KR101538388B1 - Dielectric Barrier Discharge Reactor for making Disilane, Trisilane and Tetrasilane from Silane - Google Patents

Dielectric Barrier Discharge Reactor for making Disilane, Trisilane and Tetrasilane from Silane Download PDF

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Publication number
KR101538388B1
KR101538388B1 KR1020130066750A KR20130066750A KR101538388B1 KR 101538388 B1 KR101538388 B1 KR 101538388B1 KR 1020130066750 A KR1020130066750 A KR 1020130066750A KR 20130066750 A KR20130066750 A KR 20130066750A KR 101538388 B1 KR101538388 B1 KR 101538388B1
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South Korea
Prior art keywords
discharge
gas
reaction
housing
electrode rod
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KR1020130066750A
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Korean (ko)
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KR20140144594A (en
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이이쿠보 유이치
장향자
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이이쿠보 유이치
장향자
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Priority to KR1020130066750A priority Critical patent/KR101538388B1/en
Priority to PCT/KR2014/004908 priority patent/WO2014200219A1/en
Publication of KR20140144594A publication Critical patent/KR20140144594A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/04Hydrides of silicon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/32009Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32348Dielectric barrier discharge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0824Details relating to the shape of the electrodes
    • B01J2219/0826Details relating to the shape of the electrodes essentially linear
    • B01J2219/083Details relating to the shape of the electrodes essentially linear cylindrical
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0871Heating or cooling of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873Materials to be treated
    • B01J2219/0875Gas

Abstract

The present invention relates to a dielectric barrier discharge reactor for producing disilane, trisilane and tetrasilane, and more particularly, to a reactor capable of producing disilane as well as trisilane and tetrasilane in a continuous process The inside of the reaction apparatus is composed of a discharge electrode rod connected to the high frequency device and a porous tube surrounding the discharge electrode rod. By adjusting the material of the discharge electrode rod, the distance between the discharge electrode rod and the porous pipe, Trisilane, and tetrasilane. The present invention also relates to a dielectric barrier discharge reactor for producing disilane, trisilane and tetrasilane having a high yield.

Description

[0001] The present invention relates to a dielectric barrier discharge reactor for producing disilane, trisilane and tetrasilane,

The present invention relates to a DBD (Dielectric Barrier Discharge) reactor capable of continuously producing disilane, trisilane and tetrasilane in silane.

Generally, pyrolysis reaction or catalytic reaction can be used as a method for producing disilane from silane, but the yield of these steps does not exceed 2 to 3%.

This is because it is difficult to control the reaction to disilane due to the similarity of the thermodynamic velocities of a number of reactions which can proceed in the silane. The actual reaction of the disilane is the solid formation reaction made by the polymer reaction and the silane Decomposition reaction.

In order to control the polymerization rate or pyrolysis rate of silane more precisely, high-frequency plasma or plasma is used. Since plasma requires a vacuum pressure, Escape.

US Pat. No. 5,478,453 discloses a technology using Dielectric Barrier Discharge (DBD), which is a region of high frequency, but the reactor of this technology has the following disadvantages.

It is impossible to control the liquid level in the reactor, the clogging of the feed line due to the piled disilane liquid and the reduction of the area of the reactor zone, the disilane produced is continuously exposed at a high frequency, Or the possibility of polymer formation.

In addition, since the product is trapped in the reactor, a substantial continuous process is impossible because Hisilane, etc., which is a side reaction, freezes at -120 to -145 DEG C or increases the viscosity of the liquid.

Accordingly, it is an object of the present invention to develop a reaction apparatus capable of solving the above problems and continuously producing disilane, trisilane and tetrasilane from silane.

SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and an object of the present invention is to provide a DBD (Dielectric Barrier Discharge) reaction device capable of continuously producing disilane, trisilane and tetrasilane in silane A porous tube is disposed inside the reaction zone and the condensation zone to divide the reaction zone and the condensation zone to adjust the separation distance between the discharge electrode and the discharge housing or between the discharge electrode and the porous tube to increase the reaction efficiency to increase the yield, And a versatile dielectric barrier discharge reaction device which can be used for the production of disilane and trisilane and tetrasilane.

