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WO1992009719A1 - Procede de depot d'elements de groupe 15 et/ou de groupe 16 - Google Patents

Procede de depot d'elements de groupe 15 et/ou de groupe 16 Download PDF

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Publication number
WO1992009719A1
WO1992009719A1 PCT/AU1991/000533 AU9100533W WO9209719A1 WO 1992009719 A1 WO1992009719 A1 WO 1992009719A1 AU 9100533 W AU9100533 W AU 9100533W WO 9209719 A1 WO9209719 A1 WO 9209719A1
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Prior art keywords
group
semiconductor
compound
formula
feedstock
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PCT/AU1991/000533
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English (en)
Inventor
Geoffrey Norman Pain
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The Commonwealth Industrial Gases Limited
Monash University
Australian And Overseas Telecommunications Corporation Limited
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Publication of WO1992009719A1 publication Critical patent/WO1992009719A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02551—Group 12/16 materials
    • H01L21/02562—Tellurides
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/90—Antimony compounds
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/0257—Doping during depositing
    • H01L21/02573—Conductivity type
    • H01L21/02576—N-type
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/0257—Doping during depositing
    • H01L21/02573—Conductivity type
    • H01L21/02579—P-type
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD

Definitions

  • the present invention relates to a method for the deposition of Group 15 and/or Group 16 elements on a substrate.
  • Group 15 elements are also known as Group VA elements:specifically nitrogen (N), phosphorus (P), arsenic (As), antimony (Sb) and bismuth (Bi).
  • Group 16 elements are also known as the Group VIA elements: specifically oxygen (0), sulphur (S), selenium (Se), tellurium (Te) and polonium (Po).
  • MCT pseudobinary alloy- mercury cadmium telluride
  • MOCVD metal organic chemical vapour deposition
  • MOVPE metal organic vapour phase epitaxy
  • aims are (a) the realization of regions with controlled electrical characteristics through the depth of the layer and (b) the creation, through doping, of p-n electrical junctions where p-type and n-type materials have holes and electrons respectively, as the excess carriers.
  • the range of devices which can be made incorporating p-n junctions include detectors, light emitting diodes, lasers, solar cells and high speed transistors.
  • One approach to n-on-p junctions in MCT is to grow the MCT at high temperatures where the equilibrium cation vacancy defect level is high, resulting in as-grown p- type behaviour. The layer is then subjected to ion implantation and subsequent annealing to produce the junction.
  • n-type MCT arises through electrically active damage in the layer and is largely independent of the chemical nature of the implanted element.
  • This approach is laborious, expensive and it can be difficult to reproduce due to the commonly observed n-type skin on the p-type material.
  • more sophisticated devices require highly perfect crystals for optimum performance and could not be made from implant-damaged material.
  • Another approach is to make p-on-n junctions by shallow implantation of arsenic ions into MOCVD grown MCT which has a weak unintentional n-type character followed by an activation anneal, as described in L.O. Bubulac, D. D. Edwall, D. McConnell, R.E. DeWames, E.R. Blasejewski and E.R. Gertner, "P-on-n arsenic -activated junctions in MOCVD LWIR HgCdTe/GaAs", Semicond. Sci. Technol., 1990, 5, S45-S48.
  • This approach however inevitably leads to dopant concentration grading dependent on the implantation and interdiffusion profiles.
  • MCT grown at low temperatures by MOCVD is generally n-type without deliberate doping as reported for example in G.N. Pain et al., "Large-area HgTe-CdTe superlattices and Hg*L_ x Cd x Te multilayers on GaAs and sapphire substrates grown by low-temperature metalorganic chemical vapour deposition", J. Vacuum Sci. Technol., 1990, A 8(2), 1067-1077. Thus it is of prime importance to develop p-type doping capability at low growth temperatures in order to fully exploit the MOCVD process.
  • P-type doping has been achieved with Group 1 elements by molecular beam epitaxy as reported in P. S. Wijewarnasuriya, I.K. Sou, Y.J. Kim, K.K. Mahavadi, S. Sivananthan, M. Boukerche and J.P. Faurie, "Electrical properties of Li-doped Hg*L_ ⁇ Cd ⁇ Te (100) by molecular beam epitaxy", Appl. Phys. Lett., 1987, 51(24), 2025-2027.
