TW202214878A - Method and device for separating oxide film from surface of indium-bismuth alloy - Google Patents

Abstract

The present invention provides a method for separating oxide film from surface of indium-bismuth alloy, including: providing a sleeve that has two opposite openings; inserting an indium-bismuth alloy, on which an oxide film layer is formed, into the sleeve through the openings; applying a heat to the sleeve so that the indium-bismuth alloy is melted and maintained liquid, and that the oxide film layer is thicken to a certain thickness and soften to be attached to an inner wall of the sleeve; applying an external force to the liquid indium-bismuth through the openings so that the liquid indium-bismuth breaks through the oxide film layer and the oxide film layer thus forms a breach, allowing the liquid indium-bismuth to flow out of the sleeve from the breach with the oxide film layer remained in the sleeve. The present invention also provides a device for separating oxide film from surface of indium-bismuth alloy.

Description

Method and device for separating oxide film on surface of indium bismuth alloy

The invention relates to a separation method of oxide film on the surface of indium-bismuth alloy. The indium-bismuth alloy is placed in a sleeve, a heat energy is given to the sleeve to melt the indium-bismuth alloy to maintain a liquid state, and the oxide film layer reaches a thickness. The oxide film layer is softened and attached to the inner wall of the sleeve, and then external force is applied to make the indium-bismuth alloy break through the oxide film layer, so that the indium-bismuth alloy flows out of the sleeve, and the oxide film layer remains in the sleeve.

Driven by the vigorous development of the optoelectronic industry, the global demand for TFT-LCD displays has increased, making ITO transparent conductive films the main use of metal indium. According to the statistics of the National Geological Survey of the United States, the total global indium production and demand were 820 tons and 1,500 tons respectively in 2014-2015, resulting in an increasingly serious dilemma of indium resources in short supply. In order to solve the above situation, indium metal recovery has begun to receive attention. At present, indium metal metallurgy technology includes dry metallurgy and wet metallurgy: the dry metallurgy method is to heat the metal together with the necessary additives to a high temperature in a furnace to make it molten. , generate the required chemical reaction, and separate the crude indium metal, and then refine the crude metal; the wet metallurgical method is to use a solvent or impregnating agent to leaching the metal to be recovered from the ore, and the impregnating liquid is chemically or electrochemically or electrochemically leached. After appropriate treatment, the metal is recovered from the solution.

Dry metallurgy, such as the Republic of China Patent Publication No. I496895, "A Method for Recycling Metal Indium or Indium Alloy", discloses a method for reducing indium-containing oxide waste and recovering metal indium or indium alloy: inserting indium-containing oxide waste into A reduction furnace, which introduces a reducing gas into the reduction furnace and heats it to reduce the oxide waste, and separates the molten metal indium or alloy containing indium obtained by the reduction to the lower part of the reduction furnace for metal recovery. Department is recycled.

In the above-mentioned bulletin No. I496895, in order to obtain unoxidized indium alloy, reducing gas needs to be introduced into the reduction furnace for heating to obtain unoxidized indium alloy, which is costly in recycling and complicated in production.

In view of the above-mentioned shortcomings of the currently used method for separating oxide film on the surface of indium-bismuth alloy, the present invention proposes a method for separating oxide film on the surface of indium-bismuth alloy, comprising the following steps:

A sleeve has two opposite openings, and an indium-bismuth alloy with an oxide film layer on the surface is inserted into the sleeve from the above-mentioned openings; a thermal energy is given to the sleeve to melt the indium-bismuth alloy to maintain a liquid state, and the heat can make the oxidized The film layer is softened and attached to the inner wall of the sleeve; an external force is applied to the liquid indium-bismuth alloy from the opening, so that the indium-bismuth alloy breaks through the oxide film layer, and the oxide film layer thus forms a break, allowing the indium-bismuth alloy to break through. The bismuth alloy flows out of the sleeve from the break, and the oxide film layer remains in the sleeve.

Further, the sleeve is stopped to give the heat energy to cool the sleeve and the oxide film layer, and a thrust is applied to the oxide film layer to remove the oxide film layer along the sleeve.

