Source: http://www.google.com/patents/US7673856?dq=5,579,517
Timestamp: 2016-10-28 09:51:16
Document Index: 94879598

Matched Legal Cases: ['art.\n6', 'Application No. 2001', 'Application No. 2001', 'art,\n9', 'art 102', 'art 102', 'art 25', 'art 25']

Patent US7673856 - Vaporizer and various devices using the same and an associated vaporizing method - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsA vaporizer has gas passage formed inside of main body of a dispersion part, a gas inlet opening to introduce pressurized carrier gas into gas passage, a part to supply raw materials solution to carrier gas passing gas passage, a gas outlet to send carrier gas including dispersed raw material solution...http://www.google.com/patents/US7673856?utm_source=gb-gplus-sharePatent US7673856 - Vaporizer and various devices using the same and an associated vaporizing methodAdvanced Patent SearchTry the new Google Patents, with machine-classified Google Scholar results, and Japanese and South Korean patents.Publication numberUS7673856 B2Publication typeGrantApplication numberUS 11/496,407Publication dateMar 9, 2010Filing dateAug 1, 2006Priority dateJan 18, 2001Fee statusPaidAlso published asCN1531753A, CN1966762A, CN1966762B, CN100595910C, EP1361610A1, EP1361610A4, EP1361610B1, US7246796, US20040113289, US20080193645, WO2002058141A1Publication number11496407, 496407, US 7673856 B2, US 7673856B2, US-B2-7673856, US7673856 B2, US7673856B2InventorsMasayuki Toda, Masaki Kusuhara, Masaru Umeda, Mitsuru FukagawaOriginal AssigneeKabushiki Kaisha Watanabe ShokoExport CitationBiBTeX, EndNote, RefManPatent Citations (36), Non-Patent Citations (2), Referenced by (14), Classifications (44), Legal Events (2) External Links: USPTO, USPTO Assignment, EspacenetVaporizer and various devices using the same and an associated vaporizing method
US 7673856 B2Abstract
A vaporizer has gas passage formed inside of main body of a dispersion part, a gas inlet opening to introduce pressurized carrier gas into gas passage, a part to supply raw materials solution to carrier gas passing gas passage, a gas outlet to send carrier gas including dispersed raw material solution to vaporization part, a dispersion part to flow through gas passage having a part to cool, a vaporization pipe connected with a reaction part and gas outlet of dispersion part of the device, and a heater to heat vaporization pipe is provided, a vaporization part to heat and vaporizes the carrier gas where raw materials solution is dispersed is provided, and a radiation prevention portion having small hole for the outside of gas outlet is provided.
1. A vaporization method, the vaporization method comprising the steps of:
introducing raw material solution into a gas passage, shearing/atomizing the raw material solution by jetting a carrier gas including oxygen to the introduced raw material solution to obtain raw material mist;
supplying the raw material mist to a vaporization part for making it vaporize; and
feeding the raw material solution forcefully by using helium having low gas solubility.
2. The vaporization method of claim 1, wherein said jetting of said carrier gas is performed at a speed of 10 to 200 m/s.
3. The vaporization method of claim 1, wherein the raw material solution is introduced at a rate in a range of 0.005 to 2 cc/mm.
4. The vaporization method of claim 1, wherein at least one of the carrier gas and the raw material gas is made to assume a spiral flow and a straightly advancing flow that flows in a spiral flow upper layer concomitant in area downstream from a portion where the raw material solution was introduced.
5. The vaporization method of claim 1, further comprising a step of cooling the raw material mist between a portion introducing the raw material solution and said vaporization part.
6. The vaporization method of claim 1, wherein the vaporization part includes a vaporization part; and further comprising a set of uniformly heating the wall of the vaporization tube by using a heat medium that consists of at least one of a liquid and a gas with a large thermal capacity.
7. The vaporization method of claim 1, further comprising a step of controlling the quantity of flowing of raw material solution with precision by using the liquid mass flow controller, after degasifying the helium that has dissolved slightly.
8. The vaporization method of claim 7, further comprising a step of controlling the temperature of the raw material solution, a helium forced feed container, and the liquid mass flow controller, and pipings before and behind to a given temperature.
