JP2008184349A - Cylindrical member and silicon deposition apparatus using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To deposit silicon deposited on the lower part of the cylindrical member more easily than the upper part, and the whole of the cylindrical member has to be replaced when the damage on the lower part proceeds. In addition, the replacement work is not easy, the collection efficiency is lowered, and it is difficult to manufacture silicon at low cost.
A cylindrical shape in which a plurality of reaction members 6a to 6d for depositing silicon 5 by contacting a silane-based gas on the inner surface is stacked up and down, and the inner surface extends downward and is inclined. This is the member 6. The silicon 5 deposited on the upper reaction member hardly falls while contacting the lower reaction member, and falls in the vertical direction as it is, so that damage to the lower reaction member is suppressed and the life can be extended. In addition, since the reaction members 6a to 6d need to be replaced only after the damage has progressed, the cost of parts can be reduced, and the replacement can be easily performed in a short time. It can be manufactured at low cost.
[Selection] Figure 1

Description

  The present invention relates to a cylindrical member used in an apparatus for producing silicon, which is a raw material for semiconductors or solar cells, and a silicon deposition apparatus using the cylindrical member.

  Conventionally, various methods are known as methods for producing silicon as a raw material for semiconductors or solar cells, and typical examples thereof include the Siemens method and the melt precipitation method.

  The Siemens method is a method for producing silicon that is mainly used as a raw material for semiconductors. In this method, a filament, which is a base material for deposition, is placed in a reaction vessel and heated by energization, and trichlorosilane or monosilane is introduced. In this method, silicon is deposited by contacting the filament. Although this method can obtain high-purity silicon, it requires a lot of labor to collect the deposited silicon, the deposition efficiency is poor, and a large amount of power is consumed to heat the filament, which makes the silicon expensive. There was a problem. Therefore, a method for manufacturing inexpensive silicon has been desired. The melt deposition method devised in response to such a demand is said to be an epoch-making manufacturing method, and the deposition rate of silicon is one order of magnitude faster than the Siemens method, and is mainly used as a raw material for solar cells. This is a method for producing silicon.

  FIG. 7 is a conceptual diagram showing the main part of a silicon deposition apparatus using the melt deposition method proposed in Patent Document 1, wherein (a) shows a state in which silicon is deposited on the surface of a cylindrical member, b) shows a state in which molten silicon has dropped from the surface of the cylindrical member.

  The silicon deposition apparatus 20 includes a raw material gas supply port 21 for supplying a silane-based gas such as trichlorosilane or dichlorosilane, a heating means 23 for generating electromagnetic waves, and a heating system 23 heated by the heating means 23. The cylindrical member 25 that deposits silicon 24 by contacting gas, the partition member 26 that isolates the heating means 23 from the atmosphere in which the cylindrical member 25 exists without blocking electromagnetic waves, and the deposited and dropped silicon 24 are collected. The casing 22 is provided with a recovery part 27 and an exhaust gas outlet 28.

  The sealing gas is supplied from the sealing gas supply port 29 provided between the cylindrical member 25 and the source gas supply port 21 so that the silicon 24 does not precipitate on the surface other than the inner surface which is the precipitation region of the cylindrical member 25. Supply to prevent contact with silane-based gas.

  When manufacturing silicon 24 using such a silicon deposition apparatus 20, the cylindrical member 25 is heated by the heating means 23, the temperature of the inner surface of the cylindrical member 25 is lower than the melting point of the silicon 24, For example, hold at 1400 ° C. Next, a silane-based gas is supplied from the source gas supply port 21, and silicon 24 is deposited in a solid state on the heated portion of the inner surface of the cylindrical member 25. At the same time, hydrogen, argon, or the like, which is a sealing gas, is supplied from the sealing gas supply port 29 to prevent the silicon 24 from being deposited on the surface of the cylindrical member 25 other than the heated inner surface.

  After the silicon 24 is deposited, the supply of the silane gas is stopped and the supply amount of the seal gas is reduced, and then the temperature of the inner surface of the cylindrical member 25 is maintained at a temperature slightly higher than the melting point of the silicon 24, for example, 1500 ° C. Then, the silicon 24 deposited on the cylindrical member 25 is melted only at the portion in contact with the cylindrical member 25, and most of the silicon 24 is agglomerated and falls to the collection unit 27.

  The exhaust gas that has not contributed to the reaction is sequentially discharged from the exhaust gas outlet 28 and is recovered and purified to be reused as a raw material gas.

FIG. 8 is a perspective view showing a cylindrical member described in Patent Document 2. As shown in FIG. This cylindrical member 30 is formed in an octagonal pyramid shape by joining trapezoidal plate-like parts to each other with a sealing agent containing a ceramic material powder having a contact angle with the silicon melt of 45 ° or more. . Further, since it is difficult to integrally mold a large cylindrical member, a cylindrical member in which a plurality of cylindrical or hexagonal cylindrical parts are stacked by joining with a sealant has been proposed.
International Publication No. 2002/100777 Pamphlet JP-A-2005-187259

  However, when the silicon deposition apparatus 20 proposed in Patent Document 1 is used, the silicon 24 can be manufactured more efficiently and inexpensively than the apparatus using the Siemens method. However, when the deposition of the silicon 24 is repeated, The lower part of the inner surface of the cylindrical member 25 is more likely to deposit silicon 24, so damage to the lower part of the cylindrical member 25 is greater, but partial replacement is not possible, so the entire cylindrical member 25 is replaced. Had to do. Further, since the silicon deposition apparatus 20 has been increased in size in order to increase the deposition amount of silicon 24, this cylindrical member 25 has also become larger, and such a large cylindrical member 25 has a high cost, Furthermore, since the replacement work is not easy, there is a problem that the collection efficiency is lowered and the production cost of the silicon 24 is increased accordingly.

  Moreover, when the cylindrical member 30 shown in FIG. 8 described in Patent Document 2 is used in the silicon deposition apparatus 20 described in Patent Document 1, damage in the lower portion is smaller than when the cylindrical member 30 is a cylinder. However, the damage to the lower part was still great, and when the lower part was damaged, the entire tubular member 30 had to be replaced. Further, the cylindrical member in which a plurality of cylindrical and hexagonal cylindrical parts are stacked by joining with a sealing agent also has the same problem as the cylindrical member 25 of Patent Document 1.

  The present invention has been devised in order to solve the above-mentioned problems, and by extending the life by suppressing the variation in damage of the cylindrical member, partial replacement is possible even if the damage has progressed and needs to be replaced. An object of the present invention is to provide a cylindrical member capable of producing high-purity silicon efficiently and inexpensively because it can be easily performed. Another object of the present invention is to provide a silicon deposition apparatus that can efficiently and inexpensively produce high-purity silicon using this cylindrical member.