Further, before applying the external force to the liquid indium-bismuth alloy, the thermal energy continues to heat the sleeve and the indium-bismuth alloy for a period of time between 50 minutes and 80 minutes.

Further, when the thermal energy temperature is between 100 degrees Celsius and 150 degrees Celsius, the external force is between 700 N/m ² and 1200 N/m ² .

Further, the thermal energy can reach a thickness of the oxide film layer, and the thickness is between 0.2 mm and 1.2 mm.

The present invention further provides an indium bismuth alloy surface oxide film separation device with the above-mentioned indium bismuth alloy surface oxide film separation method, the indium bismuth alloy surface oxide film separation device includes a body and a heating unit. The body has a sleeve and a rod, the sleeve has two opposite openings, the rod can move into the sleeve; the heating unit is arranged in the sleeve; the indium-bismuth alloy is inserted into the sleeve , the indium-bismuth alloy in the sleeve is melted and maintained in a liquid state by the heating unit, the thermal energy softens the oxide film layer to soften and adhere to the inner wall of the sleeve, and then extends into the sleeve through the rod through the opening The indium bismuth alloy exerts an external force to make the indium bismuth alloy break through the oxide film layer, and the oxide film layer thus forms a break, so that the indium bismuth alloy flows out of the sleeve from the break, and the oxide film layer remains the casing.

Further, the openings are respectively a feeding port and a feeding port, and the feeding port is tapered from the feeding port to the discharging port.

Further, the sleeve has a first sleeve and a second sleeve in communication, and the cross-sectional area of the first sleeve is larger than the cross-sectional area of the second sleeve.

Further, the inner wall of the sleeve is a rough surface, and the rough surface has a plurality of rough structures, and each of the rough structures has an inclined guide surface, and the inclined guide surfaces extend obliquely toward the same opening direction.

Further, the inner wall of the sleeve is a rough surface, and the rough surface has a plurality of rough structures, and each of the rough structures has an inclined guide surface, and the inclined guide surfaces extend obliquely toward the same opening direction.

Further, the roughness of the rough surface is between 0.8 microns and 50 microns.

The above technical features have the following advantages:

1. In the present invention, the indium-bismuth alloy is placed in the casing, and thermal energy is given to the casing to maintain the indium-bismuth alloy in a molten liquid state, and then an external force is applied to the indium-bismuth alloy from the opening through the rod, so that the liquid indium-bismuth alloy breaks through. It is covered with an oxide film layer and flows out of the casing along another opening.

2. The tapered sleeve of the present invention generates a pressure difference when an external force is applied, and the surface tension of the indium-bismuth alloy to break through the oxide film layer is increased by the pressure difference, and at the same time, the oxide film layer is more closely attached to the inner wall of the sleeve, not It will flow out of the casing with the liquid indium-bismuth alloy.

3. The inner wall of the sleeve of the present invention has rough structures, and the inclined guide surfaces of these rough structures extend obliquely toward the same opening, so the oxide film layer attached to the inner wall of the sleeve can be guided by the inclination during cooling. The surface of the oxide film is poured out, and the rough structure of the inner wall provides sufficient friction. When the liquid indium-bismuth alloy flows out along the break, the oxide film layer is left in its original position and is not taken out by the liquid indium-bismuth alloy. outside the casing.

4. The sleeve of the present invention uses copper metal. Because the thermal expansion coefficient of copper metal and indium-bismuth alloy is very different, when the sleeve is cooled, the thermal expansion coefficient is large enough to make the shrinkage stress greater than the adhesion, and the oxide film layer can be easily removed from the sleeve. The inner wall of the tube is stripped.

5. By controlling the temperature of the heat source between 100 and 150 degrees Celsius, the thickness of the oxide film layer is between 0.2mm and 1.2mm, so that the oxide film layer is sufficiently attached to the inner wall of the casing. When an appropriate external force is applied, when the liquid indium-bismuth alloy flows out from the crack, the oxide film layer has enough strength to maintain its shape without being washed and broken by the liquid indium-bismuth alloy, because no fragments are involved in the liquid indium-bismuth alloy. , and achieve the purpose of clean separation.

