The present invention relates to thermal treatment equipment used in a manufacturing process in which a thermal treatment must be achieved in as short a time as possible, for example, by the process for activating thermal treatment after ion implantation of impurities into SiC.
After impurities such as phosphor or nitrogen have been ion implanted into SiC substrate, a thermal treatment at a temperature as high as 1500° C. or higher is necessary in order to generate an impurities activating carrier. For such thermal treatment, it has already been reported to use a resistive heating oven, however, such resistive heating ovens inconveniently take an unacceptably long time until a temperature rises to about 1500° C. or higher. Furthermore, a duration of approximately 30 minutes is required for an effective thermal treatment and inevitably Si evaporates from the SiC substrate surface, resulting in irregularities on the substrate surface. In addition, not only Si but also the impurities are evaporated, so the impurities ion implanted region exhibits an unacceptably high resistance value, and it is not possible to fabricate a normal SiC element. Thermal treatment using high frequency heating has also been reported, however, such method may lead to uneven temperature distribution since the substrate is heated from its peripheral zone. High-speed thermal treatment equipment and a method using an infrared lamp have also been employed. According to this method, the temperature can rise to about 1700° C. in one minute and evaporation of Si from SiC substrate surface restrained. While it is possible for this method to achieve the temperature rise in a desired short time by convergence of infrared rays for heating, application of this method is limited to thermal treatment of the SiC substrate having a size on the order of 1 cm2. In other words, this method is not suitable for mass production of SiC elements. In view of such problem encountered by the method and equipment of well known art, there is a serious need for a thermal treatment equipment so improved that even a SiC substrate having a diameter of about 2 inches or larger can be heated to a desired high temperature in a short time with a practically even temperature distribution.
Kazuo Arai and Sadafumi Yoshida: “Principle and Application of SiC element” published by Ohmsha, p. 110.
As has been described above, the thermal treatment equipment relying on the infrared lamp of prior art cannot be used for mass production of the SiC element from the SiC substrate having a diameter of several centimeters or larger. While the thermal treatment method using the high frequency oven has already been proposed, this method results in that the temperature in the peripheral zone is relatively high while the temperature in the central zone is relatively low. Therefore, the temperature distribution becomes significant and, in the SiC substrate, an area in which the impurities are adequately activated and an area in which the impurities are not adequately activated appear in the SiC substrate. Eventually, the in-plane unevenness of the electric properties of the SiC element becomes so serious that such equipment cannot be used for mass production of or for industrialization of SiC elements.
In view of the problem as has been described above, it is a principal object of the present invention to provide a thermal treatment equipment improved so that a SiC substrate having a diameter of several inches or larger can be rapidly heated to a temperature as high as about 1200° C. or higher with a high in-plane evenness by heating a peripheral zone of a substrate using high frequency induction and by heating a central zone of the sample using infrared lamps while the substrate and a stage thereof are covered with a shield plate.
In the case of heating the substrate at a high temperature by infrared lamps used with a quartz column, the conventional equipment has been accompanied also with another problem such that various impurities generated from the substrate stage may cling to the quartz column and obstruct transmission of the infrared rays. In view of this problem, it is also an object of the present invention to provide a thermal treatment equipment improved so that a quartz plate is interposed between the substrate or the stage thereof and the quartz column and thereby various impurities generated from the stage of the substrate are prevented from clinging to the quartz column.
In the case of heating by the infrared lamp, the temperature of the substrate becomes higher in the central zone than in the peripheral zone, as illustrated by
The object set forth above is achieved, according to the present invention, by thermal treatment equipment comprising a vacuum chamber allowing thermal treatment to be carried out in vacuum or various gas atmospheres, an electrically conductive sample stage provided within the vacuum chamber, and a sample placed on the sample stage. A high frequency coil surrounds the sample stage, and an infrared generator, consisting of a single or plural infrared waveguide quartz column(s), is placed above and/or below the sample. An infrared lamp and a rotary elliptical reflector both placed on one end of the infrared waveguide quartz column, and a coaxial double-wall quartz tube is placed inside the high frequency coil so that cooling water may flow between this coaxial double wall quartz tube, wherein the infrared lamp is water or air cooled by cooling water or air flowing outside the infrared lamp in order to prevent the sample from being heated by the infrared lamp.
The present invention may be implemented also in various preferred manners. In the thermal treatment equipment according to claim 1, a quartz plate is interposed between the sample and the infrared waveguide quartz column as also described in claim 2. In the thermal treatment equipment according to claim 1 or 2, the sample and the sample stage are covered with a shield plate as described in claim 3.
In the thermal treatment equipment according to any one of claims 1 through 3, the sample stage is covered with an electrically conductive shield plate provided with a gap having a dimension in a range of about 1 mm to about 30 mm as described in claim 4.
In the thermal treatment equipment according to any one of claims 1 through 4, one or both of the sample stage and the shield plate is or are made of tungsten, molybdenum or tantalum as described in claim 5.
