B2F4 manufacturing process

Patent metadata

Field	Value
Publication number	US-9938156-B2
Application number	US-201214350543-A
Country	US
Kind code	B2
Filing date	Oct 9, 2012
Priority date	Oct 10, 2011
Publication date	Apr 10, 2018
Grant date	Apr 10, 2018

Abstract

A reaction system and method for preparing compounds or intermediates from solid reactant materials is provided. In a specific aspect, a reaction system and methods are provided for preparation of boron-containing precursor compounds useful as precursors for ion implantation of boron in substrates. In another specific aspect, a reactor system and methods are provided for manufacture of boron precursors such as B 2 F 4 .

First claim

What is claimed is:

1. A reactor system comprising:
a reaction zone for contacting BF 3 gas with boron-containing solids under temperature and pressure conditions effective to form an intermediate species;
an opening for allowing an unreacted portion of BF 3 gas and the intermediate species to exit the reaction zone into a condensation zone for effecting reaction between the intermediate species and the unreacted portion of the BF 3 gas to form a reaction product comprising B 2 F 4 wherein the condensation zone effects reaction between the intermediate species and the unreacted portion of the BF 3 gas to form a reaction product comprising B 2 F 4 by cooling the intermediate species and the unreacted portion of the BF 3 gas in a cryogenic temperature range and wherein the cryogenic temperature range is controlled by use of a hydraulic lift configured to translate a vessel containing material that can cool at cryogenic temperatures, in a selected one of upward and downward directions, between an uppermost position and a lowermost position;
a recovery zone for recovering the reaction product and unreacted BF 3 gas; and
a recycling zone for recycling the recovered unreacted BF 3 gas to the reaction zone, wherein the recycling zone comprises a purification zone effective to reduce impurities in the unreacted BF 3 gas.

2. A reactor system comprising:
a reaction zone for contacting BF 3 gas with boron-containing solids under temperature and pressure conditions effective to form an intermediate species; the reaction zone comprises a double-walled quartz jacket;
an opening for allowing an unreacted portion of BF 3 gas and the intermediate species to exit the reaction zone into a condensation zone for effecting reaction between the intermediate species and the unreacted portion of the BF 3 gas to form a reaction product comprising B 2 F 4 ; the condensation zone comprises a stainless steel vessel and a seal surrounding the opening, the seal sealingly connecting the reaction zone to the condensation zone, wherein the seal is effective to sealingly connect the reaction zone to the condensation zone under vacuum or super-atmospheric pressures;
a recovery zone for recovering the reaction product and unreacted BF 3 gas; and
a recycling zone for recycling the recovered unreacted BF 3 gas to the reaction zone, wherein the recycling zone comprises a purification zone effective to reduce impurities in the unreacted BF 3 gas.

3. The reactor system of claim 2 , wherein the seal comprises an O-ring including a perfluoroelastomer material disposed beneath a split flange, the split flange effective to maintain a pressure on the seal.

4. An apparatus for production of B 2 F 4 , comprising:
a reactor containing a boron reactant that is reactive with boron trifluoride, BF 3 , to yield boron fluoride, BF, wherein said reactor is configured to provide process conditions effective for reaction of BF 3 and said boron reactant to yield BF as a reaction product, and to discharge BF and unreacted BF 3 as a reactor effluent;
a source of BF 3 arranged to supply BF 3 to the reactor;
a condensation zone configured to receive the reactor effluent from the reactor and to provide process conditions effective for condensation of BF and BF 3 to yield B 2 F 4 ; and
a recirculation loop for flowing to the reactor unreacted BF 3 recoverable from the condensation, wherein the recirculation loop comprises a purification unit configured to purify recirculated BF 3 flowed to the reactor, wherein the purification unit comprises a freeze-pump-thaw purification unit.

5. The apparatus of claim 4 , wherein the reactor contains elemental boron as said boron reactant.

6. The apparatus of claim 5 , wherein the elemental boron is in a monocrystalline form comprising crystal planes of differing reactivity to boron trifluoride, and a major fraction of surface area of said elemental boron exposed to boron trifluoride as said boron reactant comprises surface area of a crystal plane having higher reactivity to boron trifluoride than other crystal plane(s) of said monocrystalline boron.

7. A method for production of B 2 F 4 , using the reactor of claim 4 , said method comprising:
reacting boron reactant in a reaction zone of the reactor with said source of BF 3 arranged to supply boron trifluoride, BF 3 , to the reactor to yield boron fluoride, BF; said reactor configured to provide process conditions effective for reaction of BF 3 and said boron reactant to yield BF as a reaction product, and to discharge BF and unreacted BF 3 as a reactor effluent;
condensing BF and unreacted BF 3 from said reacting, to yield B 2 F 4 in said condensation zone configured to receive the reactor effluent from the reactor and to provide process conditions effective for condensation of BF and BF 3 to yield B 2 F 4 ;
purifying unreacted BF 3 recovered from said condensing in the recirculation loop, said recirculation loop for flowing to the reactor unreacted BF 3 recoverable from the condensation comprises a freeze-pump-thaw purification unit configured to yield purified BF 3 ; and
recirculating said purified BF 3 to the reaction zone of the reactor, wherein said purifying comprises freeze-pump-thaw purification.

8. The method of claim 7 , wherein said boron is in a monocrystalline form comprising crystal planes of differing reactivity to boron trifluoride, and a major fraction of surface area of said monocrystalline boron exposed to boron trifluoride in said reacting comprises surface area of a crystal plane having higher reactivity to boron trifluoride than other crystal plane(s) of said monocrystalline boron-containing solid.

Assignees

• Entegris Inc

Inventors

• Byl Oleg
• Jones Edward E
• Pydi Chiranjeevi
• Sweeney Joseph D

Classifications

• B01J19/0073

  Sealings (sealings for pressure vessels per se F16J15/00) · CPC title

• B01J19/129

  Radiofrequency · CPC title

• B01J2219/0886

  Gas-solid · CPC title

• B01J3/03

  Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor · CPC title

• C01B35/061 Primary

  Halides · CPC title