US9271341B2 - Heat treatment apparatus that performs defect repair annealing - Google Patents

Heat treatment apparatus that performs defect repair annealing Download PDF

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US9271341B2
US9271341B2 US12/955,020 US95502010A US9271341B2 US 9271341 B2 US9271341 B2 US 9271341B2 US 95502010 A US95502010 A US 95502010A US 9271341 B2 US9271341 B2 US 9271341B2
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electrode
heated
heat treatment
temperature
sample
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US20120055915A1 (en
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Ken'etsu Yokogawa
Masatoshi Miyake
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Hitachi High Tech Corp
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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
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B7/00—Heating by electric discharge
    • H05B7/18—Heating by arc discharge

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  • the present invention relates to a semiconductor fabrication apparatus that fabricates semiconductor devices. More particularly, the present invention is concerned with a heat treatment apparatus that performs activation annealing or defect repair annealing, which is preceded by doping of an impurity and intended to control the conductivity of a semiconductor substrate, and oxidation or the like of the surface of the semiconductor substrate.
  • SiC silicon carbide
  • GaN gallium nitride
  • a process of fabricating various types of power devices using SiC as a substrate material is almost identical to a process in which Si is used as the substrate material, though the size or the like of the substrate is different between the SiC substrate and Si substrate.
  • a heat treatment process is cited. What is referred to as the heat treatment process is represented by activation annealing that is preceded by ion implantation of an impurity and intended to control the conductivity of the substrate.
  • the activation annealing is performed at the temperature ranging from 800° C. to 1200° C.
  • the temperature ranging from 1800° C. to 2000° C. is necessary in terms of the material properties.
  • a resistive heating furnace described, for example, in Japanese Patent Application Laid-Open Publication No. 2009-32774 is known.
  • an annealing apparatus of an induction heating type described in, for example, Japanese Patent Application Laid-Open Publication No. 2010-34481 is known.
  • a first problem lies in heat efficiency. Heat dissipation from a furnace body is dominated by radiation, and a radiant quantity increases in proportion to a biquadrate of temperature. Therefore, if a region to be heated is wide, energy efficiency necessary to heating markedly degrades. For a resistive heating furnace, a double-tube structure is usually adopted in order to avoid contamination caused by a heater. The region to be heated therefore gets wider. In addition, since a sample to be heated recedes from a heat source (heater) due to the presence of a double tube, it is necessary to set the heater to the temperature higher than the temperature of the sample to be heated. This also becomes a factor of largely degrading the efficiency.
  • the heat capacity of the region to be heated gets very large, and it takes much time to raise or lower the temperature. Accordingly, the time it takes to eject the sample to be heated after the sample to be heated is inputted gets longer. This becomes a factor of decreasing a throughput, or a factor of intensifying the surface roughness of the sample to be heated, which will be described later, because the time during which the sample to be heated stays in a high-temperature environment gets longer.
  • a second problem is concerned with wastage of a furnace material.
  • Materials capable of coping with 1800° C. and being adopted as the furnace material are limited.
  • a high-purity material of a high melting point is necessary.
  • the furnace material capable of being used for SiC is graphite or SiC itself.
  • a sintered SiC compact or a material having the surface thereof coated with SiC according to a chemical vapor phase deposition method is adopted. These materials are usually expensive. If a furnace body is large, a considerable cost is necessary to replacement. The higher the temperature is, the shorter the service life of the furnace body is. The cost of replacement gets higher than that in the normal Si process.
  • the induction heating method described in Japanese Patent Application Laid-Open Publication No. 2010-34481 is a method of heating an object of heating by feeding a high-frequency induction current to the object of heating or a placement member on which the object of heating is placed.
  • the induction heating method enjoys high heat efficiency.
  • the electric resistivity of the object of heating is low, a large induction current is necessary to heating.
  • the absolute value of the heat efficiency of an entire heating system is not always high (a heat loss occurring in an induction coil or the like is large). The induction heating method is therefore confronted with a problem on heat efficiency.
  • Heating uniformity is determined with the induction current that flows into the object of heating or the placement member on which the object of heating is placed.
  • the heating uniformity may not be sufficiently attained for a planar disk like the one employed in device fabrication. If the heating uniformity is poor, there is a fear that the object of heating may be broken due to a thermal stress during rapid heating. This becomes a factor of decreasing a throughput because of the necessity of lowering a speed of a temperature rise to such an extent that a stress is not generated. Further, similarly to the resistive heating furnace method, steps of producing and removing a cap film that prevents evaporation of Si from a SiC surface at the time of extremely high temperature are additionally necessary.
  • An object of the present invention is to provide a heat treatment apparatus that even when annealing SiC at high temperature, can exhibit a low heat capacity and perform uniform heating.
