JPH086239Y2 - Tubular site for temperature detection - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention is directed to the treatment of monosilane, silicon halides, and other metal hydrides, or silicon or silicon and other metal hydrides by thermal decomposition or hydrogen reduction reaction. It relates to improvement of a tubular site for temperature detection, which is necessary for controlling a reaction temperature of a reaction furnace in which an alloy with a metal is deposited on a substrate.

[Prior Art] In order to control the reaction temperature of vapor phase growth, a method of detecting the substrate temperature or the surface temperature of the grown crystal and feeding it back to an electric heating apparatus for the substrate has been conventionally used.

As the means for detecting the temperature, one is a method of directly measuring the temperature of the substrate portion with a thermocouple, and another is the outside of the vapor phase growth reactor through a site provided on the side wall of the reactor as in the present invention. There is a method in which the temperature of the surface of the grown crystal is measured by an infrared radiation thermometer.

Compared to thermocouples, the latter infrared radiation thermometer does not require loading on the substrate, is easy to maintain, and has a few errors because it directly measures the temperature of the grown crystal surface. Although many are adopted, if a large amount of fine particles are suspended in the meantime because of the distance from the object to be detected, an error is likely to occur in the measurement due to the influence thereof.

[Problems to be solved by the invention] When manufacturing silicon or alloys of silicon with other metals by vapor phase epitaxy, metal halide, phosphine (PH ₃ ), diborane (B ₂ H _2
When various kinds of gases such as hydrides such as ₆ ) are used as starting materials, atomized substances float in the space inside the reactor and the temperature of the growing crystal surface cannot be measured. Above all, the addition of high concentration of PH ₃ makes the above phenomenon remarkable.

[Means for Solving the Problems] The present invention has been made to solve the above problems, and in a tubular site for temperature detection for detecting temperature from outside the furnace, which is provided upright from the reactor wall, An auxiliary tube that has an outer diameter smaller than the inner diameter of the tubular site, one end of which is near the sight glass and the other end of which is near the surface of the temperature-detecting body in the furnace, is inserted into the inner wall of the tubular site through a seal member. And at any position on the inner wall of the tubular site between the sight glass and the seal member closest to the sight glass, a configuration is provided in which a gas for in-tube replacement gas is provided, reaching the surface of the grown crystal from the sight glass. By filling the space to be filled with an inert gas such as hydrogen gas, nitrogen gas or argon gas which is constantly supplied from the gas inlet, the site of atomized substances generated in the vapor phase growth reactor The infrared radiation thermometer from outside the reactor prevents
The temperature of the surface of the grown crystal can be accurately measured.

Alternatively, an inner tube having an outer diameter smaller than the inner diameter of the tubular site is fixed at one end while keeping airtightness between the inner wall surface of the tubular site and the other end positioned near the sight glass. Between the one end and the sight glass, at an arbitrary position on the inner wall of the tubular site, an inlet for the gas for pipe replacement is provided, and further an auxiliary pipe having an outer diameter smaller than the inner diameter of the tubular site,
It is inserted into the inner wall surface of the tubular site via a seal member, and one end surface is supported by a convex portion provided on the inner wall surface of the tubular site on the reactor side of the inner tube, and the other end surface is near the surface of the temperature detection object. As described above, it is possible to measure the temperature of the surface of the grown crystal with high accuracy.

Alternatively, the inner tube having an outer diameter smaller than the inner diameter of the tubular site is fixed at one end while keeping airtightness between the inner wall surface of the tubular site and the other end positioned near the sight glass, Between the section and the site glass, at an arbitrary position on the inner wall of the tubular site, an inlet for the gas for pipe replacement is provided, and an auxiliary pipe having an outer diameter smaller than the inner diameter of the tubular site is provided.
The inner wall surface of the tubular site is inserted through a seal member,
The one end face is supported by the end face of the inner tube on the reaction furnace side, and the other end face is configured to reach the vicinity of the surface of the temperature-detecting body, so that it is possible to measure the temperature of the grown crystal surface with high accuracy, similarly to the above. To do.

Furthermore, the end face of the auxiliary pipe facing the temperature-detected body side is cut obliquely or in steps to form a tip portion, and the tip portion may be located on the upstream side of the air flow on the temperature-detected body surface, It is effective to reduce the inner diameter of the auxiliary pipe toward the temperature detector side.

