JPH03100145A - Production of aluminum alloy plate having white color tone after anodic oxidation treatment - Google Patents
Production of aluminum alloy plate having white color tone after anodic oxidation treatmentInfo
- Publication number
- JPH03100145A JPH03100145A JP23914289A JP23914289A JPH03100145A JP H03100145 A JPH03100145 A JP H03100145A JP 23914289 A JP23914289 A JP 23914289A JP 23914289 A JP23914289 A JP 23914289A JP H03100145 A JPH03100145 A JP H03100145A
- Authority
- JP
- Japan
- Prior art keywords
- less
- aluminum alloy
- range
- intermetallic compounds
- treatment
- 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.)
- Granted
Links
- 238000011282 treatment Methods 0.000 title claims abstract description 88
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 230000003647 oxidation Effects 0.000 title abstract description 8
- 238000007254 oxidation reaction Methods 0.000 title abstract description 8
- 229910000765 intermetallic Inorganic materials 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000000956 alloy Substances 0.000 claims abstract description 32
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 30
- 238000005266 casting Methods 0.000 claims abstract description 28
- 230000001105 regulatory effect Effects 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 238000007743 anodising Methods 0.000 claims description 70
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 28
- 238000007788 roughening Methods 0.000 claims description 24
- 239000010407 anodic oxide Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims 3
- 230000007547 defect Effects 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000005096 rolling process Methods 0.000 abstract 1
- 235000019646 color tone Nutrition 0.000 description 38
- 230000007797 corrosion Effects 0.000 description 17
- 238000005260 corrosion Methods 0.000 description 17
- 230000000694 effects Effects 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000002048 anodisation reaction Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 7
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 239000004566 building material Substances 0.000 description 4
- 238000005097 cold rolling Methods 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 4
- 238000005098 hot rolling Methods 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- 238000004040 coloring Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- 229910018084 Al-Fe Inorganic materials 0.000 description 2
- 229910018192 Al—Fe Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 235000019445 benzyl alcohol Nutrition 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009749 continuous casting Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 241000218642 Abies Species 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000012733 comparative method Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Landscapes
- Continuous Casting (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
この発明は陽極酸化処理を施して使用される用途のアル
ミニウム合金材料、特にビルのカーテンウオールや内装
材などの建材、あるいは器物、容器、電気計測機器筐体
、装飾品等に使用されるアルミニウム合金板材の製造方
法に関するものである。[Detailed Description of the Invention] Industrial Application Field This invention is applicable to aluminum alloy materials used after anodizing, especially building materials such as curtain walls and interior materials of buildings, as well as utensils, containers, and electrical measuring instruments. The present invention relates to a method for manufacturing aluminum alloy plates used for housings, decorative items, etc.
従来の技術
一般にカーテンウオールや内装材などの建材、あるいは
器物、容器、電気計測機器筐体などに使用されるアルミ
ニウム合金は、耐食性の観点から陽極酸化処理を施して
用いられることが多い。これらの用途の陽極酸化処理用
アルミニウム合金としては、暗灰色からシルバー系のも
のが多く、このような合金としては一般に月81050
050合金00合金、5005005合金03003合
金用されることが多く、また灰色系のものとしてはAl
−1〜4%Si合金が一般的である。また陽極酸化51
!L理としては、経済性および耐食性の点から硫酸電解
浴が多用されている。BACKGROUND OF THE INVENTION Aluminum alloys, which are generally used for building materials such as curtain walls and interior materials, or for appliances, containers, electrical measuring equipment casings, etc., are often subjected to anodizing treatment from the viewpoint of corrosion resistance. Aluminum alloys for anodizing treatment for these purposes are often dark gray to silver in color, and such alloys generally include Tsuki 81050.
050 alloy 00 alloy, 5005005 alloy 03003 alloy are often used, and as a gray type, Al
-1 to 4% Si alloys are common. Also, anodizing 51
! As the L treatment, a sulfuric acid electrolytic bath is often used from the viewpoint of economy and corrosion resistance.
ところで前述のような用途では、美観のために陽極酸化
処理後の表面に対して種々の色調を有することが要求さ
れる場合がある。陽極酸化処理板に所要の色調を与える
ための方法としては、塗装、染色、二次電解着色、合金
発色、陽極酸化処理液による発色等があるが、経済的観
点および耐食性の観点からは、陽極酸化処理のまま、特
に硫酸浴による陽極酸化処理のままでの発色が望まれて
いる。By the way, in the above-mentioned applications, the surface after anodizing treatment may be required to have various color tones for aesthetic reasons. Methods for imparting the desired color tone to anodized plates include painting, dyeing, secondary electrolytic coloring, alloy coloring, and coloring with an anodizing solution, but from an economical and corrosion-resistant perspective, anodizing It is desired to develop color even after oxidation treatment, especially after anodization treatment using a sulfuric acid bath.
各種の色調のうちでも、白色は清潔感を与え、また心理
的に安心感を与えるところから、建材等の用途において
も白色の色調が要求されることが多くなっている。しか
しながら、従来は陽極酸化処理のまま、特に硫酸浴によ
る陽極酸化処理のままで白色の色調を有する陽極酸化処
理板を得ることは極めて困難とされており、そこで従来
は陽極酸化処理後に染色を施す方法、すなわち多孔質陽
極酸化皮膜のボアに白色顔料を封じ込める方法を適用せ
ざるを得なかったのが実情である。Among various color tones, white color gives a sense of cleanliness and gives a psychological sense of security, so white color tone is increasingly required for applications such as building materials. However, it has traditionally been extremely difficult to obtain an anodized board with a white tone after anodization treatment, especially after anodization treatment using a sulfuric acid bath. The reality is that we had no choice but to apply a method of sealing the white pigment into the bores of the porous anodic oxide film.
また一方、用途や使用箇所によっては、同じ白色でもマ
ット状の無光沢の白色の色調が求められる場合もあるが
、このような無光沢の白色の色調を陽極酸化処理のまま
で得ることは従来は困難とされていた。On the other hand, depending on the application and location of use, a matte, matte white tone may be required, but it is conventionally impossible to obtain such a matte white tone by anodizing. was considered difficult.
発明が解決しようとする課題
前述のような染色法により白色の色調を有する陽極酸化
処理板を得る方法では、耐食性が極めて低く、ピルのカ
ーテンウオール等に使用すれば短期間で白色の減退が生
じてしまい、したがってこれらの用途には染色法は実際
上適用し得なかった。Problems to be Solved by the Invention The method of obtaining an anodized plate with a white tone using the dyeing method described above has extremely low corrosion resistance, and when used for curtain walls of pills, etc., the white color fades in a short period of time. Therefore, the dyeing method could not be practically applied to these applications.
ところで一般にアルミニウム合金表面を梨地処理やプラ
スト処理により粗面化すれば、合金自体の表面は白色化
することが可能であるが、従来陽極酸化処理用合金とし
て使用されているJIS 1050050合金00合金
、5005005合金03003合金、陽極酸化処理前
に前述のような粗面化により表面を白色化しておいても
、充分な程度の耐食性が得られるように陽極酸化処理を
施せば、陽極酸化処理により着色されたり白色が減退し
たりして、最終的に白色の色調が得られなくなってしま
うのが実情である。したがって粗面化処理により合金表
面を白色化した後に陽極酸化処理を施す方法は、従来の
アルミニウム合金については実際上は適用できないもの
と考えられていた。By the way, in general, if the surface of an aluminum alloy is roughened by a satin finish treatment or a blast treatment, the surface of the alloy itself can be made white. 5005005 alloy 03003 alloy, even if the surface is whitened by roughening as described above before anodizing, if anodizing is performed to obtain a sufficient degree of corrosion resistance, the color will not be colored by anodizing. The reality is that the white color decreases, and eventually it becomes impossible to obtain a white tone. Therefore, it has been thought that the method of whitening the alloy surface by surface roughening treatment and then subjecting it to anodizing treatment is not practically applicable to conventional aluminum alloys.
この発明は以上の事情を背景としてなされたもので、陽
極酸化処理のまま(特に硫酸浴による陽極酸化処理のま
ま)で白色の色調が待られるアルミニウム合金板を提供
することを基本的な目的とするものである。またこの発
明は、白色の色調のうちでもマット状の無光沢の白色の
色調が陽極酸化518理のままで得られるアルミニウム
合金板を提供することを第2の目的とする。This invention was made against the background of the above-mentioned circumstances, and its basic purpose is to provide an aluminum alloy plate that has a white color even after being anodized (particularly after being anodized in a sulfuric acid bath). It is something to do. A second object of the present invention is to provide an aluminum alloy plate in which a matte, matte white color tone among white colors can be obtained as is by anodizing 518 process.
