WO2017081924A1 - 気化器、成膜装置及び温度制御方法 - Google Patents
気化器、成膜装置及び温度制御方法 Download PDFInfo
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- WO2017081924A1 WO2017081924A1 PCT/JP2016/076453 JP2016076453W WO2017081924A1 WO 2017081924 A1 WO2017081924 A1 WO 2017081924A1 JP 2016076453 W JP2016076453 W JP 2016076453W WO 2017081924 A1 WO2017081924 A1 WO 2017081924A1
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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
- 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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- 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
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67017—Apparatus for fluid treatment
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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
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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
- C23C16/52—Controlling or regulating the coating process
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- 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
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- 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
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67098—Apparatus for thermal treatment
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- 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
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67242—Apparatus for monitoring, sorting or marking
- H01L21/67248—Temperature monitoring
Definitions
- Various aspects and embodiments of the present invention relate to a vaporizer, a film forming apparatus, and a temperature control method.
- a chemical vapor deposition (CVD) method is known as a technique for forming a thin film.
- CVD chemical vapor deposition
- a solution containing a raw material such as a metal complex hereinafter referred to as “raw material solution”
- raw material solution a solution containing a raw material such as a metal complex
- the vaporizer mixes the raw material solution and the carrier gas in the gas-liquid mixing unit, injects the raw material solution mixed with the carrier gas into the vaporizing chamber from the nozzle, and vaporizes the raw material solution by heating the vaporizing chamber.
- the temperature of the nozzle may rise together with the vaporization chamber as the vaporization chamber is heated.
- the temperature of the nozzle rises excessively, the raw material solution is heated when the raw material solution is injected from the nozzle into the vaporizing chamber. For this reason, only the solvent of the raw material solution is vaporized before the raw material, and the raw material is fixed in the nozzle, and as a result, the nozzle may be clogged.
- the disclosed vaporizer includes a gas-liquid mixing unit that mixes a solution containing a raw material and a carrier gas, a nozzle that injects a solution containing the raw material mixed by the gas-liquid mixing unit, A vaporizing chamber for vaporizing the solution containing the raw material injected by the nozzle, a first temperature adjusting mechanism for adjusting the temperature of the vaporizing chamber, and a second temperature adjusting mechanism for adjusting the temperature of the gas-liquid mixing unit; A third temperature adjusting mechanism for adjusting the temperature of the nozzle; and the second temperature adjustment by heating the vaporizing chamber to a first temperature higher than the vaporizing temperature of the raw material by the first temperature adjusting mechanism.
- the temperature of the gas-liquid mixing unit is adjusted to a second temperature lower than the first temperature by a mechanism, and the temperature between the first temperature and the second temperature is adjusted by the third temperature adjusting mechanism.
- the solution belongs to the range And a control unit for adjusting the temperature of the nozzle in the third temperature lower than the vaporization temperature of the solvent.
- FIG. 1 is a diagram for explaining a schematic configuration example of a film forming apparatus according to the first embodiment.
- FIG. 2 is a schematic cross-sectional view illustrating a configuration example of the vaporizer according to the first embodiment.
- FIG. 3 is a flowchart illustrating an example of the flow of the temperature control method according to the first embodiment.
- FIG. 4 is a diagram illustrating an example of the solvent of the raw material solution.
- FIG. 5A is a diagram showing the results of Examples 1 and 2 and Comparative Examples 1 and 2.
- FIG. 5B is a diagram showing the results of Examples 3 and 4 and Comparative Examples 3 and 4.
- FIG. 5C is a diagram showing the results of Examples 5 and 6 and Comparative Examples 5 and 6.
- FIG. 5A is a diagram showing the results of Examples 1 and 2 and Comparative Examples 1 and 2.
- FIG. 5B is a diagram showing the results of Examples 3 and 4 and Comparative Examples 3 and 4.
- FIG. 5C is a diagram showing the results of Examples 5 and 6 and Compar
- FIG. 6 is a diagram for explaining a graph showing the characteristics of Li (TMHD) and the characteristics of Co (TMHD) 3 .
- FIG. 7 is a diagram for explaining a schematic configuration example of a film forming apparatus according to another embodiment 1.
- FIG. 8 is a diagram for explaining a schematic configuration example of a film forming apparatus according to another embodiment 2.
- FIG. 1 is a diagram for explaining a schematic configuration example of a film forming apparatus according to the first embodiment.
- a film forming apparatus 10 shown in FIG. 1 forms a metal oxide film on a substrate to be processed, for example, a semiconductor wafer (hereinafter simply referred to as “wafer”) W by a CVD method.
- the film forming apparatus 10 includes a vaporizer 100 and a film forming chamber 200.
- the vaporizer 100 and the film forming chamber 200 are connected by a pipe 300.