  • lithium and other elements of Group 1 are fast diffusers in MCT, and p-type doping of MCT by MOCVD has not been reported with these elements.
  • Group 15 elements are preferred because they are slow solid-state diffusers and hence should form stable device structures.
  • Deliberate extrinsic p-type doping of CdTe by MOCVD was first reported by S.K. Ghandhi, N.R. Taskar and I.B. Bhat in "Arsenic-doped CdTe layers grown by organometallic vapour phase epitaxy", Appl. Phys. Lett., 1987, 50 (14) 900-902; N.R. Taskar, V. Natarajan, I.B. Bhat and S.K. Ghandhi "Extrinsic doped n- and p-type CdTe layers grown by organometallic vapour phase epitaxy", J. Crystal Growth, 1988, 86, 228-232.
  • n-p CdTe solar cells could have an open circuit voltage of 0.90V, a short circuit current of 22.2 mA cm ⁇ 2 and an efficiency of 21% under AMI.5 illumination.
  • p-type MCT could be grown by MOCVD with arsine at 370"C in S.K. Ghandhi, N.R. Taskar, K.K. Parat, D. Terry and I.B. Bhat, "Extrinsic p-type doping of HgCdTe grown by organometallic epitaxy", Appl. Phys. Lett., 1988, 53(17), 1641-1643 and in N.R. Taskar, I.B. Bhat, K.K.
  • TMAs trimethylarsenic
  • TMSb trimethylantimony
  • TMAs and TMSb are unsatisfactory p-type dopants for low temperature MOCVD of MCT due to their thermal stability and high vapour pressures. It is likely that both compounds would lead to carbon contamination of epilayers due to the strong element- carbon bonds.
  • One object of the present invention is to provide such a method.
  • a further object of this invention is to provide an improved method of MOCVD which is also capable of being used for p-type or n-type doping of semiconductors.
  • a method for the metal organic chemical vapour deposition of a Group 15 and/or a Group 16 element on a substrate which comprises employing as a feedstock at least one compound of the formula R 2 EER2, RE'E'R, R 2 EE'R, R 2 EE'ER 2 , RE(E'R) 2 or E(E'R) 3 ⁇ wherein E is a Group 15 element, E' is a Group 16 element and R is an organic ligand.
  • a method for the metal organic chemical vapour deposition of a material having the stoichiometry EE' on a substrate wherein E is a Group 15 element and E' is a Group 16 element, which comprises employing as a feedstock at least one compound of the formula R EE'R, R EE'ER 2 , RE(E'R) 2 or E(E'R) 3 wherein E and E' are as defined above and R is an organic ligand.
  • the methods of the present invention may be used in p-type or n-type doping of semiconductors.
  • Compounds suitable for use as a feedstock in the p- type doping method of the present invention generally possess the following characteristics:
  • the dopant atom should have a low interdiffusion coefficient at the growth temperature.
  • a method for p-type doping of a II-VI semiconductor which comprises depositing one or more dopants while growing the semiconductor by employing as the feedstock to a metal organic chemical vapour deposition process at least one low vapour pressure compound of the formula R 2 EER 2 , RE'E'R, R 2 EE'R, R 2 EE'ER 2 , RE(E'R) 2 or E(E'R) , wherein E is a Group 15 element, E' is a Group 16 element and R is an organic ligand.
  • Examples of compounds suitable for use as a feedstock in the p-doping method of the invention and which possess the aforementioned characteristics include tetraethyldiarsine (Et 2 AsAsEt 2 )and tetraethyldistibine (Et 2 SbSbEt 2 ).
  • Low vapour pressure refers to pressures less than lmm Hg at room temperature.
  • the p-type doping method of the present invention may be used to produce the commercially significant p- type MCT.
  • a method for n-type doping of a III-V semiconductor which comprises depositing one or more dopants while growing the semiconductor by employing as the feedstock to a metal organic chemical vapour deposition process at least one low vapour pressure compound of the formula RE'E'R, R 2 EE'R, R 2 EE'ER 2 ,
  • E is a Group 15 element
  • E' is a Group 16 element
  • R is an organic ligand
  • the present invention also provides a method for the metal organic chemical vapour deposition of a material having the stoichemistry EE'X on a substrate, wherein E is a Group 15 element, E' is a Group 16 element and X is a halogen which comprises employing as a feedstock at least one compound of the formula R 2 EE'R, R 2 EE'ER 2 , RE(E'R) 2 or E(E'R) , wherein E and E' are as defined above and R is an organic ligand, together with a separate volatile source of halogen.
  • the Group 15 elements are selected from phosphorus, arsenic, antimony and bismuth and the Group 16 elements are selected from sulphur, selenium and tellurium.
  • the organic ligands are suitably of the type which will be non-deleterious when used in the methods of the invention. Examples include alkyl, cycloalkyl, vinyl, alkoxy and aryl, each of which may be optionally substituted. A suitable optional substituent is alkyl.