[Operation] According to the temperature detecting tubular site of the present invention, for example, hydrogen gas supplied from the gas inlet is sealed by the sealing member provided between the tubular site and the auxiliary pipe, or the inner pipe and the site inner wall surface. The fixed portions of and direct the flow toward the sight glass along the side surface of the auxiliary tube. Since the gas is always supplied, it fills the inside of the auxiliary tube and prevents the atomized substance from entering the tube from the growth reactor side, and it creates a space from the surface of the grown crystal to the sight glass of the tubular site. Keep it clear. Therefore, the temperature of the surface of the grown crystal can be accurately detected by the infrared radiation thermometer provided outside.

Also, if you cut the end face diagonally or in steps,
Prevents the atomized substance from trying to enter the tube due to the air flow generated on the substrate surface.

When the inner diameter of the auxiliary pipe is reduced toward the temperature detection target side, the flow velocity of the gas for pipe replacement at the tip portion is higher than that of the auxiliary pipe whose diameter is not reduced.

[Reference Example] A graphite substrate 7 of 3 × 23 × 810 mm was set in a reactor for vapor phase growth having an internal volume of 40 l equipped with the conventional tubular site 2 for temperature detection shown in FIG. Heating by direct energization, substrate surface temperature is measured by a radiation thermometer (not shown) through the tubular site, and this is hooded back to a power source to hold at 1000 ° C., where SiH ₄ , PH ₃ , G
176.4 cc / mi of carrier gas H ₂ for cC1 ₄ and Ge1 ₄ respectively
The silicon-germanium alloy was deposited on the substrate receiver through the n., 2.64 cc / min., 612 mg / min., and 71.6 cc / min.

The supply amount of the raw material was adjusted by increasing the increase amount of the surface area with the growth of the silicon-germanium alloy at the same rate.

In the reaction furnace, after the introduction of the raw material gas, a mist-like substance starts to float in a few minutes, which vortexes in the tubular site with the passage of time, and the measured value by the radiation thermometer is in the range of ± 10 ° C, Electric power supplied to the substrate is +10 of expected power
Hunting in the range of + 20% made feedback control of the substrate surface temperature impossible.

[Embodiment 1] FIG. 1 shows an embodiment of a tubular site for temperature detection according to the present invention.

A quartz auxiliary tube 3 having an inner diameter of 21 mm is provided in the temperature detecting tubular site 2 provided upright from the reactor wall 1, one end face 4 of which is near the sight glass 5 and the other end face 6 is the temperature inside the furnace. It is inserted into the inner wall of the tubular site via O-rings (sealing members) 8 and 8A so as to reach the vicinity of the surface of the base body 7 which is the detection body. Further, an inlet 9 for the gas for pipe replacement is provided on the inner wall of the tubular site between the sight glass 5 and the O-ring 8 closest to the sight glass.

In addition, when setting the products in the reactor, the O-rings 8 and 8A that remain
A part of the O-ring 8A was cut to replace the air between them.

 Other configurations are the same as those used in the reference example.

An attempt was made to deposit a silicon-germanium alloy under the same conditions as in the reference example, using the vapor phase growth reactor equipped with the tubular site according to the embodiment of the present invention shown in FIG. While performing deposition was purged auxiliary tube at 40 cc / min. For H ₂ from the inlet 9 of the pipe replacement gas tubular sites.

A mist was put in the reactor, but the quartz auxiliary tube 3 was always kept clear without any intrusion.

The substrate surface temperature was controlled at 1000 ° C ± 2 ° C, and the temperature measured by a radiation thermometer showed good agreement within a range of ± 1 ° C.

[Embodiment 2] Next, a different embodiment of the present invention shown in FIG. 2 will be described. In the description of this embodiment, the same components as those of the first embodiment of the present invention will be designated by the same reference numerals and redundant description will be omitted.

In the embodiment shown in FIG. 2, the first embodiment of the present invention is described.
The main difference is that the inner surface of the tubular site is kept airtight and fixed at one end 11 and the other end 12 reaches the sight glass 5 with a stainless steel inner tube 13 and a convex portion 14 on the inner wall of the tubular site. That is, a quartz auxiliary tube 3 is provided, which is in contact with one end surface 4 and the other end surface 6 is close to the surface of the base 7. The quartz-made auxiliary tube 3 has an O-ring (sealing member) 8, similar to the first embodiment.
It is inserted into the inner wall of the tubular site 2 via 8A. Further, the inflow port 9 for the gas for pipe replacement is provided on the inner wall of the annular site between the one end 11 of the stainless inner pipe and the sight glass 5.

In addition, in this embodiment, the on-pipe site is joined by the flange portion to form a two-stage structure.

An attempt was made to deposit a silicon-germanium alloy under the same conditions as in the reference example, using the vapor phase growth reactor equipped with the tubular site according to the embodiment of the present invention shown in FIG. During the deposition, the inside of the auxiliary pipe was purged with 40 cc / min. Of H ₂ from the inflow port 9 for the gas for pipe replacement at the tubular site.

