Method and apparatus for chemical synthesis

• US 20030017092A1
• Filed: 07/16/2002
• Published: 01/23/2003
• Est. Priority Date: 07/19/2001
• Status: Active Grant

• Current Assignee: ASM IP Holding B.V. (ASM International NV)
• Original Assignee: ASM America Incorporated (ASM International NV)
• Inventors: Todd, Michael A.
• Granted Patent: US 6,858,196 B2
• Time in Patent Office: Days
• US Class Current: 422/186.03
• CPC Class Codes: B01J 19/088 giving rise to electric discharges for heating purposes H05B7/00; for the production of ozone C01B13/11, H01T19/00
• CPC Class Codes: B01J 2219/00191 Control algorithm
• CPC Class Codes: B01J 2219/0286 Steel
• CPC Class Codes: B01J 2219/0809 employing two or more electrodes
• CPC Class Codes: B01J 2219/083 cylindrical
• CPC Class Codes: B01J 2219/0849 Corona pulse discharge
• CPC Class Codes: B01J 2219/0879 Solid
• CPC Class Codes: C01B 33/04 Hydrides of silicon

Abstract

An apparatus is provided for synthesis and collection of higher order chemical compounds from lower order precursors. The apparatus includes a first silent electric discharge reactor configured to synthesize an intermediate product (e.g., disilane) from a precursor chemical (e.g., monosilane). A second silent electric discharge reactor is connected downstream of the first reactor. This second reactor is configured to convert the intermediate product into the higher order chemical compound (e.g., trisilane). Multiple condensation traps are also connected to receive effluent from the second reactor, which will generally include the compound of interest as well as unreacted precursor and intermediate product. In the illustrated embodiment, a parallel second condensation traps is also included to shunt flow and continue collection while the chemical of interest is removed for purification. Moreover, parallel second condensation traps for the intermediate product and unreacted (or recombined) precursor allow continued collection while the contents of the first traps are recycled in the reactor(s).

Claims

1. An apparatus for synthesis and collection of higher order chemical compounds from lower order precursors, comprising:

a first silent electric discharge reactor configured to synthesize an intermediate product from a precursor chemical;

a source of the precursor chemical connected upstream of the first reactor;

a second silent electric discharge reactor connected downstream of the first reactor, the second reactor configured to convert the intermediate product into a higher order chemical compound; and

a plurality of condensation traps connected to receive effluent from the second reactor.

2. The apparatus of claim 1, wherein the plurality of condensation traps comprises at least a first trap for the higher order chemical compound, a first trap for the intermediate product and a first trap for the precursor chemical in the effluent from the second reactor.

3. The apparatus of claim 2, further comprising a second trap for the higher order chemical compound, a second trap for the intermediate product and a second trap for the precursor chemical in the effluent from the second reactor, the second traps being arranged in parallel with the first traps to facilitate shunting flow individually into the second traps while collected fluids are removed from the corresponding first traps.

4. The apparatus of claim 3, further comprising a feedback line from the first and second traps for the intermediate product to the second reactor for recycling the intermediate product.

5. The apparatus of claim 4, wherein the higher order chemical compound comprises trisilane, the intermediate product comprises disilane and the precursor chemical comprises monosilane.

6. The apparatus of claim 1, wherein the condensation traps are configured for periodic warming for removal of collected chemicals therefrom.

7. A method of synthesizing silicon compounds, comprising:

feeding silicon precursors into an electric discharge reactor, wherein the silicon precursors are broken down and recombined to produce additional silane compounds;

feeding products of the reactor to a downstream series of condensation traps, which recover a higher order silane in one trap and lower order silanes in at least one other trap; and

periodically removing the higher order silane to a storage device.

8. The method of claim 7, further comprising periodically recovering the lower order silanes and recycling the recovered lower order silanes for further reactions producing the higher order silane.

9. The method of claim 7, wherein the series of condensation traps comprises a series of parallel condensation traps for each recovered silane.

10. The method of claim 9, further comprising recycling an intermediate product recovered in a first lower order condensation trap while continuing to condense the intermediate product in a second lower order condensation trap, arranged in parallel with the first lower order condensation trap, from ongoing reactions in the reactor.

11. The method of claim 7, wherein the higher order silane comprises trisilane and the lower order silanes comprise disilane and monosilane.

12. The method of claim 11, further comprising providing separate condensation traps for recovering trisilane, disilane and monosilane.

13. The method of claim 12, further comprising, once a first trisilane condensation trap has been sufficiently filled, shunting flow from ongoing reactions in the reactor to a second trisilane condensation trap, while products in the first trisilane condensation trap are removed to a storage device.

14. The method of claim 13, further comprising distilling to purify the trisilane after removing from the first trisilane condensation trap and prior to storing in the storage device.

15. The method of claim 7, wherein the electric discharge reactor comprises two silent electric discharge reactors in series, an upstream one of the reactors being optimized to produce an intermediate product and a downstream one of the reactors being optimized to employ the intermediate product in producing another product.

17. The apparatus of claim 16, wherein the silicon precursor comprises monosilane and the first silicon compound comprises disilane.

18. The apparatus of claim 17, further configured to provide further monosilane separately to the second reactor.

19. The apparatus of claim 17, wherein the higher order silane comprises trisilane and reactions in the second reactor yield a higher percentage of trisilane compared with reactions in the first reactor.

20. The apparatus of claim 15, wherein conditions in the first reactor are optimized for disilane production, and conditions in the second reactor are optimized for trisilane production.

16. An apparatus for synthesizing a higher order silane, comprising:

a first discharge reactor configured to produce a first silicon compound from a silicon precursor; and

a second discharge reactor connected downstream of the first discharge reactor, the second discharge reactor receiving the first silicon compound from the first discharge reactor and converting it into the higher order silane.

21. A silent electric discharge apparatus configured for synthesizing higher order silane from monosilane precursors, comprising:

a silent electric discharge reactor, having a source of monosilane connected thereto;

a condensation trap connected downstream of the reactor for collecting reaction products; and

a source of disilane connected upstream of the silent electric discharge reactor.

22. The apparatus of claim 21, wherein the source of disilane comprises an upstream reactor provided with a source of monosilane.

23. The apparatus of claim 22, further comprising a gas line selectively communicating condensed reaction products in the condensation trap with the silent electric discharge reactor.

24. The apparatus of claim 21, wherein the source of disilane comprises the condensation trap downstream of the reactor and a gas line selectively communicating condensed reaction products in the condensation trap with the silent electric discharge reactor.