WI題を解決するための手段
前述のような課題を解決するため本発明者等が鋭意実験
・検討を重ねた結果、アルミニウム合金の成分組成を適
切に調整するとともに、製造プロセス、特に鋳塊の加熱
条件を適切に調整して、最終板における金属間化合物を
調整することによって、陽極酸化処理のままで白色の色
調が得られることを見出し、この発明をなすに至った。Means for Solving the WI Problem In order to solve the above-mentioned problems, the inventors of the present invention have conducted extensive experiments and studies, and have found that the composition of the aluminum alloy has been appropriately adjusted, and the manufacturing process, especially the ingot, has been improved. It was discovered that by appropriately adjusting the heating conditions and adjusting the intermetallic compounds in the final plate, a white color tone could be obtained as is after the anodization treatment, and this invention was achieved.
またこの場合、陽極酸化処理前に表面に粗面化処理を施
しておけば、陽極酸化処理後に一層白色度が優れかつ無
光沢の白色の色調が得られることを見出した。In this case, it has also been found that if the surface is roughened before the anodizing treatment, a matte white color tone with even better whiteness can be obtained after the anodizing treatment.
具体的には、請求項1〜4の発明は、陽極酸化処理前の
粗面化を行なわずに、陽極酸化処理後に白色の色調が得
られるようにしたアルミニウム合金板の製造方法を提供
するものである。Specifically, the inventions of claims 1 to 4 provide a method for manufacturing an aluminum alloy plate in which a white tone can be obtained after anodizing treatment without roughening the surface before anodizing treatment. It is.
すなわち先ず請求項1の発明のアルミニウム合金板の製
造方法は、l”eを0.8〜z、owt%含有しかつS
iが0゜2wt%以下に規制され、残部がAlおよび不
可避的不純物よりなる合金を素材とし、その合金を35
〜150u/鴎のI造速度でDC鋳造した後、鋳塊に5
50〜630℃の範囲内の温度で0.5〜24時間加熱
処理を施し、その後圧延して最終板厚とし、これにより
金属間化合物の90%以上が大きさ5趨以下であってか
つ金属間化合物の総量が2.5〜7wt%の範囲内にあ
り、しかも金属間化合物AZ6 Fe1とAl3Feの
比がAl6Fe/<Af3Fe+Af6Fe)≦0.1
の範囲内にあるアルミニウム合金板を得ることを特徴と
するものである。That is, first of all, the method for producing an aluminum alloy plate of the invention of claim 1 contains 0.8 to z owt% of l"e and S
The material is an alloy in which i is regulated to 0°2wt% or less, and the balance is Al and unavoidable impurities.
After DC casting at a production rate of ~150u/kao, the ingot was
Heat treatment is performed at a temperature in the range of 50 to 630°C for 0.5 to 24 hours, and then rolled to give the final thickness, so that at least 90% of the intermetallic compounds are of size 5 or less and are metal. The total amount of intermetallic compounds is within the range of 2.5 to 7 wt%, and the ratio of intermetallic compounds AZ6 Fe1 to Al3Fe is Al6Fe/<Af3Fe+Af6Fe)≦0.1
The present invention is characterized by obtaining an aluminum alloy plate within the range of .
また請求項2の発明のアルミニウム合金板の製造方法は
、Feを0.8〜2.0wt%含有するとともに、M
n 0.05〜0.2wt%、M(J 0.05〜1.
5wt%、Cr 0.05〜0.1wt%のうちの1種
または2種以上を含有し、かつSiが0.2wt%以下
に規制され、残部がA2および不可避的不純物よりなる
合金を素材とし、請求項1の発明と同様に処理して、前
記同様に金属間化合物が規制されたアルミニウム合金板
ををることを特徴とするものである。Further, the method for manufacturing an aluminum alloy plate according to the invention of claim 2 includes Fe containing 0.8 to 2.0 wt%, and M
n 0.05-0.2wt%, M(J 0.05-1.
5 wt%, Cr 0.05 to 0.1 wt%, or more, Si is regulated to 0.2 wt% or less, and the balance is A2 and unavoidable impurities. This invention is characterized in that it is processed in the same manner as in the invention of claim 1 to produce an aluminum alloy plate in which intermetallic compounds are regulated in the same manner as described above.
さらに請求項3の発明のアルミニウム合金板の製造方法
は、請求項1の発明と同様にして得られたアルミニウム
合金板に対し、さらにH2SO4濃度が10〜25四島
の硫酸電解浴を用いて浴温度15〜30℃、電流密度0
.5A/lii以上1.OA/1M未満で陽極酸化処理
を施して膜厚10〜25IJmの陽極酸化皮膜を形成す
ることを特徴とするものである。Furthermore, the method for producing an aluminum alloy plate according to the invention of claim 3 further includes using a sulfuric acid electrolytic bath having a H2SO4 concentration of 10 to 25 to 100% by temperature. 15-30℃, current density 0
.. 5A/lii or more1. It is characterized in that it is anodized at less than OA/1M to form an anodic oxide film with a thickness of 10 to 25 IJm.
また請求項4の発明のアルミニウム合金板の製造方法は
、請求項2の発明と同様にして得られたアルミニウム合
金板に対し、請求項3の発明と同様な陽極酸化処理を施
すことを特徴とするものである。Furthermore, the method for producing an aluminum alloy plate according to the invention of claim 4 is characterized in that the aluminum alloy plate obtained in the same manner as the invention of claim 2 is subjected to the same anodizing treatment as the invention of claim 3. It is something to do.
一方請求項5、請求項6の発明は、いずれも陽極酸化処
理前に粗面化処理を施して、陽極酸化処理後に無光沢の
白色の色調が得られるようにしたアルミニウム合金板の
製造方法を提供する。On the other hand, the inventions of claims 5 and 6 both provide a method for producing an aluminum alloy plate in which a surface roughening treatment is performed before anodizing treatment so that a matte white color tone is obtained after the anodizing treatment. provide.
すなわち請求項5の発明のアルミニウム合金板の製造方
法は、Feを0.8〜2. owt%含有しかつSlが
0.2宵t%以下に規制され、残部がAlおよび不可避
的不純物よりなる合金を素材とし、その合金を35〜1
50闇/11tlの鋳造速度でDC鋳造した後、鋳塊に
550〜630℃の範囲内の温度で0.5〜24時間の
加熱処理を施した後、圧延して最終板厚とし、その後表
面に粗面化処理を施して表面の色調を白色に調整し、さ
らにその粗面化処理後の板に対し、H2804濃度が1
0〜25V@1%の硫酸電解浴を用いて浴温度15〜3
0℃、電流密度0.5A/dg!以上1.OA/ds1
未満で陽極酸化処理を施して膜厚10〜25IJIIの
陽極酸化皮膜を形成することを特徴とするものである。That is, in the method for producing an aluminum alloy plate according to the fifth aspect of the invention, Fe is contained in a range of 0.8 to 2. owt% and whose Sl is regulated to 0.2t% or less, with the balance being Al and unavoidable impurities, and the alloy is
After DC casting at a casting speed of 50 mm/11 tl, the ingot is heat treated at a temperature within the range of 550-630°C for 0.5-24 hours, then rolled to the final thickness, and then the surface The surface color tone of the surface is adjusted to white by roughening treatment, and after the roughening treatment, the H2804 concentration is 1.
Bath temperature 15-3 using 0-25V@1% sulfuric acid electrolytic bath
0℃, current density 0.5A/dg! Above 1. OA/ds1
The method is characterized in that an anodic oxidation treatment is performed to form an anodic oxide film having a thickness of 10 to 25 IJII.
また請求項6の発明のアルミニウム合金板の製造方法は
、Feを0.8〜2.owt%含有するとともに、M
n 0.05〜0.2wt%、fVIG 0.05〜1
.5wt%、Q r 0.05〜0.lt%のうちの1
1または2種以上を含有し、かつSiが0.2wt%以
下に規制され、残部が八2および不可避的不純物よりな
る合金を素材とし、請求項5の発明と同様な処理を施す
ことを特徴とするものである。Further, in the method for manufacturing an aluminum alloy plate according to the invention of claim 6, Fe is contained in a range of 0.8 to 2. Contains owt% and M
n 0.05-0.2wt%, fVIG 0.05-1
.. 5wt%, Q r 0.05-0. 1 of lt%
The material is made of an alloy containing one or more of two or more types, in which Si is regulated to 0.2 wt% or less, and the remainder is 82 and unavoidable impurities, and is subjected to the same treatment as the invention of claim 5. That is.