- the vaporizer 100 vaporizes a solution containing a raw material (hereinafter referred to as “raw material solution” as appropriate) to generate a raw material gas.
- the raw material is, for example, Li (TMHD).
- the source gas generated by the vaporizer 100 is supplied to the film forming chamber 200 via the pipe 300. Details of the vaporizer 100 will be described later.
- the film forming chamber 200 performs a film forming process on the wafer W using the source gas generated by the vaporizer 100.
- the film formation chamber 200 has, for example, a substantially cylindrical side wall, and includes a susceptor 222 on which the wafer W is horizontally placed in an internal space surrounded by the side wall, the top wall 210 and the bottom wall 212.
- the side wall, the top wall 210 and the bottom wall 212 are made of a metal such as aluminum or stainless steel.
- the susceptor 222 is supported by a plurality of cylindrical support members 224 (only one is shown here).
- a heater 226 is embedded in the susceptor 222, and the temperature of the wafer W placed on the susceptor 222 can be adjusted by controlling the power supplied from the power source 228 to the heater 226.
- An exhaust port 230 is formed in the bottom wall 212 of the film forming chamber 200, and an exhaust system 232 is connected to the exhaust port 230. Then, the inside of the film formation chamber 200 can be decompressed to a predetermined degree of vacuum by the exhaust system 232.
- a shower head 240 is attached to the top wall 210 of the film forming chamber 200.
- a pipe 300 is connected to the shower head 240, and the raw material gas generated by the vaporizer 100 is introduced into the shower head 240 via the pipe 300.
- the shower head 240 has a diffusion chamber 242 and a number of gas discharge holes 244 communicating with the diffusion chamber 242.
- the source gas introduced into the diffusion chamber 242 of the shower head 240 via the pipe 300 is discharged toward the wafer W on the susceptor 222 from the gas discharge hole 244.
- the source gas from the vaporizer 100 is supplied as follows.
- a raw material solution from a raw material supply source (not shown) is supplied to the vaporizer 100 and a carrier gas from a carrier gas supply source (not shown) is supplied, the raw material together with the carrier gas is supplied to the vaporization chamber provided in the vaporizer 100.
- the solution is discharged as droplets, and the raw material solution is vaporized to generate a raw material gas.
- the source gas generated in the vaporizer 100 is supplied to the film formation chamber 200 via the pipe 300, and a desired film formation process is performed on the wafer W in the film formation chamber 200.
- FIG. 2 is a schematic cross-sectional view illustrating a configuration example of the vaporizer according to the first embodiment.
- the vaporizer 100 includes a gas-liquid mixing unit 110, a nozzle 120, a vaporization chamber 130, a heater 141, a heater power supply 142, a heat medium flow path 151, a heat medium flow path 152, a heat medium unit 153, It has a heat medium transport pipe 161, a heat medium unit 162, and a control device 170.
- the gas-liquid mixing unit 110 mixes the raw material solution and the carrier gas.
- a raw material solution supply pipe 111 and a carrier gas supply pipe 112 are connected to the gas-liquid mixing section 110.
- the raw material solution is supplied from a raw material solution supply source (not shown) to the gas-liquid mixing unit 110 via the raw material solution supply pipe 111.
- the carrier gas is supplied from a carrier gas supply source (not shown) to the gas-liquid mixing unit 110 via the carrier gas supply pipe 112.
- the raw material solution mixed with the carrier gas by the gas-liquid mixing unit 110 flows into the nozzle 120.
- the nozzle 120 injects the raw material solution mixed with the carrier gas by the gas-liquid mixing unit 110 into the vaporizing chamber 130.
- a heat medium flow path 121 is formed inside the nozzle 120.
- the heat medium flow path 121 is formed, for example, in an annular shape inside the nozzle 120.
- a heat medium adjusted to a predetermined temperature by the heat medium unit 162 is supplied to the heat medium flow path 121 via the heat medium transport pipe 161.
- the vaporization chamber 130 vaporizes the raw material solution sprayed by the nozzle 120. Specifically, the vaporization chamber 130 vaporizes the raw material solution using heat transmitted from the heater 141.
- a piping 300 is connected to the vaporization chamber 130 via an exhaust device 131.
- a raw material gas obtained by vaporizing the raw material solution in the vaporizing chamber 130 is discharged to the pipe 300 by the exhaust device 131 and supplied to the film forming chamber 200 through the pipe 300.
- the heater 141 is provided outside the vaporization chamber 130 so as to cover the circumference of the vaporization chamber 130.
- the heater 141 generates heat upon receiving a current supplied from the heater power supply 142.
- surroundings of the heater 141 are covered with the heat insulating material 141a.
