KR101745308B1 - Method for controlling trace elements in low melting metals - Google Patents

Method for controlling trace elements in low melting metals Download PDF

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Publication number
KR101745308B1
KR101745308B1 KR1020150085773A KR20150085773A KR101745308B1 KR 101745308 B1 KR101745308 B1 KR 101745308B1 KR 1020150085773 A KR1020150085773 A KR 1020150085773A KR 20150085773 A KR20150085773 A KR 20150085773A KR 101745308 B1 KR101745308 B1 KR 101745308B1
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South Korea
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metal
tube
heating means
impurity element
cooling
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KR1020150085773A
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Korean (ko)
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KR20160148945A (en
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윤재식
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한국기초과학지원연구원
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Priority to KR1020150085773A priority Critical patent/KR101745308B1/en
Priority to CN201580059461.9A priority patent/CN107075716A/en
Priority to PCT/KR2015/008683 priority patent/WO2016036030A1/en
Publication of KR20160148945A publication Critical patent/KR20160148945A/en
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/28—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The present invention relates to a method for controlling a trace element of a low melting point metal, comprising the steps of: a) charging a boat containing a metal to be refined into a tube, b) heating means provided on the outer surface of the tube, C) the target metal in the portion where the heating means is located is locally heated to become a molten zone in a liquid state, d) the region of the metal object excluding the molten portion is in a solid state E) cooling the molten metal as the heating means is moved toward the other end side of the target metal at a constant speed along the longitudinal direction of the tube, and e) , The impurity element is moved to the other end of the target metal due to the property that the impurity element contained in the target metal collects in the molten portion The step of focusing control may be made, including.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a method for controlling low-

The present invention relates to a method for controlling a trace element of a low melting point metal, and more particularly, to a method for controlling a trace element contained in a metal to increase the purity of the metal, The present invention relates to a method for controlling a trace element of a low melting point metal, which can control a trace element contained in a low melting point metal.

The conventional process for removing impurities in a single crystal solid to increase the purity is referred to as zone refining.

FIG. 1 briefly illustrates the principle of such a zone purification method. A narrow ring-shaped heater is used to heat and melt the rod-shaped monocrystalline ingot. The molten zone gradually moves from one end of the ingot to the other as the heater moves . At this time, when the main material, which has been melted and liquid, is recrystallized as the heater moves, the tendency to make crystals among the same materials causes the impurity to move to the molten portion in the liquid state at the liquid and solid interface.

That is, the ingot partly repeats the melting-crystallization process, and the impurities gradually move along the moving direction of the heater and finally gather at one end. This process is repeated several times, and at the end, one end of the ingot with denser impurities is cut off to obtain a high-purity crystal.

A related art is described in Korean Patent Laid-Open Publication No. 2003-0005722 ("Dry metallic germanium manufacturing method and its refining apparatus").

The purification apparatus according to the prior art is shown in FIG. 2, and the purification process will be briefly described with reference to FIG. After the metal germanium has been completely melted by heating the rotary tube (3) with the heater (4) after putting the germanium into the inside of the rotary tube and vacuuming the inside of the rotary tube, the heater is rotated in the axial direction of the rotary tube . At this time, impurities in the metal germanium move with the transfer of the heater 4 from the high temperature part to the low temperature part, and finally, the metal germanium is purified by cutting the tip where the impurities are gathered.

However, the purification method described in the above-mentioned prior art is a method of purifying germanium having a melting point of 958.5 ° C. In the case of low melting metals such as Ga and In (metal materials practically used at a melting point of Pb melting at 327.4 占 폚), even when the heater moves, the melted portion remains in a liquid state without recrystallization There is a problem that the impurities can not be collected on one side. That is, the prior art has a problem that it can not be applied to purification of a low melting point metal.

Korean Patent Laid-Open Publication No. 2003-0005722 ("Method for producing dry metallic germanium and its refining apparatus")

Disclosure of Invention Technical Problem [8] The present invention has been conceived to solve the problem that it is not easily melted and recrystallized when refining a low melting point metal having a melting point of 327.4 [deg.] C or less. The object of the present invention is to effectively control the trace elements contained in the low melting point metal, And a method for controlling a trace element of a low melting point metal, which enables a refining step of high purity of the metal.