  • a heat treatment apparatus including a pair of parallel plate electrodes, a high-frequency power supply that applies a high-frequency voltage to the pair of parallel plate electrodes so as to discharge between the pair of parallel plate electrodes, a temperature measurement instrument that measures the temperature of a sample to be heated which is disposed in the pair of parallel plate electrodes, a gas introduction unit that introduces a gas into the pair of parallel plate electrodes, reflection mirrors that surround the pair of parallel plate electrodes, and a control unit that controls the output of the high-frequency power supply.
  • the control unit references the temperature measured by the temperature measurement instrument, and controls the output of the high-frequency power supply so as to control the heat treatment temperature for the sample to be heated.
  • a heat treatment apparatus including a high-frequency power supply, a lower electrode on which a sample to be heated is placed, an upper electrode to which the high-frequency power supply is connected and which is located at a position opposite to the position of the lower electrode, a gas introduction unit that introduces a gas, which is used to produce plasma due to discharge, into the space between the upper electrode and lower electrode, and upper and lower reflection mirrors that cover the upper and lower electrodes via a space.
  • a heat treatment apparatus that even when annealing SiC at high temperature, can exhibit a low heat capacity and achieve uniform heating.
  • inclusion of reflection mirrors suppresses a radiation loss and permits high-temperature heat treatment.
  • FIG. 1A is a diagram showing a basic construction of a heat treatment apparatus in accordance with a first embodiment of the present invention employing plasma;
  • FIG. 1B is a diagram showing the relationship between a thermal electron current and electrode temperature
  • FIG. 1C is a diagram for use in explaining the fact that a radiation loss is minimized by reflection mirrors
  • FIG. 2A is a sectional view of a discharge formation unit included in a heat treatment apparatus in accordance with a second embodiment of the present invention employing plasma;
  • FIG. 2B is a sectional view of another discharge formation unit included in the heat treatment apparatus in accordance with the second embodiment of the present invention employing plasma;
  • FIG. 3 is a diagram showing a basic construction of a heat treatment apparatus in accordance with a third embodiment of the present invention employing plasma (a state in which treatment is under way);
  • FIG. 4 is a diagram showing the basic construction of the heat treatment apparatus in accordance with the third embodiment of the present invention employing plasma (a state in which treatment has been completed).
  • FIG. 5 is a diagram showing an example of a sequence of basic actions of the heat treatment apparatus shown in FIG. 1A .
  • a sample to be heated is disposed in a pair of parallel plate electrodes in which a gap ranging from 0.1 mm or more to 2 mm or less is created, and the gap is filled with a gas that contains as a main raw material a rare gas (helium (He), argon (Ar), krypton (Kr), xenon (Xe), or the like) whose pressure is close to atmospheric pressure.
  • a high-frequency voltage is applied to the pair of parallel plate electrodes in order to produce plasma.
  • the gas is heated with the plasma, whereby the sample to be heated is thermally treated.
  • a heat treatment apparatus Owing to heating of a gas with plasma, a heat treatment apparatus can be provided for fabrication of semiconductor devices that needs extremely high temperature of about 2000° C. Eventually, heating efficiency can be improved, a throughput can be improved due to shortening of a heating treatment time, a cost of operation such as a cost incurred by wastage of a furnace material can be reduced, and the surface roughness of a sample to be heated caused by extremely high temperature can be suppressed.
  • FIG. 1A shows a basic construction of a heat treatment apparatus in accordance with the present embodiment employing plasma. To begin with, the construction of the heat treatment apparatus will be described below.
  • a sample to be heated 1 is placed in a pair of parallel plate electrodes including an upper electrode 2 and a lower electrode 3 .
  • the sample to be heated 1 was placed on the lower electrode 3 , and the gap 4 between the upper electrode 2 and lower electrode 3 was 0.8 mm.
  • the sample to be heated 1 has a thickness ranging from 0.5 mm to 0.8 mm.
  • a dent in which the sample to be heated 1 is locked is formed in the lower electrode 3 on which the sample to be heated 1 is placed, though it is not shown in the drawing.
  • the circumferential corners of the upper electrode 2 and lower electrode 3 that are opposed to each other are tapered or rounded. This is intended to suppress localization of plasma due to concentration of an electric field at the corner of the electrode.
  • a high-frequency power is fed from a high-frequency power supply 6 to the upper electrode 2 over a feeder line 5 .
  • 13.56 MHz was adopted as the frequency of the high-frequency power supply 6 .
  • the lower electrode 3 is grounded over a feeder line 7 .
  • the feeder lines 5 and 7 are made of graphite that is a material made into the upper electrode 2 and lower electrode 3 alike.
  • a matching circuit 8 (M.B in the drawing stands for matching box) is interposed between the high-frequency power supply 6 and upper electrode 2 .
  • a structure for efficiently feeding the high-frequency power from the high-frequency power supply 6 to the plasma produced between the upper electrode 2 and lower electrode 3 is thus realized.