作 用
先ず素材アルミニウム合金の成分限定理由について説明
する。Function First, the reason for limiting the composition of the aluminum alloy material will be explained.
Fe:
FeはAl−Fe系の金属間化合物を生成して、陽極酸
化処理後の色調を決定付ける重要な元素である。すなわ
ち、鋳塊加熱条件(均質化処理条件)との組合せによっ
て金属間化合物Al6Feが増加すれば陽極酸化処理後
の色調が白色になる。Fe: Fe is an important element that generates an Al-Fe-based intermetallic compound and determines the color tone after anodizing treatment. That is, if the intermetallic compound Al6Fe increases in combination with the ingot heating conditions (homogenization treatment conditions), the color tone after the anodization treatment becomes white.
1”e量が2.0wt%を越えれば粗大化合物が増加し
て陽極酸化処理後の色調が黄味を帯びるようになり、一
方1”e量がo、 awt%未満ではAl−Fe系金属
間化合物の絶対数が少なく、全体に色が浅くなって白色
と言うよりもシルバー系となる。したがってFelは0
.8〜2.owt%の範囲内とした。If the 1"e amount exceeds 2.0 wt%, coarse compounds will increase and the color tone after anodizing will become yellowish, while if the 1"e amount is less than o, awt%, Al-Fe based metal The absolute number of interstitial compounds is small, and the overall color is shallower, making it more silvery than white. Therefore, Fel is 0
.. 8-2. It was set within the range of % by weight.
Si:
Siは鋳塊中に樅の本組織と称される異常ll114I
lを生成させやすい。鋳塊に樅の本組織が発生すれば、
圧延板を陽極酸化処理した際に表面にストリークスと称
される帯状の模様が生じ、外観を損なう。この樅の本組
織の発生を防ぐためには、Si圭を0.2wt%以下に
規制する必要がある。Si: Si has an abnormality called fir main structure in the ingot.
It is easy to generate l. If the fir structure occurs in the ingot,
When a rolled plate is anodized, band-like patterns called streaks are produced on the surface, which impairs the appearance. In order to prevent the occurrence of this fir-like structure, it is necessary to restrict Si to 0.2 wt% or less.
以上のFe、Siのほかは基本的にはAlおよびその他
の不可避的不純物とすれば良いが、必要に応じてMn、
MG、Qrのうちの1!#または2種以上を添加しても
良い。これらの添加理由、添加量限定理由は次の通りで
ある。In addition to the above Fe and Si, basically Al and other unavoidable impurities can be used, but if necessary, Mn,
MG, one of Qr! # or two or more types may be added. The reason for these additions and the reason for limiting the amount added are as follows.
Mn :
Mnは鋳塊中のAffi6Feを安定化し、樅の本組織
を発生しにくくする元素であり、特にSilが0.1〜
0.2wt%程度と比較的多い場合に、Mnの添加によ
る樅の本組織発生防止効果が大きい。Mn: Mn is an element that stabilizes Affi6Fe in the ingot and makes it difficult to generate fir structure, especially when Sil is 0.1~
When Mn is added in a relatively large amount of about 0.2 wt%, the effect of preventing the formation of this structure in fir is large.
Mn量が0.05 wt%未満では上述の効果が不充分
であり、一方0.2wt%を越えれば陽極酸化処理後の
色調が赤味を帯び、この発明で目的とする無彩色系から
外れてしまう。したがってMnを添加する場合のMn添
加量は0.05〜G、2wt%とした。If the amount of Mn is less than 0.05 wt%, the above-mentioned effect will be insufficient, while if it exceeds 0.2 wt%, the color tone after anodizing will be reddish and will deviate from the achromatic color system aimed at in this invention. I end up. Therefore, when adding Mn, the amount of Mn added was 0.05-G, 2 wt%.
M9: M9は強度向上のために添加されることがある。M9: M9 is sometimes added to improve strength.
Mchlが0.05 wt%未満では強度向上効果が充
分に得られず、一方1 、5wt%を越えれば鋳塊に樅
の本組織が発生しやすくなってしまう。したがってM9
を添加する場合のM9添加量は0.05〜1.5vt%
の範囲内とした。If Mchl is less than 0.05 wt%, a sufficient strength-improving effect cannot be obtained, while if it exceeds 1.5 wt%, the fir structure tends to occur in the ingot. Therefore M9
When adding M9, the amount of M9 added is 0.05 to 1.5vt%
was within the range of
Cr: Crも強度向上のために添加されることがある。Cr: Cr may also be added to improve strength.
Cr量が0.05 wt%未満では強度向上効果が充分
に得られず、一方0.1wt%を越えれば陽極酸化処理
後の色調が黄味を帯びるようになり、白色から外れる。If the Cr amount is less than 0.05 wt%, a sufficient strength improvement effect cannot be obtained, while if it exceeds 0.1 wt%, the color tone after the anodizing treatment becomes yellowish and deviates from white.
したがってCrを添加する場合のCr添加量は0.05
〜0.1wt%の範囲内とした。Therefore, when adding Cr, the amount of Cr added is 0.05
It was set within the range of ~0.1 wt%.
また一般のアルミニウム合金においては、鋳塊の結晶粒
微細化のために微量のT i NもしくはTiおよびB
を添加することがあるが、この発明の場合も微量のTi
もしくはTiおよびBが添加されても良く、これらの添
加による結晶粒微細化効果によって圧延板のキメ、スト
リークスを防止する効果が青られる。その場合、Tiが
0.003wt%未満では上記の効果が得られず、一方
7iが0.15 wt%を越えればTiA1’3の粗大
金属間化合物が生成されるおそれがあるから、Tiは0
、003〜0.15 wt%の範囲内とすることが好ま
しい。またBはTiとの共存により結晶粒微細化効果を
発揮するが、BがIppH未満ではその効果が得られず
、1100pp1を越えれば粗大T r 82粒子によ
る線状欠陥が発生するから、Bは1〜100ppHの範
囲内とすることが望ましい。In addition, in general aluminum alloys, trace amounts of TiN or Ti and B are added to refine the grains of the ingot.
However, in the case of this invention, a trace amount of Ti is also added.
Alternatively, Ti and B may be added, and the grain refinement effect of these additions enhances the effect of preventing texture and streaks in the rolled plate. In that case, if Ti is less than 0.003 wt%, the above effect cannot be obtained, while if 7i exceeds 0.15 wt%, a coarse intermetallic compound of TiA1'3 may be generated.
, 003 to 0.15 wt%. In addition, B exhibits a crystal grain refining effect when it coexists with Ti, but this effect cannot be obtained if B is less than IppH, and if it exceeds 1100pp1, linear defects will occur due to coarse T r 82 particles. It is desirable that the pH is within the range of 1 to 100 ppH.
次に製造条件について説明する。Next, manufacturing conditions will be explained.
先ず前述のような成分組成範囲内のアルミニウム合金の
溶湯を常法にしたがって溶製し、鋳造速度35〜150
闇/1111にてDC鋳造(半連続鋳造)する。ここで
、鋳造速度は鋳塊における樅の木lll14m発生に影
響し、鋳造速度が通過ぎれば樅の本組織が発生しやすく
なる。鋳造速度が35a/噛未満では生産性が低過ぎて
経済的ではなく、一方150朋/ mnを越えれば樅の
本組織が発生して圧延板にストリークスが生じ、外観を
損なう。したがって鋳造速度は35〜150馴/馳の範
囲内とした。First, a molten aluminum alloy within the above-mentioned composition range is melted according to a conventional method, and the casting speed is 35 to 150.
DC casting (semi-continuous casting) in darkness/1111. Here, the casting speed affects the formation of fir trees in the ingot, and if the casting speed is too high, the fir structure is likely to occur. If the casting speed is less than 35 mm/mn, the productivity is too low to be economical, while if it exceeds 150 mm/mn, fir grain structure will occur and streaks will occur in the rolled plate, spoiling the appearance. Therefore, the casting speed was set within the range of 35 to 150 m/h.
