US20030145789A1 - Gas supply device for precursors with a low vapor pressure - Google Patents

Gas supply device for precursors with a low vapor pressure Download PDF

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Publication number
US20030145789A1
US20030145789A1 US10/203,191 US20319102A US2003145789A1 US 20030145789 A1 US20030145789 A1 US 20030145789A1 US 20319102 A US20319102 A US 20319102A US 2003145789 A1 US2003145789 A1 US 2003145789A1
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United States
Prior art keywords
gas
intermediate storage
storage device
precursor
gas supply
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Abandoned
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US10/203,191
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English (en)
Inventor
Hartmut Bauch
Lars Bewig
Lutz Klippe
Thomas Kupper
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Schott AG
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Schott Glaswerke AG
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Assigned to SCHOTT GLAS reassignment SCHOTT GLAS ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BAUCH, HARTMUT, BEWIG, LARS, KLIPPE, LUTZ, KUPPER, THOMAS
Publication of US20030145789A1 publication Critical patent/US20030145789A1/en
Priority to US11/014,488 priority Critical patent/US7413767B2/en
Assigned to SCHOTT AG reassignment SCHOTT AG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SCHOTT GLAS
Abandoned legal-status Critical Current

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    • 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

Definitions

  • the invention relates to a gas supply device for precursors with a low vapor pressure, especially for CVD coating systems according to the characterizing portion of claim 1.
  • CVD coating systems chemical vapor deposition
  • the coatings which may also consist of a series of different thin layers, must satisfy very high requirements with regard to their properties.
  • the deposition In order to achieve such properties the deposition must also be of very high quality. This includes the deposition rate as a deposition parameter, for example, which has a considerable effect on the coating quality.
  • the deposition rate is fundamentally determined by the partial pressure of a gaseous precursor. Therefore, the partial pressure must be set very precisely and must not fluctuate.
  • Special coating materials are used for coating which are delivered to the coater via selected precursors.
  • Precursors used for producing TiO 2 /SiO 2 alternating coatings are titanium tetrachloride (TiCl 4 ) or hexamethyl disiloxane (HDMSO), for example, which, under normal conditions, have a low vapor pressure far below the atmospheric pressure. Such a low vapor pressure is usually too low for an adequate deposition rate required for industrial coating. Therefore, the precursors must be heated up to a first evaporation temperature in a supply container so as to generate an adequate vapor pressure.
  • the gas supply device In order to prevent the precursor from condensing on the way to the coater, the gas supply device must then be heated between the supply container and the coater to a second temperature, which is higher than the first evaporation temperature.
  • Nb 2 O 2 /SiO 2 alternating coatings can also be produced offering the advantage that they tend less toward crystallization. Moreover, NbO 2 can be deposited at higher deposition rates. Additionally, the coefficient of expansion of Nb 2 O 5 is more suitable to that of SiO 2 than the coefficient of expansion of TiO 2 , so that thicker alternating coatings can be produced with Nb 2 O 5 . However, for the production of Nb 2 O 5 coatings only precursors with comparatively low vapor pressure are available whose vapor pressure under normal conditions is even far below the vapor pressure of the HMDSO and TiCl 4 precursors.
  • NbCl 5 A commercially available Nb compound with the highest vapor pressure, NbCl 5 , will not have a pressure of 50 mbar until a temperature of approx. 170° C. is reached.
  • the temperature dependence of the vapor pressure of NbCl 5 is illustrated in the bottom curve in FIG. 1. Therefore, a gas supply device for uniformly supplying a PICVD coating system with NbCl 5 vapor would have to be maintained at said temperature.
  • a gas supply device for providing precursors with a low vapor pressure with a supply container for a precursor and an intermediate storage device for buffering and mixing the vaporous precursor with other gases is known (JP 2-25 09 77 A2).
  • the supply container is thermostatted to a first temperature T 1 and the intermediate storage device is thermostatted to a second temperature T 2 where the first temperature T 1 is lower than the second temperature T 2 so as to prevent condensation of the precursor in the intermediate storage device.
  • a carrier gas is delivered to the supply container which transports the precursor to the intermediate storage device and from there to a reaction chamber.
  • the gas supply device can be provided with a second supply container from which a second precursor is delivered to the intermediate storage device by means of a carrier gas so as to mix the two precursors and the carrier gas.
  • the intermediate storage device and the equipment connected to the intermediate storage device must be maintained at the high temperature T 2 , which makes maintenance work time-consuming because of the required cooling down period, and the materials and equipment must be able to withstand the high temperature T 2 .
  • the aim of the invention is to develop a gas supply device for a precursor with a low vapor pressure such that maintenance and repair work on an intermediate storage device can be completed easily and quickly and using cost-effective components for the intermediate storage device and its elements without having to limit the maximum achievable mass flow rate of the precursor.
  • a gas supply device of the invention for precursors with a low vapor pressure has a supply container for storing a first precursor with a low vapor pressure, an intermediate storage device for intermediate storage of the first precursor evaporated in the supply container, a first gas line connecting the supply container to the intermediate storage device, and a second gas line for removing the gas from the intermediate storage device.