  The cylindrical member of the present invention is a cylindrical member disposed in a reaction chamber for silicon deposition provided with a heating means for generating electromagnetic waves, and the cylindrical member has an inner surface in contact with a silane-based gas. A plurality of reaction members for depositing silicon are stacked one above the other, and the reaction member is characterized in that its inner surface extends downward and is inclined.

  The cylindrical member of the present invention is characterized in that, in the above configuration, the reaction member has a truncated cone shape.

  Moreover, the cylindrical member of the present invention is characterized in that, in the above configuration, the reaction member has a truncated pyramid shape.

  In the tubular member of the present invention, in each of the above-described configurations, the reaction members adjacent to each other in the upper and lower sides are positioned such that the inner edge of the lower surface of the upper reaction member is located inside the inner edge of the upper surface of the lower reaction member It is characterized by that.

  Moreover, the cylindrical member of the present invention is characterized in that, in each of the above-described configurations, the reaction member adjacent to the upper and lower sides is such that the upper reaction member is engaged with the lower reaction member. is there.

  Moreover, the cylindrical member of the present invention is characterized in that, in each of the above configurations, the reaction member is made of a silicon nitride sintered body.

  Moreover, the cylindrical member of the present invention is characterized in that, in each of the above-described configurations, the reaction member has an inner surface polished.

  Furthermore, the silicon deposition apparatus of the present invention is characterized in that the cylindrical member of the present invention having any one of the above configurations is disposed in a reaction tank for silicon deposition having heating means for generating electromagnetic waves. Is.

  According to the cylindrical member of the present invention, this cylindrical member is disposed in a reaction vessel for silicon deposition having heating means for generating electromagnetic waves, and the cylindrical member is contacted with silane-based gas on its inner surface to form silicon. The reaction member is formed by stacking up and down, and the reaction member is inclined so that the inner surface extends downward, so that the silicon deposited on the upper reaction member is the lower reaction. Since it falls almost while falling in contact with the member and falls in the vertical direction as it is, damage to the reaction member on the lower side is suppressed, and since the damage variation is small, the life can be extended. In addition, when replacing a damaged reaction member, it is only necessary to replace the damaged reaction member, so that the part cost can be reduced.

  Further, according to the cylindrical member of the present invention, when the reaction member is in the shape of a truncated cone, the inner surface that the silane-based gas contacts is inclined downward, the horizontal section is circular, and damage is concentrated. Since there is no such part, damage variation in one reaction member is less likely to occur. Furthermore, since the individual reaction members do not require joining to a plurality of parts and can be easily molded, the molding cost can be reduced.

  Further, according to the cylindrical member of the present invention, when the reaction member is in the shape of a truncated pyramid, the reaction member can be formed by joining plate-like bodies having a simple shape. The molding cost of the member can be reduced.

  Further, according to the cylindrical member of the present invention, the reaction members adjacent in the vertical direction are melted when the inner edge of the lower surface of the upper reaction member is located inside the inner edge of the upper surface of the lower reaction member. Since the silicon in the form of droplets can be dropped in the vertical direction from the inner edge of the lower surface of the upper reaction member, it does not easily penetrate into the gap between the upper and lower reaction members, and the damage variation of the reaction members is small. Thus, the silicon collection efficiency can be hardly lowered.

  Further, according to the cylindrical member of the present invention, when the upper reaction member is engaged with the lower reaction member, the reaction members adjacent in the vertical direction can be easily replaced partially. In addition, since it is not necessary to bond the reaction members using a bonding agent, the cylindrical member is not damaged due to deterioration of the bonding agent even if silicon is deposited repeatedly.

  Further, according to the cylindrical member of the present invention, when the reaction member is made of a silicon nitride-based sintered body, the carbon component that is excellent in thermal conductivity and mechanical properties at high temperature and causes a decrease in the purity of silicon. Therefore, high-purity silicon can be efficiently deposited.

  Further, according to the cylindrical member of the present invention, when the inner surface of the reaction member is polished, the inner surface of the reaction member becomes smooth and the influence of the anchor effect is suppressed, so that the reaction member is deposited on the inner surface of the reaction member. Since silicon easily falls, the silicon collection efficiency can be increased.

  Furthermore, the silicon deposition apparatus according to the present invention has a high-purity silicon because the cylindrical member having any one of the above-described structures is disposed in a reaction tank for silicon deposition having heating means for generating electromagnetic waves. While being able to manufacture efficiently and inexpensively, it can be set as the apparatus for precipitation excellent in durability.

  Hereinafter, an example of an embodiment of a cylindrical member of the present invention and a silicon deposition apparatus using the same will be described.

  FIG. 1 shows an example of an embodiment of a cylindrical member of the present invention and a silicon deposition apparatus using the same, and FIG. 1A shows an example of an embodiment of a cylindrical member and a silicon deposition apparatus of the present invention. It is sectional drawing shown, (b) is an expanded sectional view of the S section in (a).

  A silicon deposition apparatus 1 shown in FIG. 1A includes a reaction tank 3 having a source gas supply port 2 for supplying a silane-based gas such as trichlorosilane or dichlorosilane, and a heating means 4 such as a heater for generating electromagnetic waves. The heating member 4 is separated from the cylindrical member 6 that is heated by the heating unit 4 to contact the silane-based gas on the inner surface to deposit silicon 5 and the atmosphere in which the cylindrical member 6 exists without blocking electromagnetic waves. It is comprised from the partition member 7, the collection | recovery part 8 which collect | recovers the deposited silicon 5, and the waste gas exit 9 which discharges | emits the silane type gas which did not contribute to reaction.

  Further, a seal gas is supplied from the seal gas supply port 10 to prevent contact with the silane-based gas so that the silicon 5 does not precipitate on the surface other than the inner surface which is the precipitation region of the cylindrical member 6.

  In the silicon 5 deposition method using the silicon deposition apparatus 1, the cylindrical member 6 is heated by the heating means 4 so that the temperature of the inner surface of the cylindrical member 6 is higher than the melting point of the silicon 5, for example, 1500 ° C. Next, a silane-based gas is supplied to the reaction vessel 3 from the raw material gas supply port 2, and at the same time, a seal is formed to prevent the silicon 5 from being deposited on the surface other than the inner surface of the cylindrical member 6. This is a method in which a gas such as hydrogen or argon which is a sealing gas is supplied from a gas supply port 10, and a silane-based gas is brought into contact with a heated cylindrical member 6 to deposit silicon 5.