Other objects and advantages of the present invention will be described hereinafter and will be understood by the embodiments of the present invention. Further, the objects and advantages of the present invention can be realized by the means and the combination shown in the claims.

According to the present invention, there is provided a means for solving the above problems, comprising: a discharge housing (10) into which a raw material gas flows and a reaction gas is discharged; A discharging electrode rod 20 connected to the high frequency generating connection device and discharged through the discharge housing 10; An insulation member (30) installed at the outer circumference of the discharge electrode (20) in the discharge housing (10); A cooling means 40 installed at an outer circumference of the discharge housing 10 to adjust a reaction temperature of the discharge housing 10 to be heated; And a control unit.

INDUSTRIAL APPLICABILITY As described above, the present invention can produce disilane, trisilane, and tetrasilane at a high yield.

In addition, the present invention has the effect of continuously producing disilane and trisilane and tetrasilane.

Further, the present invention has a simple structure as compared with the conventional reaction apparatus, which is easy to manufacture, and has an advantageous effect in terms of stability and economy.

1 is a front cross-sectional view of a first embodiment of a dielectric barrier discharge reactor for the production of disilane, trisilane and tetrasilane according to the present invention.
2 is a front cross-sectional view of a second embodiment of a dielectric barrier discharge reactor for the production of disilane, trisilane and tetrasilane according to the present invention.
3 is a front cross-sectional view of a third embodiment of a dielectric barrier discharge reactor for the production of disilane, trisilane and tetrasilane according to the present invention.

Before describing in detail several embodiments of the invention, it will be appreciated that the application is not limited to the details of construction and arrangement of components set forth in the following detailed description or illustrated in the drawings. The invention may be embodied and carried out in other embodiments and carried out in various ways. It should also be noted that the device or element orientation (e.g., "front,""back,""up,""down,""top,""bottom, Expressions and predicates used herein for terms such as "left,"" right, "" lateral, " and the like are used merely to simplify the description of the present invention, Or that the element has to have a particular orientation. Also, terms such as " first "and" second "are used herein for the purpose of the description and the appended claims, and are not intended to indicate or imply their relative importance or purpose.

The present invention has the following features in order to achieve the above object.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings. Prior to this, terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms, and the inventor should appropriately interpret the concepts of the terms appropriately It should be interpreted in accordance with the meaning and concept consistent with the technical idea of the present invention based on the principle that it can be defined.

Therefore, the embodiments described in this specification and the configurations shown in the drawings are merely the most preferred embodiments of the present invention and do not represent all the technical ideas of the present invention. Therefore, It is to be understood that equivalents and modifications are possible.

According to the first embodiment of the present invention, a raw material gas of a silane (SiH4) gas, a helium gas, or a hydrogen gas mixture is introduced into the interior of the reactor, and a reaction gas outlet (10) having a discharge electrode (12) formed therein; A discharging electrode rod 20 connected to the high frequency generating connection device and discharged through the discharge housing 10; An insulation member (30) installed at the outer circumference of the discharge electrode (20) in the discharge housing (10); A cooling means 40 installed at an outer circumference of the discharge housing 10 to adjust a reaction temperature of the discharge housing 10 to be heated; And a control unit.

In the second embodiment, a source gas of one of a silane (SiH4) gas, a helium gas, and a hydrogen gas mixture is introduced into the inside, and a reaction gas discharge port 12 through which the reaction gas generated inside is discharged is formed. A housing (10); A discharging electrode rod 20 connected to the high frequency generating connection device and discharged through the discharge housing 10; An insulation member (30) installed at the outer circumference of the discharge electrode (20) in the discharge housing (10); A cooling means 40 installed at an outer circumference of the discharge housing 10 to adjust a reaction temperature of the discharge housing 10 to be heated; A space between the discharge electrode rod 20 and the discharge housing 10 is divided into a reaction zone A and a condensation zone B so that the discharge electrode rod 20 is installed in the discharge housing 10, So that the generated reaction gas can be quickly discharged through the porous tube 50 without being exposed to the discharge in the reaction zone for a long period of time