  • the gas supply device is also called a gas generator.
  • the gas removed via the second gas line on the intermediate storage device serves to supply the coaters with the gaseous first precursor.
  • Coaters are especially CVD coating systems or the like.
  • Precursors are also frequently called educt species, starting materials or coating material.
  • Precursors with a low vapor pressure should be understood to mean solid or liquid coating compounds with a vapor pressure of less than 10 mbar at temperatures of 50° C., for example.
  • the evaporation rate of the first precursor in the supply container depends on the temperature T 1 and on the partial pressure of the first precursor in the supply container.
  • the evaporation rate increases as the temperature rises. If the vaporous precursor is now removed for the intermediate storage device the precursor is very quickly replaced because of the evaporation.
  • the saturation vapor pressure of the precursor is virtually maintained. Because the saturation vapor pressure depends very highly on the temperature (see FIG. 2) a minor change in the temperature T 1 can achieve a significant change in the pressure p 1 .
  • a valve for example, for adjusting the mass flow between the intermediate storage device and the supply container, its conductance can be set such that the mass flow through the valve is affected only by the pressure p 1 on the inlet side and that it is independent of the pressure p 2 on the outlet side (locking conditions).
  • the pressure p 1 is preferably twice as high as the pressure p 2 .
  • the first metering device is advantageously a controllable mass flow controller so that on the one hand, control is possible via a control unit or a regulator, and on the other hand, the mass flow flowing between the supply container and the intermediate storage device can be measured.
  • gas is discharged via a second metering device from the intermediate storage device to a gas outlet.
  • gas can be discharged continuously from the intermediate storage device.
  • the second metering device can be adjusted such that when the pressure p 2 is exceeded gas can be discharged from the intermediate storage device so as to maintain a constant pressure in the intermediate storage device.
  • the outlet can also be used for evacuating and purging the intermediate storage device.
  • the second metering device can be a flow control valve, where the cross-section can be adjusted for discharging the gas.
  • a carrier gas is delivered into the first gas line between the supply container and the intermediate storage device.
  • the carrier gas can be an inert gas, a second precursor or a gas mix with a second precursor.
  • Carrier gases are used in CVD processes for transporting the precursors more rapidly to the object to be coated and for removing reaction products or impurities from there. Therefore, the carrier gas transports the first precursor faster through the gas supply device, and mixing the first precursor with the carrier gas has the additional advantageous effect that as a result of diluting the first precursor its partial pressure in the intermediate storage device is lower than the total pressure p 2 in the intermediate storage device.
  • the temperature T 2 is restricted by the lower limit at which the temperature-dependent saturation vapor pressure is higher than the partial pressure of the first precursor in the intermediate storage device, which prevents condensation.
  • TaCl 5 or a Ta alcoholate can preferably be used.
  • TIPT titanium isopropylate
  • AICl 3 can preferably be used.
  • the first mass flow controller 6 is used for measuring the mass flow from the supply container 2 to the intermediate storage device 4 and for adjusting the mass flow rate to a specified value.
  • first mass flow controller 6 and the intermediate storage device 4 another line enters the first gas line 3 .
  • a second mass flow controller 9 is disposed.
  • a carrier gas or another reaction gas in the present case oxygen (O 2 )
  • O 2 oxygen
  • the NbCl 5 precursor is then mixed with the carrier gas and delivered to the intermediate storage device 4 .
  • oxygen is supplied through the second mass flow controller 9 into the first gas line 3 .
  • Appropriate control of the mass flow controllers 6 and 9 achieves that the second mass flow controller 9 delivers a mass flow of oxygen proportional to the first mass flow controller 6 .
  • the mass flow of the oxygen is 19 times higher than the mass flow of NbCl 5 , resulting in a mixing ratio of 5% NbCl 5 gas and 95% oxygen in the intermediate storage device 4 .
  • the intermediate storage device is maintained at a total pressure of 40 mbar.
  • the partial pressure of the NbCl 5 in the intermediate storage device is approx. 2 mbar, which is clearly below the saturation vapor pressure of 4 mbar at 120° C. (see FIG. 1) and which prevents condensation of NbCl 5 .
  • the pressure p 2 in the intermediate storage device 4 is controlled by means of the flow control valve 15 .
  • the mass flow controllers are set for constant flow rates.
  • the pressure p 2 is controlled via a variable control of the mass flow rates of the mass flow controllers 6 , 9 at a constant ratio.
  • the mass flow through the first metering valve depends solely on its conductance and the pressure p 2 in the intermediate storage device 4 and it is independent of the pressure in the gas exchange station 11 . Therefore, in order to obtain a constant mass flow from the intermediate storage device 4 to the gas exchange station 11 and continuing to the deposition system 14 , it is not necessary to provide another mass flow controller because the mass flow rate is determined via the constant pressure p 2 and the conductance setting of the first metering valve.
  • the functional method of the two gas supply devices 19 , 20 ; 19 ′, 20 ′ substantially corresponds to the gas supply device 1 of FIG. 2 with the difference that the temperature T 1 of the supply area 19 and the temperature T 2 of the intermediate storage area 20 are optimized for the temperature dependence of the precursor in the supply container 2 , and the temperature T 4 in the supply area 19 ′ and the temperature T 5 in the intermediate storage area 20 ′ are optimized for the temperature-dependent course of the vapor pressure of the second precursor in the supply container 2 ′.