In view of the above technical features, the main functions of the method for separating the oxide film on the surface of the indium-bismuth alloy and the device thereof of the present invention will be clearly presented in the following embodiments.

Please refer to FIGS. 1 to 3 , an indium-bismuth alloy surface oxide film separation device includes a main body 1 and a heating unit 2 . The main body 1 has a sleeve 11 and a rod 12, the sleeve 11 is made of copper metal, and has a feed port 111 and a discharge port 112, and the feed port 111 to the discharge port 112 In a tapered shape, the rod 12 can move into the sleeve 11 ; the heating unit 2 is covered outside the sleeve 11 .

And the operation method of the oxide film separation device on the surface of the indium bismuth alloy is as follows:

An indium bismuth alloy 3 of an oxide film layer 31 on the solid surface layer is placed into the sleeve 11 from the feed port 111 .

The heating unit 2 imparts a thermal energy to the sleeve 11 to melt the indium-bismuth alloy 3, and the temperature of the thermal energy is between 100 degrees Celsius and 150 degrees Celsius. The solid indium-bismuth alloy 3 has a base phase of BiIn2 phase or BiIn Phase, when the solid indium-bismuth alloy 3 is melted into the liquid indium-bismuth alloy 3, the plurality of liquid indium-bismuth alloys 3 will be fused into one piece, and in the process of melting into one piece, the specific gravity of the oxide film layer 31 is higher than that of the indium-bismuth alloy 3. The indium bismuth alloy 3 is lighter, so that the oxide film layer 31 will flow out of the liquid indium bismuth alloy 3 to cover the liquid indium bismuth alloy 3, and the surface of the indium bismuth alloy 3 will also be oxidized to make the oxide film The layer 31 reaches a thickness, which usually needs to be heated by the heat source for about 1 minute to 20 minutes, so that the oxide film layer 31 has strength, and is broken and broken under pressure, and the outer oxide film layer 31 will adhere to the The thickness of the inner wall 113 of the sleeve 11 is between 0.2 mm and 1.2 mm. The oxide film layer 31 is an amorphous film and will be broken when pressed. The color of the oxide film layer 31 is white and translucent.

The thermal energy continues to heat the sleeve 11 and the indium-bismuth alloy 3 for a period of time between 50 and 80, which not only melts the indium-bismuth alloy 3, but also softens the oxide film layer and adheres to the sleeve. inner wall. It should be noted that when the thickness of the oxide film layer 31 is between 0.2 mm and 1.2 mm, the oxide film layer 31 is sufficient to adhere to the inner wall 113 .

The rod 12 extends from the feed port 111 to exert an external force on the indium-bismuth alloy 3 in liquid state. The external force is between 700N/m ² and 1200N/m ² , and it is difficult to break through the external force below 700N/m ² The oxide film layer 31, the external force exceeding 1200N/m ² is easy to break the oxide film layer 31 into pieces, and then mix into the liquid indium bismuth alloy 3. It should be noted that when the thermal energy temperature is higher, the required The lower the external force is, a pressure difference is generated in the tapered sleeve 11 by the external force, and the pressure difference makes the indium bismuth alloy 3 break through the surface tension of the oxide film layer 31, so that the oxide film layer 31 Therefore, a break 32 is formed, so that the indium bismuth alloy 3 flows out of the sleeve 11 from the break 32, and the oxide film layer 31 is still attached to the inner wall of the sleeve 11 within the range of the stress parameter, breaking the The thickness of the suspended oxide film layer 31 at the mouth is sufficient, so that the film strength is sufficient to maintain the shape, the oxide film layer 31 will not be further cracked, and the film fragments flow out of the sleeve 11 with the liquid indium bismuth alloy 3 .

Stop giving the thermal energy to the sleeve 11 to cool the sleeve 11 and the oxide film layer 31 , and apply a thrust to the oxide film layer 31 to peel off the oxide film layer 31 from the sleeve 11 .