  Note that the silane-based gas that has not contributed to the reaction is sequentially discharged as exhaust gas from the exhaust gas outlet 9, and is recovered and purified to be reused as raw material gas.

  As shown in FIG. 1B, the cylindrical member 6 of the present invention is configured such that a plurality of reaction members 6a to 6d for depositing silicon 5 by contacting a silane-based gas on the inner surface thereof are stacked one above the other. At the same time, it is important that the reaction members 6a to 6d have their inner surfaces extending downward and inclined.

  In particular, the angle between the vertical direction and the inner surfaces of the reaction members 6a to 6d is preferably 1 ° or more and 10 ° or less. In this range, for example, the silicon 5 deposited on the reaction member 6a disposed on the upper side hardly falls while contacting the inner surface along the lower reaction member 6b and falls in the vertical direction as it is. Since the silicon 5 deposited on the member 6a is less likely to come into contact with the lower reaction members 6b to 6d, variation in damage among the reaction members 6a to 6d is suppressed. Moreover, even if damage is advanced due to repeated use and the reaction members 6a to 6d need to be replaced, it is only necessary to replace any of the reaction members 6a to 6d that have progressed damage. it can. Further, when the plurality of reaction members 6a to 6d are in the shape of a truncated cone, the individual reaction members 6a to 6d do not need to be joined to a plurality of parts and can be easily formed. Can be reduced.

  The cylindrical member 6 constituted by stacking the truncated cone-shaped reaction members 6a to 6d vertically has an inner diameter of 300 to 350 mm on the uppermost surface of the reaction member 6a, for example. The inner diameter of the lower surface is 328 to 385 mm, and the height is 800 to 1000 mm.

  Next, FIG. 2 is a perspective view showing another example of the embodiment of the reaction member shown in FIG.

  The reaction member 6e shown in FIG. 2 has a truncated pyramid shape, and the inner surface extends downward and is inclined. In this case, since the plate-like body 61 having a simple shape can be joined with the joining agent 62 to form the reaction member 6e, the molding cost can be reduced. The reaction member 6e is an example of an octagonal truncated cone shape, but may be another truncated pyramid shaped reaction member such as a hexagonal truncated pyramid shape, a quadrangular truncated pyramid shape, or a dodecagonal truncated pyramid shape. As the bonding agent 62 for bonding the plate-like body 61 and the plate-like body 61, a material containing silicon nitride or sialon which is a ceramic is preferable from the viewpoint of excellent corrosion resistance to the silicon 5.

  The size of the cylindrical member 6 constituted by stacking the reaction members 6e in the shape of a truncated pyramid vertically is, for example, that the length of the diagonal line connecting the inner edges on the uppermost surface is 300 to 350 mm, and the inner edge on the lowermost surface is The length of the connecting diagonal line is 328 to 385 mm, and the height is 800 to 1000 mm.

  FIG. 3 shows another example of the embodiment of the cylindrical member and silicon deposition apparatus of the present invention. FIG. 3A shows another example of the embodiment of the cylindrical member and silicon deposition apparatus of the present invention. It is sectional drawing, (b) is an expanded sectional view of the S section in (a). In the following drawings, the same members as those in FIG. 1 are denoted by the same reference numerals.

  As shown in FIG. 3A, in the reaction members 6a to 6d constituting the cylindrical member 6 of the present invention, as shown in the enlarged sectional view of the S portion in FIG. It is preferable that the inner edge of the lower surface of the upper reaction member 6a is located inside the inner edge of the upper surface of the lower reaction member 6b. As a result, even if the silicon 5 is melted into droplets, it can be dropped in the vertical direction from the inner edge of the lower surface of the upper reaction member 6a, so that the silicon 5 is placed between the upper and lower reaction members 6a and 6b. The reaction member 6a, 6b is less likely to penetrate into the gap, and the variation in the damage of the reaction members 6a, 6b is reduced, so that the replacement frequency is reduced and the collection efficiency of the silicon 5 is hardly lowered.

  At this time, the distance between the inner edge of the lower surface of the upper reaction member 6a and the inner edge of the upper surface of the lower reaction member 6b (d shown in FIG. 3B) is preferably 0.2 to 0.4 mm. .

  4A and 4B show another example of the embodiment of the silicon deposition apparatus of the present invention. FIG. 4A is a sectional view of the silicon deposition apparatus, and FIG. 4B is an enlarged sectional view of the S part in FIG. It is.

  In the reaction members 6a to 6d constituting the cylindrical member 6 of the present invention, the upper reaction member 6a is engaged with the lower reaction member 6b, as shown in the enlarged sectional view of the S part in FIG. It is preferable. Accordingly, the reaction members 6a to 6d are easily exchanged partially, and the reaction members 6a to 6d are bonded to each other using a bonding agent to stabilize the plurality of reaction members 6a to 6d in a stacked state. Since it is not necessary to bond, even if the silicon 5 is continuously deposited, the tubular member 6 is not damaged due to deterioration of the bonding agent.

  Also in this case, as in the example shown in FIG. 3, the inner edge of the lower surface of the upper reaction member 6a adjacent to the upper and lower sides is located inside the inner edge of the upper surface of the lower reaction member 6b. Is preferred. As a result, even if the silicon 5 is melted and formed into droplets, it can be dropped in the vertical direction from the inner edge of the lower surface of the upper reaction member 6a. The reaction member 6a, 6b is less likely to penetrate into the gap, and the variation in damage of the reaction members 6a, 6b is reduced, so that the replacement frequency is reduced and the collection efficiency of the silicon 5 is hardly lowered.

  The distance between the inner edge of the lower surface of the upper reaction member 6a and the inner edge of the upper surface of the lower reaction member 6b (d shown in FIG. 4B) is also preferably 0.2 to 0.4 mm. .

  Next, FIGS. 5A and 5B are cross-sectional views showing other examples of embodiments of the cylindrical member and the silicon deposition apparatus of the present invention, respectively.

  As in the example illustrated in FIG. 5A, the reaction members 6 a to 6 d constituting the cylindrical member 6 may be stacked so that the height sequentially increases from the upper side to the lower side. With such a configuration, for example, since the upper reaction member 6a that must be removed when the reaction member 6b is replaced is lightweight, the reaction members 6a to 6d can be replaced more easily.

  Moreover, like the example shown in FIG.5 (b), you may stack reaction members 6a-6d by changing the inclination-angle of the outer surface of the cylindrical member 6, and an inner surface. With such a configuration, the lower side of each of the reaction members 6a to 6d that are easily damaged is thick, so that the life of the reaction members 6a to 6d can be further extended.

