KR101503491B1 - Process for trimethylgallium with high yield - Google Patents

Abstract

The present invention relates to a method for producing trimethylgallium, and more particularly, to a method for producing trimethylgallium having a high yield from gallium in a powder state and a methyl group in a liquid state using a magnesium catalyst.
According to the present invention, there is provided a method of manufacturing a semiconductor device, comprising the steps of stirring magnesium powder in an argon atmosphere, mixing gallium powder into the magnesium powder, mixing ether with a mixture of the magnesium powder and the gallium powder to form a first solution Adding methyl iodide to the first solution to form a second solution, mixing the second solution with the ether and mexylen to form a third solution, heating the third solution And a step of allowing the third solution that has been heated to stand at room temperature to obtain trimethylgallium.

Description

[0001] The present invention relates to a process for producing trimethylgallium having a high yield,

The present invention relates to a method for producing trimethylgallium, and more particularly, to a method for producing trimethylgallium having a high yield from gallium in a powder state and a methyl group in a liquid state using a magnesium catalyst.

BACKGROUND ART [0002] GaAs-based semiconductor materials as semiconductor light emitting devices have been used in light emitting diode (LED) devices and laser devices. The color (wavelength) of light emitted from these semiconductor light emitting devices ranges from infrared light to red light. However, in the case of recording information on an optical disk by using a laser beam generated from these semiconductor light emitting elements, the density of the recorded information is limited because the wavelength of the laser beam is long even if more precise information is recorded. For this reason, there has been a demand for a semiconductor light emitting element (semiconductor laser diode) capable of generating a laser beam having a shorter wavelength. Accordingly, the development of a short-wavelength light emitting device using a III-V compound semiconductor material containing nitrogen (hereinafter referred to as a nitride-based semiconductor material) has progressed.

Since the nitride based semiconductor material has a wide band gap of 2 eV or more, a short wavelength light emitting element capable of emitting light in a wide range from orange to ultraviolet rays can be obtained. Currently, a general method of manufacturing a short-wavelength light-emitting device includes a step of laminating semiconductor layers formed of mixed crystals having different compositions of a predetermined metal and nitrogen selected from In, Ga, and Al in sequence so as to enable light emission with a desired wavelength And the composition of each semiconductor layer are determined, and crystal growth is performed based on the structure of the device and the composition of the semiconductor layer to form a semiconductor layer, thereby fabricating a light emitting device.

For example, as a crystal growth method for producing a blue light emitting element containing GaN as a main component, an organic metal such as trimethyl gallium (TMGa), trimethyl aluminum (TMAl), trimethyl indium (TMIn) ammonia (NH ₃₎ is used.

The blue light emitting device using trimethylgallium, which is a main component material, is widely used in various industrial applications such as home appliances, remote controllers, electric sign boards, displays, and various automation devices. As a result, the demand for trimethylgallium (TMGa) to be. However, the production volume of domestic companies supplying domestic semiconductor device companies is limited, and most of them are imported from abroad. As a result, the device makers are having difficulty in competitiveness with foreign companies in price competitiveness and customer service.

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Background art related to the present invention includes trimethylgallium disclosed in Korean Patent Laid-Open Publication No. 10-2006-0053239 (published on May 19, 2006), a method for producing the same, and a gallium nitride thin film formed from trimethylgallium.

An object of the present invention is to provide a method for producing trimethylgallium, which has a high yield from gallium in a powder state and a methyl group in a liquid state using a magnesium catalyst, and which is simple in the production process.

According to another aspect of the present invention, there is provided a method for producing trimethylgallium, comprising the steps of stirring magnesium powder in an argon atmosphere, mixing gallium powder in the magnesium powder, A step of mixing a mixture of gallium powder and an ether as a solvent to form a first solution, adding methyl iodide to the first solution to form a second solution, mixing the ether and mexylene in the second solution Forming a third solution, raising the temperature of the third solution, and leaving the elevated temperature of the third solution at room temperature to obtain trimethylgallium.

In the stirring step, the magnesium powder is preferably stirred at 2500 rpm for 1 hour while maintaining the temperature at 60 ° C in an ultrasonic generator.

The mixing of the magnesium powder with the gallium powder may be performed by stirring the magnesium powder and the gallium powder at 2500 rpm for 1 hour while maintaining the temperature at 60 ° C in an ultrasonic generator.

The ethers include diisopentyl ether, dibutyl ether, diisopropyl ether, and diethyl ether And the like.

In the step of forming the second solution, it is preferable that the methyl iodide is dropwise added dropwise to the first solution in an ultrasonic generator.

Stirring the third solution in an ultrasonic generator for 30 minutes to 60 minutes before the step of raising the temperature of the third solution.

