JPS6188492A - Luminous body and manufacture thereof - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

Detailed Description of the Invention "Field of Industrial Application" The present invention is a method for electrochemically encapsulating a reduced element metal in the pores of a superficial porous layer formed by anodizing an aluminum plate. The present invention relates to a light emitting body and a method for manufacturing the same.

``Prior art'' Conventionally, as a solid light emitting material using an activator of rare earth elements such as manogane, europium (Eul), or terbium (Tb), which are not unstable organic substances, for example, niobium was alloyed with 0.37! of aluminum wire. 1 piece of phosphoric acid solution,
By producing orange EL light during anodization at 140 V, or by fabricating an aluminum-terbium alloy film by vacuum simultaneous evaporation method, and dipping it in an ammonium borate bath.
By anodizing C, the green color E unique to terbium is produced.
(2) It is known that four types of light emission can be obtained. Furthermore, it has also been reported that Eu is added to Ta by vacuum simultaneous evaporation method, and red EL emission is caused while this is anodized.

``Problems to be solved by the invention'' However, in any case, the above conventional methods require adding rare earth elements etc. to aluminum as an alloy.
Therefore, it becomes extremely expensive as a solid-state light emitting body, which is a big problem in practical use.

"Means for Solving the Problems" In view of the above, the present invention provides Mn; Go, Zn in the pores of a porous layer formed by anodizing an aluminum plate.
The present invention provides a light emitting body configured to encapsulate a reduction element metal such as , Ce or the like. The light emitter is made by anodizing an aluminum plate to form a porous layer.
This is immersed in a sulfate solution consisting of a reduction element metal to adsorb and encapsulate the reduction element metal in the pores of the porous layer, and then re-anodized to activate it with a transition metal element. Manufactured by crystallizing a sulfuric acid film.

"Function" According to the present invention, without using conventional alloying means,
It is possible to efficiently encapsulate and immobilize reduced elemental metals in the pores of the porous layer of an aluminum anodic oxide film using an inexpensive electrochemical method.

"Example" The drawing is a conceptual diagram showing an example of manufacturing a light emitting body according to an embodiment of the present invention. First, an aluminum plate 1 to be used has a purity of about 99.99X, and its surface is For example, 10% of an ethyl alcohol/perchloric acid bath with a volume ratio of 4:1.
Below °C lol! ! In addition to forming it smoothly by means such as electrolytic polishing β in step 1, as a degreasing treatment, approximately 5% of Na
After immersion treatment in OH at 60 to 65°C for about 12 minutes, it is desirable to thoroughly wash with water once. This pretreated aluminum plate 1 is heated to DC 17 to 20 V, current density 5
0 mA/cm2-8011IA/Cm2, liquid i]5~
11 in a 10X sulfuric acid bath at 20 °C.
When subjected to oxidation treatment, as shown in FIG. 1, a porous layer 3 having numerous fine pores 2 can be formed on its surface and a barrier layer 4 can be formed on its bottom.

Through such anodic oxidation treatment, it becomes possible to form holes 2 in the porous PR layer 3 with a diameter of approximately 150 pores (n pores/cm2) and a thickness of 100 μm or more. The thickness of the porous layer 3 can be controlled to a desired thickness by appropriately controlling the current application time during the positive oxidation treatment to 10 to 60 minutes.
The thickness of the barrier layer 4 formed in the boundary region between the aluminum plate 1 and the base material of the aluminum plate 1 is about 200 degrees.

After the second anodic oxidation step, as shown in Fig. 2, in a sulfuric acid bath of about 10X, a low voltage of about DC5 to IOV, a current density of 5 to 1011 persons/CW12, several minutes to 10
By performing secondary anodic oxidation treatment under the conditions of
It is preferable to form two finer holes at the bottom of the pores in order to increase the sealing area of the reduced element metal and to strengthen and stabilize its activation ability.