9. The vaporization method of claim 8, wherein the temperature is controlled within a range of 5 to 20� C., when a SBT thin film is to be formed.
10. The vaporization method of claim 9, wherein the temperature is controlled within a range of 12�1� C. when a SBT thin film is to be formed.
11. A vaporization method, the vaporization method comprising the steps of:
controlling the temperature of the raw materials solution, a helium forced feed container, and a liquid mass flow controller, and pipings before and behind to a given temperature.
12. A film forming method comprising the steps of:
introducing a carrier gas into a gas passage from a gas inlet;
introducing one or more raw material solutions in the carrier gas in the gas passage to obtain a raw material mist;
supplying the raw material mist to into a vaporizing part from a jet port to obtain a material gas;
introducing an oxidizing gas into the material gas; and
supplying the material gas including the oxidizing gas into a film forming chamber,
wherein another oxidizing gas is introduced from the gas inlet or the jet port.
13. The film forming method of claim 12, wherein said carrier gas is introduced into a gas passage at a speed of 10-200 m/s.
14. The film forming method of claim 12, wherein the raw material solutions are introduced at a rate in a range of 0.005 to 2 cc/min.
15. The film forming method of claim 12, wherein the carrier gas flows in the gas passage spirally and straightly.
16. The film forming method of claim 12, further comprising a step of cooling the raw material mist between a portion introducing the raw material solutions and said jet port.
17. The film forming method of claim 12, wherein the vaporization part includes a vaporization part; and further comprising a set of uniformly heating the wall of the vaporization tube by using a heat medium that comprises of at least one of a liquid and a gas with a large thermal capacity.
18. The film forming method of claim 12, further comprising a step of feeding the raw material solutions by helium.
19. The film forming method of claim 18, further comprising a step of controlling the quantity of flowing of the raw material solutions by liquid mass flow controller, after degassing.
20. The film forming method of claim 19, further comprising a step of controlling the temperature of the raw material solutions, a helium gas container, and the liquid mass flow controller, and pipes.
21. The film forming method of claim 20, wherein the temperature is controlled within a range of 5 to 20� C., when a SBT film is to be formed.
22. The film forming method of claim 21, wherein the temperature is controlled within a range of 11 to 13� C., when a SBT film is to be formed.
The Applicants claim priority to and incorporate by reference U.S. patent application Ser. No. 10/466,528 filed Dec. 8, 2003, Japanese Patent Application No. 2001-010827, filed Jan. 18, 2001 and Japanese Patent Application No. 2001-392833, filed Nov. 18, 2001.
The present invention relates to a vaporizer and a vaporizing method, which is preferably used for a deposition device such as a MOCVD, as well as a other various devices.
However, in an application after 256M DRAM, a three-dimensional capacitor structure is required. (BaxSr1-x)TiO3, Pb(ZryTi1-y)O3, (PbaL1-a)(ZrbTi1-b)O3 are regarded as promising materials which have the higher relative dielectric constant than the above-described oxides and can be expected to apply to the DRAM.
Moreover, recently, a layered structure of Bi group which has a very similar crystal structure to the one of a superconductive material greatly attracts the attention because it has a high dielectric constant, has a self polarization characteristic of a ferroelectric, and is superior as a nonvolatile memory. Generally, the thin film formation of SrBi2TaO9 ferroelectric is done by MOCVD (metalorganic chemical vapor deposition) method—the practical and promising method. The raw material of the ferroelectric thin film includes, for instance, three kinds of organometallic complex, Sr(DPM)2, Bi(C6H5)3, and Ta(OC2H5)5, melt respectively in THF (Tetorahidorofran), hexane, and other solvents, and this combination is used as a raw material solution. Sr(Ta(OEt)6)2 and Bi(OtAm)3 can be melted in hexane and other solvents and used as a raw material solution. Note that DPM is an abbreviation of bis(diphenylphosphino) methane.
