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 PDFInfo
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- 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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- discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/04—Hydrides of silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
- H01J37/32348—Dielectric barrier discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
- B01J2219/0807—Processes 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
- B01J2219/0807—Processes 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
- B01J2219/0824—Details relating to the shape of the electrodes
- B01J2219/0826—Details relating to the shape of the electrodes essentially linear
- B01J2219/083—Details relating to the shape of the electrodes essentially linear cylindrical
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0871—Heating or cooling of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0873—Materials to be treated
- B01J2219/0875—Gas
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
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
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
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
In a third embodiment, a
The
In addition, the
The insulating
The
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
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
The
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
The cooling means (not shown) is installed at the outer periphery of the
The upper and lower ends of the
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
An example of the first embodiment constructed as above is as follows.
Using the pipe-
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
The second embodiment for this purpose includes a
The
The
An
The
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
An example of the second embodiment configured as described above is as follows.
A 1/4
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
The third embodiment for this purpose includes a
The
The
The
The cooling means 40 is spaced apart from the inside of the
The
The cooling
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
Any one of PFA (Perfluoro alkoxy), PTFE (Polytetrafluoroethylene), Glass, Quartz, Ceramic, Silicon rubber may be used as the insulating
The gap between the
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 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 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 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.
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.
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.
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 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 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.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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KR1020130066750A KR101538388B1 (en) | 2013-06-11 | 2013-06-11 | Dielectric Barrier Discharge Reactor for making Disilane, Trisilane and Tetrasilane from Silane |
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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KR1020130066750A KR101538388B1 (en) | 2013-06-11 | 2013-06-11 | Dielectric Barrier Discharge Reactor for making Disilane, Trisilane and Tetrasilane from Silane |
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KR20140144594A KR20140144594A (en) | 2014-12-19 |
KR101538388B1 true KR101538388B1 (en) | 2015-07-22 |
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KR1020130066750A KR101538388B1 (en) | 2013-06-11 | 2013-06-11 | Dielectric Barrier Discharge Reactor for making Disilane, Trisilane and Tetrasilane from Silane |
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DE102020211833A1 (en) | 2020-09-22 | 2022-03-24 | Evonik Operations Gmbh | Process for the production of oligomeric hydridosilanes from SiH4 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
Family Cites Families (1)
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EP2052097B1 (en) * | 2006-07-31 | 2016-12-07 | Tekna Plasma Systems, Inc. | Plasma surface treatment using dielectric barrier discharges |
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- 2014-06-03 WO PCT/KR2014/004908 patent/WO2014200219A1/en active Application Filing
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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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KR20140144594A (en) | 2014-12-19 |
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