A method of controlling a trace element of a low melting point metal according to the present invention comprises the steps of: a) charging a boat containing a metal to be refined into a tube (S100); b) a step S200 in which the heating means provided on the outer surface of the tube is located on one side of the end of the target metal; c) a step S300 in which the metal in the portion where the heating means is located is locally heated to become a molten zone in a liquid state; d) cooling (S400) the target metal so that a region of the target metal excluding the molten portion becomes a crystal zone; And e) as the heating means is moved toward the other end side of the target metal at a constant speed along the longitudinal direction of the tube, the molten metal is moved as well. Depending on the property of the impurity element contained in the metal to be collected in the molten metal (S500) in which the impurity element is moved to the other end of the target metal and concentrated.

In addition, the step d) includes cooling the cooling water to a predetermined temperature (S410), supplying the cooling water to the micro tube provided to contact the outer surface of the boat (S420), and cooling the cooling water through the micro tube And cooling the target metal by circulation (S430).

Further, after the step (e), the step (f) may include cutting the other end of the metal to which the impurity element is concentrated to obtain a metal of high purity (S600).

After the step a), a1) the inside of the tube is evacuated (S110); And a2) forming a process atmosphere by injecting an atmospheric gas into the tube (S120).

In the present invention, the target metal may be any one selected from Ga, In, Bi, Pb, Sn, Li, Na and Rb.

Also, steps d) and e) may be performed simultaneously, and steps b) to e) may be repeatedly performed.

According to the present invention, the molten metal and the crystallized portion of the target metal can be formed by controlling the cooling temperature of the target metal, the heating temperature of the heating means, and the moving speed of the heating means.

In the conventional refining method, it is impossible to purify a metal having a low melting point due to the problem that the melted portion of the metal is not recrystallized despite the movement of the heater. However, the method for controlling a trace element of a low melting point metal according to the present invention, The present invention is advantageous in that the high refinement refining process can be performed for the low melting point metal by performing the step of cooling the metal so that the region where the metal is melted can be effectively recrystallized simultaneously with the movement of the heater.

Further, in the control method according to the present invention, since the cooling temperature, the heating temperature of the heater, and the moving speed of the heater are mutually adjusted, the portion to be removed after the process is completed can be minimized, thereby maximizing the yield of the process.

1 is a view showing the principle of the zone refining method
2 is a schematic diagram of a conventional metal germanium purification apparatus
3 is a block diagram showing a method for controlling a trace element of a low melting point metal according to the present invention
FIG. 4 is a diagram showing a configuration of a control device using a method for controlling a trace element of a low melting point metal according to the present invention
5 is a schematic view showing the principle of a method of controlling a trace element of a low melting point metal according to the present invention
FIG. 6 is a schematic view of an embodiment of the heating means and the cooling means according to the present invention
Fig. 7 is a view showing another embodiment of the heating means and the cooling means according to the present invention

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Reference will now be made in detail to the present embodiments of the present invention, examples of which are illustrated in the accompanying drawings.

The following drawings are provided as examples for allowing a person skilled in the art to sufficiently convey the idea of the present invention. Therefore, the present invention is not limited to the drawings and may be embodied in other forms. In addition, like reference numerals designate like elements throughout the specification.

In this case, unless otherwise defined, technical terms and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In the following description and the accompanying drawings, A description of known functions and configurations that may unnecessarily obscure the description of the present invention will be omitted.

FIG. 3 is a block diagram showing a method for controlling a trace element in a low melting point metal according to the present invention, FIG. 4 is a diagram illustrating a control apparatus using a trace element control method for a low melting point metal according to the present invention, Is a schematic diagram showing a principle of a method of controlling a trace element of a low melting point metal according to the present invention.

As shown in FIG. 3, the present invention may include steps a) to e).

The step a) is a step in which the boat 200 containing the low melting point metal to be purified (hereinafter referred to as the 'target metal 10') is charged into the tube 100 (S100).

The object metal 10 is a typical low melting point metal such as Ga, In, Bi, Pb, Sn, and the like. The object of the present invention is to provide a control method capable of purifying a low melting point metal, Li, Na, and Rb.

At this time, the target metal 10 is in a bulk ingot form and is loaded in the center of the inside of the tube 100 while being contained in the boat 200 as shown in FIG.

A1) a step S110 in which the inside of the tube 100 is evacuated after the step a), and a2) a step S120 in which a process atmosphere is formed by injecting an atmospheric gas into the tube 100, I make it.