In a third embodiment, a discharge housing 10 having an insulator 14 formed on its inner periphery; A source gas of a silane (SiH4) gas, a helium gas, or a hydrogen gas mixture is introduced into the discharge housing 10 and the reactive gas is discharged through the reaction gas outlet 12 formed in the discharge housing 10, A discharging electrode rod 20 connected to the high frequency generating coupling device and discharged; An insulation member (30) installed at the periphery of the discharge electrode bar (20); A cooling means 40 penetrating into the discharge electrode rod 20 to control the reaction temperature of the discharge housing 10 heated by condensing the reaction gas; A porous tube 50 (50) is provided between the discharge electrode rod 20 and the cooling means 40 to divide the space between the discharge electrode rod 20 and the cooling means 40 into a reaction zone A and a condensation zone B ); And a control unit.

The discharge electrode rod 20 is insulated from the discharge housing 10 through an insulating bushing 61, an insulating gasket 62 and an insulating member 30.

In addition, the discharge housing 10 and the discharge electrode rod 20 may be made of a metal material through which electric power is supplied.

The insulating member 30 is formed of any one of PFA (Perfluoro alkoxy), PTFE (Polytetrafluoroethylene), Glass, Quartz, Ceramic and Silicon rubber do.

The discharge electrode bar 20 and the porous pipe member 50 are characterized in that a gap between the discharge electrode bar 20 and the porous pipe member 50 is maintained between 0.5 and 3 mm.

Further, the reaction zone (A) and the condensation zone (B) are characterized by a volume ratio of 10: 1 to 1:10.

Hereinafter, a dielectric barrier discharge reaction device for producing disilane, trisilane and tetrasilane according to a preferred embodiment of the present invention will be described in detail with reference to FIGS. 1 to 3. FIG.

As shown in the figure, the dielectric barrier discharge reactor for producing disilane, trisilane and tetrasilane according to the present invention is capable of continuously producing disilane, trisilane, tetrasilane, etc. in silane, A housing 10, a discharge electrode rod 20, an insulating member 30, a cooling means 40, and a porous tube 50.

The dielectric barrier discharge reactor for the production of such disilane and trisilane and tetrasilane of the present invention has three embodiments

As shown in FIG. 1, the dielectric barrier discharge reaction device for producing disilane, trisilane and tetrasilane in the first embodiment is a basic pipe type using a dielectric barrier discharge (DBD) (10), a discharge electrode rod (20), an insulating member (30), and a cooling means (not shown).

The discharge housing 10 has a tubular shape with open upper and lower ends and an empty interior. A source gas (for example, a SiH4 gas, a helium gas, a hydrogen gas mixture, or the like) is supplied to the upper end of the discharge housing 10, And a reaction gas outlet 12 through which the reaction gas (e.g., disilane, trisilane, tetrasilane, etc.) generated in the discharge housing 10 is discharged is formed at the lower end of the reaction gas outlet 12 Respectively.

The discharge electrode rod 20 is a metal pipe or a metal rod. The discharge electrode rod 20 protrudes to a predetermined length from the discharge electrode rod 20 and protrudes from the discharge electrode rod 20. (Not shown) for generating high frequency waves.

In the high frequency generator, the resonance frequency is determined according to the reaction conditions for 120 V, and in the present invention, the frequency is maintained at 20 to 100 kHz, preferably 20 to 50 kHz.

The insulating member 30 is formed on the outer periphery of the discharging electrode bar 20 and is formed in a tube shape or the like so as to be integrated with the discharging electrode bar 20, It is prevented from being directly energized with the battery 10.

The cooling means (not shown) is installed at the outer periphery of the discharge housing 10 and has an inlet 41 and an outlet 42 through which various cooling members (e.g., refrigerant) In order to allow the internal temperature of the discharge housing 10 heated by the separate heating means (e.g., various devices capable of heating the discharge housing 10 such as a heater) to be a predetermined reaction temperature desired by the user, (10) is cooled so that the reaction temperature can be controlled. The cooling means may be a cooling coil wound around the outer circumference of the discharge housing 10 in the form of a coil or a cooling jacket covering the outer circumference of the discharge housing 10 because the inside thereof is hollow in the longitudinal direction. ). ≪ / RTI >

The upper and lower ends of the discharge housing 10 in which the discharge electrode bar 20 is installed are provided with discharge electrodes 20 through the center of the discharge bushing 60, The electrode rod 20 and the discharge housing 10 are completely insulated from each other and all the devices connected to the discharge housing 10 except for the pipe connected to the discharge electrode rod 20 and the high frequency generating connection device Should be.