次いで、鋳塊に対し550〜630℃の範囲内の温度で
0.5〜24時間の加熱を施す。この鋳塊加熱は、−船
釣な鋳塊組織均質化のために必要であるばかりでなく、
陽極酸化処理後の色調に大きな影響を及ぼす。すなわち
この鋳塊加熱によって鋳塊中の金属間化合物Aβ6Fe
がA11a Feに変態し、後述するように最終板厚の
板においてAss )”e/ (Aj!s Fe+Aj
>3Fe)の値がo、ia下になって、圧延板の陽極酸
化処理後に白色の色調ををることが可能となる。鋳塊加
熱温度が550℃未満では、最終板厚の板における
ARs Fe/ (Aj!s Fe+Al3Fe)の値
が0.1より大きくなり、陽極酸化処理後の色調として
灰色が強くなり、白色とは言えなくなる。一方鋳塊加熱
温度が630℃を越えれば、結晶粒の粗大化が生じて陽
極酸化処理後にストリークスが生じ、また場合によって
は局部溶融が生じることもある。Next, the ingot is heated at a temperature in the range of 550 to 630°C for 0.5 to 24 hours. This ingot heating is not only necessary for homogenizing the ingot structure, but also
It has a great effect on the color tone after anodizing. That is, by heating the ingot, the intermetallic compound Aβ6Fe in the ingot
transforms into A11a Fe, and as will be described later, in the final thickness of the plate Ass )”e/ (Aj!s Fe+Aj
>3Fe) becomes below o, ia, and it becomes possible to obtain a white color tone after anodizing the rolled plate. When the ingot heating temperature is less than 550°C, the value of ARs Fe/ (Aj!s Fe+Al3Fe) in the final plate thickness becomes larger than 0.1, and the color tone after anodizing treatment becomes more gray, and the color is not white. I can't say it anymore. On the other hand, if the ingot heating temperature exceeds 630°C, crystal grains will become coarser, streaks will occur after anodizing treatment, and local melting may occur depending on the case.
したがって鋳塊加熱温度は550℃〜630℃の範囲内
とする必要がある。また鋳塊加熱時間が0.5時間未満
では上述の効果が充分に得られず、一方24時間を越え
ても効果は飽和し、コスト上昇を招くだけであるから、
0.5〜24時間に限定した。Therefore, the ingot heating temperature needs to be within the range of 550°C to 630°C. Furthermore, if the ingot heating time is less than 0.5 hours, the above-mentioned effects will not be sufficiently obtained, while if it exceeds 24 hours, the effect will be saturated and the cost will only increase.
It was limited to 0.5 to 24 hours.
上述のような鋳塊加熱の後、熱間圧延および冷間圧延を
行なって最終板厚とする。ここで、熱間圧延は常法にし
たがって行なえば良いが、鋳塊の加熱温度以下で行なう
のが一般的である。熱間圧延の直後、あるいは冷間圧延
の間には、中間焼鈍を行なっても良い。中間焼鈍は、2
50〜450℃で0.5〜12時間行なうのが一般的で
ある。After heating the ingot as described above, hot rolling and cold rolling are performed to obtain the final thickness. Here, hot rolling may be carried out according to a conventional method, but it is generally carried out at a temperature below the heating temperature of the ingot. Intermediate annealing may be performed immediately after hot rolling or during cold rolling. Intermediate annealing is 2
Generally, the heating is carried out at 50 to 450°C for 0.5 to 12 hours.
このようにして得られた最終板の圧延板においては、金
属間化合物が次のように規制されている必要がある。す
なわち、
■ 金属間化合?!lAi!6FeとAl3Feの比(
重量化)が、
Al6Fe/<Aj’3Fe+Al5Fe)≦0.1を
満たしていること。In the final rolled plate thus obtained, intermetallic compounds must be regulated as follows. In other words, ■ Intermetallic compound? ! lAi! The ratio of 6Fe and Al3Fe (
weight) satisfies Al6Fe/<Aj'3Fe+Al5Fe)≦0.1.
■ 金属間化合物の全数のうち90%以上が大きさ5#
以下であること。■ More than 90% of the total number of intermetallic compounds are size 5#
Must be below.
■ 金属間化合物のalが2.5〜7wt%の範囲内に
あること。(2) Al of the intermetallic compound must be within the range of 2.5 to 7 wt%.
これらの金属間化合物に関する限定理由は次の通りであ
る。The reasons for the limitations regarding these intermetallic compounds are as follows.
Als Fe/ (Al3Fe+AJFs Fe)の値
が0,1を越えれば、陽極酸化処理後の色調が灰色がか
ってきて、白色とは言えなくなる。また5顯を越える大
径の金属間化合物が10wt%を越えれば、陽極酸化処
理後の色調が浅くなり、白色から外れる。さらに金属間
化合物のIIが2.5wt%未満では陽極酸化処理後の
色調が浅くなり、充分な白色が得られない。一方金属間
化合物の4@量が7wt%を越えれば、陽極酸化処理後
の色調が黄味を帯びて、白色とは言えなくなる。If the value of Als Fe/(Al3Fe+AJFs Fe) exceeds 0.1, the color tone after the anodizing treatment becomes grayish and cannot be called white. Furthermore, if the amount of intermetallic compounds with a diameter exceeding 5 mm exceeds 10 wt%, the color tone after anodizing becomes shallow and deviates from white. Furthermore, if the amount of II of the intermetallic compound is less than 2.5 wt%, the color tone after the anodizing treatment becomes shallow, and a sufficient white color cannot be obtained. On the other hand, if the amount of 4@ of the intermetallic compound exceeds 7 wt%, the color tone after the anodizing treatment becomes yellowish and cannot be called white.
このように最終板厚の圧延板における金属間化合物を所
定の条件範囲内に規制しておくことによって、その後陽
極酸化処理を施せば白色の色調を得ることができる。こ
こで、請求項1および請求項2の発明の方法では、金属
間化合物を所定の条件範囲内に規制した最終板厚の圧延
板を得るまでの工程で全プロセスは終了するが、請求項
3および請求項4の発明のプロセスでは、さらにその最
終板厚の板に対して積極的に陽極酸化処理を施すまでの
プロセスを含む。By regulating the intermetallic compounds in the rolled sheet of final thickness within a predetermined condition range in this manner, a white color tone can be obtained by subsequently performing anodizing treatment. Here, in the method of the invention according to claims 1 and 2, the entire process is completed until a rolled plate with a final thickness in which the intermetallic compound is regulated within a predetermined condition range is obtained. The process of the invention according to claim 4 further includes a process of actively anodizing the plate having the final thickness.
陽極酸化処理にあたっては、予め表面の汚れおよび表面
の欠陥を除去しておくため、脱脂およびエツチングを行
なうのが一般的である。エツチングは、苛性ソーダ系の
アルカリエツチングを行なうのが通常である。そして陽
極酸化処理自体は、H28041度が10〜25vo1
%の硫酸浴を用イ、浴温度15〜30℃、電流密度0.
5A/dd以上1.OA /d未満で行ない、膜厚10
〜25μmの陽極酸化皮膜を生成させる。Before anodizing, degreasing and etching are generally performed to remove surface stains and surface defects in advance. Etching is usually performed using caustic soda-based alkaline etching. And the anodizing process itself is H28041 degree 10~25vo1
% sulfuric acid bath, bath temperature 15-30°C, current density 0.
5A/dd or more1. Conducted at less than OA/d, film thickness 10
Produce an anodic oxide film of ~25 μm.
ここで、硫酸浴のH2SO4濃度がIOV@1%未満で
は陽極酸化処理後の色調が黄味を帯びるようになり、ま
た皮膜の多孔度が減少して浴電圧が高くなる。一方82
8041度が25vo1%を越えれば、表面が荒れて陽
極酸化皮膜が柔かくなる。また浴温度が15℃未満では
陽極酸化処理後の色調に黄味が強くなって白色からずれ
てしまい、一方30℃を越えれば陽極酸化処理後の耐食
性が低下してしまう。さらに電流密度は、1.OA/d
gi以上では陽極酸化処理後の色調が黄味を帯びて、白
色からずれてしまい、一方0.5A/dIi未満では、
所要の膜厚の陽極酸化皮膜を生成するためにかなりの時
間を要してしまって生産性を阻害するとともに、耐食性
も低下する。また生成される陽極酸化皮膜の膜厚が10
趨未満では充分な耐食性が得られず、一方30/Jaを
越えるまで厚くすることは経済的でなく、しかも陽極酸
イヒ処理後の色調が黄味を帯びて白色からずれる。Here, if the H2SO4 concentration of the sulfuric acid bath is less than IOV@1%, the color tone after the anodizing treatment becomes yellowish, and the porosity of the film decreases, resulting in a high bath voltage. On the other hand 82
If 8041 degrees exceeds 25 vol%, the surface will become rough and the anodic oxide film will become soft. Further, if the bath temperature is less than 15°C, the color tone after the anodizing treatment will become more yellowish and will deviate from white, while if it exceeds 30°C, the corrosion resistance after the anodizing treatment will decrease. Furthermore, the current density is 1. OA/d
If it is more than gi, the color tone after anodizing becomes yellowish and deviates from white, while if it is less than 0.5A/dIi,
It takes a considerable amount of time to produce an anodic oxide film of the required thickness, which impedes productivity and also reduces corrosion resistance. In addition, the thickness of the anodic oxide film produced is 10
If the thickness is less than 30/Ja, sufficient corrosion resistance cannot be obtained, while increasing the thickness to more than 30/Ja is not economical, and furthermore, the color tone after the anodic acid treatment becomes yellowish and deviates from white.