  • a He gas can be introduced at a pressure, which ranges from 0.1 atm. to 10 atm., by means of a gas introduction unit 10 .
  • the pressure of the gas to be introduced is monitored by a pressure detection unit 11 .
  • the gas can be exhausted from the container 9 by a vacuum pump connected to an exhaust vent 12 .
  • the container 9 is deaerated to be vacuum at a step preceding introduction of the He gas.
  • the gas is introduced by the gas introduction unit 10 until the gas has a predetermined pressure.
  • the atmosphere in the container 9 can be brought to an atmosphere of a desired pure gas (He in the present embodiment).
  • the predetermined pressure can be retained by combining introduction of a certain amount of gas, which is performed by the gas introduction unit 10 , with exhaustion thereof.
  • the gas introduction unit can be controlled by the control unit 18 .
  • the upper electrode 2 and lower electrode 3 in the container 9 are surrounded by reflection mirrors 13 each formed with a paraboloid of revolution.
  • a protective quartz plate 14 is interposed between the upper electrode 2 and the reflection mirror 13 and between the lower electrode 3 and the reflection mirror 13 .
  • the reflection mirror 13 formed with the paraboloid of revolution is constructed by optically polishing the paraboloid of a metallic substrate, and plating or vapor-depositing gold on the polished surface.
  • a coolant channel 15 is formed in the metallic substrate of the reflection mirror 13 . Cooling water is poured into the channel so that the temperature of the metallic substrate can be held constant.
  • the upper electrode 2 or lower electrode 3 can be measured through a window 16 using a radiation thermometer 17 .
  • the radiation thermometer 17 is used to measure the temperature of the sample to be heated 1 .
  • the result of the measurement by the radiation thermometer 17 is processed by the control unit 18 , and the output of the high-frequency power supply 6 is automatically controlled so that the temperature of the sample to be heated 1 becomes desired temperature.
  • the temperature of the sample to be heated 1 can be considered to be identical to the temperature of the upper electrode 2 or lower electrode 3 , or especially, to the temperature of the lower electrode 3 .
  • the gap 4 between the upper electrode 2 and lower electrode 3 is set to 0.8 mm by means of an up-and-down mechanism 20 (the same applies to the distance between the upper electrode 2 and the sample to be heated 1 ).
  • the container 9 is deaerated by the vacuum pump, which is connected through the exhaust vent 12 , until the pressure therein becomes 1 Pa or less, and is then brought to a vacuum state by means of a vacuum valve 21 .
  • a He gas is introduced from the gas introduction unit 10 to the container 9 until the gas pressure becomes a desired one. In the present embodiment, the He pressure in the container 9 was set to 1 atm. (1013 hectopascal).
  • a high-frequency power is applied from the high-frequency power supply to the upper electrode 2 via the matching circuit 8 through a power introduction terminal 19 over the feeder line 5 .
  • He plasma is produced in a glow discharge region in the gap 4 .
  • the high-frequency power to be fed to the upper electrode 2 was set to 2000 W.
  • the high-frequency energy is absorbed by electrons contained in the plasma, and atoms or molecules of the raw gas are heated due to collision of the electrons.
  • the frequency of collision of the electrons with the gas atoms and molecules is so high that a thermal equilibrium state is established, that is, the temperature of the electrons and the temperature of the atoms and molecules become nearly equal to each other.
  • the temperature of the raw gas can be readily raised to the temperature ranging from 1000° C. to 2600° C.
  • the sample to be heated 1 is heated due to contact of the heated high-temperature gas and radiation thereof.
  • the temperature of the sample to be heated 1 can be raised from the temperature, which is 70% or more of the gas temperature, to the temperature nearly equal to the gas temperature.
  • the surface of the upper electrode 2 opposed to the sample to be heated 1 is also heated and comes to have the temperature nearly equal to the temperature of the sample to be heated.
  • a percentage at which thermal energy is emitted due to radiation is high (a magnitude of radiation increases in proportion to the fourth power of temperature). Therefore, radiation from the upper electrode 2 contributes to heating of the sample to be heated.
  • the sample to be heated 1 can be heated from several hundreds of degrees to the temperature necessary to activate SiC (ranging from about 1800° C. to about 2000° C.).
  • the planar plasma is used as a heat source to heat the sample to be heated 1 . This makes it possible to uniformly heat the planar sample to be heated 1 .
  • a high-temperature portion is limited to the upper electrode 2 and the lower electrode 3 including the sample to be heated 1 .
  • the heat capacity of a region to be heated can be extremely reduced, and the temperature of the sample to be heated can be raised or lowered at a high speed.