In the thermal treatment equipment according to any one of claims 1 through 4, one or both of the sample stage and the shield plate is or are made of carbon or SiC coated carbon as described in claim 6.
In the thermal treatment equipment according to any one of claims 1 through 6, the high frequency wave has a frequency less than about 50 kHz as described in claim 7.
In the thermal treatment equipment according to any one of claims 1 through 7, further comprising a mechanism adapted to adjust a distance between one end surface of the quartz column and the sample in a range from about 0.5 mm to about 20 mm as described in claim 8.
In the thermal treatment equipment according to any one of claims 1 through 8, further comprising a sample temperature control means adapted to measure a temperature of the sample stage or the sample itself by a pyrometer or a thermocouple and thereby control the voltage or current applied to the infrared lamp or the high frequency coil as described in claim 9.
In the thermal treatment equipment according to any one of claims 1 through 9, the quartz column is arranged in a tilted posture as described in claim 10.
In the thermal treatment equipment according to any one of claims 1 through 10, wherein said equipment is programmed so that the SiC substrate is heated from a room temperature to about 1200° C. or higher in from about 10 seconds to about 5 minutes, maintained at such temperature for about 10 seconds to about 10 minutes and thereafter the SiC substrate is cooled to a temperature lower than about 1200° C. in about 10 seconds to about 30 minutes as described in claim 11.
In, the thermal treatment equipment according to claim 11, said equipment is programmed so that the SiC substrate is previously heated to a temperature lower than about 1200° C., then heated from a room temperature to about 1200° C. or higher in about 10 seconds to about 5 minutes and thereafter cooled to a temperature lower than about 1200° C. in about 10 seconds to about 30 minutes as described in claim 12.
The present invention has a unique construction as has been described above and provides an effect as follows.
The thermal treatment equipment as defined in claim 1 comprises a vacuum chamber allowing thermal treatment to be carried out in vacuum or various gas atmospheres, an electrically conductive sample stage provided within the vacuum chamber, and a sample placed on the sample stage. A high frequency coil surrounds the sample stage, and an infrared generator consisting of a single or plural infrared waveguide quartz column(s) is placed above and/or below the sample. An infrared lamp and a rotary elliptical reflector are both placed on one end of the infrared waveguide quartz column, and a coaxial double-wall quartz tube placed inside the high frequency coil so that cooling water may flow between this coaxial double wall quartz tube. The infrared lamp is water or air cooled by cooling water or air flowing outside the infrared lamp in order to prevent the sample from being heated by the infrared lamp. Such equipment allows a temperature to rise from a room temperature up to about 1800° C. as rapidly as in about 1 minute and to ensure a temperature distribution having unevenness as negligible as ±50° C. without any anxiety of equipment destruction.
The thermal treatment equipment defined in claim 2 corresponding to the equipment according to claim 1, wherein a quartz plate is interposed between the sample and the infrared waveguide quartz column wherein the quartz plate prevents any impurities from clinging to the end surface of the infrared waveguide quartz column, so the infrared irradiation can be carried out for a long period without exchanging the infrared waveguide quartz column. The quartz plate is exchanged when it is desired.
The thermal treatment equipment defined in claim 3 corresponding the equipment according to claim 1 or 2, wherein the sample and the sample stage are covered with a shield plate which allows a temperature to rise up to about 1200° C. or higher rapidly.
The thermal treatment equipment defined in claim 4 corresponding to the equipment according to any one of claims 1 through 3, wherein the sample stage is covered with an electrically conductive shield plate provided with a gap having a dimension in a range of about 1 mm to about 30 mm is effective to prevent an induction heating by the high frequency wave and to restrain a temperature rise of the coaxial double quartz tube due to a temperature rise of the electrically conductive shield plate.
The thermal treatment equipment defined in claim 5 corresponding to the equipment according to any one of claims 1 through 4, wherein one or both of the sample stage and the shield plate are made of tungsten, molybdenum or tantalum is effective to prevent the shield plate from being molten even at a high temperature and thereby prevents the shield plate from changing from its initial shape.
The thermal treatment equipment defined in claim 6 corresponding to the equipment according to any one of claims 1 through 4, wherein one or both of the sample stage and the shield plate are made of carbon or SiC coated carbon which allows the thermal treatment to be stabilized even at a high temperature.
The thermal treatment equipment defined in claim 7 corresponding to the equipment according to any one of claims 1 through 6, wherein the high frequency wave has a frequency less than about 50 kHz promotes the high frequency wave to propagate into the sample so that a zone of the sample in the vicinity of its center can be sufficiently heated so as to minimize unevenness of the temperature distribution.
The thermal treatment equipment defined in claim 8 corresponding to the equipment according to any one of claims 1 through 7, further comprising a mechanism adapted to adjust a distance between one end surface of the quartz column and the sample in a range from about 0.5 mm to about 20 mm improve a heating effect of the infrared rays.
The thermal treatment equipment defined in claim 9 corresponding to the equipment according to any one of claims 1 through 8, further comprising a sample temperature control means adapted to measure a temperature of the sample stage or the sample itself by a pyrometer or a thermocouple and control the voltage or current applied to the infrared lamp or the high frequency coil to allow outputs of the infrared lamp and the high frequency wave to be controlled and, thereby, the temperature of the substrate to be controlled.