Characteristics of a raw material for a
Boiling point (� C.) and
FIGS. 7( a) and (b) are cross-sectional views showing a variant of a gas passage of a vaporizer for MOCVD, both according to an embodiment 4;
FIG. 9 shows a rod used for the vaporizer for MOCVD according to the embodiment 5, (a) being a side view thereof, (b) an X-X cross-sectional view, and (c) a Y-Y cross-sectional view;
FIGS. 16( a) and (b) both are cross-sectional views showing the vaporizer for MOCVD of the prior art;
Main body of a dispersion part,
Gas passage,
Raw material solution,
Raw material supply hole,
Gas outlet,
Dispersion part,
9a, 9b,
9c, 9d:
Means to cool (cooling water),
Vaporizing tube,
Heating means (heater),
Vaporizing part,
Connection part,
Oxygen introduction means (first oxygen
(oxidation gas) supply opening),
Raw material supply inlet,
30a, 30b,
30c, 30d
31a, 31b,
31c, 31d
Reservation tank,
Carrier gas bomb,
Reaction pipe,
Radiation prevention portion,
Oxygen introduction means (second
oxygen (oxidation gas))
Upstream ring
Downstream ring
303a, 303b
Heat transmission passage
Heat conversion board
Gas vent gas nozzle
Heat medium inlet
Heat medium outlet
Heat introduction medium
Heat outlet medium
In this embodiment, in addition, the radiation prevention part 102 that has a small hole 101 outside the gas outlet 7 is installed. The numerals 103, 104 represent seal materials such as an O ring. This radiation prevention part 102 may be composed, for instance, of teflon, stainless steel, ceramic, etc. In addition, it is preferable to make of use a material excellent in heat conduction. According to the finding of the present inventor, the gas in gas passage 2 is overheated, in the prior art, by the heat in the vaporization part, such as the radiant heat through the gas outlet 7. Therefore, the low melting point elements in the gas tend to deposit in the vicinity of the gas outlet 7, even if it is cooled with cooling water 18.
FIG. 4 shows the details of the reserve tank. The reserve tank is filled with the raw material solution 5 and, for instance, 1.0 to 3.0 kgf/cm2 of the carrier gas 3 (for instance, inert gas Ar, He, Ne) is sent to the respective reservoir tank 32 a-32 d (an inner capacity 300 cc, made by SUS). The raw material solution is pushed up in the tube on the side contacting with the solution, because the interior of the reservoir tank is pressurized by the carrier gas, and transferred under pressure to a mass flow controller (made by STEC, full-scale flow 0.2 cc/min). A flowing quantity is controlled here, and it is transported from a raw material supply port 29 of the vaporizer to the raw material supply hole 6.
Sr(DPM)2 0.04 cc/min Bi(C6H5)3 0.08 cc/min Ta(OC2H5)5 0.08 cc/min THF 0.2 cc/min Carrier gas: Nitrogen gas
10˜350 m/s The device shown in FIG. 8 was used as the vaporization device. However, the rod 10 where a spiral groove was not formed as shown in FIG. 9, was used as the rod. The raw material solution is supplied from the raw material supply hole 6, while the carrier gas is changed in speed variously. The groove 67 a was supplied with Sr(DPM) 2, groove 67 b with Bi(C6H5)3, groove 67 c with Ta(OC2H5)5 and groove 67 d with solvent such as THF, respectively, from the raw material supply hole. Heating in the vaporization part was not executed, the raw material gas was collected at the gas outlet 7, and the particle diameter of the raw material solution was measured in the collected raw material gas.
Hexaethoxy strontium tantalum Sr[Ta(OC2H5)6]2 0.1 mole solution (Solvent: Hexane) 0.02 ml/min Tori-t-amyloxide bismuth Bi(O-t-C5H11)3 0.2 mole solution (Solvent: Hexane) 0.02 ml/min First carrier Ar=200 sccm (introduced into the gas inlet 4) First carrier O2=10 sccm (introduced into the gas inlet 4) Second carrier Ar=20 sccm (introduced into the gas inlet 200) Second carrier O2=10 sccm (introduced into the gas inlet 200) Reactant oxygen O2=200 sccm (introduced into lower part 25 of the dispersion jet part) Reactant oxygen temperature 216� C. (control the temperature by a separately installed heater before introducing from the lower part of the dispersion jet part) Wafer temperature 475� C. Space temperature 299� C. Space distance 30 mm Temperature of shower head 201� C. Reaction pressure 1 Torr Deposition time 20 minutes
SBT film thickness about 300 nm (depositing speed about 150 nm/min) SBT composition
Hexaethoxy strontium tantalum Sr[Ta(OC2H5)6]2 0.1 mole solution (Solvent: Hexane) 0.02 ml/min Tori-t-amyloxide bismuth Bi(O-t-C5H11)3 0.2 mole solution (Solvent: Hexane) 0.02 ml/min First carrier Ar=200 sccm (introduced into the gas inlet 4) First carrier O2=10 sccm (introduced into the gas inlet 4) flow into the vaporizer and are drawn to the vacuum pump via the second valve and the automatic pressure regulating valve. The pressure gauge is controlled by the automatic pressure regulating valve to 4 Torr, at this time. A few minutes after the wafer is transferred, if the temperature is steady, the following gas flows into the reaction chamber thereof, the first valve is opened and the second valve is shut to start depositing.