  • the sample to be heated can be heated uniformly on a planar basis, even if the temperature thereof is raised rapidly, a risk that a break or the like may stem from non-uniformity in the temperature of the sample to be heated 1 is low. Therefore, the temperature of the sample to be heated can be raised or lowered at a high speed, and the time it takes to complete a series of heating treatment steps can be shortened. Owing to this advantage, a throughput of heating treatment can be improved. In addition, unnecessarily long stay of the sample to be heated 1 in a high-temperature atmosphere can be suppressed. Roughness on the SiC surface stemming from evaporation of Si from SiC heated at high temperature can be minimized.
  • the temperature of the sample to be heated 1 is nearly identical to the temperature of the lower electrode 3 , when the temperature of the lower electrode 3 is measured with the radiation thermometer 17 , the temperature of the sample to be heated 1 can be measured. Since the control unit 18 controls the output of the high-frequency power supply 6 by referencing the result of the measurement of the temperature of the sample to be heated 1 performed by the radiation thermometer 17 , the temperature of the sample to be heated 1 can be highly precisely controlled (1800° C. ⁇ 10° C. or less).
  • the sample to be heated 1 was heated up to 1800° C., which was necessary to activation of a SiC device succeeding ion implantation, and annealed for 1 min.
  • uniformity represented by an in-plane resistivity of the sample to be heated that is ⁇ 3% or less was attained.
  • glow discharge when sustained, heating can be achieved uniformly on a planar basis.
  • formation of plasma is localized. Uniform heating becomes hard to do.
  • the temperature of the sample to be heated becomes several thousands of degrees or more, that is, becomes unnecessarily high, and it becomes hard to control the temperature.
  • the upper limit of a range of temperatures up to which the sample to be heated is heated is preferably about 2000° C. at which glow discharge can be sustained.
  • the temperature is equal to or larger than 2000° C., a quantity of thermal electrons emitted from the electrode surface increases to the gap 4 . Eventually, a risk that a transition may be made to arc discharge gets higher.
  • a transition to arc discharge is, as mentioned previously, largely related to emission of thermal electrons deriving from a temperature rise at an electrode. Glow discharge is sustained with emission of secondary electrons from the electrode. However, when the quantity of thermal electrons exceeds that of secondary electrons, discharge becomes unstable and makes a transition to the arc discharge.
  • the quantity of thermal electrons emitted from the electrode is expressed by the Richardson-Dushman's formula (1) presented below, and determined with the temperature of the electrode material and a work function.
  • J denotes a quantity of emitted thermal electrons per unit area
  • m denotes a mass of electrons
  • k denotes a Boltzmann coefficient
  • e denotes an elementary electric charge
  • h denotes a Planck constant
  • T denotes an absolute temperature of an electrode
  • W denotes a work function of an electrode material.
  • FIG. 1B shows the relationships between the quantities of emitted thermal electrons of tungsten (W), silicon carbide (SiC), and carbon (C) deduced from the formula (1) and the temperature.
  • Tungsten is cited for reference because it is widely adopted as a thermal electron source.
  • the quantity of thermal electrons exceeds the quantity of secondary electrons, and the temperature at which a transition is made from glow discharge to arc discharge ranges from about 1800° C. to about 2100° C.
  • An electrode material employed in the present embodiment is carbon or SiC (which may be coated over carbon). Both of SiC and carbon are larger than tungsten in terms of the work function. Therefore, as long as the temperature remains unchanged, the quantity of thermal electrons is smaller than that from tungsten. Since the transition to arc discharge is determined with the quantity of thermal electrons, when carbon or SiC is adopted as the electrode material, the temperature at which the transition to arc discharge is made is higher than that observed when tungsten is adopted.
  • the temperature determined with a quantity of thermal electrons emitted from carbon which is identical to the quantity of thermal electrons emitted from tungsten at the time of a transition to arc discharge is the temperature at which a transition is made to arc discharge
  • the temperature ranges from about 2030° C. to about 2300° C. Therefore, when a carbon electrode is employed, glow discharge can be sustained at about 2000° C. or less, and heating based on glow discharge can be achieved.
  • the temperature ranges from 1900° C. to 2200° C. Heating based on glow discharge can be achieved at about 1900° C. or so. In reality, emission of thermal electrons will not overwhelm sustention of discharge at a lower limit of temperatures at which glow discharge is sustained. Therefore, glow discharge can be sustained at about 2000° C. at most irrespective of whether it is caused by a carbon electrode or SiC electrode.
  • the minimization of the radiation loss is implemented by the reflection mirrors 13 .
  • the reflection mirror 13 is formed by coating a paraboloid of revolution, which is optically polished, with gold that upgrades the reflectance of infrared light.
  • the reflection mirrors 13 are disposed to cover the upper electrode 2 and lower electrode 3 with the paraboloids of revolution with which the reflection mirrors are formed. Thus, radiant light can be reflected to the perimeters of the upper electrode 2 and lower electrode 3 that are regions to be heated. This permits the minimization of the radiation loss.