The thermal treatment equipment defined in claim 10 corresponding to the equipment according to any one of claims 1 through 9, wherein the quartz column is tilted to allow many quartz columns to be used and, thereby, the infrared irradiation area to be enlarged.
The thermal treatment equipment defined in claim 11 corresponds to the equipment according to any one of claims 1 through 10, wherein said equipment is programmed so that the SiC substrate is heated from a room temperature to about 1200° C. or higher in about 10 seconds to about 5 minutes, then maintained at such temperature for about 10 second to about 10 minutes and thereafter the SiC substrate is cooled to a temperature lower than about 1200° C. in about 10 seconds to about 30 minutes. With such an arrangement, a resistance value of the SiC substrate ion-implanted with impurities such as phosphor, nitrogen, aluminum or boron can be adequately lowered and, at the same time, evaporation of Si from the SiC substrate leading to the undesirable surface irregularities can be prevented. In this way, a high quality SiC element can be manufactured.
The thermal treatment equipment defined in claim 12 corresponds to the equipment according to claim 11, wherein said equipment is programmed so that the SiC substrate is previously heated to a temperature lower than about 1200° C., then heated from a room temperature to about 1200° C. or higher in about 10 seconds to about 5 minutes and thereafter cooled to a temperature lower than about 1200° C. in about 10 seconds to about 30 minutes. With such an arrangement also, a resistance value of the SiC substrate ion-implanted with impurities such as phosphor, nitrogen, aluminum and boron can be adequately lowered and, at the same time, evaporation of Si from the SiC substrate leading to the undesirable surface irregularities can be prevented. In this way, high quality SiC element can be manufactured.
These and other features, objects and advantages of the present invention will become apparent upon reading the following description thereof together with reference to the accompanying drawings.
FIGS. 4(1)-4(6) are schematic views which illustrate various placements of the infrared lamps;
In the following description, structural elements are identified by the following reference numerals:
Referring to
Heat conduction from the sample stage 10 heated by infrared rays causes the temperature of sample 12, such as the SiC substrate, to rise. On the other hand, inductive heating by high frequency wave is applied to a high frequency coil 7 from a high frequency oscillator and heats by induction the sample stage 10, thereby causing the temperature of sample 12 to rise through thermal conduction. In the case of the sample 12 which is electrically conductive, the sample 12 itself also is heated by an inductive heating effect by high frequency RF energy. A shield plate 11 is provided in order to restrain heat dissipation. If this shield plate 11 is made of electrically conductive material, the temperature of shield plate 11 itself would rise similarly to the sample stage 10 and heat the members surrounding the sample stage 10, such as the quartz tube 6 for cooling water, eventually leading to destruction by melting or fissure. To avoid such an undesirable result, shield plate 11 is made similarly to the sample stage 10 of a high melting point metallic material, such as tungsten, molybdenum or tantalum or high purity carbon or SiC coated carbon. A gap 20, as illustrated in
To maximize an effect of infrared irradiation, a raising and lowering mechanism 9 vertically moves the infrared waveguide quartz column 3 so that the temperature may rise as rapidly as possible and the temperature may be distributed as evenly as possible. If the end surface 3a of the infrared waveguide quartz column 3 smears, transmission of the infrared rays as well as rise of the temperature will be obstructed. To solve this problem, a quartz plate 13 is placed on the sample stage 10 and thereby prevents any impurities coming from the sample stage 10 to contaminate the end surface 3a of the infrared waveguide quartz column 3. Taking into account the fact that the thermal treatment is carried out in various atmospheres, for example, vacuum, argon, nitrogen, helium or hydrogen, the components of the equipment directly serving for the thermal treatment are arranged within a vacuum chamber 4 which is provided with a vacuum pumping exhaust port 8 communicating with a vacuum pump and a gas inlet port 16.
Outside the shield plate 11, the coaxial double-walled cylindrical quartz tube 6 and cooling water tube 5 are provided to prevent the temperature in the vicinity of the sample stage 10 from rising excessively and destroying the equipment. The temperature of the sample can be measured by a thermocouple and an infrared temperature sensor, and the temperature can be controlled. There is provided a temperature sensor pickup port 14 for a lead wire of the thermocouple and a temperature sensor port 15 for the infrared temperature sensor. A temperature control circuit 23 is coupled to each of the quartz lamps 1 to the temperature sensors and to the RF coils 7 to control the temperature profile to which the sample is exposed, as shown, for example, in
In the case of heating by the infrared lamps alone during less than 30 sec (
While the SiC substrate has been described and illustrated as an example of the sample, the sample is not limited to the SiC.
It will become apparent to those skilled in the art that various modifications to the preferred embodiment of the invention as described herein can be made without departing from the spirit or scope of the invention as defined by the appended claims.
Number | Date | Country | Kind |
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2004-47295 | Feb 2004 | JP | national |