- the heater power supply 142 adjusts the temperature of the vaporization chamber 130 according to the control of the control device 170. Specifically, when the heater power supply 142 receives the “first temperature control signal” from the control device 170, a predetermined current is supplied to the heater 141 to cause the heater 141 to generate heat, thereby causing the heater power supply 142 to exceed the vaporization temperature of the raw material. The temperature of the vaporizing chamber 130 is adjusted to a high temperature T1. If the temperature of the vaporizing chamber 130 rises excessively, when the raw material solution is vaporized, the raw material is thermally decomposed and converted into another substance.
- the temperature T1 is preferably higher than the vaporization temperature of the raw material and lower than the temperature at which the raw material is thermally decomposed.
- the heater power source 142 is an example of a “first temperature adjustment mechanism”, and the temperature T1 is an example of a “first temperature”.
- the heat medium flow channel 151 is provided outside the gas-liquid mixing unit 110 so as to cover the periphery of the gas-liquid mixing unit 110.
- the heat medium flow path 151 is connected to the heat medium flow path 152 and allows the heat medium supplied from the heat medium unit 153 to flow through the heat medium flow path 152. Further, the periphery of the heat medium passage 151 is covered with a heat insulating material 151a.
- the heat medium flow path 152 is provided outside the carrier gas supply pipe 112 so as to cover the periphery of the carrier gas supply pipe 112 connected to the gas-liquid mixing unit 110.
- the heat medium flow path 152 is connected to the heat medium unit 153 and allows the heat medium supplied from the heat medium unit 153 to flow therethrough. Further, the periphery of the heat medium flow path 152 is covered with a heat insulating material 152a.
- the heat medium unit 153 adjusts the temperature of the gas-liquid mixing unit 110 and the temperature of the carrier gas supply pipe 112 according to the control of the control device 170. Specifically, when the heat medium unit 153 receives the “second temperature control signal” from the control device 170, the heat medium unit 153 circulates the heat medium using the heat medium flow path 151 and the heat medium flow path 152. The temperature of the gas-liquid mixing unit 110 and the temperature of the carrier gas supply pipe 112 are adjusted to a temperature T2 lower than the temperature T1. That is, the heat medium adjusted to a predetermined temperature by the heat medium unit 153 flows into the heat medium flow path 152, flows through the heat medium flow path 152, and heats or cools the carrier gas supply pipe 112. 151 flow into.
- the heat medium that has flowed into the heat medium flow path 151 flows through the heat medium flow path 151 to heat or cool the gas-liquid mixing unit 110, and returns to the heat medium unit 153 via the heat medium flow path 152.
- the temperature is adjusted to a predetermined temperature by the medium unit 153 and is circulated again through the heat medium flow path 152 and the heat medium flow path 151.
- the temperature of the gas-liquid mixing part 110 and the temperature of the carrier gas supply pipe 112 are adjusted to a temperature T2 lower than the temperature T1.
- the heat medium unit 153 is an example of a “second temperature adjustment mechanism”, and the temperature T2 is an example of a “second temperature”.
- the heat medium transport pipe 161 is connected to the heat medium flow path 121 in the nozzle 120, and transports the heat medium adjusted to a predetermined temperature by the heat medium unit 162 to the heat medium flow path 121.
- the heat medium unit 162 adjusts the temperature of the nozzle 120 according to the control of the control device 170. Specifically, when receiving the “third temperature control signal” from the control device 170, the heat medium unit 162 circulates the heat medium using the heat medium transport pipe 161 and the heat medium flow path 121 in the nozzle 120. By adjusting the temperature, the temperature of the nozzle 120 is adjusted to the temperature T3.
- the temperature T3 belongs to a temperature range between the temperature T1 and the temperature T2, and is lower than the vaporization temperature of the solvent of the raw material solution.
- the heat medium adjusted to a predetermined temperature by the heat medium unit 162 flows into the heat medium flow path 121 in the nozzle 120 via the heat medium transport pipe 161, flows through the heat medium flow path 121, and moves the nozzle 120. Heated or cooled, returned to the heat medium unit 162 through the heat medium transport pipe 161, adjusted to a predetermined temperature by the heat medium unit 162, and circulated again through the heat medium transport pipe 161 and the heat medium flow path 121. To do. Thereby, the temperature of the nozzle 120 is adjusted to the temperature T3.
- the heat medium unit 162 is an example of a “third temperature adjustment mechanism”
- the temperature T3 is an example of a “third temperature”.
- the control device 170 includes, for example, a central processing unit (CPU) and a storage device such as a memory, and controls various operations of the vaporizer 100 by reading and executing a program stored in the storage device. For example, the control device 170 controls each part of the vaporizer 100 so as to perform a temperature control method described later. As a detailed example, the control device 170 adjusts the temperature of the vaporization chamber 130 to a temperature T1 higher than the vaporization temperature of the raw material by the heater power supply 142. And the control apparatus 170 adjusts the temperature of the gas-liquid mixing part 110 to the temperature T2 lower than the temperature T1 by the heat medium unit 153.