  • FIG. 1C shows a radiant spectrum emitted from an electrode having 1800° C., and the reflectance of gold (Au) having been polished to have a mirror surface.
  • Au gold
  • the reflectance thereof decreases with respect to visible light (600 nm or less), but the high reflectance (ranging from 95% to 98%) is retained with respect to the nearly entire radiant spectrum available at 1800° C.
  • the reflectance of about 97% on average is ensured. In reality, since various losses are produced, the reflectance is about 90% on average.
  • the mirror surface having the reflectance is used to form the reflection mirrors 13 shown in FIG. 1A , a loss caused by radiation can be minimized.
  • the mirror surfaces of the reflection mirrors 13 exhibit the reflectance of about 90% with respect to radiant light. However, since the reflection mirrors 13 provide multipath reflection, absorbed radiant energy causes the temperature of the reflection mirrors 13 to rise. A heat loss transferred from the upper electrode 2 and lower electrode 3 through a He gas atmosphere leads to a rise in the temperature of the reflection mirrors 13 . When the temperature of the reflection mirrors 13 becomes several hundreds of degrees or more, there arises a possibility that the sample to be heated 1 may be contaminated due to a decrease in the reflectance, which derives from deterioration of the mirror surfaces, and emission of an impurity.
  • the coolant channel 15 is formed in the metallic substrate of each of the reflection mirrors 13 so that cooling water can flow through the channel.
  • the protective quartz plates 14 are interposed between the reflection mirrors 13 and the upper electrode 2 or lower electrode 3 .
  • the protective quartz plates 14 have the capability to prevent contamination of the surfaces of the reflection mirrors 13 by an entity emitted from the upper electrode 2 and lower electrode 3 that have extremely high temperature (a sublimate of graphite or a product of an added gas), or to prevent invasion of a contaminate, which has a possibility of being mixed in the sample to be heated, 1 from any of the reflection mirrors 13 .
  • a heat treatment apparatus that can exhibit a low heat capacity and perform uniform heating can be provided.
  • an amount of gas to be introduced during heat treatment should preferably range from 10 sccm to 10000 sccm.
  • the gap 4 is set to 0.8 mm. Even when the gap 4 ranges from 0.1 mm to 2 mm, the same advantage can be exerted. Even when the gap is narrower than 0.1 mm, discharge can be formed. However, unfavorably, a high-precision facility becomes necessary to maintain the parallelism between the upper electrode 2 and lower electrode 3 , and alteration (roughness) of an electrode surface adversely affects plasma. In contrast, when the gap 4 exceeds 2 mm, degradation in the ignitability of plasma or an increase in a radiation loss occurring in the gap unfavorably poses a problem.
  • the pressure at which plasma is formed is 1 atm.
  • the same actions can be performed even when the pressure ranges from 0.1 atm. to 10 atm.
  • the heat treatment apparatus is allowed to act under a pressure lower than 0.1 atm.
  • a heat loss caused by heat transfer from the upper electrode 2 and lower electrode 3 through a gaseous atmosphere can be minimized.
  • a transition from glow discharge to arc discharge deriving from a temperature rise can be suppressed.
  • the pressure is lower than 0.1 atm., ions in the plasma enter the sample to be heated 1 while gaining relatively high energy. This is unfavorable because the sample to be heated may be damaged.
  • kinetic energy that damages a crystalline surface is 10 electronvolt (eV) or more.
  • ions When ions are accelerated to gain the kinetic energy exceeding 10 eV, they damage the sample to be heated. Therefore, it is necessary to restrict the energy of ions, which enter the sample to be heated 1 , to 10 eV or less.
  • Ions contained in plasma are accelerated with a voltage developed in an ion sheath formed on the surface of the sample to be heated 1 , and then enter the sample to be heated. The voltage in the ion sheath is developed with an energy difference between ions and electrons in a plasma bulk.
  • the thickness of the ion sheath usually ranges from several tens of micrometers to several hundreds of micrometers.
  • the mean free path of He ions is 20 ⁇ m or less in an He atmosphere of 0.1 atm. or less and 1800° C. This raises the possibility that: the number of times of collision in the ion sheath may range about 1 to 10; a percentage by which ions are accelerated with a voltage close to a voltage equivalent to the potential difference may get larger; and ions having energy which exceeds 10 eV may enter the sample to be heated.
  • He is adopted as a raw gas to be used to produce plasma.
  • a rare gas such as Ar, Xe, or Kr
  • the same advantages can be exerted.
  • He used to describe the actions is superior in ignitability of plasma at a pressure near atmospheric pressure and safety, the thermal conductivity of the gas is so high that a heat loss caused by heat transfer through a gaseous atmosphere is relatively large.
  • a gas of a large mass such as Ar is poor in the thermal conductivity. This is advantageous in terms of heat efficiency.
  • a carbon protective film that prevents surface roughness deriving from heating can be formed on the surface of the sample to be heated 1 in a stage preceding heating.