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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)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
US10/203,191 2000-02-10 2001-01-27 Gas supply device for precursors with a low vapor pressure Abandoned US20030145789A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US11/014,488 US7413767B2 (en) 2000-02-10 2004-12-16 Gas supply method in a CVD coating system for precursors with a low vapor pressure

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10005820A DE10005820C1 (de) 2000-02-10 2000-02-10 Gasversorungsvorrichtung für Precursoren geringen Dampfdrucks
DE10005820.5 2000-02-10

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US11/014,488 Division US7413767B2 (en) 2000-02-10 2004-12-16 Gas supply method in a CVD coating system for precursors with a low vapor pressure

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EP (1) EP1264002B1 (ja)
JP (1) JP4772246B2 (ja)
CN (1) CN1234908C (ja)
AT (1) ATE291105T1 (ja)
AU (1) AU2001228504A1 (ja)
CA (1) CA2399477A1 (ja)
DE (2) DE10005820C1 (ja)
HK (1) HK1052031A1 (ja)
TW (1) TW527435B (ja)
WO (1) WO2001059176A1 (ja)

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CA2399477A1 (en) 2001-08-16
DE50105618D1 (de) 2005-04-21
TW527435B (en) 2003-04-11
CN1234908C (zh) 2006-01-04
JP4772246B2 (ja) 2011-09-14
EP1264002B1 (de) 2005-03-16
JP2003527481A (ja) 2003-09-16
CN1418261A (zh) 2003-05-14
US20050132959A1 (en) 2005-06-23
HK1052031A1 (en) 2003-08-29
ATE291105T1 (de) 2005-04-15
US7413767B2 (en) 2008-08-19

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