GB2151662A - Device for enriching a carrier gas with the vapour of a slightly volatile material for chemical vapour deposition method - Google Patents
Device for enriching a carrier gas with the vapour of a slightly volatile material for chemical vapour deposition method Download PDFInfo
- Publication number
- GB2151662A GB2151662A GB08427276A GB8427276A GB2151662A GB 2151662 A GB2151662 A GB 2151662A GB 08427276 A GB08427276 A GB 08427276A GB 8427276 A GB8427276 A GB 8427276A GB 2151662 A GB2151662 A GB 2151662A
- Authority
- GB
- United Kingdom
- Prior art keywords
- carrier gas
- wall
- mixture
- groove
- metal member
- 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.)
- Granted
Links
Classifications
-
- 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
- C23C16/44—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 method of coating
- C23C16/448—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 method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4481—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 method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The device comprises a container (1) having a heatable inner space (3) for receiving a fine-particle, sparingly volatile material or mixture of materials, a gas inlet (4) and a gas outlet (5), and the container (1) comprises a removable tightly-fitting metal member (2), having a groove (3) preferably wound in the form of a spiral or in a zigzag-like or meander-like manner provided in at least one outer wall of the metal member, and said outer wall being in contact with an inner wall, preferably the bottom, of the container, in such manner that the groove forms the said inner space. The device has a long flow path and can easily be cleaned. <IMAGE>
Description
SPECIFICATION
Device for Enriching a Carrier Gas with the Vapour of a Sparingly Volatile Material
The invention relates to a device for enriching a carrier gas or carrier gas mixture with the vapour or vapours of a sparingly volatile material or mixture of materials present in the form of solid particles, comprising a container having a heatable inner space for receiving the material or mixture of materials which is provided with an inlet for the carrier gas and an outlet for the enriched carrier gas, the pipes opening into the inner space in such manner that the carrier gas during operation of the device flows through the material or the mixture of materials.
Such a device is known from DE-OS 31 36 895.
The known device consists of an evaporation vessel with cover. Inside the evaporation vessel a sieve is present on which during operation of the device a starting material is present in the form of a powder.
A heating element is provided below the sieve or in the proximity thereof in the evaporation vessel.
From a carrier gas storage container an inlet leads to the evaporation vessel, the inlet opening below the sieve. From the inner space of the evaporation vessel above the sieve a vapour outlet leads to a reactor in which a reactive deposition from the gaseous phase takes piace in which hence a CVDmethod is carried out.
The investigations which have led to the present invention relates to the enrichment of carrier gases with gases for the reactive deposition in particular of rare earth metals (Ill-B-metal) and rare earth metal compounds (Ill-B-compounds), respectively, and of thorium and thorium compounds, from the gaseous phase. Since the starting compounds in question for the CVD-method as a rule are present as metalorganiccompounds in powder form at room temperatu re--only these are slightly volatile already with slight heating-the starting compound is transported by a carrier gas to a substrate surface on which layers are to be deposited. The carrier gas, preferably a noble gas, in particular argon, flows through a saturator which is filled with the starting compound in powder form and is heated to a suitable temperature.
The device known from DE-OS 31 36 895 suffers from the disadvantage of having only a short flow path of the gas through the gas-forming material.
The yield of reaction gas for the CVD-method and its concentration in the gasflow, respectively, are correspondingly low.
It is the object of the invention to provide a device of the kind mentioned in the opening paragraph, in particular a saturator, which has a long flow path.
According to the invention this object is achieved in that the container comprises a removable tightly fitting metal member, that at least one groove is provided in at least one outer wall of the metal member, and that said outer wall is in contact with an inner wall of the container in such manner that the groove forms the said inner space.
In order to achieve a flow path which is as long as possible, the groove must be as long as possible.
For this purpose it is advantageous for the groove to
be wound in the form of a spiral or in a zigzag-like or
meander-like manner.
The outer wall of the metal member in which the
groove is provided is preferably in contact with the
bottom of the vessel. From this it follows that the
groove is preferably provided in the lower side of the metal member. However, it is also possible for the groove to be provided in the side walls of the
metal member.
In order to avoid particles of the material or
mixture of materials being dragged along by the carrier gas it is advantageous to provide a gas
permeable member between the gas outlet and the
inner space.
The device according to the invention has the advantage that it can be filled in a simple manner with the fine-particle vapour-forming material or
mixture of materials, for example a powder. For example, for filling a saturator according to the invention the groove formed in the lower side of a copper block is pressed down to the bottom of a tray or pan of V2A noble steel filled just sufficiently with the powder. During operation, the carrier gas flows through the groove thus filled.
A helical construction of the groove has the additional advantage that by means of a rotary movement in the spiral outer direction a dense filling of the grooves with the powder is achieved and at the same time the bottom contact of the contacting surfaces becomes really good.