- CPU central processing unit
- a storage device such as a memory
- the control apparatus 170 adjusts the temperature of the nozzle 120 to temperature T3 which belongs to the temperature range between the temperature T1 and the temperature T2 by the heat medium unit 162, and is lower than the vaporization temperature of the solvent of a raw material solution.
- the temperature adjustment by the heater power supply 142, the temperature adjustment by the heat medium unit 153, and the temperature adjustment by the heat medium unit 162 are, for example, the above-mentioned “first temperature adjustment signal”, “second temperature adjustment signal”, And “third temperature adjustment signal”.
- the temperature T3 corresponds to an intermediate value between the temperature T1 and the temperature T2, for example, and is lower than the vaporization temperature of the solvent of the raw material solution.
- the raw material is, for example, Li (TMHD).
- FIG. 3 is a flowchart illustrating an example of the flow of the temperature control method according to the first embodiment.
- the raw material is Li (TMHD).
- the controller 170 of the vaporizer 100 adjusts the temperature Th of the vaporization chamber 130 to a temperature T1 higher than the vaporization temperature of the raw material by the heater power supply 142 (step S101).
- Tsol ° C.
- the temperature condition to be satisfied by the vaporization chamber 130 is expressed by the following equation (1).
- the temperature T1 that is, the temperature Th of the vaporization chamber 130 is preferably lower than the temperature at which the raw material is thermally decomposed as described above. That is, since the thermal decomposition temperature of the raw material Li (TMHD) is 280 ° C., the following formula (2) is derived from the above formula (1).
- control device 170 adjusts the temperature Tm of the gas-liquid mixing unit 110 to a temperature T2 lower than the temperature T1 by the heat medium unit 153 (step S102). At this time, the control device 170 adjusts the temperature of the carrier gas supply pipe 112 together with the temperature of the gas-liquid mixing unit 110 to the temperature T2.
- the control device 170 adjusts the temperature Tn of the nozzle 120 to a temperature T3 that belongs to a temperature range between the temperature T1 and the temperature T2 and is lower than the vaporization temperature of the solvent of the raw material solution by the heat medium unit 162. (Step S103). In the present embodiment, the control device 170 adjusts the temperature Tn of the nozzle 120 to a temperature T3 corresponding to an intermediate value between the temperature T1 and the temperature T2 and lower than the vaporization temperature of the solvent of the raw material solution.
- the temperature condition to be satisfied by the nozzle 120 is expressed by the following equation (3).
- Tn (Th + Tm) / 2 ⁇ Tsov ... (3)
- the solvent of the raw material solution is selected so that the temperature condition represented by the above formula (2) and the temperature condition represented by the above formula (3) are satisfied.
- the solvent of the raw material solution is selected so that the following expressions (4) and (5) are satisfied.
- FIG. 4 is a diagram illustrating an example of the solvent of the raw material solution. That is, as the solvent of the raw material solution, acetonitrile, gamma butyrolactone, diethyl ether, 1,2-dimethoxyethane, dimethyl sulfoxide, 1,3-dioxolane, ethylene carbonate, methyl formate, 2-methyltetrahydrofuran, 3-methyl-2- Examples include oxazolidinone, propylene carbonate, sulfolane, formamide, N, N-dimethylformamide, glyme, diglyme, triglyme, tetraglyme, benzaldehyde, acetophenone, benzophenone, tetrahydrofuran, toluene, cyclohexanone, mesitylene, and diphenyl
- a solvent having a relative dielectric constant of 7.0 or more and a dipole moment of 1.7 D or more that is, acetonitrile, gamma butyrolactone, dimethyl sulfoxide, Ethylene carbonate, methyl formate, propylene carbonate, sulfolane, formamide, N, N-dimethylformamide, glyme, diglyme, benzaldehyde, acetophenone, benzophenone, tetrahydrofuran and cyclohexanone are preferred.
- processing procedure shown in FIG. 3 is not limited to the above-described order, and may be appropriately changed within a range that does not contradict the processing contents.
- the above steps S101 and S102 may be executed in parallel.
- the temperature of the vaporization chamber 130 is adjusted to the temperature T1 higher than the vaporization temperature of the raw material, and the gas-liquid mixing unit 110 is adjusted to the temperature T2 lower than the temperature T1.
- the temperature is adjusted, and the temperature of the nozzle 120 is adjusted to a temperature T3 that belongs to a temperature range between the temperature T1 and the temperature T2 and that is lower than the vaporization temperature of the solvent of the raw material solution.
- the temperature of the nozzle 120 is adjusted independently of the temperature of the vaporization chamber 130 and the temperature of the gas-liquid mixing unit 110, so that the nozzle 120 can be cooled appropriately and the material in the nozzle 120 is prevented from sticking. can do.