The aluminum plate 1 having the porous layer 3 as described above is then immersed in a sulfate solution of a transition element IH group and an oxalic acid solution to form a porous layer 3 as shown in FIG.
A reduction element metal or its compound 5 is placed in each hole 2.2A of E
2>R adsorption. In the case of Eu2 (SO4) as the sulfate solution used in such immersion adsorption treatment, the concentration was a saturated solution, and the immersion time and temperature were 20 to 40'C for 10 minutes or more. The reduction element metal to be adsorbed is Mn.

In addition to Co, Zn, Ce, etc., Sn, Fe, 8g,
Metals such as In, Mg, V, N1, MOlCr, Ila, or Cu can be used.

Such a porous layer 3 is made of N in order to crystallize it.
aHSO, tN)l, ISO, and +7) molar ratio 1:
1.15, and subjected to tertiary anodization treatment in a molten salt with a liquid temperature of about 1700 C or a 2 mol/l) h2Co3 aqueous solution,
The film layer 3 is crystallized, washed with water and dried. As for the tertiary anodizing treatment conditions, in the case of a molten salt bath, the current density is about 30 to 40 III^/cI112, Na2Co, and in the case of a bath, the current density is about 100 to 200+++ persons/cm.
2, and a 99.992 aluminum plate or platinum plate can be used for the counter electrode.

In the light emitting body 6 constructed as described above, each pore 2 of the porous layer 3 is filled with a monomeric polyacetylene conductive material (not shown) or is appropriately sealed in boiling distilled water. , it is preferable to aim at immobilization of the inclusions. Also,
As the emission excitation means for the luminous body 6, ultraviolet excitation, ultraviolet excitation,
Various means such as electron beam excitation or electric field excitation can be employed.

"Effects of the Invention" According to the luminescent material and the manufacturing method thereof according to the present invention, reduced element metals or other compounds can be efficiently and stably encapsulated in an aluminum anodic oxide film using an inexpensive biochemical method. This makes it possible to reduce the cost of the product.In addition, the light emitting operation of the light emitter is stable, and the light emitting operation speed is also low (7). Provide advantages such as tζ4M.

[Brief explanation of the drawing]

Figures 1, 2 and 3 conceptually illustrate the manufacturing process of a luminous body according to an embodiment of the present invention. Fig. 2 is a process diagram for forming a porous layer by the primary anodic oxidation process.
ii. Oxidation treatment process diagram, and FIG. 3 is an immersion adsorption process diagram in which transition element gold, metal, or a compound thereof is immersed and adsorbed into the porous layer obtained in the above process to obtain a luminescent material. The names of the symbols in the attached drawings are as follows. 1 Nialuminum plate 2: Hole 2A: Microscopic hole 3: Porous layer 4: Parrya calendar 5: Enclosed reduction element metal 6: Luminous body ) 1. Indication of the case 1982 Patent No. 199728 2. Name of the invention Luminescent body and its manufacturing method 3. Person making the amendment Relationship to the case Patent applicant M”Fir 1-12 Shiba Daimon, Minato-ku, Tokyo No. 15 M
”X (Name) Nippon Mectron Co., Ltd. 4. Agent Address: 300-12, (02981)
74-235] 6. Number of inventions increased by amendment None (contents of amendment) (1) The scope of claims of the FiAMfi document will be corrected as shown in the attached sheet. (2) "Niobium" in the second line of page 2 of the specification is replaced with "neodymium (
Nd) Correct it as J. (3) Correct "and" in lines 6 to 7 of page 5 of the same page to "or". (4) "Biography" on page 6, line 16 is corrected to "electricity." (Claims) (1) A light-emitting body characterized in that a metal made of a transition element is enclosed in the pores of a porous layer formed by anodizing an aluminum plate. (2) The aluminum plate is anodized to form a porous layer, which is immersed in a sulfate solution containing a reduced metal and then an oxalic acid solution, and then re-anodized. A method for producing a luminescent material.

Claims (2)

[Claims] (1) A light-emitting body characterized in that a metal made of a transition element is enclosed in the pores of a porous layer formed by anodizing an aluminum plate. (2) Luminescence characterized by subjecting an aluminum plate to anodizing treatment to form a porous layer, immersing this in a sulfate solution and oxalic acid solution consisting of a reduced element metal, and then subjecting it to re-anodizing treatment. How the body is manufactured.