一方請求項5および請求項6の発明のプロセスの場合は
、既に述べたようにして最終板厚の圧延板とした後、表
面に粗面化処理を施してから陽極酸化処理を施す。この
粗面化処理は、陽極酸化処理前の下地を予め白色化して
おくためのものであり、このように陽極酸化処理前の下
地を粗面化処理により白色化しておくことによって、陽
極酸化処理後の色調の白色度が増すとともに、マット状
の無光沢の白色が青られる。On the other hand, in the case of the process of the invention of claims 5 and 6, after the rolled plate of the final thickness is obtained as described above, the surface is roughened and then anodized. This surface roughening treatment is to whiten the base before anodizing treatment. By roughening the base before anodizing treatment in this way, it is possible to The whiteness of the later tones increases and the matte matte white becomes blue.
粗面化処理は、機械的粗面化、化学的粗面化、もしくは
電気化学的粗面化のいずれを適用しても良い。機械的粗
面化法としてはブラッシング、ブラスト等がある。化学
的粗面化法は、酸性浴による処理、アルカリ性浴による
処理に大別され、酸性浴による処理としては酸性弗化ア
ンモニウム系浴や燐酸浴による梨地処理などがあり、ア
ルカリ性浴による処理としては苛性ソーダ浴による梨地
処理などがある。さらに電気化学的方法としては、塩酸
もしくは硝酸浴中での交流電解グレイニングなどがある
。The surface roughening treatment may be mechanical roughening, chemical roughening, or electrochemical roughening. Mechanical surface roughening methods include brushing, blasting, and the like. Chemical surface roughening methods are broadly divided into treatments using acidic baths and treatments using alkaline baths. Treatments using acidic baths include satin finish using acidic ammonium fluoride baths and phosphoric acid baths, and treatments using alkaline baths include There is a satin finish treatment using a caustic soda bath. Further electrochemical methods include alternating current electrolytic graining in a hydrochloric acid or nitric acid bath.
なおこのような粗面化処理を行なった後の陽極酸化処理
は、既に述べた硫酸浴による陽極酸化処理と同じ条件で
行えば良い。Note that the anodizing treatment after such surface roughening treatment may be performed under the same conditions as the anodic oxidation treatment using the sulfuric acid bath described above.
以上のように、請求項1および請求項2の発明の方法は
、金属間化合物が所定の条件範囲内に規制された最終板
厚の圧延板を冑るものであって、このような圧延板にそ
の後陽極酸化処理を施すことによって、白色度の優れた
板を得ることができる。また請求項3および請求項4の
発明の方法は、前述のような最終板厚の圧延板にさらに
陽極酸化処理を施すものであって、これによって実際に
白色の板を得ることができる。一方請求項5および請求
項6の発明の方法では、陽極酸化51!L理前に予め粗
面化を施しておき、その後陽極酸化処理を施すことによ
って、光沢のないマット状の表面であってしかも白色度
の優れた板を得ることができる。As described above, the method of the invention of claims 1 and 2 is for removing a rolled plate having a final thickness in which intermetallic compounds are regulated within a predetermined condition range, and By subsequently subjecting the material to anodizing treatment, a board with excellent whiteness can be obtained. Further, in the method according to the third and fourth aspects of the invention, the rolled plate having the final thickness as described above is further subjected to an anodizing treatment, whereby a white plate can actually be obtained. On the other hand, in the method of the invention of claims 5 and 6, anodization 51! By roughening the surface beforehand and then anodizing it, it is possible to obtain a plate with a matte surface without gloss and excellent whiteness.
なお陽極酸化処理後の白色の色調については、ハンター
の色差式(JIS 、78730参照)による明度指数
りとクロマティクネス指数a、bの値によって評価する
ことができる。すなわち、明度指数のL値は高いほど白
く、一方りロマティクネス指数は着色度についてのもの
であってそのa値は高いほど赤味が強く、b値は高いは
と黄味が強いことをあられす。したがってL値が高くか
つa値、b値が零に近いほど、白色度が優れていると言
うことができる。ちなみに、請求項1〜4の発明の場合
は、陽極酸化処理後のL値、al、b値が、L〉75、
−2 <a< 2、−2 <b< 2を満たすことがで
きる。一方請求項5,6の発明の場合は、陽極酸化処理
後のL値、a値、b値が、L〉78、−2 <a< 2
、−2 <i)< 2を満たすことができる。Note that the white color tone after the anodizing treatment can be evaluated by the values of the brightness index and the chromaticness index a and b according to Hunter's color difference formula (see JIS, 78730). In other words, the higher the L value of the lightness index, the whiter it is, while the Romanticness index is about the degree of coloration, and the higher the A value, the stronger the reddish tinge, and the higher the B value, the stronger the yellowish tinge. . Therefore, it can be said that the higher the L value and the closer the a value and b value are to zero, the better the whiteness is. Incidentally, in the case of the inventions of claims 1 to 4, the L value, al, and b value after the anodizing treatment are L>75,
−2 < a < 2, −2 < b < 2 can be satisfied. On the other hand, in the case of the inventions of claims 5 and 6, the L value, a value, and b value after the anodizing treatment are L>78, -2 <a<2
, -2 < i) < 2 can be satisfied.
実施例
[実施例1]
第1表に示す合金1101〜9の溶湯を常法にしたがっ
て溶製し、第2表中に示すような鋳造速度(主に65m
m/min、一部は175mm/min)で半連続鋳造
法(DC鋳造法)によって断面寸法400謔×1000
層の鋳塊を鋳造した。得られた各鋳塊の一部をスライス
して、鋳塊組織を調べた。Examples [Example 1] Molten metals of alloys 1101 to 9 shown in Table 1 were melted according to a conventional method, and the casting speeds shown in Table 2 (mainly 65 m
The cross-sectional size is 400mm x 1000mm by semi-continuous casting method (DC casting method) at
A layer of ingot was cast. A portion of each obtained ingot was sliced to examine the ingot structure.
その結果を第2表中に併せて示す。第2表に示すように
、鋳造速度を175u/噛とした比較法、およびSil
が高い比較合金懇6、MQmが高い比較合金NQ8では
、樅の本組織が発生し、不合格と判定された。The results are also shown in Table 2. As shown in Table 2, the comparative method using a casting speed of 175u/mesh and the Sil
Comparative alloy No. 6 with a high MQm and comparative alloy NQ8 with a high MQm had fir structure and were determined to be rejected.
各合金No、 1〜9の鋳塊のうち、樅の本組織で代表
される異常が生じなかった鋳塊、すなわち合格と判定さ
れた鋳塊(合金NQ1〜5.7.9;いずれも鋳造速度
は65顛/1Iih)について固剤後、第3表中に示す
ような条件で鋳塊加熱(主に600℃×10h「、一部
は530℃x 10hr)を行ない、400℃で熱間圧
延を施して板厚61111の熱延板とした。次いで板厚
4Mまで冷間圧延した後、350℃×5h「の中間焼鈍
を行ない、さらに板厚2,5闇まで冷間圧延した。Among the ingots of each alloy No. 1 to 9, the ingots in which no abnormality represented by the fir main structure occurred, that is, the ingots judged to be acceptable (alloys NQ1 to 5.7.9; all of them are cast After solidification, the ingot was heated at 400°C (mainly 600°C x 10h, some at 530°C x 10hr) under the conditions shown in Table 3. This was rolled to obtain a hot-rolled plate having a thickness of 61111 mm.Then, it was cold-rolled to a thickness of 4M, intermediate annealing was performed at 350°C for 5 hours, and further cold-rolled to a thickness of 2.5 mm.
その後、各板について5%NaOH水溶液でエツチング
し、水洗後納酸でデスマット処理を行なった。次いでH
2SO4濃度15Vl1%の@酸浴を用いて、浴温20
℃、電流密度0.8A/da!で陽極酸化処理を行ない
、それぞれWA厚15顯の陽極酸化皮膜を生成させた。Thereafter, each plate was etched with a 5% NaOH aqueous solution, washed with water, and then desmutted with nitric acid. Then H
Using an acid bath with a 2SO4 concentration of 15Vl1%, the bath temperature was 20
℃, current density 0.8A/da! An anodic oxidation treatment was carried out to produce an anodic oxide film having a WA thickness of 15 mm.