A further advantage of the device according to the invention is that its parts, after removing the metal member, can easily be cleaned.
Afew embodiments of the invention are shown in a drawing and will be described in greater detail hereinafter. In the drawing:
Fig. 1 is a sectional view of a saturator,
Fig. 2 shows a removable metal member (metal insert) with spiral-like groove, and
Fig. 3 shows a removable metal member (metal insert) with meander-like groove.
The sequence in time of the operation of the saturatorshown in Figure 1 is as follows.
First, fine gas-forming powder is filled in a container 1 of noble steel. A tightly fitting copper block 2 having a spiral groove 3 in its lower side is then pressed firmly on the powder, namely by means of a rotary movement against the subsequent direction of flow, and is fitted to the carrier gas inlet 4 and locked buy a pin (not shown).
The gas outlet 5 is in the centre of the copper block and comprises a mesh grid and Awl203 wool provided in front of it. This combined sieve is to prevent emanation of the powder.
A further copper insert, for example a hollow cylinder with sealing and outlet aperture (not shown) may be provided above the copper block 2 and be clamped on the saturator block with fixed pressure by means of a bayonet. The space between the copper insert and the saturator block then forms a mixing chamber for further CVD starting gases.
Via its outlet nozzle the substrate to be coated may then be provided in a reactor (not shown).
Fig. 2 shows a metal member 2 having a spiral-like groove 3 and Fig. 3 shows a metal member 2 having a meander-like groove 3 in which the carrier gas inlet is referenced 4 and the gas outlet is referenced 5.
The outer walls of the saturator and reactor consists of V2A noble steel and are constructed so as to be high vacuum-tight. They are present in a furnace having a separate heating for the saturator and for the reactor and the mixing chamber. During operation the latter are at a slightly higher temperature than the saturator so as to avoid deposition on the wall of the III B starting compound. After a series of coatings, cleaning of the saturator and a renewed filling with the starting compound as a rule is necessary since many of the powdered metalorganic starting compounds used start to dissociate already near the melting point, but exactly there also have the highest vapour pressure realisable in the long run. Moreover, a successive decomposition by contact with the agressive compounds (for example WF6 and HF) formed during the CVD method may be caused.
For cleaning purposes the whole arrangement can be taken apart wtih few manipulations and be cleaned by means of a brush in dilute solutions of detergents followed by rinsing with water and ethanol.
In using the saturator thorium acetyl acetonate (Th(AA)4) and thorium trifluoroacetyl acetonate (Th (3 FAA)4) were used as powdered starting compounds and argon was used as a carrier gas.
The saturator temperature for the filling with
Th(AA)4 was 160 C+5 C and for the Th(3FAA)4 filling it was 100 to 1 20 C. The reactor temperature was 200- above the saturation temperature. As deposition rates for the layers containing thorium approximately 0.1 to 0.4 pmlmin were reached which strongly reduced forTh(AA)4 in the each time third coating and for Th(3FAA)4 could be realised for approximately 6 coatings, the duration of a coating being at most 4 hours.
Claims (5)
1. A device for enriching a carrier gas or mixture of carrier gases with the vapour or vapours of a sparingly volatile material or mixture of materials present in the form of solid particles, comprising a container having a heatable inner space for receiving the material or mixture of materials which is provided with an inletforthe carrier gas and an outlet for the enriched carrier gas, the pipes opening into the inner space in such manner that the carrier gas during operation of the device flows through the material or the mixture of materials, characterized in that the container comprises a removable tightly fitting metal member, that at least one groove is provided in at least one outer wall of the metal member, and that said outer wall is in contact with an inner wall of the container in such manner that the groove forms the said inner space.
2. A device as claimed in Claim 1, characterized in that the groove is wound in the form of a spiral or in a zigzag-like or meander-like manner.
3. A device as claimed in Claim 1 or 2, characterized in that the outer wall of the metal member in which the groove is provided is in contact with the bottom of the vessel.
4. A device as claimed in Claim 1,2 or 3, characterized in that a gas-permeable member is provided between the gas outlet and the inner wall.