  Next, FIG. 6 is a cross-sectional view showing another example of the embodiment of the cylindrical member and silicon deposition apparatus of the present invention.

  As in the example shown in FIG. 6, the partition wall member 7 may be configured by stacking a plurality of partition wall members 7 a to 7 d as the partition wall member 7 disposed outside the cylindrical member 6. With such a configuration, even if the partition wall member 7 is partially damaged, only one of the damaged partition wall members 7a to 7d needs to be replaced. Can be reduced.

  The cylindrical member 6 is preferably made of a silicon nitride sintered body. Since the silicon nitride-based sintered body is excellent in thermal conductivity and mechanical properties at high temperatures and does not contain a carbon component that causes the purity of the silicon 5 to be reduced, the high-purity silicon 5 is efficiently precipitated. Can be collected.

During deposition of the silicon 5, since the cylindrical member 6 to be used at a high temperature of about 1500 ° C., since it preferably has high thermal conductivity and strength in this temperature range, the tubular member 6, the composition formula Si _{6 -Z Al Z O Z N 8-} Z and β- siAlON represented by (z = 0.1 to 1) and a main phase, Al, Si, RE (RE is a group 3 element of the periodic table) composition ratio of each Al RE-Al-Si-O- in which Al ₂ O ₃ is 5 to 50% by mass in terms of ₂ O ₃ , SiO ₂ and RE ₂ O ₃ , SiO ₂ is 5 to 20% by mass, and the balance is mainly RE ₂ O ₃ The grain boundary phase composed of N is included in the range of 4 to 20% by volume with respect to the sintered body composed of the main phase and the grain boundary phase, and Fe silicide particles are 0.02% relative to the sintered body in terms of Fe. It is more preferable to form a silicon nitride sintered body containing ˜3 mass%.

Composition formula _{Si 6-Z Al Z O Z} N 8-Z main phase of which represented β- SiAlON by (z = 0.1 to 1) is Al in the _{β-Si 3 N 4, O} , is N components in solid solution The main phase is composed of crystals, and the value of the solid solution amount z affects the thermal conductivity and strength of the silicon nitride sintered body. When the solid solution amount z is small, the sinterability is lowered, so the firing temperature has to be increased in an attempt to promote densification, and as a result, abnormal grain growth occurs and the strength at high temperature may be reduced. There is. On the other hand, if the solid solution amount z is large, the crystal symmetry of β-Si ₃ N ₄ is impaired and the thermal conductivity of the crystal is lowered, so that the thermal conductivity at high temperature of the silicon nitride sintered body is lowered. . As a result, since the heat dissipation characteristics of the cylindrical member 6 are lowered, if the silicon 5 is repeatedly deposited, the residual thermal stress is likely to accumulate, and the cylindrical member 6 is likely to break due to the increased residual thermal stress. From such a viewpoint, by setting the solid solution amount z to 0.1 to 1, it is possible to obtain a silicon nitride sintered body having high thermal conductivity and high strength at high temperatures. In particular, the solid solution amount z is more preferably 0.35 to 0.70.

  Here, the solid solution amount z can be calculated as follows. That is, a silicon nitride-based sintered body is pulverized to a particle size of 200 mesh or less, and a high-purity α-silicon nitride powder (E product made by Ube Industries, Ltd.) is used as a sample for correcting the diffraction angle in the powder X-ray diffraction method. -10 grade, Al content of 20 ppm or less) is added and mixed uniformly in a mortar, and the analysis range 2θ is set to 33 to 37 ° by the powder X-ray diffraction method, the scanning step width is set to 0.002 °, Cu -Measure the profile intensity with the Kα line (λ = 1.54056 mm). The angle is corrected using the maximum peak value obtained from the angle correction sample.

That is, the difference (Δ2θ ₁ ) between the average 2θ of the top 10 points of α (102) appearing every 0.002 ° of α (102) appearing near 2θ = 34.565 ° and 34.565 ° (α2θ ₁ ), and α appearing near 2θ = 35.333 ° 210), the difference (Δ2θ ₂ ) between the average 2θ of the top 10 peak intensities obtained every 0.002 ° and 35.333 ° (Δ2θ ₂ ) is obtained, and the average (Δ2θ ₁ + Δ2θ ₂ ) / 2 of the difference is taken as the corrected Δ2θ. Next, the angle obtained by correcting the average 2θ of the top 10 peak intensities obtained every 0.002 ° of β (210) appearing near 2θ = 36.055 ° by the correction Δ2θ is the peak position of β (210) of the inner cylinder 2 ( 2θ _β ). Then, the lattice constant a (Å) is calculated by substituting the peak position (2θ _β ), λ = 1.40556Å, and (hkl) = (210) into the following equation.

sin ² θ _β = λ ² (h ² + hk + k ² ) / (3a ² ) + λ ² l ² / (4c ² )
In this equation, the calculated lattice constant a (Å) and the lattice constant a (Å) −solid solution amount z described in KH Jack, J. Mater. Sci., 11 (1976) 1135-1158, FIG. From this graph, the solid solution amount z can be determined.

The grain boundary phase consists RE-Al-SiO-N, Al, Si, the component ratio of RE is _{Al 2 O 3, SiO 2,} RE 2 O 3 in terms of in _Al 2 _{O 3} is from 5 to 50 mass %, SiO ₂ is 5 to 20% by mass, and the balance is mainly RE ₂ O ₃ , and it is preferable that the content is 4 to 20% by volume with respect to the sintered body composed of the main phase and the grain boundary phase. . In the present invention, the composition ratio of the grain boundary phase is expressed with the sum of Al ₂ O ₃ , SiO ₂ , RE ₂ O ₃ and N being 100 mass%.

Here, in general, an oxide containing RE-Al-Si-O promotes densification of silicon nitride and sialon. Powder materials such as Al ₂ O ₃ , SiO ₂ , and RE ₂ O ₃ react as the temperature rises, generate a liquid phase that wets well with silicon nitride and sialon above 1400 ° C, then dissolve silicon nitride and sialon By doing so, a grain boundary phase composed of RE-Al-Si-O-N is formed.

The composition ratio of Al in the grain boundary phase affects the thermal conductivity and strength of the silicon nitride sintered body. If the composition ratio of Al is too low or too high, there is a high possibility that the composition will be deviated from the RE ₂ O ₃ —Al ₂ O ₃ —SiO ₂ -based lowest liquid layer generation composition (hereinafter referred to as “low melting point composition”). For this reason, the firing temperature must be increased, and when the firing temperature is increased, crystals in which Al, O, and N components are dissolved in β-Si ₃ N ₄ are coarsened, and the strength at high temperatures is reduced. At the same time, when the Al composition ratio is too high, the solid solution amount z tends to be larger than 1, the thermal conductivity of the silicon nitride sintered body is lowered, and the grain boundary phase is easily eroded. .