- clogging of the nozzle 120 can be stably suppressed.
- Example 6 the temperature Th of the vaporization chamber 130 is adjusted to a temperature T1 higher than the vaporization temperature Tsol of Li (TMHD) as a raw material, and the temperature Tm of the gas-liquid mixing unit 110 is set to a temperature T2 lower than the temperature T1.
- the temperature Tn of the nozzle 120 was adjusted to a temperature T3 corresponding to an intermediate value between the temperature T1 and the temperature T2 and lower than the vaporization temperature Tsov of the solvent Y of the raw material solution.
- Examples 1 to 6 the following solvent was used as the solvent Y of the raw material solution.
- Examples 1 and 2 Mesitylene
- Examples 3 and 4 Toluene
- Examples 5 and 6 Tetrahydrofuran
- Comparative Examples 1 and 2 In Comparative Examples 1 and 2, unlike Examples 1 and 2, the temperature Th of the vaporization chamber 130 was adjusted to a temperature lower than the vaporization temperature Tsol of the raw material Li (TMHD). Comparative Examples 1 and 2 are the same as Examples 1 and 2 in other points.
- Comparative Examples 3 and 4 In Comparative Examples 3 and 4, unlike Examples 3 and 4, the temperature Th of the vaporization chamber 130 was adjusted to a temperature lower than the vaporization temperature Tsol of the raw material Li (TMHD). Comparative Examples 3 and 4 are the same as Examples 3 and 4 in other points.
- Comparative Example 5 (Comparative Example 5)
- the temperature Th of the vaporization chamber 130 is adjusted to a temperature lower than the vaporization temperature Tsol of the raw material Li (TMHD), and the intermediate value between the temperature T1 and the temperature T2 is set.
- the temperature Tn of the nozzle 120 was adjusted to a temperature higher than the vaporization temperature Tsov of the solvent Y of the raw material solution. Comparative Example 5 is the same as Examples 5 and 6 in other points.
- Comparative Example 6 In Comparative Example 6, unlike Examples 5 and 6, the temperature Th of the vaporization chamber 130 was adjusted to a temperature lower than the vaporization temperature Tsol of the raw material Li (TMHD). Comparative Example 6 is the same as Examples 5 and 6 in other points.
- FIG. 5A is a diagram showing the results of Examples 1 and 2 and Comparative Examples 1 and 2.
- FIG. 5B is a diagram showing the results of Examples 3 and 4 and Comparative Examples 3 and 4.
- FIG. 5C is a diagram showing the results of Examples 5 and 6 and Comparative Examples 5 and 6.
- the temperature Th of the vaporization chamber 130 is adjusted to the temperature T1
- the gas-liquid mixing unit 110 is adjusted to the temperature T2.
- the second embodiment is different from the first embodiment in that Li (TMHD) and Co (TMHD) 3 are used as raw materials. Therefore, the description of the same configuration as that of the first embodiment is omitted.
- the vaporizer 100 vaporizes the raw material solution to generate the raw material gas.
- the raw material is Li (TMHD) and Co (TMHD) 3
- the raw material solution is a mixed solution containing Li (TMHD) and Co (TMHD) 3 as the raw material.
- the source gas generated by the vaporizer 100 is supplied to the film forming chamber 200 via the pipe 300.
- the solvent of the raw material solution is selected so that the following equations (8) and (9) are satisfied.
- the vaporization temperature of the raw material is Tsol, Li (° C.), and the temperature of the vaporization chamber 130 is Th, Li. It is represented by the formula (10).
- the temperatures Th and Li of the vaporization chamber 130 are preferably lower than the temperature at which the raw material is thermally decomposed. That is, since the thermal decomposition temperature of Li (TMHD) is 280 ° C., the following equation (11) is derived from the above equation (10).
- the vaporization temperature of the solvent of the raw material solution is Tsov, Li
- the temperature of the nozzle 120 is Tn, Li
- the temperature of the gas-liquid mixing unit 110 is Tm, Li.
- the vaporization temperature of the raw material is Tsol, Co (° C.) and the temperature of the vaporization chamber 130 is Th, Co, assuming that the raw material is only Co (TMHD) 3 , the vaporization chamber 130 is satisfied.
- the power temperature condition is expressed by the following equation (17).
- temperature Th, Co of the vaporization chamber 130 is lower than the temperature which a raw material thermally decomposes. That is, since the thermal decomposition temperature of Co (TMHD) 3 is 250 ° C., the following equation (18) is derived from the above equation (17).
- the temperature condition to be satisfied by the nozzle 120 is expressed by the following equation (19).
- FIG. 6 is a diagram for explaining a graph showing the characteristics of Li (TMHD) and the characteristics of Co (TMHD) 3 .