A mist was trapped in the reactor, but the auxiliary tube was kept clear without any intrusion.

The substrate surface temperature was controlled at 1000 ° C ± 2 ° C, and the temperature measured by a radiation thermometer showed good agreement within a range of ± 1 ° C.

The structure according to the first embodiment is
There was a risk that the quartz auxiliary tube 3 and the sight glass 5 would collide with each other and be damaged. However, in the configuration according to the present embodiment, since the stainless steel inner tube 13 is fixed to the tubular site 2, such a thing is not possible. Absent.

[Embodiment 3] Another embodiment of the present invention shown in FIG. 3 will be described. In the description of this embodiment, the same components as those of the second embodiment of the present invention will be designated by the same reference numerals and duplicate description will be omitted.

In the embodiment shown in FIG. 3, the second embodiment of the present invention is described.
The main difference is that the inner wall of the tubular site of the configuration of Example 2 does not have a convex portion, and the one end 11 of the inner tube 13 made of stainless steel on the reaction furnace side and the one end face 4 of the auxiliary tube 3 made of quartz are Being directly supported.

An attempt was made to deposit a silicon-germanium alloy under the same conditions as in the reference example, using the vapor phase growth reactor equipped with the tubular site according to the embodiment of the present invention shown in FIG. During the deposition, the auxiliary pipe was diversified with 40 cc / min of H ₂ from the inflow port 9 for the gas for pipe substitution at the tubular site.

A mist was trapped in the reactor, but the auxiliary tube was kept clear without any intrusion.

The substrate surface temperature was controlled at 1000 ° C ± 2 ° C, and the temperature measured by a radiation thermometer showed good agreement within a range of ± 1 ° C.

Also according to the present embodiment, the sight glass 5 as in the second embodiment.
It is possible to prevent damage.

[Embodiment 4] Still another embodiment of the present invention shown in FIG. 4 will be described. In the description of this embodiment, the same components as those of the first embodiment of the present invention will be designated by the same reference numerals and redundant description will be omitted.

In the embodiment shown in FIG. 4, the first embodiment of the present invention is described.
The main difference is that the end surface of the quartz auxiliary tube 3A on the side of the base body 7 is obliquely cut to form a tip portion 100, and the tip portion 100 is positioned on the upstream side of the air flow flowing on the surface of the base body. It is located in.

The end surface of the auxiliary tube 3A on the side of the sight glass 5 is supported by a stopper 20 provided on the inner wall of the tubular site 2.

Using a vapor phase growth reactor having a tubular site according to an embodiment of the present invention shown in FIG. 4, an attempt was made to deposit a silicon-germanium alloy under the same conditions as in the reference example. During the deposition, the inside of the auxiliary pipe was barged with 40 cc / min. Of H ₂ from the inflow port 9 for the pipe replacement gas at the tubular site.

A mist was trapped in the reactor, but the auxiliary tube was kept clear without any intrusion.

The substrate surface temperature was controlled at 1000 ° C ± 2 ° C, and the temperature measured by a radiation thermometer showed good agreement within a range of ± 1 ° C.

According to this embodiment, the end face of the quartz auxiliary pipe 3A on the side of the substrate 7 is obliquely cut, and the side closest to the substrate is directed toward the upstream side of the air flow flowing on the substrate surface.
It is possible to prevent the entrainment of airflow into 3A and to further suppress the intrusion of atomized substances.

[Embodiment 5] Another embodiment of the present invention shown in FIG. 5 will be described. In the description of this embodiment, the same components as those in the fourth embodiment of the present invention will be designated by the same reference numerals, and the duplicated description will be omitted.

In the embodiment shown in FIG. 5, the fourth embodiment of the present invention is provided.
The main difference is that the inner diameter of the quartz auxiliary tube 3B is reduced toward the temperature detection object side.

Also, the degree of this diameter reduction should not interfere with the optical path from the substrate necessary for temperature detection.

An attempt was made to deposit a silicon-germanium alloy under the same conditions as in the reference example, using a vapor phase growth reactor equipped with a tubular site according to an embodiment of the present invention shown in FIG. While performing deposition was purged auxiliary tube at 20 cc / min. For H ₂ from the inlet 9 of the pipe replacement gas tubular sites.

A mist was trapped in the reactor, but the auxiliary tube was kept clear without any intrusion.

The substrate surface temperature was controlled at 1000 ° C ± 2 ° C, and the temperature measured by a radiation thermometer showed good agreement within a range of ± 1 ° C.