  Further, the composition ratio of Si in the grain boundary phase also affects the thermal conductivity and strength of the silicon nitride sintered body. When the composition ratio of Si is low, the possibility of deviating from the low melting point composition increases, and the strength at a high temperature decreases as in the case of Al. On the other hand, when the composition ratio of Si is high, the composition approaches a low melting point composition. For this reason, the bonding force at high temperatures between atoms constituting the grain boundary phase is weakened. Both rate and strength decrease.

From this viewpoint, Al, Si, RE (RE is a Group 3 element of the Periodic Table) Each component ratio _{Al 2 O 3, SiO 2,} RE 2 O 3 in terms of in _Al 2 _{O 3} 5 to 50 wt% , SiO ₂ is preferably 5 to 20% by mass, and the balance is mainly RE ₂ O ₃ , and this constituent ratio not only improves the sinterability but also increases the interatomic bonding force of the grain boundary phase even at high temperatures. Since it can hold | maintain, it is effective in the improvement of the heat conductivity and intensity | strength in high temperature.

  The volume ratio of the grain boundary phase to the sintered body affects the corrosion resistance and strength of the silicon nitride sintered body. If the volume ratio of the grain boundary phase is too high, the metal powder of the workpiece W tends to adhere to the grain boundary phase, and if it is too low, the strength decreases. It is preferable that the volume ratio of the grain boundary phase to the sintered body is 4 to 20% by volume. By setting the volume ratio within this range, a silicon nitride-based sintered body with less metal powder sticking and high strength is obtained. be able to.

Such a composition ratio of Al ₂ O ₃ , SiO ₂ , RE ₂ O ₃ and a volume ratio of the grain boundary phase can be obtained as follows. First, each ratio (mass%) of RE and Al in the sintered body was measured by ICP (Inductivity Coupled Plasma) spectroscopy, and this ratio (mass%) was set to RE ₂ O ₃ and Al ₂ O ₃ , respectively. Convert to the ratio (mass%). Next, the ratio of all oxygen in the sintered body was measured by an oxygen analysis method using an oxygen analyzer (TC-136 type) manufactured by LECO, and the ratio of oxygen in RE ₂ O ₃ and Al ₂ O ₃ was determined. The ratio of the remaining oxygen is subtracted and converted into the ratio (mass%) of SiO ₂ . The balance in the sintered body is regarded as Si ₃ N _4, and each ratio (mass%) is set to the respective theoretical density (Y ₂ O ₃ : 5.02 g / cm ³ , Er ₂ O ₃ : 8.64 g / cm ³ , Yb _2). O ₃ : 9.18 g / cm ³ , Lu ₂ O ₃ : 9.42 g / cm ³ , Al ₂ O ₃ : 3.98 g / cm ³ , SiO ₂ : 2.65 g / cm ³ , Si ₃ N ₄ : 3.18 g / cm ³ ) To calculate the volume ratio of the grain boundary phase.

Next, the ratio (mass%) of nitrogen (N) contained in the grain boundary phase is calculated using energy dispersive X-ray spectroscopy (EDS), and Al ₂ O ₃ , SiO ₂ , RE ₂ O ₃ and The composition ratio of the grain boundary phase is calculated with the sum of the ratios (mass%) of nitrogen (N) as 100%. However, since the composition ratio of nitrogen contained in the grain boundary phase of the silicon nitride-based sintered body used in the present invention is a very small amount and is usually 0.1% by mass or less, it will be referred to as RE ₂ O ₃ hereinafter. .

  The RE in the grain boundary phase may be a Group 3 element of the periodic table, such as Er, Yb, Lu, etc., but RE is preferably Y. This is because Y is a light element among the Group 3 elements of the periodic table, so that phonon propagation is good and effective in improving the thermal conductivity of the grain boundary phase. Further, the four-point bending strength and thermal conductivity at temperatures of 1400 to 1500 ° C. may be measured in accordance with JIS R 1604-1995 and JIS R 1611-1997, respectively.

  In addition, the Fe silicide particles in the sintered body affect the fracture toughness, thermal shock resistance, thermal conductivity, and strength of the sintered body. It is preferable to constitute a silicon nitride sintered body containing 0.02 to 3% by mass.

  Fe silicide has a large coefficient of thermal expansion and is thought to generate residual stress on β-sialon particles and grain boundary phase, and has the effect of improving the fracture toughness of the sintered body. It is also effective for improving. In addition, it acts as a wedge that prevents the sliding of β-sialon particles when grain boundary sliding, which is a form of fracture at high temperature, occurs, and has the effect of improving strength at high temperature. It is also effective for improvement. The Fe silicide acts as one of the liquid phase components during firing, and is effective in improving the sinterability. If Fe silicide particles are less than 0.02% by mass in terms of Fe with respect to the sintered body, the fracture toughness and strength at high temperatures of the sintered body cannot be sufficiently increased. In addition, since Fe silicide has a low thermal conductivity, if the Fe silicide particles exceed 3% by mass in terms of Fe with respect to the sintered body, the thermal conductivity of the sintered body decreases. The form of Fe silicide can be confirmed by powder X-ray diffraction or elemental analysis using an X-ray microanalyzer (EPMA). It can also be quantified by ICP spectroscopy.

Note that Fe silicide is interspersed as particles having a particle size of 50 μm or less, preferably 2 to 30 μm in the grain boundary phase composed of β-sialon particles or RE-Al—Si—O—N. _{and, FeSi 2, FeSi, Fe 3} Si, is preferably present in the form of _Fe 5 Si _3, it is preferable that particularly FeSi ₂ (JCPDS # 35-0822).

  Further, it is preferable that the cylindrical member 6 is polished rather than the inner surface being a ceramic skin surface or the like. If the inner surface is polished, the surface becomes smooth and the influence of the anchor effect is suppressed, so that the silicon 5 deposited on the inner surface of the cylindrical member 6 is likely to fall, so that the collection efficiency of the silicon 5 can be increased. it can.

Further, the partition member 7, similar to the tubular member 6, represented by β- SiAlON by a composition formula _{Si 6-Z Al Z O Z} N 8-Z (z = 0.1~1) and a main phase, Al, Si, RE (RE is periodic table group 3 element) composition ratio is each _{Al 2 O 3, SiO 2,} RE 2 O 3 in terms of in _Al 2 _{O 3} is 5 to 50 mass%, SiO ₂ is 5 to 20 mass %, With the balance being mainly RE ₂ O ₃ , the grain boundary phase composed of RE—Al—Si—O—N in the range of 4 to 20% by volume with respect to the sintered body composed of the main phase and the grain boundary phase. It is preferable to form a silicon nitride sintered body that contains and contains Fe silicide particles in an amount of 0.02 to 3% by mass in terms of Fe.