Using the dielectric barrier discharge reactor for the production of disilane, trisilane and tetrasilane in the first embodiment as described above, the yield from silane to disilane is maintained under the condition (amount of source gas, The distance between the discharge electrode rod 20 and the discharge housing 10 and the internal temperature of the discharge housing 10 and the like as well as disilane as well as trisilane and tetrasilane ) Can be made continuous.

An example of the first embodiment constructed as above is as follows.

Using the pipe-shaped discharge housing 10 of the 5/8 inch 350 mm flange 63 type, the 1/4 inch discharge electrode bar 20 and the 3/8 inch PFA insulating member 30, (The dielectric barrier discharge reaction device for producing disilane and trisilane and tetrasilane of the present invention), the discharge electrode rod 20 is connected to the high frequency generator, and the reaction device and related devices are all grounded do.

SiH4 gas of 0.01 L / min, helium gas of 0.5 L / min and hydrogen gas of 0.5 L / min were injected into the reaction apparatus at room temperature, and the generated gas (reaction gas) was detected by GC- ionization detector and GC-mass (mass-selective detector), the results showed that 73% yield of disilane and 6.8% trisilane (0.3%) were obtained at 0.3 to 0.35 W / cm3, 35 kHz and 1.5 psig pressure, , And 0.1% of tetra silane.

As shown in FIG. 2, the device for producing a dielectric barrier discharge for the production of disilane, trisilane and tetrasilane in the second embodiment is characterized in that disilane or the like accumulated in a liquid at a low temperature is no longer exposed to high frequency in the reaction zone (A) Or a porous pipe-type device capable of efficiently passing through the discharge housing 10 without adversely affecting the reaction zone A or reducing the area of the reaction zone A. The cryogenic reaction system Cryogenic reaction system).

The second embodiment for this purpose includes a discharge housing 10, a discharge electrode rod 20, an insulating member 30, a cooling means 40 and a porous tube 50. The discharge housing 10, the discharge electrode 20 ), The insulating member 30, and the cooling means 40 are similar to the first embodiment described above.

The discharge housing 10 is open at its both ends and is hollow inside and has flanges 63 and insulating bushings 60 and 61 and insulating gaskets 62 at both ends thereof. A raw material gas discharge port 13 for discharging the raw material gas to be used and a reaction gas discharge port 12 for discharging the reaction gas generated in the discharge housing 10 in a liquid phase, Respectively.

The discharge electrode rod 20 is electrically connected to the high frequency generating connection device and is inserted into the discharge housing 10 so that the insulating member 30 is formed on the outer periphery of the discharge electrode rod 20, And an insulating bushing 61 is installed at an end portion of the discharge housing 10 located inside the discharge housing 10 so that a porous tube 50 to be described later is fixed at a predetermined distance from the electrode rod.

An inlet port 41 and an outlet port 42 of the cooling member are formed on the outer circumference of the discharge housing 10 and a cooling means 40 for adjusting the reaction temperature in the discharge housing 10 is provided.

The porous tube 50 has a plurality of holes (the hole size of the porous tube 50 is 2 to 3 mm and has a 20 to 30% open / close ratio) on the outer circumference of the tube. (10) so that the discharge electrode rod (20) described above is located in the discharge porous pipe member (50). That is, the porous pipe 50 is positioned between the discharge housing 10 and the discharge electrode bar 20 and is not in contact with any of the structures of the porous pipe 50 and the discharge housing 10, A reaction zone A is formed in the interior of the porous pipe 50 between the porous pipe 50 and the discharge electrode bar 20 and the outside of the porous pipe 50 (B) is formed between the condensing zone (B). At this time, the volume ratio of the reaction zone (A) to the condensation zone (B) is preferably about 2: 3.