For example, referring to FIG. 4, after the target metal 10 is charged into the tube 100, a vacuum pump 110 connected to the tube 100 is used to vacuum the inside of the tube 100, Thereafter, hydrogen gas is introduced through the nozzle 120 to create a hydrogen atmosphere. At this time, although hydrogen is used as the atmosphere gas, various gases other than hydrogen can be used.

In step b), the heating means 300 provided on the outer surface of the tube 100 is positioned on one side of the target metal 10 (S200).

Since the heating means 300 is provided on the outer surface of the tube 100 as described above, the heating means 300 is spaced apart from the target metal 10 in the tube 100 and locally heats the target metal 10. As the heating means 300, a normal heater, a plasma generator, or the like can be used.

In a subsequent step c), a molten zone 11 is formed in a liquid state by locally heating a certain region of the target metal 10 adjacent to the portion where the heating means 300 is located (S300).

Next, in step d), the target metal 10 is cooled (S400) so that the area of the target metal 10 excluding the molten part 11 becomes a crystal zone 12 in a solid state (S400) In the step e), as the heating means 300 is moved toward the other end side of the target metal 10 at a constant speed along the longitudinal direction of the tube 100, the molten portion 11 is also moved along with the target metal 10 The trace elements contained in the target metal 10 are moved to the other end of the target metal 10 and concentrated by the property that the included trace elements are gathered in the molten portion 11 at step S500.

At this time, it is preferable that the steps d) and e) are performed simultaneously. Also, the steps b) to e) may be repeated several times in order to obtain the target metal 10 of desired purity.

Thereafter, f) step S600 of obtaining a high-purity target metal 10 by cutting the other end of the metal 10 to which a trace element is concentrated may be performed.

As described above, the target metal 10 is a low melting point metal having a low melting point. For example, Ga metal, a typical low-melting metal, has a melting point of 29.76 ° C which is lower than the human body temperature. It is very difficult to locally melt the Ga metal because it melts easily in the human hand.

Specifically, in the case of a low melting point metal such as Ga metal, the process of recrystallization of the molten portion 11 into the crystal portion 12 takes a very long time. In this process, the molten portion 11 Can be crystallized as it is without moving along with the movement of the heating means 300. Furthermore, even if the heating means 300 has moved, the molten portion 11 may remain in the liquid state have.

A more serious problem is that as the number of repeating steps b) to e) increases, the atmospheric gas in the tube 100 is heated and the temperature inside the tube 100 continuously increases, It is more intense.

Therefore, in the method of controlling a trace element of a low melting point metal according to the present invention, a cooling step like the step d) is essential.

Hereinafter, a process of controlling the trace elements of the target metal 10 will be described in more detail with reference to FIGS.

the heating means 300 provided on the outer surface of the tube 100 in the step b) is located on one side of the end side of the target metal 10 after the initial conditions are made through the steps a) to a2), c) The fused portion 11 is formed at one end of the target metal 10 by the heating means 300. Step d) and step e) are then carried out simultaneously.

That is, as the heating means 300 gradually moves from one end side to the other end side of the target metal 10 along the longitudinal direction of the tube 100, the molten portion 11 is also bent at one end of the target metal 10 And moves to the other end. At the same time, as the heating means 300 moves from the target metal 10, the melted portion 11 which has been melted is effectively recrystallized to cool the target metal 10 so as to become the crystal portion 12. At this time, at the interface where the melted portion is recrystallized by the solid portion 12 after the heating means 300 has passed, trace elements such as impurities contained in the target metal 10 are gathered toward the molten portion 11 And the concentration of the trace elements in the molten metal 11 gradually increases as the molten metal 11 moves, and finally the molten metal is concentrated on the other end of the metal 10.

Thereafter, in step f), the target metal 10 is taken out and partially analyzed to confirm a point where the concentration of the trace element starts to increase sharply, and then a certain region of the other end of the target metal 10 is cut off, The metal (10) can be obtained. As described above, if the trace metal element is not removed sufficiently so that the target metal 10 has a desired purity, steps b) to e) may be repeated several times.

That is, according to the present invention, as the heating means 300 moves, the melted portion is effectively recrystallized by performing the d) step (cooling step) at the same time as the e) step (the molten part moving step) . Therefore, the present invention is advantageous in that it is possible to purify the object metal 10 which is low in melting point and is not easily recrystallized by melting, so that the refining process can be performed at a high purity.

4 and 5 for performing the step d) as described above. 6 and 7 illustrate various embodiments of the heating means 300 and the cooling means 500 according to the present invention. Hereinafter, an example of step d) will be described in detail with reference to FIGS.