- the solid line indicates the characteristic of Li (TMHD)
- the broken line indicates the characteristic of Co (TMHD) 3 .
- the solvent of the raw material solution is the above formula (8) and formula (9). Is selected to be satisfied.
- clogging of the nozzle 120 can be stably suppressed as in the first embodiment.
- the film forming apparatus 10 has one vaporizer 100 for one film forming chamber 200
- the disclosed technique is not limited thereto.
- the film forming apparatus 10 may have two vaporizers for one film forming chamber 200.
- a film forming apparatus having two vaporizers for one film forming chamber 200 will be described as a film forming apparatus according to another embodiment.
- FIG. 7 is a diagram for explaining a schematic configuration example of a film forming apparatus according to another embodiment 1.
- the film forming apparatus 10 according to another embodiment 1 is different from the film forming apparatus 10 described with reference to FIG. 1 in that one film forming chamber 200 has two vaporizers. Therefore, the description of the same configuration as the film forming apparatus 10 described in FIG. 1 is omitted.
- the 7 has vaporizers 100a and 100b and a film formation chamber 200.
- the film formation apparatus 10 shown in FIG. The vaporizer 100a and the film formation chamber 200 are connected by a pipe 300a, and the vaporizer 100b and the film formation chamber 200 are connected by a pipe 300b.
- the vaporizer 100a vaporizes a raw material solution containing Li (TMHD) as a raw material to generate a raw material gas.
- the source gas generated by the vaporizer 100a is supplied to the film forming chamber 200 through the pipe 300a.
- the configuration of the vaporizer 100a is the same as that of the vaporizer 100 described in FIG.
- the solvent of the raw material solution is selected so that the temperature condition regarding Li (TMHD) as the raw material is satisfied, that is, the following equations (24) and (25) are satisfied.
- Tm temperature of the gas-liquid mixing unit 110 (° C.)
- the vaporizer 100b vaporizes a raw material solution containing Co (TMHD) 3 as a raw material to generate a raw material gas.
- the raw material gas generated by the vaporizer 100b is supplied to the film forming chamber 200 through the pipe 300b.
- the configuration of the vaporizer 100b is the same as that of the vaporizer 100 described in FIG.
- the solvent of the raw material solution is selected so that the temperature condition regarding Co (TMHD) 3 as the raw material is satisfied, that is, the following equations (26) and (27) are satisfied.
- a shower head 240 a is attached to the top wall 210 of the film forming chamber 200.
- a pipe 300a and a pipe 300b are connected to the shower head 240a.
- the raw material gas generated by the vaporizer 100a that is, the raw material gas obtained by vaporizing the raw material solution containing Li (TMHD) as the raw material
- TMHD raw material solution containing Li
- a raw material gas generated in the vaporizer 100b that is, a raw material gas obtained by vaporizing a raw material solution containing Co (TMHD) 3 as a raw material
- the shower head 240a has a diffusion chamber 242a and a number of gas discharge holes 244a communicating with the diffusion chamber 242a.
- the raw material gas introduced into the diffusion chamber 242a of the shower head 240a through the pipe 300a and the raw material gas introduced into the diffusion chamber 242a of the shower head 240a through the pipe 300b are mixed in the diffusion chamber 242a and discharged. It is discharged toward the wafer W on the susceptor 222 from the hole 244a.
- FIG. 8 is a diagram for explaining a schematic configuration example of a film forming apparatus according to another embodiment 2.
- the film forming apparatus 10 according to another embodiment 2 is different from the film forming apparatus 10 described with reference to FIG. 7 in the structure of the shower head. Therefore, the description of the same configuration as the film forming apparatus 10 described in FIG. 7 is omitted.
- a shower head 240 b is attached to the top wall 210 of the film forming chamber 200.
- a pipe 300a and a pipe 300b are connected to the shower head 240b.
- the raw material gas generated in the vaporizer 100a that is, the raw material gas obtained by vaporizing the raw material solution containing Li (TMHD) as the raw material
- the raw material gas generated in the vaporizer 100b that is, the raw material gas obtained by vaporizing the raw material solution containing Co (TMHD) 3 as the raw material
- the shower head 240b is introduced into the shower head 240b via the pipe 300b.
- the shower head 240b includes a diffusion chamber 242b, a number of gas discharge holes 244b communicating with the diffusion chamber 242b, a diffusion chamber 242c, and a number of gas discharge holes 244c communicating with the diffusion chamber 242c.
- the source gas introduced into the diffusion chamber 242b of the shower head 240b via the pipe 300a is discharged toward the wafer W on the susceptor 222 from the gas discharge hole 244b. Further, the source gas introduced into the diffusion chamber 242c of the shower head 240b via the pipe 300b is discharged toward the wafer W on the susceptor 222 from the gas discharge hole 244c. Then, the source gas discharged from the gas discharge hole 244b and the source gas discharged from the gas discharge hole 244c are mixed in the film forming chamber 200.