  • the organic ligand is a C 2 _ 2 o alkyl group, more preferably ethyl, tert-butyl, iso-propyl, 1-ethylpropyl or 2-ethylbutyl.
  • Suitable materials having a stoichiometry of EE' include AsSe and BiTe.
  • An example of a material having a stoichiometry of EE'X is SbTel.
  • the grown film or the substrate may be of any suitable known type for example, metals, alloys, glasses, oxides, chalcogenides, pnictides, superconductors, semiconductors, polycrystalline powders, amorphous powders and bulk crystals.
  • II-VI semiconductors examples include ZnSe, CdTe and HgTe.
  • III-V semiconductors examples include InSb and InP.
  • the compound ethyltellurodiethylstibine (Et 2 SbTeEt), which is suitable for use in the methods of the invention, is novel and accordingly contributes a further aspect of the present invention.
  • EtTeSbEt ethyltellurodiethylstibine
  • Related compounds are the direct reaction of the appropriate ditelluride or diselenide with the diarsine, distibine or dibismuthine.
  • the reaction can be conducted in the absence of solvent, in which case distillation of the low boiling product is unnecessary, as taught in H. Breunig, W.W. du Mont and T. Severengir "Dimethyl( -tolyltelluro)stibine", Organometallic Syntheses (R.B.King and J.J. Eisch eds.). Volume 4, Elsevier, Amsterdam, 1988 p.587-8.
  • Other synthetic routes include treatment of e.g. the salt NaTeR with the dialkylhalide of As, Sb or Bi.
  • the methods of the invention may be performed in any suitable known MOCVD reactor, for example, the reactor described in G. N. Pain et al., "Large area HgTe-CdTe superlattices and Hg* j __ ⁇ Cd ⁇ Te multilayers on GaAs and sapphire substrates grown by low-temperature metal organic chemical vapour deposition", J. Vac. Sci. Technol., 1990, A8(2), 1067-77.
  • Tetraethyldistibine is also prepared in good yield by reduction of diethylantimonybromide with magnesium as reported in H.J. Breunig, V. Breunig-Lyriti and T.P. Knobloch “Einfache Synthesen von Tetramethyl- und Tetraethyldistiban” Chemiker Science, 1977, 101, 399- 400, where the boiling point was 55°C at 0.02 mm Hg.
  • Tetraethyldiarsine has a low vapour pressure of 1 mm Hg at 20°C compared to trimethylarsine which has vapour pressure of 227.3 mm Hg at the same temperature.
  • the binuclear derivatives have considerably lower vapour pressures than the mononuclear species and fulfil a prime requirement for p-type dopants.
  • Tetraethyldibismuthine, the propyl, isopropyl and butyl derivatives have been reported by H.J. Breunig and D. Mueller "Et4Bi 2 : a binuclear bismuth compound” Angew. Chem. 1982, 94(6), 448; "R 4 Bi 2 ; tetraalkyldibismuthines” Z. Naturforsch. 1983, B38(2), 125-129. The methyl derivative disproportionates to trimethylbismuth and bismuth at 25°C as reported in A.J. Ashe and E.G. Ludwig, Jr. "A reinvestigation of Paneth's violet compound.
  • distibines react with diselenides and ditellurides to give R 2 SbE'R' e.g. Et 2 SbTeR', H.J. Breunig and H.
  • a stoichiometric quantity of diethylditelluride was added to a sample of tetraethyldistibine in a stainless steel bubbler, held at - 78°C, and the vessel was slowly warmed to room temperature. The bubbler was carefully evacuated at room temperature in order to remove traces of starting materials, leaving the product EtTeSb(Et) 2 , as a low vapour pressure liquid, in near quantitative yield.
  • the compound was characterized by nuclear magnetic resonance spectroscopy, *--H, delta 2.48 (quartet), 1.5 (multiplet), 1.48 (triplet), 1.23 (triplet) 2 J( 1 H, 125 Te) 25.0 Hz, 7.6 HZ (-TeEt), 3 J( 1 H, --H) 7.7 Hz (-SbEt 2 ); 13 C ⁇ 1 H ⁇ , delta 21.2, 11.8, 5.9, -10.9; mass spectrometry 338.1 (P + ), 309.1 (P-Et), 281.0 (P-Et-C 2 H ), 250.9 (SbTe).
  • a thin layer of doped CdTe was grown followed by a thin layer of undoped HgTe and the process was repeated until the desired thickness of material was deposited.
  • the multilayer film was annealed and solid-state interdiffusion yielded p-type MCT.
  • Room temperature Hall effect measurements using gold metallization yielded calculated hole mobilities of 40-100 cm 2 /Vsec and hole concentrations of 9 x lO 1 ⁇ to 10 17 cm -3 .
  • V:B 0 (mV)
  • V:B 0 (mV)
  • n 2.176E+16 cm"-3
  • V: B 0 (mV )
  • Rh 138.1E+3 Ohm/sq
  • Rh 74.74
  • the sample had high carrier (2 x lO- * **-** electrons cm” ) concentration at room temperature and at 77K which is believed to be due to tellurium doping. It is also possible that a high concentration sheet of carriers is present.
  • the carrier mobility was calculated ignoring effects of the MCT layer and ranged from 1.3 to 3.4 x 10 3 cm 2 /Vsec (average over 8 devices 2.23 x 10 3 ) at room temperature, with a slight increase at 77K.