  • gaseous oxygen is added after completion of heating (in a stage in which the temperature of the sample to be heated 1 is decreased to some extent) in order to produce plasma, the carbon-series coating can be removed.
  • graphite coated with silicon carbide according to a chemical vapor deposition (CVD) method is used to form the upper electrode 2 and lower electrode 3 .
  • CVD chemical vapor deposition
  • a member produced by coating graphite with thermolytic carbon, a member produced by vitrifying a graphite surface, a compound of carbon and a high-melting point metal (tantalum (Ta), tungsten (W), or the like), or SiC (sintered compact, single crystal, or polycrystalline material) is adopted, the same advantages can be exerted.
  • the feeder lines 5 and 7 are, similarly to the upper electrode 2 and lower electrode 3 , made of graphite. Heat dissipated from the upper electrode 2 and lower electrode 3 is transferred over the feeder lines 5 and 7 and then lost. Therefore, it is necessary to limit heat transfer over the feeder lines 5 and 7 to a minimal necessary level.
  • the sectional area of the feeder lines 5 and 7 made of graphite has to be as small as possible, and the length thereof has to be as long as possible.
  • the sectional area of the feeder lines 5 and 7 is made extremely small and the length thereof is made too long, a high-frequency power loss on the feeder lines 5 and 7 increases. This invites degradation in heating efficiency for the sample to be heated 1 .
  • the sectional area of the feeder lines 5 and 7 made of graphite is set to 12 mm 2 , and the length thereof is set to 40 mm. The same advantages can be exerted as long as the sectional area ranges from 5 mm 2 to 30 mm 2 and the length ranges from 30 mm to 100 mm.
  • heat dissipation from the upper electrode 2 and lower electrode 3 which determines heating efficiency is, as mentioned above, dominated mainly by (1) radiation, (2) heat transfer through a gaseous atmosphere, and (3) heat transfer over the feeder lines 5 and 7 .
  • the primary one is (1) radiation.
  • the reflection mirrors 13 are used to suppress the radiation. Heat dissipation over the feeder lines 5 and 7 is minimized by, as mentioned above, optimizing the sectional area of the feeder lines and the length thereof.
  • the size of the container 9 becomes too large for a region to be heated. Once the distance of 30 mm or more is preserved, while the size of the container 9 is suppressed, heat dissipation due to heat transfer through a gaseous atmosphere can be suppressed. Needless to say, when Ar or the like exhibiting low thermal conductivity is adopted or a gas pressure is decreased (0.1 atm. or more), heat transfer through the gaseous atmosphere can be further suppressed.
  • 13.56 MHz is employed in bringing about electric discharge. This is because since 13.56 MHz is a frequency for industrial use, a power source is available at a low cost. In addition, a criterion for leakage of an electromagnetic wave is so low that the cost of the apparatus can be lowered. However, needless to say, heating can be achieved at any other frequency under the same principles. In particular, a frequency that is equal to or larger than 1 MHz and falls below 100 MHz is preferred for the present invention. At a frequency lower than 1 MHz, a high-frequency voltage needed to feed power necessary to heating gets higher. This is unfavorable because abnormal discharge (unstable discharge or discharge occurring other than the space between the upper electrode and lower electrode) occurs and it becomes hard to perform stable actions. A frequency exceeding 100 MHz is not preferred because the impedance in the gap between the upper electrode 2 and lower electrode 3 is low and it becomes hard to develop a voltage necessary to produce plasma.
  • the reflection mirrors 13 , upper electrode 2 , and lower electrode 3 may be made large in size, and the plural samples to be heated 1 may be disposed on the lower electrode 3 .
  • the number of samples to be heated capable of being treated at a time may be increased.
  • a high-frequency power suitable for the size of the upper electrode 2 and lower electrode 3 (nearly proportional to the area of the upper electrode 2 and lower electrode 3 ) has to be fed.
  • a large container may be used, and plural pairs of the reflection mirrors 13 , and plural pairs of the upper electrode 2 and lower electrode 3 may be disposed.
  • the number of samples to be heated capable of being treated at a time may be increased.
  • the reflection mirrors 13 are formed with paraboloids of revolution, even when planar reflection mirrors are disposed on the perimeters of the upper electrode 2 and lower electrode 3 , the same advantages are exerted.
  • FIG. 5 shows an example of a sequence of basic actions to be performed in the heat treatment apparatus shown in FIG. 1A .
  • FIG. 5 is concerned with a case where formation and removal of a surface protective film that prevents the surface roughness of a sample to be heated are performed concurrently with a series of heating treatment steps.
  • a rare gas (He) 180 that is a base material and a fluorocarbon gas 190 to be used to form the surface protective film are introduced.
  • Electrical discharge is formed with a relatively low power (500 W), and a protective film is formed on the surface of the sample to be heated (treatment time 230 ).