  A manufacturing method for obtaining such a cylindrical member 6 of the present invention will be described.

First, a silicon nitride powder in which the β conversion ratio of the silicon nitride powder is 40% or less and the solid solution amount z in the composition formula Si _6-Z Al _Z O _Z N _8-Z is 0.5 or less, and an additive Each component of Al ₂ O ₃ , SiO ₂ , RE ₂ O ₃ , and Fe ₂ O ₃ as components is wet-mixed using a barrel mill, a rotary mill, a vibration mill, a bead mill or the like, and pulverized into a slurry.

Here, the total of the powders of Al ₂ O ₃ , SiO ₂ , and RE ₂ O ₃ that are additive components is, when the total sum of the silicon nitride powder and the powder of these additive components is 100% by volume, What is necessary is just to make it 4-20 volume%.

  There are two types of silicon nitride, α-type and β-type, due to the difference in crystal structure of silicon nitride. The α type is stable at low temperatures, the β type is stable at high temperatures, and the phase transition from α type to β type occurs irreversibly at 1400 ° C or higher.

Here, the β conversion is the sum of the peak intensities of the α (102) diffraction line and the α (210) diffraction line obtained by the X-ray diffraction method, I _α , β (101) diffraction line and β ( 210) This is a value calculated by the following equation, where I _β is the sum of the peak intensities with the diffraction line.

β conversion rate = {I _β / (I _α + I _β )} × 100 (%)
The β conversion rate of the silicon nitride powder affects the strength and fracture toughness value of the silicon nitride sintered body. The reason why silicon nitride powder having a β conversion rate of 40% or less is used is that both strength and fracture toughness values can be increased. Silicon nitride-based powders with a β conversion ratio exceeding 40% become the core of grain growth in the firing step, tend to be coarse crystals with a low aspect ratio, and both strength and fracture toughness values decrease. In particular, it is preferable to use a silicon nitride-based powder having a β conversion rate of 10% or less, whereby the solid solution amount z can be made 0.1 or more.

  Further, the solid solution amount z affects the thermal conductivity of the silicon nitride sintered body, and using a powder having a solid solution amount z of 0.5 or less results in an acicular crystal structure having an aspect ratio of 5 or more after sintering. This is because both the strength and the thermal conductivity of the silicon nitride sintered body can be increased. When the solid solution amount z exceeds 0.5, the silicon nitride powder becomes the nucleus of grain growth in the firing step, and the solid solution amount z of β-sialon that becomes the main phase after sintering tends to exceed 1, and the thermal conductivity. May decrease.

  The media used for pulverizing the silicon nitride-based powder can be media composed of various sintered bodies such as silicon nitride, zirconia, and alumina. However, a material that does not easily contain impurities, or silicon nitride having the same material composition. A medium made of a sintered material is suitable.

Note that the silicon nitride powder is pulverized until the particle size (D ₉₀ ) at which the cumulative volume is 90% when the total cumulative volume of the particle size distribution curve is 100% is 3 μm or less. This is preferable from the viewpoints of improvement in cohesion and acicularization of the crystal structure. The particle size distribution obtained by grinding can be adjusted by the outer diameter of the media, the amount of the media, the viscosity of the slurry, the grinding time, and the like. In order to reduce the viscosity of the slurry, it is preferable to add a dispersant, and in order to pulverize in a short time, it is preferable to use a powder having a particle size (D ₅₀ ) of 1 μm or less with a cumulative volume of 50% in advance.

  Next, the obtained slurry is passed through a mesh having a particle size smaller than 200 mesh and then dried to obtain granules. Moreover, it is preferable for moldability to mix organic binders, such as paraffin wax, polyvinyl alcohol (PVA), and polyethyleneglycol (PEG), with respect to 100 mass% of powder at the stage of a slurry. Drying may be performed with a spray dryer, and there is no problem even if other methods are used.

  Next, the obtained granule is formed into a truncated cone-shaped body having a relative density of 45 to 60% by using a cold isostatic pressing method (CIP). If the molding pressure is in the range of 50 to 300 MPa, it is preferable from the viewpoint of improving the density of the molded body and the collapsibility of the granules. The obtained molded body is cut by a step for engaging with the lower portion if the reaction member 6a, the upper and lower portions if the reaction members 6b and 6c, and the upper portion if the reaction member 6d. And it is better to degrease in nitrogen atmosphere or vacuum atmosphere. The degreasing temperature varies depending on the type of the added organic binder, but it is preferably 900 ° C. or less, and particularly preferably 500 to 800 ° C.

Next, the molded body is placed in a firing furnace using a graphite resistance heating element used for firing a general silicon nitride shaped body and fired. In the firing furnace, a co-material containing components such as Al ₂ O ₃ , SiO ₂ , and RE ₂ O ₃ may be disposed in order to suppress volatilization of the components contained in the compact.

Further, as a method of arranging the molded body, if a method of embedding the molded body in a silicon nitride powder or a silicon carbide powder is used, it can be fired in the air in an electric furnace. When such a method is used, since the molded body is embedded in the powder, oxygen gas in the atmosphere is shut off, and the firing atmosphere is substantially a nitrogen atmosphere. About temperature, it heats up in a vacuum atmosphere from room temperature to 300-1000 degreeC, Then, nitrogen gas is introduce | transduced and nitrogen partial pressure is maintained at 50-300 kPa. At this time, since the open porosity of the compact is about 40 to 55%, the compact is sufficiently filled with nitrogen gas. In the vicinity of 1000 to 1400 ° C., additive components Al ₂ O ₃ and RE ₂ O ₃ undergo a solid phase reaction to form a liquid phase component, and β-sialon is precipitated in a temperature range of about 1400 ° C. or higher. Densification starts. β-sialon is a solution in which Al ³⁺ , N ³⁻ and O ²⁻ are substituted and dissolved in the Si ⁴⁺ position of β-Si ₃ N ₄ , and Si ₃ N ₄ -AlN—Al ₂ O ₃ —SiO ₂ type As shown in many phase diagrams (for example, KH Jack, J. Mater. Sci., 11 (1976) 1135-1158, Fig. 11), the stable region of the β-sialon phase is Si ₃ N ₄ -Al ₂ O. N ³⁻ is insufficient to stabilize the valence with respect to the _3- SiO ₂ system, and it is necessary to supply N ³⁻ from the outside. This is because the nitrogen gas filled in the molded body becomes N ^{3 −,} and the solid solution amount z of β-sialon can be lowered by keeping the nitrogen partial pressure low.