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Abstract
Description
まず、実施形態1にかかる成膜装置について図面を参照しながら説明する。図1は、実施形態1にかかる成膜装置の概略構成例を説明するための図である。図1に示す成膜装置10は、被処理基板例えば半導体ウエハ(以下、単に「ウエハ」という)W上にCVD法により金属酸化物膜を成膜する。成膜装置10は、気化器100と、成膜室200とを有する。気化器100と、成膜室200とは配管300によって接続されている。
Tsov>{11.94ln(Ph)+157.38+Tm}/2 …(5)
ただし、Ph:気化室の圧力(kPa)
実施例1~6では、原料であるLi(TMHD)の気化温度Tsolよりも高い温度T1に気化室130の温度Thを調整し、温度T1よりも低い温度T2に気液混合部110の温度Tmを調整し、温度T1と温度T2との中間値に対応し、かつ、原料溶液の溶媒Yの気化温度Tsovよりも低い温度T3にノズル120の温度Tnを調整した。
実施例1,2:メシチレン
実施例3,4:トルエン
実施例5,6:テトラヒドロフラン
比較例1,2では、実施例1,2とは異なり、原料であるLi(TMHD)の気化温度Tsolよりも低い温度に気化室130の温度Thを調整した。比較例1,2では、それ以外の点において、実施例1,2と同様である。
比較例3,4では、実施例3,4とは異なり、原料であるLi(TMHD)の気化温度Tsolよりも低い温度に気化室130の温度Thを調整した。比較例3,4では、それ以外の点において、実施例3,4と同様である。
比較例5では、実施例5,6とは異なり、原料であるLi(TMHD)の気化温度Tsolよりも低い温度に気化室130の温度Thを調整し、温度T1と温度T2との中間値に対応し、かつ、原料溶液の溶媒Yの気化温度Tsovよりも高い温度にノズル120の温度Tnを調整した。比較例5では、それ以外の点において、実施例5,6と同様である。
比較例6では、実施例5,6とは異なり、原料であるLi(TMHD)の気化温度Tsolよりも低い温度に気化室130の温度Thを調整した。比較例6では、それ以外の点において、実施例5,6と同様である。
図5Aは、実施例1,2及び比較例1,2の結果を示す図である。図5Bは、実施例3,4及び比較例3,4の結果を示す図である。図5Cは、実施例5,6及び比較例5,6の結果を示す図である。
実施形態2は、原料として、Li(TMHD)及びCo(TMHD)3を用いる点が実施形態1と異なる。したがって、実施形態1と同様の構成については、説明を省略する。
Tsov>{11.94ln(Ph)+157.38+Tm}/2 …(9)
ただし、Ph:気化室の圧力(kPa)
ただし、Ph,Li:原料がLi(TMHD)のみであると仮定した場合の気化室の圧力(kPa)
ただし、Ph,Co:原料がCo(TMHD)3のみであると仮定した場合の気化室の圧力(kPa)
なお、上記実施形態では、成膜装置10が1つの成膜室200に対して1つの気化器100を有する例を説明したが、開示技術はこれに限定されない。例えば、成膜装置10は、1つの成膜室200に対して2つの気化器を有しても良い。以下、他の実施形態にかかる成膜装置として、1つの成膜室200に対して2つの気化器を有する成膜装置について説明する。
Tsov>{11.94ln(Ph)+157.38+Tm}/2 …(25)
ただし、Ph:気化室130の圧力(kPa)
Tsov:原料溶液の溶媒の気化温度(℃)
Tm:気液混合部110の温度(℃)
Tsov>{17.744ln(Ph)+45.483+Tm}/2 …(27)
100 気化器
110 気液混合部
111 原料溶液供給管
112 キャリアガス供給管
120 ノズル
121 熱媒流路
130 気化室
131 排気装置
141 ヒータ
141a 断熱材
142 ヒータ電源
151 熱媒流路
151a 断熱材
152 熱媒流路
152a 断熱材
153 熱媒ユニット
161 熱媒輸送管
162 熱媒ユニット
170 制御装置
200 成膜室
210 天壁
212 底壁
222 サセプタ
224 支持部材
226 ヒータ
228 電源
230 排気ポート
232 排気系
240 シャワーヘッド
242 拡散室
244 ガス吐出孔
300 配管
Claims (9)
- 原料を含む溶液とキャリアガスとを混合する気液混合部と、
前記気液混合部によって混合された前記原料を含む溶液を噴射するノズルと、
前記ノズルによって噴射された前記原料を含む溶液を気化する気化室と、
前記気化室の温度を調整する第1の温度調整機構と、