According to this embodiment, since the diameter of the quartz auxiliary pipe 3B is reduced toward the substrate 7, the inside of the auxiliary pipe can be purged with a small amount of gas.

[Advantage of the Invention] The temperature-detecting tubular site of the present invention can keep the space between the growth crystal surface and the sight glass extremely clear, so that no error occurs in the measurement.

Since it is structurally simple, it can be easily applied to conventional reactors. In addition, the gas supplied from the gas inlet is very small, and since it is sufficient to supply a part of the carrier gas, it is not necessary to provide special additional equipment.

In particular, the end face is obliquely or stepwise cut, and the part of this end face that is closest to the temperature-detecting body is located on the upstream side of the air flow, and there is little entrainment of the air flow from the end face. The effect is remarkable.

Further, the auxiliary pipe whose inner diameter is reduced toward the temperature detection target can be purged with a smaller amount of gas. Therefore, since a natural convection in the reactor is not disturbed, a homogeneous deposit layer can be obtained.

[Brief description of drawings]

FIG. 1 is a sectional view of a tubular site for temperature detection according to an embodiment of the present invention. FIG. 2 is a sectional view of a tubular site for temperature detection according to another embodiment of the present invention. FIG. 3 is a cross-sectional view of a tubular site for temperature detection according to still another embodiment of the present invention. FIG. 4 is a sectional view of a temperature detecting tubular site according to still another embodiment of the present invention. FIG. 5 is a sectional view of a tubular site for temperature detection according to another embodiment of the present invention. FIG. 6 is a sectional view of a conventional tubular site for temperature detection. 1 ... Reactor wall, 14 ... Convex part 2 ... Tubular site, 20 ... Stopper 3,3A, 3B ... Auxiliary tube, 100 ... Tip part 4 ... One end surface of auxiliary tube 5 ... Sight glass 6 ... the other end surface of the auxiliary pipe 7 ... base 8,8A ... O-ring 9 ... gas inlet 11 ... one end of the inner pipe 12 ... other end of the inner pipe 13 ... inner pipe

Claims (5)

[Scope of utility model registration request] 1. A temperature-detecting tubular site which is provided upright from a reactor wall for detecting temperature from outside the furnace, has an outer diameter smaller than the inner diameter of the tubular site, and one end face of which is near the site glass. , The other end surface reaches the vicinity of the surface of the temperature-detecting body in the furnace, the inner wall of the tubular site, the auxiliary tube inserted through a seal member, and the tubular member between the sight glass and the seal member closest to the sight glass. A tubular site for temperature detection, which is provided at an arbitrary position on the inner wall of the site and is provided with an inflow port for the gas for pipe replacement. 2. A tubular site for temperature detection, which is provided upright from the reactor wall and is for detecting temperature from the outside of the furnace, having an outer diameter shorter than the entire length of the tubular site and smaller than the inner diameter of the tubular site, An inner tube fixed at one end while keeping airtightness with the inner wall surface of the tubular site, and the other end inserted so as to reach the vicinity of the sight glass; An inlet for the gas for pipe replacement, which is provided at an arbitrary position on the inner wall of the site, and is further inserted into the inner wall surface of the tubular site via a seal member, and the inner wall surface of the tubular site closer to the reaction furnace than the inner tube. A tubular site for temperature detection, comprising: an auxiliary pipe whose one end face is supported by a convex portion provided on the other end and the other end face reaches the vicinity of the surface of the temperature detection object. 3. A tubular site for temperature detection, which is provided upright from the reactor wall and is for detecting temperature from the outside of the furnace, having an outer diameter shorter than the entire length of the tubular site and smaller than the inner diameter of the tubular site, An inner tube fixed at one end while keeping airtightness with the inner wall surface of the tubular site, and the other end inserted so as to reach the vicinity of the sight glass; An inlet for the gas for pipe replacement, which is provided at an arbitrary position on the inner wall of the site, and is further inserted into the inner wall surface of the tubular site via a seal member, and one end face of the inner pipe at the end face on the reactor side. The tubular site for temperature detection, characterized in that the tubular site for temperature detection is provided with an auxiliary pipe whose other end surface reaches the vicinity of the surface of the body to be detected. 4. An end surface of the auxiliary pipe on the temperature detection body side, which is cut obliquely or stepwise to have a tip portion,
The auxiliary tube is inserted into the inner wall of the tubular site so that the tip of the end face is closest to the temperature-detecting body on the upstream side of the air flow near the surface of the temperature-detecting body. The tubular site for temperature detection according to any one of 1 to 3. 5. The tubular site for temperature detection according to any one of claims 1 to 4, wherein the inner diameter of the auxiliary pipe is reduced toward the temperature detection target.