That is, in the stage until the open porosity reaches from 40 to 55% to 5%, it is necessary to set the nitrogen partial pressure as low as possible, and it is important to set it to 50 to 300 kPa. When the nitrogen partial pressure exceeds 300 kPa, substitutional solid solution of Al ³⁺ , N ³⁻ , and O ²⁻ progresses with respect to β-Si ₃ N ₄ , the solid solution amount z tends to exceed 1, and the thermal conductivity decreases. To do. When the nitrogen partial pressure is less than 50 kPa, the equilibrium nitrogen partial pressure of β-sialon is reduced, and the decomposition reaction of β-sialon proceeds to melt Si, so that a normal silicon nitride sintered body cannot be obtained. Further, when the temperature exceeds 1800 ° C., substitutional solid solution of Al ³⁺ , N ³⁻ , and O ²⁻ advances, the solid solution amount z tends to exceed 1, and the thermal conductivity decreases. When the sintering progresses and the open porosity is less than 5%, the supply amount of nitrogen gas into the silicon nitride sintered body is reduced, so the nitrogen partial pressure may exceed 300 kPa. It may be fired at a temperature of 1800 ° C. or higher. Ultimately, by proceeding densification to a relative density of 96% or more, the truncated cone-shaped reaction members 6a to 6d made of a silicon nitride-based sintered body having high strength and heat conduction at high temperatures can be obtained.

  Further, in order to obtain a truncated pyramidal reaction member 6e as shown in FIG. 2, a plate-like body 61 is formed by a plate-like silicon nitride sintered body having a simple shape by the method described above, and this plate It can be obtained by bonding the shaped bodies 61 together with a bonding agent 62.

  In order to obtain a fine crystal structure in the silicon nitride sintered body, the firing temperature may be set to 1700 ° C. or higher and lower than 1800 ° C. Further, it is desirable from the economical viewpoint that the nitrogen partial pressure is set to 150 kPa or less after the temperature is raised in a vacuum atmosphere. In order to promote further densification, a gas pressure sintering process or a hot isostatic pressing (HIP) process of 200 MPa or less may be performed when the open porosity becomes 5% or less. In this case, after promoting the sintering to an open porosity of 1% or less and a relative density of 97% or more, further 99% or more, a gas pressure sintering process or a hot isostatic pressing (HIP) process is performed. Is preferred.

In addition, the added Fe ₂ O ₃ powder reacts with β-sialon, which is the main phase, by firing to release oxygen components and produce Fe silicide particles.

  And it is preferable to grind | polish an inner surface with an internal cylinder grinder etc. with respect to several reaction member 6a-6d which comprises the cylindrical member 6 obtained with the manufacturing method mentioned above, and arithmetic mean height Ra is 0.5 micrometer. The following is more preferable. This arithmetic average height Ra can be measured according to JIS B 0601-2001. By polishing the reaction members 6a to 6d in this way, the inner surface becomes smooth and the influence of the anchor effect is suppressed, so that the silicon 5 deposited on the inner surfaces of the reaction members 6a to 6d is likely to fall. The collection efficiency can be increased.

  Finally, the reaction members 6a to 6d are stacked from the bottom in the order of the reaction members 6d, 6c, 6b, and 6a, so that the cylindrical member 6 whose inner surface extends downward and is inclined can be obtained. In this cylindrical member 6, for example, the silicon 5 deposited on the inner surface of the upper reaction member 6a hardly falls while contacting the lower reaction member 6b, and falls in the vertical direction as it is. The damage of the member 6b can be suppressed, and since the damage variation of the reaction members 6a to 6d is small, the life of the cylindrical member 6 can be extended. Further, when the reaction members 6a to 6d are replaced, it is only necessary to replace the damaged part, so that the cost of parts of the cylindrical member 6 and the silicon deposition apparatus 1 can be reduced.

  Furthermore, the silicon deposition apparatus 1 of the present invention in which the excellent cylindrical member 6 is arranged in the reaction tank 3 for silicon deposition provided with the heating means 4 for generating electromagnetic waves is composed of high-purity silicon 5 Can be manufactured efficiently and inexpensively, and a device with excellent durability can be obtained.

  Details of the embodiments of the present invention will be described below.

(Example 1)
First, the cylindrical member 6 of the present invention was produced in the following procedure. As the shape of the cylindrical member 6, the sample 1 has a plurality of reaction members 6 a to 6 d stacked up and down as shown in FIG. As shown in FIG. 3, the inner edge of the lower surface of the upper reaction member 6a is located inside the inner edge of the upper surface of the lower reaction member 6b. Sample 3 is an upper reaction as shown in FIG. The member 6a is engaged with the lower reaction member 6b.

Silicon nitride powder (average particle diameter D ₅₀ = 3 μm, Al content is 200 ppm, oxygen content is 0.9 mass%), Y ₂ O ₃ powder (average particle diameter D ₅₀ = 0.9 μm), Al ₂ O ₃ powder ( A predetermined amount of an average particle diameter D ₅₀ = 0.5 μm) and SiO ₂ powder (average particle diameter D ₅₀ = 1.9 μm) are prepared, pulverized and mixed for 72 hours using a vibration mill, and composed of a mixed powder of D ₉₀ = 1.5 μm. A slurry was prepared. Next, 5% by mass of polyvinyl alcohol (PVA) is added to 100% by mass of the mixed powder, and this is passed through a # 400 mesh to remove foreign matter. Got. And this granule was made into the molded object of each sample shape by the cold isostatic pressing method (CIP), and it cut as needed. Then, after removing polyvinyl alcohol (PVA) in a nitrogen atmosphere at 600 ° C., it is placed in a firing furnace using a graphite resistance heating element and fired at 1750 ° C. for 15 hours with the nitrogen partial pressure maintained at 110 kPa. As a result, a sintered body was obtained. As a result of measuring the porosity of this sintered body by the Archimedes method, the porosity was 2% or less. Further, it is fired again at 1800 ° C. for 5 hours in nitrogen of 300 kPa, and is made of a silicon nitride sintered body having a relative density of 97% or more. The inner diameter of the uppermost surface of the reaction member 6a is 350 mm. A cylindrical member 6 having an inner diameter of 380 mm and a height of 850 mm on the lowermost surface was obtained.

