナ粒子で、一部γ−アルミナの生成がみられた。The obtained alumina particles have an X-ray I of more than 90% or α-
Formation of γ-alumina was observed in some of the alumina particles.
平均粒径は8μmでほぼ球形であった。この粒子の重装
密度は2.80r/y、軽装密度は2.12r/eaで
あり、この粒子の安息角を測定した結果30度であり、
溶射処理前の粉末の安息角は35°であり、流動性が改
良されていることか分った。The average particle size was 8 μm and approximately spherical. The heavy density of this particle is 2.80 r/y, the light density is 2.12 r/ea, and the angle of repose of this particle is 30 degrees,
The angle of repose of the powder before thermal spraying was 35°, indicating improved flowability.
実施例2
第1表に示す条件で実施例1と同様に高純度アルミナ粉
末の溶射処理を行なった。Example 2 High purity alumina powder was thermally sprayed in the same manner as in Example 1 under the conditions shown in Table 1.
処理条件、得られた^純度アルミナ粒子の特性を第1表
1こ示す。Table 1 shows the processing conditions and characteristics of the obtained pure alumina particles.
第1表Table 1
Claims (1)
し、該粉末表面を溶融或は半溶融することを特徴とする
高純度アルミナ粒子の製造方法。 2)酸素過剰の高温火炎中に投入する高純度アルミナ粉
末が高純度アルミナ100重量部に対し塩酸0.1〜1
重量部添加したものであることを特徴とする特許請求の
範囲第1項記載の方法。[Claims] l) A method for producing high-purity alumina particles, which comprises: introducing high-purity alumina powder into a sieve flame with excess oxygen, and melting or semi-melting the powder surface. 2) High-purity alumina powder added to a high-temperature flame with excess oxygen contains 0.1 to 1 part of hydrochloric acid per 100 parts by weight of high-purity alumina.
The method according to claim 1, characterized in that part by weight is added.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57205088A JPS5997527A (en) | 1982-11-22 | 1982-11-22 | Manufacture of high purity alumina particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57205088A JPS5997527A (en) | 1982-11-22 | 1982-11-22 | Manufacture of high purity alumina particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5997527A true JPS5997527A (en) | 1984-06-05 |
Family
ID=16501223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57205088A Pending JPS5997527A (en) | 1982-11-22 | 1982-11-22 | Manufacture of high purity alumina particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5997527A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62191420A (en) * | 1986-02-17 | 1987-08-21 | Showa Alum Ind Kk | Spherical corundum particle and production thereof |
| JPH05294613A (en) * | 1991-11-28 | 1993-11-09 | Showa Denko Kk | Spherical corundum particle |
| WO2024128321A1 (en) * | 2022-12-16 | 2024-06-20 | デンカ株式会社 | Powder of spherical alumina particles |
-
1982
- 1982-11-22 JP JP57205088A patent/JPS5997527A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62191420A (en) * | 1986-02-17 | 1987-08-21 | Showa Alum Ind Kk | Spherical corundum particle and production thereof |
| JPH05294613A (en) * | 1991-11-28 | 1993-11-09 | Showa Denko Kk | Spherical corundum particle |
| WO2024128321A1 (en) * | 2022-12-16 | 2024-06-20 | デンカ株式会社 | Powder of spherical alumina particles |
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