EP0105328A4 - Reinigung von silikonhaliden. - Google Patents

Reinigung von silikonhaliden.

Info

Publication number
EP0105328A4
EP0105328A4 EP19830901472 EP83901472A EP0105328A4 EP 0105328 A4 EP0105328 A4 EP 0105328A4 EP 19830901472 EP19830901472 EP 19830901472 EP 83901472 A EP83901472 A EP 83901472A EP 0105328 A4 EP0105328 A4 EP 0105328A4
Authority
EP
European Patent Office
Prior art keywords
impurities
silicon
trichlorosilane
organosiloxane
boron
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP19830901472
Other languages
English (en)
French (fr)
Other versions
EP0105328A1 (de
Inventor
William David Kray
John Simon Razzano
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
General Electric Co
Original Assignee
General Electric Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by General Electric Co filed Critical General Electric Co
Publication of EP0105328A1 publication Critical patent/EP0105328A1/de
Publication of EP0105328A4 publication Critical patent/EP0105328A4/de
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/10778—Purification

Definitions

  • This invention relates to the preparation of trichlorosilane for the manufacture of electronic grade silicon and, more particularly, to novel methods for removing trace impurities of electrical donor contaminates, especially boron and other Lewis acid or proton donor-type impurities.
  • Silicon of extremely high purity is required for sophisticated electronics uses such as in semiconductors and transistors. It is well known that even trace impurities can seriously impair the performance of silicon-containing electronic components.
  • Elemental silicon for semiconductor use is generally prepared by reduction of silicon halides, such as silicon tetrachloride (SiCl 4 ), trichlorosilane (HSiCl 3 ) and dichlorosilane (H 2 SiCl 2 ), with hydrogen, zinc, sodium or metal hydrides. Silicon may also be derived from thermal decomposition of silane (SiH 4 ), but this latter material is hard to work with because it burns explosively on contact with air.
  • boron One of the most difficult impurities to remove from high purity silicon is boron. Whereas other common impurities such as copper, iron and manganese are comparatively easy to remove by conventional techniques (e.g., zone refining, crystal pulling), boron has physical properties so similar to silicon that separation is accomplished only by repeated trials. Moreover, concentrating purification efforts on the starting materials, e.g., chlorosilanes, is likewise difficult because boron forms corresponding compounds with similar properties.
  • the method of this invention involves contacting the boron halide or other Lewis acid impurity present in a silicon halide solution with a molar excess of an organosiloxane, heating the solution to cause a reaction between the impurities and the siloxane to yield compounds of lower vapor pressure than the silicon halide, and then distilling the pure silicon halide off, leaving the siloxane-bound impurities behind.
  • This method is very effective for removing boron contaminates, especially from solutions of silicon chlorides, such as trichlorosilane.
  • the boron concentration in a solution of trichlorosilane can be reduced by the treatment of the present invention to less than 50 parts per trillion (ppt) .
  • a "Lewis acid” is any substance that will take up an electron pair to form a covalent bond (i.e., "electron-pair acceptor”). This includes the “proton donor” concept of the Lowry-Br ⁇ nsted definition of acids.
  • boron trifluoride (BF 3 ) is a typical Lewis acid, as it contains only six electrons in its outermost electron orbital shell. BF 3 tends to accept a free electron pair to complete its eight-electron orbital.
  • siloxane compounds suitable for the purposes herein are any organosiloxanes which will react with the boron or other impurity present in the silicon halide solution to form impurity-siloxane compounds (e.g., borosiloxane) having a lower vapor pressure than the solution to be purified, such that a pure silicon-containing solution may be distilled from the reaction vessel, leaving the impurity-siloxane compounds behind.
  • impurity-siloxane compounds e.g., borosiloxane
  • siloxanes include alkyl, aryl, halogenated alkyl, halogenated aryl or hydrogen substituted alkyl or aryl cyclotrisiloxanes and cyclotetrasiloxanes such as hexamethylcyclotri siloxane, octamethylcyclotetrasiloxane, polydimethyl siloxane fluids, dimethyl (methyl hydrogensiloxane copolymers and other cyclic siloxane monomers. Cyclotrisiloxanes, alkyl cyclotrisiloxanes, halogenated alkyl cyclotrisiloxanes are preferred; hexamethylcyclotrisiloxane is most preferred.
  • the siloxanes are added to the contaminated silicon halides solution in an amount which will ensure reaction of the siloxanes with the Lewis acid impurities. Best results are obtained if this amount is a large molar excess, for example 5-100 times, based on the concentration of the contaminate. However, any amount of siloxane suitable to effectively bind the impurities present in the solution is contemplated.
  • the mixture is heated to drive the reaction of the siloxanes with the Lewis acid impurities.
  • very high temperatures i.e. , temperatures over 200 oC
  • the reaction may not be sufficient to effectively remove all of the BCl 3 .
  • a reaction temperature range from 25oC to about 200°C is preferred, from about 80oC to about 130°C is most preferred, but higher temperatures are also contemplated so long as the reaction products will not be distilled in the same fraction as the silicon halide, and thereby confound the purification. Best results have been obtained at about 100oC.
  • reaction is allowed to proceed until substantially all of the impurities are bound to siloxane compounds.
  • the time will of course vary according to materials used, temperature used, pressure, etc. Simple experimentation will readily lead to the optimum reaction period for a given purification.
  • the final step in the purification of the present invention is to distill the pure silicon halide from the reaction solution.
  • the decreased volatility of the siloxane-bound impurities compared to the silicon halides makes this final distillation possible.
  • the distillation may be carried out at atmospheric pressures or at higher pressure so long as the temperature of the liquid material does not exceed the decomposition temperature of the borates formed in the process. It is preferred to maintain the temperature of the liquid below about 200oC.
  • TCS trichlorosilane
  • BCl 3 boron trichloride
  • the charge to the distillation vessel was 2000 g. with 99% of the material recovered, the presence of boron was less than 50 parts per trillion in each of the distilled fractions.
  • Example 1 400 parts by weight of 0.018 molar BCl 3 (5000 ppm) in TCS was placed in a reaction vessel with sufficient trimer to make the solution 0.09 molar. The reaction mixture was agitated under pressure and samples distilled periodically for analysis by infrared spectroscopy as in Example 1:

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
EP19830901472 1982-03-18 1983-03-17 Reinigung von silikonhaliden. Withdrawn EP0105328A4 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US35943782A 1982-03-18 1982-03-18
US359437 1982-03-18

Publications (2)

Publication Number Publication Date
EP0105328A1 EP0105328A1 (de) 1984-04-18
EP0105328A4 true EP0105328A4 (de) 1984-09-19

Family

ID=23413785

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19830901472 Withdrawn EP0105328A4 (de) 1982-03-18 1983-03-17 Reinigung von silikonhaliden.

Country Status (3)

Country Link
EP (1) EP0105328A4 (de)
IT (1) IT1163149B (de)
WO (1) WO1983003244A1 (de)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5660690A (en) * 1996-06-03 1997-08-26 Dow Corning Corporation Method for distilling hexamethylcyclotrisiloxane
JP4582091B2 (ja) * 2004-04-13 2010-11-17 ダイキン工業株式会社 クロロトリフルオロエチレン共重合体
EP3002262B1 (de) 2014-10-01 2018-06-27 Heraeus Quarzglas GmbH & Co. KG Verfahren zur Herstellung von synthetischem Quarzglas mittels einer polymerisierbaren Polyalkylsiloxanverbindung
CN117247018B (zh) * 2023-09-22 2025-10-31 新疆大全新能源股份有限公司 一种回收新鲜料系统重杂的方法和装置

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1330442A (fr) * 1961-08-04 1963-06-21 Merck & Co Inc Corps semiconducteur et son procédé de fabrication

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3126248A (en) * 1964-03-24 Process for producing purified
US2857249A (en) * 1956-07-03 1958-10-21 Guenter A Wolff Method of purifying silicon tetrachloride
US3403003A (en) * 1966-12-23 1968-09-24 Western Electric Co Method of removing boron from silicon tetrachloride
US3540861A (en) * 1968-02-07 1970-11-17 Union Carbide Corp Purification of silicon compounds
DE2546957C3 (de) * 1975-10-20 1980-10-23 Wacker-Chemitronic Gesellschaft Fuer Elektronik-Grundstoffe Mbh, 8263 Burghausen Verfahren zur Reinigung von Halogensilanen

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1330442A (fr) * 1961-08-04 1963-06-21 Merck & Co Inc Corps semiconducteur et son procédé de fabrication

Also Published As

Publication number Publication date
IT8320139A0 (it) 1983-03-18
IT1163149B (it) 1987-04-08
EP0105328A1 (de) 1984-04-18
WO1983003244A1 (en) 1983-09-29

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Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Designated state(s): DE

17P Request for examination filed

Effective date: 19840209

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 19851213

RIN1 Information on inventor provided before grant (corrected)

Inventor name: KRAY, WILLIAM DAVID

Inventor name: RAZZANO, JOHN SIMON