Please refer to the third and fourth figures. It should be noted that the break 32 can be generated by the rod 12 directly applying the external force to pass through the oxide film layer 31, or by the rod 12. The external force applied to the indium-bismuth alloy 3 causes the indium-bismuth alloy 3 to break through the oxide film layer 31 and flow out. In this embodiment, the indium-bismuth alloy 3 breaks through the oxide film layer 31. And flow out.

Please refer to the third and fifth figures, the inner wall 113 is a rough surface, the rough surface has a plurality of rough structures, and each of the rough structures has an inclined guide surface 1131, and the arrangement direction of the inclined guide surfaces 1131 is The roughness of the rough surface is between 0.8 μm and 50 μm in the direction of the feeding port 111 .

Please refer to FIG. 6 , when the indium bismuth alloy 3 is completely discharged from the oxide film layer 31 , since the oxide film layer 31 is attached to the inner wall 113 , the heating of the sleeve 11 is stopped to cause the sleeve 11 to be heated. The tube 11 and the oxide film layer 31 are cooled, because the thermal expansion coefficient of the oxide film layer 31 and the copper metal sleeve 11 is very different, and the oxidation of the copper metal due to heating makes the oxide film layer 31 more difficult to adhere to. For the sleeve 11, the oxide film layer 31 will peel off from the inner wall of the sleeve 11 during the cooling process to reduce the adhesion. When the thrust is applied, the oxide film layer 31 will be completely detached from the inner wall of the sleeve 11 and the oxide film layer 31 can be easily discharged along the feeding port 111 through the inclined guide surface 1131 , and the oxide film layer 31 remove.

Please refer to FIG. 7 , the sleeve 11A of the indium bismuth alloy surface oxide film separation device has another type. The sleeve 11A communicates with a first sleeve 113A and a second sleeve 114A, and the first sleeve 11A The first sleeve 113A has a penetrating feed port 111A, the second sleeve 114A has a penetrating discharge port 112A, and the cross-sectional area of the first sleeve 113A is larger than that of the second sleeve 114A. The cross-sectional area of the feed opening of the first sleeve 113A is larger than the feed opening 111A of the second sleeve 114A. Therefore, after the indium bismuth alloy 3 is placed in the first sleeve 113A and the second sleeve 114A and heated and melted, a pressure difference is generated between the inlet 111A and the outlet 112A by applying the external force , and as shown in Fig. 5, the pressure difference makes the indium bismuth alloy 3 break through the surface tension of the oxide film layer 31, so that the oxide film layer 31 forms the break 32, so that the indium bismuth alloy 3 breaks through the break 32 flows out of the sleeve 11A.

It should be noted that the difference between the above method for separating the oxide film on the surface of indium-bismuth alloy and the traditional recovery method of indium or indium alloy is that it does not need to be recovered through a reduction furnace, but only needs to be heated to soften the oxide film and attach to the sleeve. The inner wall of the indium-bismuth alloy can flow out through the external force, and the oxide film layer has sufficient strength to maintain its shape without being washed and broken by the liquid indium-bismuth alloy, because no fragments are involved in the liquid indium-bismuth alloy. Indium bismuth alloy, and achieve the purpose of clean separation.

Based on the descriptions of the above embodiments, one can fully understand the operation, use and effects of the present invention, but the above-mentioned embodiments are only preferred embodiments of the present invention, which should not limit the implementation of the present invention. Scope, that is, simple equivalent changes and modifications made according to the scope of the patent application of the present invention and the contents of the description of the invention, all fall within the scope of the present invention.