Incidentally, the tubular member 6 formed by using the silicon nitride sintered body are both represented by β- SiAlON by a composition formula _Si 5.92 _{Al 0.08} O _0.08 N _7.92 a main phase The composition ratio of Al, Si, Y is Al ₂ O ₃ , SiO ₂ , Y ₂ O ₃ conversion, respectively, Al ₂ O ₃ is 2 mass%, SiO ₂ is 15 mass%, and the balance is mainly Y ₂ O ₃ . A grain boundary phase composed of Y—Al—Si—O—N is included in a range of 10% by volume with respect to a sintered body composed of a main phase and a grain boundary phase, and Fe silicide particles are sintered in terms of Fe. It is formed from a silicon nitride based sintered body containing 0.8% by mass with respect to the bonded body.

  As a comparative example, an integrally formed cylindrical carbon cylindrical member was prepared.

  These cylindrical members 6 are arranged in the silicon deposition apparatus 1, and the cylindrical member 6 is heated by the heating means 4 so that the temperature of the inner surface of the cylindrical member 6 is a temperature equal to or higher than the melting point of the silicon 5. In order to prevent the silicon 5 from being deposited on the surface other than the inner surface of the cylindrical member 6 together with supplying the silane-based gas to the reaction vessel 3 from the source gas supply port 2. Hydrogen gas, which is a seal gas, was supplied from the seal gas supply port 10, and silicon 5 was deposited by bringing the silane-based gas into contact with the heated inner surface of the cylindrical member 6.

  As a result, in the comparative example, the melted silicon 5 falls from the lower side of the carbon cylindrical member along the inner surface of the carbon cylindrical member, so that the lower part is severely damaged. On the other hand, in the samples 1 to 3 using the cylindrical member 6 of the present invention, the silicon 5 deposited on the upper reaction member hardly falls while contacting the inner surface of the lower reaction member. Since it fell in the vertical direction, there was little damage to each reaction member 6a-6d, the dispersion | variation in damage was also small, and the lifetime was long.

  Also, in terms of cost, the comparative example shows that the lower part of the carbon tubular member is severely damaged, but the upper part was not particularly damaged, but since the partial replacement is not possible, the entire carbon tubular member is Had to be replaced. On the other hand, since it is only necessary to replace any of the damaged reaction members 6a to 6d in the samples 1 to 3 which are the cylindrical member 6 of the present invention, it can be confirmed that the component cost can be reduced. It was. Furthermore, in the comparative example, since the entire carbon tubular member has to be replaced, much time and labor are required for the replacement, but the samples 1 to 3 which are the tubular member 6 of the present invention are damaged. Since only one of the advanced reaction members 6a to 6d has to be replaced, it was possible to easily replace in a short time.

  Moreover, the carbon cylindrical member of the comparative example contained the carbon component in the deposited silicon 5, and the purity of the silicon 5 was lowered due to the material of the cylindrical member. On the other hand, samples 1 to 3, which are the cylindrical member 6 of the present invention, are made of a silicon nitride-based sintered body, so that they are excellent in thermal conductivity and mechanical properties at high temperatures and the purity of silicon 5 is lowered. Since no causative carbon component was contained, silicon 5 having high purity could be obtained.

  Moreover, the samples 1-3 of the cylindrical member 6 of this invention were produced again, and the inner surface was grind | polished. The arithmetic average height of the inner surface of the cylindrical member 6 measured according to JIS B 0601-2001 was 0.45 μm. When the cylindrical member 6 whose inner surface was polished was placed in the silicon deposition apparatus 1 and the same silicon 5 was deposited, the life was further extended with respect to the unpolished samples 1 to 3, and the operation exceeded 2000 hours. Could withstand. This is because the inner surface is polished and smooth, and the influence of the anchor effect is suppressed. Therefore, the silicon 5 deposited on the inner surfaces of the reaction members 6a to 6d is easily dropped, and thus damage is caused. This is thought to be due to further suppression.

  As described above, the silicon deposition apparatus 1 in which the cylindrical member 6 of the present invention thus excellent is arranged can manufacture the high-purity silicon 5 efficiently and inexpensively, and has an excellent durability. I was able to confirm.

An example of embodiment of the cylindrical member of this invention and the apparatus for silicon deposition is shown, (a) is sectional drawing of a cylindrical member and the apparatus for silicon deposition, (b) is an expansion of the S section in (a). It is sectional drawing. It is a perspective view which shows the other example of embodiment of the reaction member shown in FIG. The other example of embodiment of the cylindrical member of this invention and the apparatus for silicon deposition is shown, (a) is sectional drawing of a cylindrical member and the apparatus for silicon deposition, (b) is S section in (a) FIG. The other example of embodiment of the cylindrical member of this invention and the apparatus for silicon deposition is shown, (a) is sectional drawing of a cylindrical member and the apparatus for silicon deposition, (b) is S section in (a) FIG. (A) And (b) is sectional drawing which shows the other example of embodiment of the cylindrical member of this invention, and the apparatus for silicon deposition, respectively. It is sectional drawing which shows the other example of embodiment of the cylindrical member and silicon deposition apparatus of this invention. It is a conceptual diagram which shows the principal part of the conventional silicon deposition apparatus. It is a perspective view which shows the conventional cylindrical member.

Explanation of symbols

1: Silicon deposition apparatus 2: Source gas supply port 3: Reaction tank 4: Heating means 5: Silicon 6: Cylindrical members 6a, 6b, 6c, 6d, 6e: Reaction members 7: Partition members 7a, 7b, 7c, 7d: Partition member 8: Recovery part 9: Exhaust gas outlet
10: Seal gas supply port

Claims (8)

A cylindrical member disposed in a reaction chamber for silicon deposition provided with a heating means for generating electromagnetic waves, the cylindrical member having a plurality of reaction members whose inner surfaces are brought into contact with a silane-based gas to deposit silicon Are stacked in a vertical direction, and the reaction member is inclined with its inner surface extending downward. The cylindrical member according to claim 1, wherein the reaction member has a truncated cone shape. The cylindrical member according to claim 1, wherein the reaction member has a truncated pyramid shape. 4. The reaction member that is vertically adjacent to each other, wherein an inner edge of a lower surface of the upper reaction member is positioned inside an inner edge of an upper surface of the lower reaction member. The cylindrical member according to crab. The cylindrical member according to any one of claims 1 to 4, wherein the reaction member adjacent to the upper and lower sides is engaged with the reaction member on the lower side of the reaction member on the upper side. The cylindrical member according to any one of claims 1 to 5, wherein the reaction member is made of a silicon nitride sintered body. The cylindrical member according to claim 1, wherein an inner surface of the reaction member is polished. 8. A silicon deposition apparatus, wherein the cylindrical member according to claim 1 is disposed in a reaction chamber for silicon deposition provided with a heating means for generating electromagnetic waves.

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