The step d) includes cooling the cooling water to a predetermined temperature at step S410, supplying cooling water to the micro tube 510 provided to contact the outer surface of the boat 200 at step S420, (Step S430) in which the target metal 10 is cooled by circulating through the first and second metal plates. As described above, the cooling unit 500 is used to perform the step d). The cooling unit 500 includes a micro-tube 500 which is in contact with the outer surface of the boat 200 and has a zigzag- And a cooling control unit 520 for controlling the circulation of the cooling water by connecting both ends of the micro tube 510 with the opposite ends of the micro tube 510.

That is, in step d), the temperature of the cooling water is appropriately set according to the melting point of the target metal 10 through the cooling control device 520, the cooling water is cooled to the set temperature, and the cooling water is supplied to the micro- And circulates through the pipe 510 so that the region of the metal 10 contained in the boat 200 excluding the molten portion 11 is cooled to be the crystal portion 12. At this time, water, ethylene glycol, or the like may be used as the cooling water.

6 and 7, it is preferable that the heating means 300 is provided on the outer surface of the tube 100 at least one side except the side where the micro tube 510 is located.

6, when the micro tube 510 is configured to abut the lower outer surface of the boat 200, the heating means 300 may be disposed in a predetermined region of the other side except the lower outer surface of the tube 100. [ The heating means 300 may be formed in the shape of a band surrounding the tube 100 so that the micro tube 510 is in contact with the left and right outer surfaces of the boat 200 in the longitudinal direction, Or may be formed on the side surface.

In addition, in the present invention, it is preferable that the fine tube 510 is provided so as to be in contact with the outer surface of the boat 200 and the boat 200 is formed of a metal having thermal conductivity as described above. This makes it possible to rapidly conduct heat to the target metal 10, thereby improving the cooling efficiency of the target metal 10. [ In order to achieve more uniform cooling, it is preferable that an area of contact between the micro tube (510) and the lower outer side surface or the right and left outer side surfaces of the boat (200) is as wide as possible.

Therefore, the boat 200 is typically made of gold, silver, copper, aluminum or the like having a high thermal conductivity and a melting point higher than that of the low melting point metal. Among them, the boat 200 is preferably made of copper having excellent thermal conductivity .

As described above, the boat 200 formed of a metal having excellent thermal conductivity is preferably coated thinly with Teflon. This is to prevent the reaction with the target metal 10 contained in the boat 200. If the boat 200 is made only of a metal having a good thermal conductivity, it can react with the molten target metal 10 to be.

As described above, in the step d), the cooling of the target metal 10 may be performed through circulation of the cooling water, or various other methods may be applied.

The method for controlling a trace element of a low melting point metal according to the present invention is a method for controlling a trace element of a low melting point metal by controlling mutually the cooling temperature (set temperature of cooling water), the heating temperature of the heating means (300) The molten portion 11 and the crystal portion 12 are formed in the metal 10. Further, the lower the melting point of the target metal, the finer the heating temperature of the heating means 300 and the temperature of the cooling water should be.

That is, in the present invention, by appropriately controlling the temperature of the cooling water flowing through the micro-tube 510 and the heating temperature of the heating means 300, And the tangent at the intermediate point is an interface gradient (T), it is preferable to optimize the interface gradient (T) to be maximum (see FIG. 5). At this time, since the temperature of the cooling water and the heating temperature of the heating means 300 are inversely related to each other, they are mutually adjusted to find a point at which the interface slope T becomes maximum. The closer the interface slope (T) is to the vertical, the more the process yield can be maximized since the portion removed after the process is completed (cut off at the point where the trace element concentration begins to increase sharply) can be minimized.

Also, since the temperature inside the tube 100 gradually increases as the number of repetition of the process is increased as described above, the temperature in the tube 100 is continuously checked using a temperature sensor or the like, The temperature should be fine-tuned.

In addition, the moving speed of the heating means 300 should be suitably adjusted. If the moving speed is high, it is preferable to adjust the speed as low as possible because a sufficient amount of element can not be removed. However, if the moving speed is too slow, It is inappropriate in terms of bringing the interface slope (T) to the maximum, so it should be appropriately adjusted.