In the step of raising the temperature of the third solution, it is preferable to raise the temperature of the third solution to 200 DEG C or less over 3 hours.

In the step of obtaining trimethylgallium, it is preferable that the temperature-raised third solution is allowed to stand at room temperature for 6 to 12 hours.

According to the present invention, it is possible to provide a process for producing trimethylgallium having a high yield from gallium in a powder state and a methyl group in a liquid state using a magnesium catalyst.

Further, according to the manufacturing process of trimethylgallium according to the present invention, it is possible to shorten the manufacturing process while having a high yield.

1 is a flow chart illustrating a process for manufacturing trimethylgallium according to an embodiment of the present invention.
2 is an NMR graph of trimethylgallium according to an embodiment of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention, and the manner of achieving them, will be apparent from and elucidated with reference to the embodiments described hereinafter in conjunction with the accompanying drawings. However, it should be understood that the present invention is not limited to the embodiments disclosed herein but may be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the invention to those skilled in the art. Is provided to fully convey the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims. Like reference numerals refer to like elements throughout the specification.

Hereinafter, a method for producing trimethylgallium according to an embodiment of the present invention will be described with reference to FIG.

1 is a flow chart showing a process for producing trimethylgallium according to an embodiment of the present invention.

Referring to FIG. 1, a method of manufacturing trimethylgallium according to an embodiment of the present invention includes the steps of stirring magnesium powder in an argon atmosphere (S110), mixing gallium powder in the magnesium powder (S120) Forming a first solution by mixing ether and a solvent in a mixture of the magnesium powder and the gallium powder in step S130, adding methyl iodine to the first solution to form a second solution in step S140, (S160), heating the third solution (S160), and heating the third solution to room temperature to form trimethyl gallium (S170). ≪ / RTI >

In the stirring step (S110), the magnesium powder is stirred at 2500 rpm for 1 hour while maintaining 60 ° C in an ultrasonic generator.

Next, in the step of mixing the gallium powder with the magnesium powder (S120), the magnesium powder and the gallium powder are sintered for 1 hour at 2500 rpm in an ultrasonic generator maintained at 60 ° C as in the previous step followed by stirring and mixing.

Here, stirring and mixing the magnesium powder and the gallium powder in an ultrasonic generator is intended to activate the magnesium powder so that it can act as a catalyst well.

In step S130 of mixing the mixture of magnesium and gallium with the ether to form the first solution, the ether is isoamyl ether, Diisopentyl ether, dibutyl ether, diisopropyl ether, and diethyl ether , But the ether solvent usable in the embodiment of the present invention is not limited thereto.

Then, methyl iodide is added dropwise to the first solution to form a second solution (S140). In the step of forming the second solution (S140), methyl iodide is dropped into the first solution in a dropwise manner in an ultrasonic generator. The reason why methyl iodide is dropwise dropped in an ultrasonic generator is to cause a sufficient reaction by slowly adding methyl iodine in a small amount.

Next, the third solution is formed by mixing ether and me- cylene in the second solution (S150). Here, the ether may be at least one selected from diisopentyl ether, dibutyl ether, diisopropyl ether, and diethyl ether, which are used in step S130 of forming the first solution.

Here, mexylenes are used as internal standards for quantitatively calculating the amount of trimethylgallium (TMG) in NMR. In practice, the molar amount of trimethyl gallium (TMG) can be relatively calculated by comparing the mexylenic peak with the trimethylgallium (TMG) peak in NMR. Through these calculations, the yield of trimethyl gallium (TMG) can be calculated by comparing the mexylenic peak with the trimethylgallium (TMG) peak in NMR.

Next, the third solution is stirred in an ultrasonic generator for 30 minutes to 60 minutes (S155).

Here, the reason why the third solution is stirred in the ultrasonic generator for 30 minutes to 60 minutes is because the reaction time of the trimethylgallium (TMG) is 2 to 3 hours after reacting the magnesium powder with the methyl iodide It is obtained in the best yield after roughing. Methyl iodine is thoroughly mixed and stirred in an ultrasonic generator to react well with the gallium-magnesium complex.

Next, the temperature of the third solution is raised (S160). Here, it is preferable that the temperature of the third solution is raised to 200 占 폚 or less over 3 hours.

Here, the reason why the temperature of the third solution is raised over 3 hours is that the energy sufficient to cause the trimethylgallium (TMG) generation reaction to occur is externally applied. Although the reaction time is described as 3 hours, the reaction time according to the embodiment of the present invention is not limited to this, but can be varied depending on the temperature condition.

Finally, the heated third solution is left at room temperature to obtain trimethyl gallium (S170). The heated third solution is allowed to stand at room temperature for 6 to 12 hours. As a result, trimethyl gallium could be obtained at a yield of 91.9%.