In this second embodiment, when the reaction temperature needs to be maintained at a very low temperature as required, the inert gas such as disilane, trisilane, tetrasilane or the like generated therein is condensed or condensed to remain in the reaction zone A where electric discharge is generated In this case, the efficiency of the reaction is lowered, and ultimately, the reaction becomes ineffective. The second embodiment therefore compensates for these shortcomings in the low temperature reaction.

2, when the porous tube 50 is installed outside the discharge electrode rod 20 surrounded by the insulating member 30, the discharge is generated between the discharge electrode rod 20 and the porous tube 50 ), And the produced Disilane gas or the like is discharged from the reaction zone A (or the electric discharge zone), condensed on the outer wall of the discharge housing 10, and falls downward. In this case, since the generated reaction gas is no longer exposed to electric discharge, it can be prevented from being decomposed or polymerized, and the reaction zone (A) can not be changed by the condensed reaction gas, This is possible.

An example of the second embodiment configured as described above is as follows.

A 1/4 inch discharge electrode 20 and a 3/8 inch PFA insulating member 30 are used as the discharge electrode unit 10 of the flange 63 type of 1 inch in diameter and 600 mm in diameter. (The dielectric barrier discharge reaction device for producing disilane and trisilane and tetrasilane of the present invention) according to the second embodiment, the discharge electrode rod 20 is connected to the high frequency generator, And related devices are grounded.

SiH4 gas at a rate of 0.01 L / min, helium gas at a rate of 0.5 L / min, hydrogen gas at a rate of 0.5 L / min were injected into the reactor at -120 to -130 ° C, Hour mass spectrometry using in-situ mass spectrometry to obtain 85% yield of disilane, 9.2% trisilane and 0.2% tetra silane at 0.45 ~ 0.5 W / cm3, 35 kHz and 1.5 psig pressure.

The dielectric barrier discharge reactor for the production of disilane and trisilane and tetrasilane of the third embodiment differs from the first and second embodiments in that a cooling means 40 is provided in the discharge housing 10 Is not provided outside in the form of a jacket or a coil, but is provided at the center of the discharge housing (10) to condense the reaction gas generated by the reaction at the center.

The third embodiment for this purpose includes a discharge housing 10, a discharge electrode rod 20, an insulating member 30, a cooling means 40, and a porous tube 50.

The discharge housing 10 is provided with insulation gasket 62 and flange 63 at the upper and lower ends thereof and an insulating material 70 at the lower end thereof. A raw gas inlet 11 for introducing the raw material gas is formed at the upper end of the outer periphery and a reaction gas outlet 12 protruding to the outside through the heat insulating material 70 is formed at the lower end. In addition, an insulator 14 is integrally formed on the inner periphery.

The discharge electrode bar 20 is opened at its upper and lower ends and spaced apart in the longitudinal direction inside the discharge housing 10 in a state where the insulating member 30 is formed on the inner circumference. Frequency generating coupling device 21 or the high-frequency generating coupling device 21 provided at the outer periphery of the high-frequency generating coupling device 10. The discharge electrode bar 20 is installed inside the discharge housing 10 and the insulating bushing 61 is installed at the upper end of the discharge electrode bar 20. Since the insulator 14 is provided between the discharge housing 10 and the discharge electrode 20 in the raw material gas introduced through the raw material gas inlet 11 formed in the discharge housing 10, And is introduced into the discharge electrode rod 20 installed in the discharge housing 10 without being influxed.

The discharge electrode 10 and the discharge electrode rod 20 are spaced apart from each other and the discharge electrode rod 20 is present near the wall of the discharge housing 10 so that the insulator 14 So that mutual energization is prevented due to the insulator 14 positioned between the discharge housing 10 and the discharge electrode bar 20.

The cooling means 40 is spaced apart from the inside of the discharge electrode bar 20 so that one end of the cooling electrode 40 protrudes through the upper end flange 63 of the discharge housing 10. An inlet port 41 and an outlet port 42 are formed on the protruded upper side so as to allow the cooling member to flow in and out. The inlet pipe 43 formed in the inlet port 41 is provided inside the cooling unit 40 So as to be in the form of being inserted in the longitudinal direction.