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Abstract

La présente invention se rapporte à un procédé de dépôt chimique, organique et métallique en phase vapeur d'un élément de groupe 15 et/ou de groupe 16 sur un substrat, procédé qui se caractérise en ce qu'il utilise comme charge d'alimentation au moins un composé des formules R2EER2, RE'E'R, R2EE'R, R2EE'ER2, RE(E'R)2 or E(E'R)3, où E représente un élément de groupe 15, E' représente un élément de groupe 16 et R représente un ligand organique. La présente invention se rapporte aussi à des procédés de dopage de type-p d'un semi-conducteur II-VI, et de dopage de type-N d'un semi-conducteur III-V, selon le procédé décrit ci-dessus. Un nouveau composé, l'éthyltellurodiéthylstibine (Et2SbTeEt) est aussi décrit.
PCT/AU1991/000533 1990-11-23 1991-11-19 Procede de depot d'elements de groupe 15 et/ou de groupe 16 WO1992009719A1 (fr)

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AUPK3500 1990-11-23
AUPK350090 1990-11-23

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011095849A1 (fr) * 2010-02-03 2011-08-11 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Précurseurs contenant des chalcogénures, procédés de fabrication, et procédés d'utilisation de ceux-ci pour un dépôt de film mince
KR101567936B1 (ko) * 2013-11-11 2015-11-10 한국화학연구원 안티몬-텔루륨 단일 전구체, 이의 제조방법 및 이를 이용하여 박막을 형성하는 방법

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01205517A (ja) * 1988-02-12 1989-08-17 Nippon Steel Corp 気相成長方法および装置
US4999223A (en) * 1990-02-22 1991-03-12 Cvd Incorporated Chemical vapor deposition and chemicals with diarsines and polyarsines
US5015747A (en) * 1987-08-08 1991-05-14 Merck Patent Gesellschaft Mit Beschrankter Haftung Organometallic compounds

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5015747A (en) * 1987-08-08 1991-05-14 Merck Patent Gesellschaft Mit Beschrankter Haftung Organometallic compounds
JPH01205517A (ja) * 1988-02-12 1989-08-17 Nippon Steel Corp 気相成長方法および装置
US4999223A (en) * 1990-02-22 1991-03-12 Cvd Incorporated Chemical vapor deposition and chemicals with diarsines and polyarsines

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DERWENT ABSTRACT, Accession No. 89-281702/39, Class U11; & JP,A,1 205 517 (NIPPON STEEL CORP), 17 August 1989. *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011095849A1 (fr) * 2010-02-03 2011-08-11 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Précurseurs contenant des chalcogénures, procédés de fabrication, et procédés d'utilisation de ceux-ci pour un dépôt de film mince
KR101567936B1 (ko) * 2013-11-11 2015-11-10 한국화학연구원 안티몬-텔루륨 단일 전구체, 이의 제조방법 및 이를 이용하여 박막을 형성하는 방법

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