各板の陽極酸化皮膜の表面色調について、スガ試験機製
カラーメーター5N−3−HCHを用いて調べた。色調
は、ハンターの色差式による明度指数しおよびクロマテ
ィクネス指数a、bを用いて評価した。その結果を第3
表中に示す。なおここでL値〉75、−2くa値く2、
−2くb値く2を満たす場合に白色の色調と判定できる
。The surface color tone of the anodic oxide film of each board was examined using Colormeter 5N-3-HCH manufactured by Suga Test Instruments. The color tone was evaluated using the brightness index according to Hunter's color difference formula and the chromaticness indexes a and b. The result is the third
Shown in the table. Note that here, L value > 75, -2 × a value × 2,
-2 x b value x 2, it can be determined that the color tone is white.
また一方、各板について、金属間化合物の総量、5趨以
下の金属間化合物の数の割合、およびA16 Fe/
(Al3Fe+A1s Fe)の比の値を調べた。その
結果を第3表中に併せて示す。On the other hand, for each plate, the total amount of intermetallic compounds, the proportion of the number of intermetallic compounds of 5 or less, and the A16 Fe/
The ratio value of (Al3Fe+A1s Fe) was investigated. The results are also shown in Table 3.
なお、金属間化合物の量の測定は、次のようにして行な
った。すなわち、先ず試料を約0.5〜19採取し、フ
ェノール溶液100d中において170〜180℃で3
0分溶解し、さらにフェノール溶液の凝固を防ぐためベ
ンジルアルコールを140℃で50d添加した後、濾過
して、残漬をアルコールで洗浄し、さらにその残漬を重
量分析した。Note that the amount of intermetallic compounds was measured as follows. That is, first, a sample of about 0.5 to 19 mm was taken and heated in 100 d of phenol solution at 170 to 180°C for 30 minutes.
After dissolving for 0 minutes, benzyl alcohol was added for 50 d at 140° C. to prevent coagulation of the phenol solution, the solution was filtered, the residue was washed with alcohol, and the residue was analyzed by weight.
また金属間化合物の相の同定は次のようにして行なった
。すなわち、先ず試料を約0.5〜1g採取し、フェノ
ール溶液100SECにおいて170〜180℃で30
分溶解し、フェノール溶液の凝固を防ぐためにベンジル
アルコールを140℃で50−添加した後、濾過し、残
漬をアルコールで洗浄した後、その残漬をX線回折によ
り同定した。The phase of the intermetallic compound was identified as follows. That is, first, about 0.5 to 1 g of a sample was collected and heated at 170 to 180°C for 30 minutes in a phenol solution of 100 SEC.
After adding benzyl alcohol for 50 minutes at 140° C. to prevent coagulation of the phenol solution, the solution was filtered, and the residue was washed with alcohol, and the residue was identified by X-ray diffraction.
さらに金属間化合物のサイズは、試料を研磨した後、画
像解析により金属間化合物の最大長さの分布を測定した
。但し0.5m未満の微細な金属間化合物は無視した。Furthermore, the size of the intermetallic compound was determined by polishing the sample and then measuring the distribution of the maximum length of the intermetallic compound by image analysis. However, fine intermetallic compounds less than 0.5 m were ignored.
第
表
第
表
第3表に示す結果から、この発明の実施例によるアルミ
ニウム合金板材は、陽極酸化処理後の色調が白色となっ
ていることが明らかである。From the results shown in Table 3, it is clear that the aluminum alloy plate material according to the example of the present invention has a white color tone after the anodization treatment.
[実施例2]
実施例1に記載したと同様にして得られた合金騎1の圧
延板について、第4表中に示すように陽極酸化処理条件
を種々変化させ、膜厚20μmの陽極酸化皮膜を生成さ
せた。[Example 2] A rolled plate of Alloy 1 obtained in the same manner as described in Example 1 was subjected to various anodizing treatment conditions as shown in Table 4 to form an anodized film with a thickness of 20 μm. was generated.
各条件で陽極酸化処理を施した後の色調と、陽極酸化皮
膜の耐食性を調べた結果を第4表中に併せて示す。なお
耐食性は、JIS H8681に規定される陽極酸化皮
膜の耐食性試験法のうち、起電力法を用いて評価し、1
00SEC以上を合格とした。Table 4 also shows the results of examining the color tone after anodizing under each condition and the corrosion resistance of the anodic oxide film. Corrosion resistance was evaluated using the electromotive force method among the corrosion resistance test methods for anodic oxide films stipulated in JIS H8681.
00SEC or higher was considered to be a pass.
第 4 表
第4表から、請求項3、請求項4で規定している陽極酸
化処理条件を満たした場合に、耐食性が優れた白色の色
調が得られることが判る。Table 4 From Table 4, it can be seen that when the anodizing treatment conditions specified in claims 3 and 4 are satisfied, a white color tone with excellent corrosion resistance can be obtained.
[実施例3]
第1表に示す合金間1〜9について、実施例1と同様に
して鋳造した。その結果は第2表に示した通りである。[Example 3] Alloys 1 to 9 shown in Table 1 were cast in the same manner as in Example 1. The results are shown in Table 2.
得られた鋳塊のうち、合格と判定された鋳塊(合金NQ
1〜5.7,9:いずれも鋳造速度は65s / ni
h >について、第5表中に示すような条件で鋳塊加熱
(主に600℃x 10hr、一部は530℃x 10
hr)を行ない、実施例1と同様な条件で圧延(熱間圧
延−冷間圧延一中間焼鈍一冷間圧延)を行ない、板厚2
.5txaの圧延板とした。Among the obtained ingots, ingots judged to be acceptable (alloy NQ
1 to 5.7, 9: Casting speed is 65s/ni for both
h>, the ingot was heated under the conditions shown in Table 5 (mainly 600℃ x 10 hours, some at 530℃ x 10 hours).
hr) and rolled under the same conditions as in Example 1 (hot rolling - cold rolling - intermediate annealing - cold rolling), and the plate thickness was 2.
.. It was made into a rolled plate of 5txa.
次いで各圧延板について、第5表中に示すような各種の
粗面化法により粗面化して白色に調整し、その後実施例
1と同じ条件で陽極酸化処理を行なった。Next, the surface of each rolled plate was roughened by various surface roughening methods shown in Table 5 to adjust it to white, and then anodization treatment was performed under the same conditions as in Example 1.
陽極酸化処理前(粗面化処理後)の色調(L値)および
陽極酸化処理後の色調(L値、a値、b値)を調べた結
果を第5表中に示す。また陽極酸化処理後の表面の光沢
度を、入射角60°、反射角60゜で測定した結果も併
せて第5表中に示す。ここで、光沢度は、10%未満で
あれば実質的に無光沢と判定することができる。なお金
属間化合物については、実施例1について第3表中に示
した結果と同じであるから、省略する。Table 5 shows the results of examining the color tone (L value) before anodizing treatment (after surface roughening treatment) and the color tone (L value, a value, b value) after anodizing treatment. Table 5 also shows the results of measuring the glossiness of the surface after the anodizing treatment at an incident angle of 60° and a reflection angle of 60°. Here, if the glossiness is less than 10%, it can be determined that the gloss is substantially matte. Note that the results regarding the intermetallic compounds are the same as those shown in Table 3 for Example 1, so they will be omitted.
第5表から、予め圧延板表面に粗面化処理を施して白色
に調整した優、陽極酸化処理を施した本発明法によるア
ルミニウム合金板材では、陽極酸化処理後に実質的に無
光沢の白色の色調が臂られることが明らかである。From Table 5, it can be seen that the aluminum alloy plate material produced by the method of the present invention, which has been roughened in advance on the surface of the rolled plate and has been anodized, has a substantially matte white color after the anodization treatment. It is clear that the color tone is subdued.
[実施例4]
実施例3と同様にして得られた合金1IQ1の圧延板に
ついて、粗面化処理として弗化アンモニウム系処理(処
理後の表面のL値は92)を施した後、第6表中に示す
ように種々条件を変えて陽極酸化処理を施し、映厚20
μmの陽極酸化皮膜を生成させた。[Example 4] A rolled plate of alloy 1IQ1 obtained in the same manner as in Example 3 was subjected to ammonium fluoride treatment (L value of the surface after treatment was 92) as a surface roughening treatment, and then As shown in the table, anodizing was performed under various conditions, and the film thickness was 20.
An anodic oxide film of μm was produced.