1: Ontology 11: Casing 111: Feed port 112: discharge port 113: inner wall 1131: Inclined Guide Surface 12: Rods 2: Heating unit 3: Indium bismuth alloy 31: oxide film layer 32: Break 11A: Casing 111A: Feed port 112A: discharge port 113A: First casing 114A: Second casing

[Figure 1] is a block flow diagram of the method for separating the oxide film on the surface of the indium-bismuth alloy according to the present invention. [Fig. 2] is an exploded perspective view of the oxide film separation device on the surface of the indium-bismuth alloy of the present invention. [Figure 3] is a schematic diagram of the present invention extending the rod into the casing to pressurize the indium-bismuth alloy. [Figure 4] is a partial enlarged view of the indium-bismuth alloy of the present invention breaking through the oxide film. [Figure 5] is a partial enlarged view of the inner wall of the casing of the indium-bismuth alloy surface oxide film separation device of the present invention. [Fig. 6] is a schematic diagram of the present invention, in which the sleeve is turned upside down so that the oxide film peels off the inner wall and falls. [Fig. 7] is a cross-sectional view of another casing of the indium-bismuth alloy surface oxide film separation device of the present invention.

Claims (10)

A method for separating oxide film on the surface of indium-bismuth alloy, comprising: The sleeve has two opposite openings, and an indium-bismuth alloy with an oxide film layer on the surface is inserted into the sleeve from the openings; Giving a heat to the sleeve can make the indium-bismuth alloy melt and maintain a liquid state, and the heat can soften the oxide film layer and adhere to the inner wall of the sleeve; An external force is applied to the liquid indium bismuth alloy from the opening, so that the indium bismuth alloy breaks through the oxide film layer, and the oxide film layer thus forms a break, so that the indium bismuth alloy flows out of the sleeve from the break , the oxide film layer remains on the sleeve. The method for separating oxide film on the surface of indium-bismuth alloy according to claim 1, further, the sleeve is stopped to give the thermal energy to cool the sleeve and the oxide film, and a thrust is applied to the oxide film to make the oxide film Remove along the cannula. The method for separating oxide film on the surface of indium-bismuth alloy according to claim 1, further, before applying the external force to the liquid indium-bismuth alloy, the thermal energy continues to heat the sleeve and the indium-bismuth alloy for a period of time, and the time Between 50 and 80 points. The method for separating oxide film on the surface of indium-bismuth alloy as claimed in claim 1, wherein when the thermal energy temperature is between 100°C and 150°C, the external force is between 700N/m ² and 1200N/m ² . According to the method for separating the oxide film on the surface of the indium-bismuth alloy as claimed in claim 1, further, the thermal energy can reach a thickness of the oxide film, and the thickness is between 0.2 mm and 1.2 mm. A device having a method for separating oxide film on the surface of indium-bismuth alloy as described in any one of the application scopes 1 to 5, the device for separating oxide film on the surface of indium-bismuth alloy comprises: a body, a sleeve and a rod, the sleeve has two opposite openings, and the rod movably extends into the sleeve; a heating unit, arranged on the sleeve; The indium-bismuth alloy is placed in the sleeve, and the indium-bismuth alloy in the sleeve is melted and maintained in a liquid state by the heating unit. The thermal energy softens the oxide film layer and attaches to the inner wall of the sleeve, and then penetrate The rod extends into the indium bismuth alloy through the opening and exerts an external force, so that the indium bismuth alloy breaks through the oxide film layer, and the oxide film layer thus forms a break, so that the indium bismuth alloy flows out from the break to the indium bismuth alloy. Outside the casing, the oxide film layer remains in the casing. The indium-bismuth alloy surface oxide film separation device as claimed in claim 6, wherein the openings are respectively a feeding port and a discharging port, and the feeding port is tapered from the discharging port. The indium-bismuth alloy surface oxide film separation device as claimed in claim 6, wherein the sleeve has a first sleeve and a second sleeve connected in communication, and the cross-sectional area of the first sleeve is larger than that of the second sleeve cross-sectional area. The indium-bismuth alloy surface oxide film separation device as claimed in claim 6, wherein the inner wall of the sleeve is a rough surface, the rough surface has a plurality of rough structures, and the rough structures respectively have an inclined guide surface, and the inclined The guide surfaces extend obliquely in the direction of the same opening. The indium-bismuth alloy surface oxide film separation device according to claim 9, wherein the roughness of the rough surface is between 0.8 microns and 50 microns.

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