Hexaethoxy strontium tantalum Sr[Ta(OC2H5)6]2 0.1 mole solution (Solvent: Hexane) 0.02 ml/min Tori-t-amyloxide bismuth Bi(O-t-C5H11)3 0.2 mole solution (Solvent: Hexane) 0.02 ml/min First carrier Ar=200 sccm (introduced into the gas inlet 4) First carrier O2=10 sccm (introduced into the gas inlet 4) Second carrier Ar=20 sccm (introduced into the gas inlet 200) O2=10 sccm (introduced into the gas inlet 200) Reactant oxygen O2=200 sccm (introduced into the lower part 25 of the dispersion jet part) Reactant oxygen temperature 216� C. (control the temperature by a separately installed heater before introducing from the lower part of the dispersion jet part) Wafer temperature 475� C.
In addition, in the substrate surface treatment device in which a predetermined gas is sprayed on the substrate surface of the silicon substrate shown in FIGS. 22, 23 to conduct a surface treatment for the substrate surface. Such a device is desirable that has and configures an upstream ring 301 connected to a heat medium entrance 320 for flowing through a heat medium, a downstream ring 302 connected to a heat medium outlet 321 of the predetermined heat medium, and, at least, two heat transmission passages 303 a, 303 b which are connected in a parallel direction to between the upstream ring 301 and downstream ring 302 and form a passage for the heat medium, and a flow passage directed from the upstream ring 301 to downstream ring 302 between adjacent the heat transmission passage 303 a, 303 b being alternated and a heat medium circulation passage desirable to make the gas to a specified temperature.
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center rod for use in the carburetor or carburetor for mocvd, method for dispersing carrier gas, and method for vaporizing carrier gas* Cited by examinerClassifications U.S. Classification261/78.2, 392/397, 261/DIG.65, 118/726, 261/79.2International ClassificationB01F5/06, H01L27/115, B01B1/00, B01F3/04, C23C16/40, H01L21/316, C23C16/448, H01L21/02, H01L21/8246, B01D3/34Cooperative ClassificationY10S261/65, H01L27/11502, H01L27/11507, B01B1/005, C23C16/4486, H01L21/31691, B01F5/0656, C23C16/40, B01F5/0653, C23C16/409, B01F3/04021, B01D3/346, B01F5/0671, B01F5/0646, H01L28/55, B01F5/0676European ClassificationB01F5/06B3F12, B01F5/06D2V14, B01F5/06D2V6, B01F5/06B3F, H01L27/115C, B01F5/06B3G, H01L21/316D, B01F3/04B3, C23C16/40P, B01B1/00B, C23C16/40, H01L27/115C4, C23C16/448HLegal EventsDateCodeEventDescriptionAug 1, 2006ASAssignmentOwner name: KABUSHIKI KAISHA WATANABE SHOKO, JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:TODA, MASAYUKI;KUSUHARA, MASAKI;UMEDA, MASARU;AND OTHERS;REEL/FRAME:018146/0402Effective date: 20030807Owner name: KABUSHIKI KAISHA WATANABE SHOKO,JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:TODA, MASAYUKI;KUSUHARA, MASAKI;UMEDA, MASARU;AND OTHERS;REEL/FRAME:018146/0402Effective date: 20030807Mar 14, 2013FPAYFee paymentYear of fee payment: 4RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google Patents - Send FeedbackData provided by IFI CLAIMS Patent Services