各条件で陽極酸化処理を施した後の色調と、陽極酸化皮
膜の耐食性を調べた結果を第6表中に示す。なお耐食性
は、実施例3と同様に起電力法によって評価し、100
SEC以上を合格と判定した。Table 6 shows the results of examining the color tone after anodizing under various conditions and the corrosion resistance of the anodic oxide film. The corrosion resistance was evaluated by the electromotive force method in the same manner as in Example 3.
A score of SEC or above was judged as passing.
第 6 表
第6表から、陽極酸化処理前に粗面化処理を維しておい
た場合も、請求項5、請求項6で規定している条件範囲
内の陽極酸化処理を施すことによって、耐食性に優れた
白色の色調の陽極酸化皮膜が得られることが明らかであ
る。Table 6 From Table 6, even if the surface roughening treatment is maintained before the anodizing treatment, by performing the anodizing treatment within the condition range specified in claims 5 and 6, It is clear that a white-toned anodic oxide film with excellent corrosion resistance can be obtained.
発明の効果
以上の実施例から明らかなように、請求項1、請求項2
の発明の方法によれば、陽極酸化処理後の色調が白色で
かつ陽極酸化処理後にストリークス等の外観欠陥のない
アルミニウム合金板材を得ることができる。また請求項
3、請求項4の発明の方法によれば、陽極酸化処理が施
されたアルミニウム合金板材として、実際に色調が白色
でかつ外観欠陥がなく、しかも耐食性の優れた陽極酸化
処理板を得ることができる。さらに請求項5、請求項6
の発明の方法によれば、陽極酸化処理前に粗面化処理を
施して白色に調整しておくことにより、表面が無光沢の
マット状でかつ白色の色調を有する陽極酸化処理板を得
ることができる。また各発明の方法によれば染色法の場
合の如く耐食性に劣ることがないため、特に建材等の用
途に使用されるアルミニウム合金板材の製造に最適であ
る。Effects of the invention As is clear from the above embodiments, claims 1 and 2
According to the method of the invention, it is possible to obtain an aluminum alloy plate material which has a white color tone after anodizing treatment and has no appearance defects such as streaks after anodizing treatment. Further, according to the method of the invention of claims 3 and 4, an anodized aluminum alloy plate material that is actually white in color, has no appearance defects, and has excellent corrosion resistance is produced as an anodized aluminum alloy plate material. Obtainable. Furthermore, claims 5 and 6
According to the method of the invention, by performing surface roughening treatment to adjust the surface to white before anodizing treatment, an anodized plate having a matte surface with a non-glossy surface and a white tone can be obtained. I can do it. Furthermore, the methods of each invention do not suffer from inferior corrosion resistance as in the case of dyeing methods, so they are particularly suitable for manufacturing aluminum alloy plates used for building materials and the like.
Claims (6)
.2wt%以下に規制され、残部がAlおよび不可避的
不純物よりなる合金を素材とし、その合金を35〜15
0mm/minの鋳造速度でDC鋳造した後、鋳塊に5
50〜630℃の範囲内の温度で0.5〜24時間加熱
処理を施し、その後圧延して最終板厚とし、これにより
金属間化合物の90%以上が大きさ5μm以下であって
かつ金属間化合物の総量が2.5〜7wt%の範囲内に
あり、しかも金属間化合物Al_6FeとAl_3Fe
の比が Al_6Fe/(Al_3Fe+Al_6Fe)≦0.
1の範囲内にあるアルミニウム合金板を得ることを特徴
とする、陽極酸化処理後の色調が白色のアルミニウム合
金板の製造方法。(1) Contains 0.8 to 2.0 wt% Fe and 0 Si
.. The material is an alloy whose content is regulated to 2wt% or less, with the remainder consisting of Al and unavoidable impurities.
After DC casting at a casting speed of 0 mm/min, the ingot was
Heat treatment is performed at a temperature in the range of 50 to 630°C for 0.5 to 24 hours, and then rolled to give the final thickness, so that 90% or more of the intermetallic compounds have a size of 5 μm or less and the intermetallic The total amount of compounds is within the range of 2.5 to 7 wt%, and intermetallic compounds Al_6Fe and Al_3Fe
The ratio of Al_6Fe/(Al_3Fe+Al_6Fe)≦0.
1. A method for producing an aluminum alloy plate having a white color tone after anodizing treatment, characterized by obtaining an aluminum alloy plate having a color within the range of 1.
Mn0.05〜0.2wt%、Mg0.05〜1.5w
t%、Cr0.05〜0.1wt%のうちの1種または
2種以上を含有し、かつSiが0.2wt%以下に規制
され、残部がAlおよび不可避的不純物よりなる合金を
素材とし、その合金を35〜150mm/minの鋳造
速度でDC鋳造した後、鋳塊に550〜630℃の範囲
内の温度で0.5〜24時間加熱処理を施し、その後圧
延して最終板厚とし、これにより金属間化合物の90%
以上が大きさ5μm以下であつてかつ金属間化合物の総
量が2.5〜7wt%の範囲内にあり、しかも金属間化
合物Al_6FeとAl_3Feの比がAl_6Fe/
(Al_3Fe+Al_6Fe)≦0.1の範囲内にあ
るアルミニウム合金板を得ることを特徴とする、陽極酸
化処理後の色調が白色のアルミニウム合金板の製造方法
。(2) Contains 0.8 to 2.0 wt% of Fe, and
Mn0.05-0.2wt%, Mg0.05-1.5w
t%, Cr0.05 to 0.1 wt%, and Si is regulated to 0.2 wt% or less, and the balance is Al and unavoidable impurities. After DC casting the alloy at a casting speed of 35 to 150 mm/min, the ingot is heat treated at a temperature in the range of 550 to 630°C for 0.5 to 24 hours, and then rolled to a final thickness, This results in 90% of the intermetallic compounds
or more, the size is 5 μm or less, the total amount of intermetallic compounds is within the range of 2.5 to 7 wt%, and the ratio of intermetallic compounds Al_6Fe and Al_3Fe is Al_6Fe/
A method for producing an aluminum alloy plate having a white color after anodizing treatment, characterized by obtaining an aluminum alloy plate in a range of (Al_3Fe+Al_6Fe)≦0.1.
.2wt%以下に規制され、残部がAlおよび不可避的
不純物よりなる合金を素材とし、その合金を35〜15
0mm/minの鋳造速度でDC鋳造した後、鋳塊に5
50〜630℃の範囲内の温度で0.5〜24時間加熱
処理を施し、その後圧延して最終板厚とし、これにより
金属間化合物の90%以上が大きさ5μm以下であって
かつ金属間化合物の総量が2.5〜7wt%の範囲内に
あり、しかも金属間化合物Al_6FeとAl_3Fe
の比が Al_6Fe/(Al_3Fe+Al_6Fe)≦0.
1の範囲内にあるアルミニウム合金板を得、さらにその
最終板厚の合金板に対し、H_2SO_4濃度が10〜
25vol%の硫酸電解浴を用いて浴温度15〜30℃
、電流密度0.5A/dm^2以上1.0A/dm^2
未満で陽極酸化処理を施して膜厚10〜25μmの陽極
酸化皮膜を形成することを特徴とする、陽極酸化処理後
の色調が白色のアルミニウム合金板の製造方法。(3) Contains 0.8 to 2.0 wt% Fe and 0 Si
.. The material is an alloy whose content is regulated to 2wt% or less, with the remainder consisting of Al and unavoidable impurities.
After DC casting at a casting speed of 0 mm/min, the ingot was
Heat treatment is performed at a temperature in the range of 50 to 630°C for 0.5 to 24 hours, and then rolled to give the final thickness, so that 90% or more of the intermetallic compounds have a size of 5 μm or less and the intermetallic The total amount of compounds is within the range of 2.5 to 7 wt%, and intermetallic compounds Al_6Fe and Al_3Fe
The ratio of Al_6Fe/(Al_3Fe+Al_6Fe)≦0.
An aluminum alloy plate with a final thickness of 1 is obtained, and the H_2SO_4 concentration is 10 to 10.
Using a 25 vol% sulfuric acid electrolytic bath, the bath temperature is 15-30°C.
, current density 0.5A/dm^2 or more 1.0A/dm^2
A method for producing an aluminum alloy plate having a white color after anodizing treatment, characterized in that anodizing treatment is performed at less than 100 µm to form an anodized film having a thickness of 10 to 25 μm.