5. A device for enriching a carrier gas or mixture of carrier gases with the vapour or vapours of a sparingly volatile material or mixture of materials present in the device in the form of solid particles, substantially as herein described with reference to
Figures 1 and 2 orto Figure 3 of the drawings.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19833339625 DE3339625A1 (en) | 1983-11-02 | 1983-11-02 | DEVICE FOR ENRICHING A CARRIER GAS WITH THE VAPOR OF A LITTLE VOLATILE FABRIC |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| GB8427276D0 GB8427276D0 (en) | 1984-12-05 |
| GB2151662A true GB2151662A (en) | 1985-07-24 |
| GB2151662B GB2151662B (en) | 1986-07-23 |
Family
ID=6213274
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB08427276A Expired GB2151662B (en) | 1983-11-02 | 1984-10-29 | Device for enriching a carrier gas with the vapour of a slightly volatile material for chemical vapour deposition method |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JPS61110766A (en) |
| DE (1) | DE3339625A1 (en) |
| FR (1) | FR2554131B1 (en) |
| GB (1) | GB2151662B (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004007793A2 (en) * | 2002-07-17 | 2004-01-22 | Applied Materials, Inc. | Method and apparatus for providing gas to a processing chamber |
| US7122085B2 (en) | 2002-07-30 | 2006-10-17 | Asm America, Inc. | Sublimation bed employing carrier gas guidance structures |
| US7156380B2 (en) | 2003-09-29 | 2007-01-02 | Asm International, N.V. | Safe liquid source containers |
| US7601225B2 (en) | 2002-06-17 | 2009-10-13 | Asm International N.V. | System for controlling the sublimation of reactants |
| US7833353B2 (en) | 2007-01-24 | 2010-11-16 | Asm Japan K.K. | Liquid material vaporization apparatus for semiconductor processing apparatus |
| US8012876B2 (en) | 2008-12-02 | 2011-09-06 | Asm International N.V. | Delivery of vapor precursor from solid source |
| US8137462B2 (en) | 2006-10-10 | 2012-03-20 | Asm America, Inc. | Precursor delivery system |
| US9117773B2 (en) | 2009-08-26 | 2015-08-25 | Asm America, Inc. | High concentration water pulses for atomic layer deposition |
| US10876205B2 (en) | 2016-09-30 | 2020-12-29 | Asm Ip Holding B.V. | Reactant vaporizer and related systems and methods |
| US11624113B2 (en) | 2019-09-13 | 2023-04-11 | Asm Ip Holding B.V. | Heating zone separation for reactant evaporation system |
| US11634812B2 (en) | 2018-08-16 | 2023-04-25 | Asm Ip Holding B.V. | Solid source sublimator |
| US11926894B2 (en) | 2016-09-30 | 2024-03-12 | Asm Ip Holding B.V. | Reactant vaporizer and related systems and methods |
| US12054825B2 (en) | 2021-06-22 | 2024-08-06 | Applied Materials, Inc. | Bottom fed sublimation bed for high saturation efficiency in semiconductor applications |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3702923A1 (en) * | 1987-01-31 | 1988-08-11 | Philips Patentverwaltung | DEVICE FOR ENRICHING A CARRIER GAS WITH THE VAPOR OF A LITTLE VOLATILE FABRIC |
| DE3801147A1 (en) * | 1988-01-16 | 1989-07-27 | Philips Patentverwaltung | DEVICE FOR GENERATING A GAS FLOW ENRICHED WITH THE VAPOR OF A LITTLE VOLATILE FABRIC |
| JPH0269389A (en) * | 1988-08-31 | 1990-03-08 | Toyo Stauffer Chem Co | Formation of saturated vapor of solid organometallic compound in vapor growth method |
| DE3931189A1 (en) * | 1989-09-19 | 1991-03-28 | Philips Patentverwaltung | Gas flow contg. vapour of low volatility powder for CVD - obtd. using device where process can be continuous and containers having little residual powder can be refilled without disturbing gas flow |
| JPH0513166U (en) * | 1991-08-06 | 1993-02-23 | ダイワ精工株式会社 | Fishing reel fishing line stopper |
| DE19638100C1 (en) * | 1996-09-18 | 1998-03-05 | Fraunhofer Ges Forschung | Apparatus to produce vaporous reaction product from solid particles |
| US7775508B2 (en) | 2006-10-31 | 2010-08-17 | Applied Materials, Inc. | Ampoule for liquid draw and vapor draw with a continuous level sensor |
| US8343583B2 (en) | 2008-07-10 | 2013-01-01 | Asm International N.V. | Method for vaporizing non-gaseous precursor in a fluidized bed |
| US8146896B2 (en) | 2008-10-31 | 2012-04-03 | Applied Materials, Inc. | Chemical precursor ampoule for vapor deposition processes |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1204588A (en) * | 1958-04-22 | 1960-01-27 | E F Drew & Co | Apparatus for carrying out continuous chemical reactions |