The porous pipe member 50 is provided between the cooling means 40 and the discharge electrode bar 20 and is disposed between the cooling means 40 and the discharge electrode bar 20 in the reaction zone A as in the second embodiment. (Between the periphery of the discharge electrode bar 20 and the outer periphery of the porous pipe 50) and the condensation zone B (between the periphery of the porous pipe 50 and the outer periphery of the cooling means 40). Further, the upper end of the porous pipe 50 is insulated by using the insulator 61.

The cooling pipe 40 is installed in the porous tube 50 and the porous tube 50 is inserted into the discharge electrode rod 20 so that the discharge electrode rod 20 is inserted into the discharge housing 10 It has the configuration of the quadrangular tube type to be put in.

In the third embodiment, the volume of the reaction zone A is larger than the volume of the condensation zone B, which is related to the inner diameter of the reaction device in the form of a pipe. When the volume of the reaction zone (A) is larger than the volume of the condensation zone (B), the reaction gas enters the reaction zone (A) more and the efficiency increases. The third embodiment increased the yield of silane to disilane by about 10% compared to the second embodiment.

In addition, in the first, second, and third embodiments configured as described above,

The discharge housing 10 and the discharge electrode rod 20 are made of a metal material. The metal material is made of stainless steel, carbon steel, copper, Alumina (Alumina), and the like.

Any one of PFA (Perfluoro alkoxy), PTFE (Polytetrafluoroethylene), Glass, Quartz, Ceramic, Silicon rubber may be used as the insulating member 30. (Of these, PFA has the greatest electrical insulation characteristics, lowest dissipation factor, and excellent durability.)

The gap between the discharge housing 10 and the discharge electrode 20 is 0.5 to 3 mm and preferably 1 to 2 mm and the discharge electrode 20 is wound with the insulating member 30. (Gap) between the porous tube 50 and the porous tube 50 is 0.5 to 3 mm, preferably 1 to 2 mm.

Also, the volume ratio of the reaction zone (A) and the condensation zone (B) in the second and third embodiments is 10: 1 to 1:10, preferably 3: 2 to 2: 3.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. It is to be understood that various changes and modifications may be made without departing from the scope of the appended claims.

10: discharge housing 11: source gas inlet
12: reaction gas outlet 13: raw material gas outlet
14: insulator 20: discharge electrode rod
21: high frequency generating connector 30: insulating member
40: cooling means 41: inlet
42: outlet 43: inlet pipe
50: porous tube 60: insulated bushing
61: insulated bushing 62: insulating gasket
63: Flange 70: Insulation
A: Reaction zone B: Condensation zone

Claims (8)