The unillustrated reference moving means 400 is shown as a gear 410 and a belt 420 as shown in FIG. 4 as means for moving the heating means 300 along the longitudinal direction of the tube 100 But is not limited thereto. The gas control unit 121 provided at the middle of the nozzle 120 regulates the amount of the atmospheric gas to be introduced into the tube 100. The burner 600 connected to one side of the tube 100 is an explosion- And discharging the hydrogen gas.

Although the present invention has been described with reference to particular embodiments and specific embodiments thereof with reference to the accompanying drawings, it is to be understood that the invention is not limited to the disclosed embodiments, It is to be understood that the invention is not limited to the above-described embodiment, and that various modifications and changes may be made by those skilled in the art to which the present invention pertains.

That is, it goes without saying that the control device according to the present invention may be used not only for refining low-melting metal but also for refining other metals.

Therefore, the spirit of the present invention should not be construed as being limited to the embodiments described, and all of the equivalents or equivalents of the claims, as well as the appended claims, fall within the scope of the present invention.

10: Target metal
11: melting portion 12: crystal portion
100: tube 110: vacuum pump
120: nozzle 121: gas regulator
200: boat 300: heating means
400: moving means 410: gear
420: Belt 500: Cooling means
510: micro tube 520: cooling control device
600: Burner

Claims (8)

a) a step (S100) in which a boat containing the metal to be refined is charged into the tube;
b) a step S200 in which the heating means provided on the outer surface of the tube is located on one side of the end of the target metal;
c) a step S300 in which the metal in the portion where the heating means is located is locally heated to become a molten zone in a liquid state;
d) cooling (S400) the target metal so that a region of the target metal excluding the molten portion becomes a crystal zone; And
e) As the heating means is moved toward the other end side of the target metal at a constant speed along the longitudinal direction of the tube, the molten metal is moved as well, and depending on the property of the impurity element contained in the metal, (S500) in which the impurity element is moved to the other end of the target metal and concentrated;
/ RTI >
The step d)
Cooling the cooling water to a predetermined temperature (S410);
A step S420 of supplying the cooling water to the micro tube provided to contact the outer surface of the boat; And
Cooling the object metal by circulating the cooling water through the micro-tube (S430);
Wherein the impurity element is a metal.
The method according to claim 1,
The target metal may be,
Ga, In, Bi, Pb, Sn, Li, Na, and Rb.
The method according to claim 1,
A method for controlling an impurity element of a metal,
Wherein the step d) and the step e) are simultaneously performed.
The method according to claim 1,
The steps b) to e)
Wherein the impurity element is a metal.
The method according to claim 1,
A method for controlling an impurity element of a metal,
Wherein the molten metal and the crystallized portion are formed in the metal by mutually adjusting the cooling temperature of the metal, the heating temperature of the heating means, and the moving speed of the heating means.
The method according to claim 1,
After step e)
f) obtaining an object metal having a high purity by cutting the other end of the metal to which the impurity element is concentrated (S600);
Wherein the impurity element is a metal.
The method according to claim 1,
After step a)
a1) the inside of the tube is evacuated (S110); And
a2) injecting an atmospheric gas into the tube to form a process atmosphere (S120);
Wherein the impurity element is a metal.
delete
KR1020150085773A 2014-09-03 2015-06-17 Method for controlling trace elements in low melting metals KR101745308B1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
KR1020150085773A KR101745308B1 (en) 2015-06-17 2015-06-17 Method for controlling trace elements in low melting metals
CN201580059461.9A CN107075716A (en) 2014-09-03 2015-08-20 The ultramicro-element control device and control method of low-melting-point metal
PCT/KR2015/008683 WO2016036030A1 (en) 2014-09-03 2015-08-20 Method and apparatus for controlling trace elements of low-melting point metal

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Application Number Priority Date Filing Date Title
KR1020150085773A KR101745308B1 (en) 2015-06-17 2015-06-17 Method for controlling trace elements in low melting metals

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KR101745308B1 true KR101745308B1 (en) 2017-06-12

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4888051A (en) 1988-08-19 1989-12-19 Cominco Ltd. Method for the zone refining of gallium
JP2001123232A (en) * 1999-10-26 2001-05-08 Furukawa Co Ltd Method for refining gallium

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030005722A (en) 2001-07-10 2003-01-23 (주)나인디지트 Manufacturing method of metal Germanium without liquid and refining device thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4888051A (en) 1988-08-19 1989-12-19 Cominco Ltd. Method for the zone refining of gallium
JP2001123232A (en) * 1999-10-26 2001-05-08 Furukawa Co Ltd Method for refining gallium

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