  • feed of the protective film formation gas 190 is ceased, and a flow rate of the rare gas (He) 180 is lowered.
  • the discharge power 210 is raised up to a power necessary to heating (2000 W). Accordingly, the temperature 220 of the sample to be heated rises to 1800° C. (treatment time 240 ). After heating treatment is completed, the flow rate of the rare gas (He) 180 is raised for the purpose of cooling, and the discharge power 210 is decreased. When the temperature decreases to some extent (600° C.), oxygen gas 200 for use in removing the protective film is added to the rare gas 180 in order to remove the protective film (treatment time 250 ).
  • the example of the series of treatment steps has been described so far. In the sequence shown in FIG. 5 , steps of forming and removing the protective film are added.
  • a temperature measurement instrument that measures the temperature of a sample to be heated (lower electrode) which is heated with plasma generated through glow discharge formed in a pair of parallel plate electrodes, and a control unit that controls the output of a high-frequency power supply using the temperature measured by the temperature measurement instrument
  • a heat treatment apparatus that can exhibit a low heat capacity and perform uniform heating can be provided.
  • reflection mirrors that minimize a radiation loss are further included, even when SiC is annealed at high temperature, there is provided the heat treatment apparatus that can exhibit a low heat capacity and perform uniform heating.
  • FIG. 2A and FIG. 2B A second embodiment will be described in conjunction with FIG. 2A and FIG. 2B . Items that have been described in relation to the first embodiment but will not be described in relation to the present embodiment will apply to the present embodiment unless the circumstances are exceptional.
  • FIG. 2A is a sectional view of an electrical discharge formation unit included in a heat treatment apparatus in accordance with the present embodiment employing plasma.
  • FIG. 2A and FIG. 2B are enlarged view of a portion equivalent to the upper electrode 2 and lower electrode 3 included in the first embodiment.
  • the upper electrode 2 is provided with a second gas introduction unit 22 , a gas diffuse layer 23 , and gas jet holes 24 .
  • the other components are identical to those of the first embodiment shown in FIG. 1A to FIG. 1C .
  • the second gas introduction unit 22 is incorporated in the feeder line 5 .
  • a gas composition in the gap 4 in which plasma is produced is altered from a gas composition in the container 9 .
  • a He gas that is superior in ignitability for electrical discharge and in stableness is introduced from the second gas introduction unit 22 , while Ar exhibiting low thermal conductivity is introduced into the container 9 .
  • the protective film when a protective film for use in preventing surface roughness is formed on the surface of the sample to be heated 1 , if the raw gas (hydrocarbon-series gas) is mixed in a rare gas and introduced by the second gas introduction unit 22 , the protective film can be uniformly formed with a small amount of raw gas.
  • the second gas introduction unit 22 is, as shown in FIG. 2B , incorporated in the feeder line 5 , radiation in the vicinity of the upper electrode 2 is made uniform.
  • a third embodiment will be described in conjunction with FIG. 3 and FIG. 4 . Items that have been described in relation to the first or second embodiment but will not be described in relation to the present embodiment can apply to the present invention unless the circumstances are exceptional.
  • FIG. 3 and FIG. 4 are diagrams showing a basic construction of a heat treatment apparatus in accordance with the third embodiment of the present invention employing plasma.
  • FIG. 3 shows a state in which heating treatment is under way
  • FIG. 4 shows a state in which the treatment is completed.
  • an up-and-down driving mechanism 25 for the reflection mirrors 13 is added to the construction of the first embodiment shown in FIG. 1A to FIG. 1C .
  • FIG. 1A to FIG. 1C As shown in FIG.
  • the upper electrode 2 and lower electrode 3 are located as close to the reflection mirrors 13 as possible (a distance of 30 mm or more making it possible to suppress an adverse effect of heat transfer through a gaseous atmosphere described in relation to the first embodiment). This is intended to suppress a loss caused by radiation.
  • the temperature has to be lowered as quickly as possible.
  • the suppression of a radiation loss by the reflection mirrors 13 hinders cooling. Therefore, after heating treatment is completed, the up-and-down mechanism 25 is, as shown in FIG. 4 , used to separate the reflection mirrors 13 from the upper electrode 2 and lower electrode 3 .
  • the effect of the reflection mirrors 13 is minimized in order to raise a temperature-drop speed.
  • the distance between the upper reflection mirror and upper electrode 2 , and the distance between the lower reflection mirror and lower electrode 3 are adjusted so that they become identical to each other (especially, during heating treatment).
  • a first advantage lies in heating efficiency. Since the gas in the gap between the upper electrode and lower electrode as well as the upper electrode and lower electrode (sample stand) should merely be heated, the heat capacity can be drastically lowered. In addition, the upper electrode 2 and lower electrode 3 including the sample to be heated 1 are covered by the reflection mirrors formed with paraboloids of revolution. Therefore, since the sample to be heated 1 can be heated in a system in which a heating loss caused by radiation is very small, high energy efficiency can be realized and high-temperature heating can be achieved.