Mn0.05〜0.2wt%、Mg0.05〜1.5w
t%、Cr0.05〜0.1wt%のうちの1種または
2種以上を含有し、かつSiが0.2wt%以下に規制
され、残部がAlおよび不可避的不純物よりなる合金を
素材とし、その合金を35〜150mm/minの鋳造
速度でDC鋳造した後、鋳塊に550〜630℃の範囲
内の温度で0.5〜24時間加熱処理を施し、その後圧
延して最終板厚とし、これにより金属間化合物の90%
以上が大きさ5μm以下であつてかつ金属間化合物の総
量が2.5〜7wt%の範囲内にあり、しかも金属間化
合物Al_6FeとAl_3Feの比がAl_6Fe/
(Al_3Fe+Al_6Fe)≦0.1の範囲内にあ
るアルミニウム合金板を得、さらにその最終板厚の合金
板に対し、H_2SO_4濃度が10〜25vol%の
硫酸電解浴を用いて浴温度15〜30℃、電流密度0.
5A/dm^2以上1.0A/dm^2未満で陽極酸化
処理を施して膜厚10〜25μmの陽極酸化皮膜を形成
することを特徴とする、陽極酸化処理後の色調が白色の
アルミニウム合金板の製造方法。(4) Contains 0.8 to 2.0 wt% of Fe, and
Mn0.05-0.2wt%, Mg0.05-1.5w
t%, Cr0.05 to 0.1 wt%, and Si is regulated to 0.2 wt% or less, and the balance is Al and unavoidable impurities. After DC casting the alloy at a casting speed of 35 to 150 mm/min, the ingot is heat treated at a temperature in the range of 550 to 630°C for 0.5 to 24 hours, and then rolled to a final thickness, This results in 90% of the intermetallic compounds
or more, the size is 5 μm or less, the total amount of intermetallic compounds is within the range of 2.5 to 7 wt%, and the ratio of intermetallic compounds Al_6Fe and Al_3Fe is Al_6Fe/
Obtain an aluminum alloy plate within the range of (Al_3Fe+Al_6Fe)≦0.1, and then use a sulfuric acid electrolytic bath with a H_2SO_4 concentration of 10 to 25 vol% to obtain an aluminum alloy plate with a final thickness of 15 to 30°C. Current density 0.
An aluminum alloy having a white color after anodizing treatment, characterized in that it is anodized at 5 A/dm^2 or more and less than 1.0 A/dm^2 to form an anodic oxide film with a thickness of 10 to 25 μm. Method of manufacturing the board.
.2wt%以下に規制され、残部がAlおよび不可避的
不純物よりなる合金を素材とし、その合金を35〜15
0mm/minの鋳造速度でDC鋳造した後、鋳塊に5
50〜630℃の範囲内の温度で0.5〜24時間の加
熱処理を施した後、圧延して最終板厚とし、その後表面
に粗面化処理を施して表面の色調を白色に調整し、さら
にその粗面化処理後の板に対し、H_2SO_4濃度が
10〜25vol%の硫酸電解浴を用いて浴温度15〜
30℃、電流密度0.5A/dm^2以上1.0A/d
m^2未満で陽極酸化処理を施して膜厚10〜25μm
の陽極酸化皮膜を形成することを特徴とする、陽極酸化
処理後の色調が白色のアルミニウム合金板の製造方法。(5) Contains 0.8 to 2.0 wt% Fe and 0 Si
.. The material is an alloy whose content is regulated to 2wt% or less, with the remainder consisting of Al and unavoidable impurities.
After DC casting at a casting speed of 0 mm/min, the ingot was
After heat treatment for 0.5 to 24 hours at a temperature within the range of 50 to 630°C, it is rolled to obtain the final thickness, and then the surface is roughened to adjust the surface color to white. Furthermore, the plate after surface roughening treatment is heated to a bath temperature of 15 to 15% using a sulfuric acid electrolytic bath with a H_2SO_4 concentration of 10 to 25 vol%.
30℃, current density 0.5A/dm^2 or more 1.0A/d
Film thickness of 10 to 25 μm by anodizing at less than m^2
A method for producing an aluminum alloy plate having a white color after anodizing treatment, the method comprising forming an anodized film of.
Mn0.05〜0.2wt%、Mg0.05〜1.5w
t%、Cr0.05〜0.1wt%のうちの1種または
2種以上を含有し、かつSiが0.2wt%以下に規制
され、残部がAlおよび不可避的不純物よりなる合金を
素材とし、その合金を35〜150mm/minの鋳造
速度でDC鋳造した後、鋳塊に550〜630℃の範囲
内の温度で0.5〜24時間の加熱処理を施した後、圧
延して最終板厚とし、その後表面に粗面化処理を施して
表面の色調を白色に調整し、さらにその粗面化処理後の
板に対し、H_2SO_4濃度が10〜25vol%の
硫酸電解浴を用いて浴温度15〜30℃、電流密度0.
5A/dm^2以上1.0A/dm^2未満で陽極酸化
処理を施して膜厚10〜25μmの陽極酸化皮膜を形成
することを特徴とする、陽極酸化処理後の色調が白色の
アルミニウム合金板の製造方法。(6) Contains 0.8 to 2.0 wt% of Fe, and
Mn0.05-0.2wt%, Mg0.05-1.5w
t%, Cr0.05 to 0.1 wt%, and Si is regulated to 0.2 wt% or less, and the balance is Al and unavoidable impurities. After DC casting the alloy at a casting speed of 35 to 150 mm/min, the ingot is heat treated at a temperature in the range of 550 to 630°C for 0.5 to 24 hours, and then rolled to a final thickness of After that, the surface is subjected to a roughening treatment to adjust the surface color to white, and the plate after the roughening treatment is heated to a bath temperature of 15% using a sulfuric acid electrolytic bath with an H_2SO_4 concentration of 10 to 25 vol%. ~30°C, current density 0.
An aluminum alloy having a white color after anodizing treatment, characterized in that it is anodized at 5 A/dm^2 or more and less than 1.0 A/dm^2 to form an anodic oxide film with a thickness of 10 to 25 μm. Method of manufacturing the board.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP23914289A JPH0739622B2 (en) | 1989-09-14 | 1989-09-14 | Method for producing aluminum alloy plate having white color tone after anodizing treatment |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP23914289A JPH0739622B2 (en) | 1989-09-14 | 1989-09-14 | Method for producing aluminum alloy plate having white color tone after anodizing treatment |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH03100145A true JPH03100145A (en) | 1991-04-25 |
JPH0739622B2 JPH0739622B2 (en) | 1995-05-01 |
Family
ID=17040388
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP23914289A Expired - Lifetime JPH0739622B2 (en) | 1989-09-14 | 1989-09-14 | Method for producing aluminum alloy plate having white color tone after anodizing treatment |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0739622B2 (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010121164A (en) * | 2008-11-19 | 2010-06-03 | Nippon Light Metal Co Ltd | Aluminum alloy sheet having excellent moldability, and method for producing the same |
CN104619871A (en) * | 2012-08-31 | 2015-05-13 | 株式会社大纪铝工业所 | Highly heat conductive aluminum alloy for die casting, aluminum alloy die cast product using same, and heatsink using same |
JP6474878B1 (en) * | 2017-11-28 | 2019-02-27 | 株式会社Uacj | Aluminum member and manufacturing method thereof |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6249435B2 (en) * | 2012-08-10 | 2017-12-20 | 日本軽金属株式会社 | Aluminum-zinc alloy extruded material and method for producing the same |
-
1989
- 1989-09-14 JP JP23914289A patent/JPH0739622B2/en not_active Expired - Lifetime
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010121164A (en) * | 2008-11-19 | 2010-06-03 | Nippon Light Metal Co Ltd | Aluminum alloy sheet having excellent moldability, and method for producing the same |
CN104619871A (en) * | 2012-08-31 | 2015-05-13 | 株式会社大纪铝工业所 | Highly heat conductive aluminum alloy for die casting, aluminum alloy die cast product using same, and heatsink using same |
EP2871250A4 (en) * | 2012-08-31 | 2015-10-14 | Daiki Aluminium Industry Co Ltd | Highly heat conductive aluminum alloy for die casting, aluminum alloy die cast product using same, and heatsink using same |
JP6474878B1 (en) * | 2017-11-28 | 2019-02-27 | 株式会社Uacj | Aluminum member and manufacturing method thereof |
JP2019094553A (en) * | 2017-11-28 | 2019-06-20 | 株式会社Uacj | Aluminum member and its production method |
US10844506B2 (en) | 2017-11-28 | 2020-11-24 | Uacj Corporation | Aluminum member and method of manufacturing the same |
Also Published As
Publication number | Publication date |
---|---|
JPH0739622B2 (en) | 1995-05-01 |
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