前記気液混合部の温度を調整する第2の温度調整機構と、
前記ノズルの温度を調整する第3の温度調整機構と、
前記第1の温度調整機構によって前記原料の気化温度よりも高い第1の温度に前記気化室の温度を調整し、前記第2の温度調整機構によって前記第1の温度よりも低い第2の温度に前記気液混合部の温度を調整し、前記第3の温度調整機構によって前記第1の温度と前記第2の温度との間の温度範囲に属し、かつ、前記溶液の溶媒の気化温度よりも低い第3の温度に前記ノズルの温度を調整する制御部と
を有することを特徴とする気化器。 - 前記第3の温度は、前記第1の温度と前記第2の温度との中間値に対応し、かつ、前記溶液の溶媒の気化温度よりも低いことを特徴とする請求項1に記載の気化器。
- 前記第1の温度は、前記原料の気化温度よりも高く、かつ、前記原料が熱分解する温度よりも低い温度であることを特徴とする請求項1又は2に記載の気化器。
- 前記第2の温度調整機構は、
前記気液混合部へ前記キャリアガスを供給するキャリアガス供給管の温度をさらに調整し、
前記制御部は、
前記第2の温度調整機構によって前記気液混合部の温度及び前記キャリアガス供給管の温度を前記第2の温度に調整することを特徴とする請求項1に記載の気化器。 - 前記原料は、Li(TMHD)であり、
前記気化室の圧力をPh(kPa)とし、前記気液混合部の温度をTm(℃)とし、前記溶液の溶媒の気化温度をTsov(℃)とすると、前記溶液の溶媒は、以下の式(1)及び式(2)が満たされるように、選択されることを特徴とする請求項1に記載の気化器。
Ph<29 …(1)
Tsov>{11.94ln(Ph)+157.38+Tm}/2 …(2) - 前記原料は、Li(TMHD)及びCo(TMHD)3であり、
前記気化室の圧力をPh(kPa)とし、前記気液混合部の温度をTm(℃)とし、前記溶液の溶媒の気化温度をTsov(℃)とすると、前記溶液の溶媒は、以下の式(3)及び式(4)が満たされるように、選択されることを特徴とする請求項1に記載の気化器。
Ph<29 …(3)
Tsov>{11.94ln(Ph)+157.38+Tm}/2 …(4) - 前記原料は、Co(TMHD)3であり、
前記気化室の圧力をPh(kPa)とし、前記気液混合部の温度をTm(℃)とし、前記溶液の溶媒の気化温度をTsov(℃)とすると、前記溶液の溶媒は、以下の式(5)及び式(6)が満たされるように、選択されることを特徴とする請求項1に記載の気化器。
Ph<101 …(5)
Tsov>{17.744ln(Ph)+45.483+Tm}/2 …(6) - 原料を含む溶液を気化して原料ガスを生成する気化器と、
前記気化器によって生成された原料ガスを用いて成膜処理を行う成膜室と
を有し、
前記気化器は、
原料を含む溶液とキャリアガスとを混合する気液混合部と、
前記気液混合部によって混合された前記原料を含む溶液を噴射するノズルと、
前記ノズルによって噴射された前記原料を含む溶液を気化する気化室と、
前記気化室の温度を調整する第1の温度調整機構と、
前記気液混合部の温度を調整する第2の温度調整機構と、
前記ノズルの温度を調整する第3の温度調整機構と、
前記第1の温度調整機構によって前記原料の気化温度よりも高い第1の温度に前記気化室の温度を調整し、前記第2の温度調整機構によって前記第1の温度よりも低い第2の温度に前記気液混合部の温度を調整し、前記第3の温度調整機構によって前記第1の温度と前記第2の温度との間の温度範囲に属し、かつ、前記溶液の溶媒の気化温度よりも低い第3の温度に前記ノズルの温度の調整する制御部と
を有することを特徴とする成膜装置。 - 原料を含む溶液とキャリアガスとを混合する気液混合部と、
前記気液混合部によって混合された前記原料を含む溶液を噴射するノズルと、
前記ノズルによって噴射された前記原料を含む溶液を気化する気化室と、
前記気化室の温度を調整する第1の温度調整機構と、
前記気液混合部の温度を調整する第2の温度調整機構と、
前記ノズルの温度を調整する第3の温度調整機構と
を有する気化器による温度制御方法であって、
前記第1の温度調整機構によって前記原料の気化温度よりも高い第1の温度に前記気化室の温度を調整し、前記第2の温度調整機構によって前記第1の温度よりも低い第2の温度に前記気液混合部の温度を調整し、前記第3の温度調整機構によって前記第1の温度と前記第2の温度との間の温度範囲に属し、かつ、前記溶液の溶媒の気化温度よりも低い第3の温度に前記ノズルの温度を調整する
ことを特徴とする温度制御方法。
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