  • a second advantage lies in heating responsiveness and uniformity. Owing to the aforesaid construction, the heat capacity of a heating unit is so small that a rapid temperature rise and a rapid temperature drop can be achieved. Since heating of a gas due to glow discharge is used as a heat source, heating can be achieved uniformly on a planar basis owing to a spread of the glow discharge. The temperature uniformity is so high that a variance in device characteristics on the surface of the sample to be heated 1 , which derives from heat treatment, can be suppressed. At the same time, a damage caused by a thermal stress deriving from a temperature difference on the surface of the sample to be headed 1 occurring when a rapid temperature rise is attained can be suppressed.
  • a third advantage lies in minimization of the number of parts wasted during heating treatment.
  • a gas that comes into contact with the sample to be heated 1 is directly heated, a region in which the temperature rises is limited to a member disposed very close to the sample to be heated 1 , and the temperature in the region is equal to or lower than the temperature of the sample to be heated 1 . Therefore, the service life of the member is long, and a region in which a part has to be replaced with a new one because of deterioration is limited.
  • a fourth advantage lies in suppression of surface roughness of the sample to be heated 1 .
  • the sample to be heated is exposed to plasma due to atmospheric-pressure glow discharge and is thus heated.
  • plasma produced from a rare gas is employed.
  • a reactive gas is added to the rare gas in the course of a temperature rise or drop, whereby formation of a protective film and removal thereof can be consistently performed during heating. Therefore, the steps of forming and removing the protective film which are performed in an apparatus other than the heat treatment apparatus become unnecessary. This leads to a reduction in a cost of fabrication.
  • the reflection mirrors 13 are used to improve the efficiency in heating the upper electrode 2 , lower electrode 3 , and sample to be heated 1 .
  • the reflection mirrors 13 are not always necessary.
  • the reflection mirrors are intended to minimize a heat loss caused by radiant emission.
  • a structure devoid of the reflection mirrors 13 can fulfill the required role.
  • the basic construction includes the upper electrode 2 and lower electrode 3 which include the sample to be heated 1 , the high-frequency power supply 6 that feeds a high-frequency power to the electrodes, an instrument that monitors the temperature of any of the sample to be heated 1 and the upper and lower electrodes (radiation thermometer 17 ), a unit that controls the power of the high-frequency power supply 6 by referencing the monitored value of the temperature, and a mechanism that controls a region to be discharged in an atmosphere of a rare gas whose pressure ranges from 0.1 atm. to 10 atm. or a gas to be added to the rare gas in order to form a protective film or remove the protective film.
  • a rare gas whose pressure ranges from 0.1 atm. to 10 atm. or a gas to be added to the rare gas in order to form a protective film or remove the protective film.
  • the present embodiment can provide the same advantages as the first embodiment can.
  • a temperature rise/drop speed can be raised.
  • a heat treatment apparatus including:
  • control unit references the temperature measured by the temperature measurement instrument, and controls the output of the high-frequency power supply so as to control the heat-treatment temperature for the sample to be heated.
  • a heat treatment apparatus including:
  • control unit references the temperature measured by the temperature measurement instrument, and controls the output of the high-frequency power supply so as to control the heat-treatment temperature for the sample to be heated.
  • the gas introduction unit includes a first gas introduction unit and a second gas introduction unit.
  • the first gas introduction unit has a gas introduction port thereof located outside a gap created in the pair of parallel plate electrodes, while the second gas introduction unit has a gas introduction port thereof located within the gap in the pair of parallel plate electrodes.
  • the first and second gas introduction units introduce a gas independently of each other.
  • as the pair of parallel plate electrodes plural pairs of electrodes are included.
  • the control unit controls the gas introduction unit so that before heat treatment is performed on the sample to be heated or while the temperature is rising, a carbon-containing molecular gas can be added to plasma stemming from discharge in order to form a protective film, which is a carbon-series coating, on the surface of the sample to be heated.
  • the control unit extends control so that oxygen can be added to the plasma, which stems from discharge, in order to remove the protective film.
  • a heat treatment apparatus including:
  • control unit controls the gas introduction unit so that a protective film can be formed on the surface of the sample to be heated, controls the output of the high-frequency power supply so that the sample to be heated can be heated with the surface thereof coated with the protective film, and controls the gas introduction unit so that the protective film can be removed.
  • the reflection members are disposed above and below the pair of parallel plate electrodes, and the heat treatment apparatus further includes a driving mechanism that drives the reflection mirrors in up-and-down directions.
  • the heat treatment apparatus as set forth in paragraph (7) further includes a driving mechanism that drives the upper and lower reflection mirrors in up-and-down directions.
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