Here, the reason why the third solution is left at room temperature for 6 hours to 12 hours is to allow the third solution to cool slowly to room temperature and to stand for a sufficient time to obtain as much TMG as possible. TMG may be obtained even when the third solution is heated to 200 DEG C, but TMG may be dissolved in the high temperature solvent. Thus, when the third solution is allowed to stand for a sufficient time while slowly cooling to room temperature, as much trimethyl gallium as possible can be obtained. On the other hand, when the third solution is rapidly cooled, the impurities contained in the solution tend to melt or adsorb to the precipitated TMG. Therefore, it is preferable to cool the third solution as slowly as possible.

Example

The 50 mesh magnesium powder 29mM was stirred at 2500rpm for 1 hour in an ultrasonic generator while maintaining the temperature at 60 占 폚. At this time, the stirling was performed in an argon atmosphere. Next, 10 mM of gallium powder was mixed with the magnesium powder, and further, the mixture was further stuttered in the ultrasonic generator for 1 hour. To the mixture of the magnesium powder and the gallium powder was added 5 mL of isoamyl ether. In the ultrasonic generator, 53 mM of methyl iodide was dropwise added dropwise to the mixed solution over 10 minutes. 5 ml of isoamyl ether and 10 mM of methylene chloride were added to the mixed solution in which the methyl iodide was added, and then the mixed solution was stitched in an ultrasonic generator for 30 minutes. The mixed solution was heated to 190 DEG C over 3 hours, and then the mixed solution was left at room temperature for 8 hours. At this time, 1.06 g of trimethylgallium (TMG) as a product was obtained, and an NMR graph for the structural analysis thereof is shown in Fig.

2 is a result of NMR analysis of trimethylgallium according to an embodiment of the present invention.

Referring to FIG. 2, a peak of -0.3 ppm represents a hydrogen atom corresponding to the methyl group in trimethylgallium (TMG). The peak of 2.3 ppm represents a hydrogen atom corresponding to the methyl group in mexylenes. On the other hand, the peaks indicated by the remaining i-Am2O are peaks of isoamyl ether, and four isomers of hydrogen are present in the isoamyl ether. In addition, the peak of 3.0 ppm is an impurity peak.

As described in the above example, 10mM of gallium powder was added to obtain 1.06g (0.92mM) of trimethylgallium, which was confirmed to be obtained in a yield of 92%.

According to the present invention, it is possible to provide a process for producing trimethylgallium having a high yield from gallium in a powder state and a methyl group in a liquid state using a magnesium catalyst.

Further, according to the manufacturing process of trimethylgallium according to the present invention, it is possible to shorten the manufacturing process while having a high yield.

Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims. These changes and modifications may be made without departing from the scope of the present invention. Accordingly, the scope of the present invention should be determined by the following claims.

Claims (8)

(a) stirring magnesium powder in an argon atmosphere;
(b) mixing gallium powder with the magnesium powder;
(c) mixing a mixture of the magnesium powder and the gallium powder with ether as a solvent to form a first solution;
(d) adding methyl iodide to the first solution to form a second solution;
(e) mixing the second solution with ether and me- cithylene to form a third solution;
(f) heating the third solution to generate trimethyl gallium; And
(g) placing the third solution that has been heated at room temperature to obtain trimethyl gallium,
Wherein the steps (a) to (e) are performed in an ultrasonic generator.
The method according to claim 1,
In the stirring step,
Wherein the magnesium powder is stirred in an ultrasonic generator at a temperature of 60 ° C at 2500 rpm for 1 hour, thereby producing a trimethylgallium having a high yield.
The method according to claim 1,
Wherein the mixing of the gallium powder with the magnesium powder comprises:
Wherein the magnesium powder and the gallium powder are stirred at 2500 rpm for 1 hour while maintaining the temperature at 60 캜 in an ultrasonic generator.
The method according to claim 1,
The ether
Diisopentyl ether, dibutyl ether, diisopropyl ether, and diethyl ether , And the method for producing trimethylgallium has a high yield.
The method according to claim 1,
In the step of forming the second solution,
A method for producing trimethylgallium having a high yield by dropwise dropping the methyl iodide in an ultrasonic generator.
The method according to claim 1,
Before the step of raising the temperature of the third solution,
Further comprising stirring the third solution in an ultrasonic generator for 30 to 60 minutes. ≪ Desc / Clms Page number 20 >
The method according to claim 1,
In the step of raising the temperature of the third solution,
And the third solution is heated to 200 DEG C or lower over 3 hours.
The method according to claim 1,
In the step of obtaining the trimethyl gallium,
And the temperature of the third solution is allowed to stand at room temperature for 6 hours to 12 hours.

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