A discharge housing 10 in which a raw material gas of one of a silane (SiH4) gas, a helium gas, and a hydrogen gas mixture flows in and a reaction gas outlet 12 through which a reaction gas generated therein is discharged;
A discharging electrode rod 20 connected to the high frequency generating connection device and discharged through the discharge housing 10;
An insulation member (30) installed at the outer circumference of the discharge electrode (20) in the discharge housing (10);
A cooling means 40 installed at an outer circumference of the discharge housing 10 to adjust a reaction temperature of the discharge housing 10 to be heated;
Wherein the dielectric barrier discharge reactor comprises a dielectric barrier discharge reactor for producing disilane, trisilane and tetrasilane.
A discharge housing 10 in which a raw material gas of one of a silane (SiH4) gas, a helium gas, and a hydrogen gas mixture flows in and a reaction gas outlet 12 through which a reaction gas generated therein is discharged;
A discharging electrode rod 20 connected to the high frequency generating connection device and discharged through the discharge housing 10;
An insulation member (30) installed at the outer circumference of the discharge electrode (20) in the discharge housing (10);
A cooling means 40 installed at an outer circumference of the discharge housing 10 to adjust a reaction temperature of the discharge housing 10 to be heated;
A space between the discharge electrode rod 20 and the discharge housing 10 is divided into a reaction zone A and a condensation zone B so that the discharge electrode rod 20 is installed in the discharge housing 10, A porous tube (50) for preventing the generated reaction gas from being exposed to a discharge;
Wherein the dielectric barrier discharge reactor is a device for producing disilane, trisilane and tetrasilane.
A discharge housing (10) having an insulator (14) formed on its inner periphery;
A source gas of a silane (SiH4) gas, a helium gas, or a hydrogen gas mixture is introduced into the discharge housing 10 and the reactive gas is discharged through the reaction gas outlet 12 formed in the discharge housing 10, A discharging electrode rod 20 connected to the high frequency generating coupling device and discharged;
An insulation member (30) installed at the periphery of the discharge electrode bar (20);
A cooling means 40 penetrating into the discharge electrode rod 20 to control the reaction temperature of the discharge housing 10 heated by condensing the reaction gas;
A porous tube 50 (50) is provided between the discharge electrode rod 20 and the cooling means 40 to divide the space between the discharge electrode rod 20 and the cooling means 40 into a reaction zone A and a condensation zone B );
Wherein the dielectric barrier discharge reactor is a device for producing disilane, trisilane and tetrasilane.
4. The method according to any one of claims 1 to 3,
The discharge electrode rod 20 is insulated from the discharge housing 10 through an insulating bushing 60, an insulator 14 or an insulating gasket 62. The dielectric barrier for the production of disilane and trisilane and tetrasilane, Discharge reaction device.
4. The method according to any one of claims 1 to 3,
The discharge housing (10) and the discharge electrode rod (20)
Wherein a metal material to which electricity is energized is used as a dielectric barrier discharge reactor for producing disilane, trisilane and tetrasilane.
4. The method according to any one of claims 1 to 3,
The insulating member (30)
Wherein at least one of tetrafluoroethylene (PFA), perfluoroalkoxy (PTFE), polystetrafluoroethylene (PTFE), glass, quartz, ceramic and silicone rubber is used. And a dielectric barrier discharge reactor for producing the dielectric barrier discharge reactor.
The method according to claim 2 or 3,
The discharge electrode (20) and the porous tube (50)
Wherein the distance between the discharge electrode rod (20) and the porous tube (50) is kept at a distance of 0.5 to 3 mm.
The method according to claim 2 or 3,
The reaction zone (A) and the condensation zone (B)
Wherein the volume ratio of the disilane to the trisilane is from 10: 1 to 1:10.
KR1020130066750A 2013-06-11 2013-06-11 Dielectric Barrier Discharge Reactor for making Disilane, Trisilane and Tetrasilane from Silane KR101538388B1 (en)

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PCT/KR2014/004908 WO2014200219A1 (en) 2013-06-11 2014-06-03 Dielectric barrier discharge reacting apparatus for producing disilane, trisilane, and tetrasilane

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Citations (4)

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US5478453A (en) * 1993-03-11 1995-12-26 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process for preparing disilane from monosilane by electric discharge and cryogenic trapping
US6221155B1 (en) * 1997-12-15 2001-04-24 Advanced Silicon Materials, Llc Chemical vapor deposition system for polycrystalline silicon rod production
KR100893183B1 (en) * 2008-06-24 2009-04-15 (주)티에스티아이테크 Apparatus and method of manufacturing polysilicon using laser induced chemical vapor deposition
US20110305604A1 (en) * 2009-01-22 2011-12-15 Schmid Silicon Technology Gmbh Reactor for producing polycrystalline silicon using the monosilane process

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US5478453A (en) * 1993-03-11 1995-12-26 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process for preparing disilane from monosilane by electric discharge and cryogenic trapping
US6221155B1 (en) * 1997-12-15 2001-04-24 Advanced Silicon Materials, Llc Chemical vapor deposition system for polycrystalline silicon rod production
KR100893183B1 (en) * 2008-06-24 2009-04-15 (주)티에스티아이테크 Apparatus and method of manufacturing polysilicon using laser induced chemical vapor deposition
US20110305604A1 (en) * 2009-01-22 2011-12-15 Schmid Silicon Technology Gmbh Reactor for producing polycrystalline silicon using the monosilane process

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