| FR1532742A (en) * | 1967-07-19 | 1968-07-12 | Bristol Aeroplane Plastics Ltd | Method and device for mixing fluids |
| FR1581523A (en) * | 1968-05-08 | 1969-09-19 | ||
| US3801073A (en) * | 1972-12-27 | 1974-04-02 | Kates W Co | Fluid mixer |
| US4129624A (en) * | 1977-05-13 | 1978-12-12 | The W. A. Kates Company | Fluid mixer |
| JPS5635426A (en) * | 1979-08-31 | 1981-04-08 | Fujitsu Ltd | Vapor-phase epitaxial growth device |
| DE3136895A1 (en) * | 1981-09-17 | 1983-03-31 | Philips Patentverwaltung Gmbh, 2000 Hamburg | Apparatus for evaporating starting materials for the reactive separation from the gas phase |
-
1983
- 1983-11-02 DE DE19833339625 patent/DE3339625A1/en active Granted
-
1984
- 1984-10-29 GB GB08427276A patent/GB2151662B/en not_active Expired
- 1984-10-30 FR FR8416553A patent/FR2554131B1/en not_active Expired
- 1984-11-01 JP JP22903684A patent/JPS61110766A/en active Granted
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7851019B2 (en) | 2002-06-17 | 2010-12-14 | Asm International N.V. | Method for controlling the sublimation of reactants |
| US8309173B2 (en) | 2002-06-17 | 2012-11-13 | Asm International N.V. | System for controlling the sublimation of reactants |
| US7601225B2 (en) | 2002-06-17 | 2009-10-13 | Asm International N.V. | System for controlling the sublimation of reactants |
| WO2004007793A3 (en) * | 2002-07-17 | 2004-05-27 | Applied Materials Inc | Method and apparatus for providing gas to a processing chamber |
| US6905541B2 (en) | 2002-07-17 | 2005-06-14 | Applied Materials, Inc. | Method and apparatus of generating PDMAT precursor |
| US7186385B2 (en) | 2002-07-17 | 2007-03-06 | Applied Materials, Inc. | Apparatus for providing gas to a processing chamber |
| WO2004007793A2 (en) * | 2002-07-17 | 2004-01-22 | Applied Materials, Inc. | Method and apparatus for providing gas to a processing chamber |
| US7122085B2 (en) | 2002-07-30 | 2006-10-17 | Asm America, Inc. | Sublimation bed employing carrier gas guidance structures |
| US7971861B2 (en) | 2003-09-29 | 2011-07-05 | Asm International N.V. | Safe liquid source containers |
| US7156380B2 (en) | 2003-09-29 | 2007-01-02 | Asm International, N.V. | Safe liquid source containers |
| US7497420B2 (en) | 2003-09-29 | 2009-03-03 | Asm International, N.V. | Safe liquid source containers |
| US9593416B2 (en) | 2006-10-10 | 2017-03-14 | Asm America, Inc. | Precursor delivery system |
| US8137462B2 (en) | 2006-10-10 | 2012-03-20 | Asm America, Inc. | Precursor delivery system |
| US7833353B2 (en) | 2007-01-24 | 2010-11-16 | Asm Japan K.K. | Liquid material vaporization apparatus for semiconductor processing apparatus |
| US8012876B2 (en) | 2008-12-02 | 2011-09-06 | Asm International N.V. | Delivery of vapor precursor from solid source |
| US9117773B2 (en) | 2009-08-26 | 2015-08-25 | Asm America, Inc. | High concentration water pulses for atomic layer deposition |
| US10876205B2 (en) | 2016-09-30 | 2020-12-29 | Asm Ip Holding B.V. | Reactant vaporizer and related systems and methods |
| US11377732B2 (en) | 2016-09-30 | 2022-07-05 | Asm Ip Holding B.V. | Reactant vaporizer and related systems and methods |
| US11926894B2 (en) | 2016-09-30 | 2024-03-12 | Asm Ip Holding B.V. | Reactant vaporizer and related systems and methods |
| US11634812B2 (en) | 2018-08-16 | 2023-04-25 | Asm Ip Holding B.V. | Solid source sublimator |
| US11773486B2 (en) | 2018-08-16 | 2023-10-03 | Asm Ip Holding B.V. | Solid source sublimator |
| US11624113B2 (en) | 2019-09-13 | 2023-04-11 | Asm Ip Holding B.V. | Heating zone separation for reactant evaporation system |
| US12054825B2 (en) | 2021-06-22 | 2024-08-06 | Applied Materials, Inc. | Bottom fed sublimation bed for high saturation efficiency in semiconductor applications |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2554131B1 (en) | 1988-10-14 |
| DE3339625C2 (en) | 1991-01-31 |
| JPS61110766A (en) | 1986-05-29 |
| GB2151662B (en) | 1986-07-23 |
| FR2554131A1 (en) | 1985-05-03 |
| JPH0530908B2 (en) | 1993-05-11 |
| DE3339625A1 (en) | 1985-05-09 |
| GB8427276D0 (en) | 1984-12-05 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |
Effective date: 19951029 |