Vacuum reaction chamber and low-pressure chemical vapor deposition equipment
By setting up silicon carbide lining and simplified disassembly structure in the furnace tube of the vacuum reaction room, the problem of frequent maintenance and cost of maintenance caused by the concentration of the existing vacuum reaction room has been solved. Effect of production cost.
Patent Information
- Application Number
- CN202420995704.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-09
- Publication Date
- 2025-01-28
- Estimated Expiration
- 2034-05-09
AI Technical Summary
The inner wall of the quartz tube in the existing vacuum reaction chamber is concentrated due to the deposition of the polycrystalline silicon film and temperature changes, which is prone to film peeling and cracking of the quartz tube, resulting in frequent maintenance and high cost.
The use of silicon carbide lining is replaced by the inner wall of the traditional quartz tube. The silicon carbide lining has better antiplication performance, reducing the risk of cracking caused by stress concentration. Silicon carbide lining process of disassembly and cleaning.
The maintenance cycle was extended, the maintenance efficiency was improved, the stop time was reduced, the production cost was reduced, and the production efficiency was improved.
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Figure CN222411810U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of low-pressure chemical vapor deposition equipment, in particular to a vacuum reaction chamber and low-pressure chemical vapor deposition equipment. Background Art
[0002] Low-pressure chemical vapor deposition equipment is a process for depositing thin films on silicon substrates in the photovoltaic industry by chemically reacting mixed gases under low pressure and high temperature conditions to generate solid reactants and deposit them on the surface of silicon wafers to form thin films. The silicon substrate is placed in the reaction chamber, and one or more gases are introduced by reducing the pressure. These gases react in the gas phase on the surface of the silicon substrate or near the surface and are deposited on the silicon substrate to form a deposited film.
[0003] Since the reaction gas exists in the entire reaction chamber, while the reaction product grows on the silicon substrate, the gas may also react on the inner wall of the furnace tube, and the reaction product will be deposited on the inner wall of the furnace tube to form a polycrystalline silicon film. Most of the existing vacuum reaction chambers are single-layer quartz tubes. When the polycrystalline silicon film deposited on the inner wall of the quartz tube reaches a certain thickness, the film will peel off due to the difference in expansion coefficient between the polycrystalline silicon film and the quartz tube. If there is a temperature fluctuation such as power failure or cooling maintenance, a large stress concentration will occur, causing the quartz tube to crack; not only affecting the process quality, but also affecting the service life of the quartz tube. In order to solve the above technical problems, the solutions in the prior art are: first, the quartz tube is disassembled and cleaned many times, the steps are cumbersome and time-consuming; due to the hard and brittle characteristics of the quartz tube itself, the quartz tube may be broken and damaged during the disassembly and cleaning process, so each disassembly and cleaning requires a lot of inspection work, which is risky and has a short maintenance cycle. Second, the quartz tube is replaced regularly, and it is replaced before the quartz tube is damaged, so as to ensure the stable operation of the equipment at the cost of certain material and labor costs. The above two solutions have had a certain impact on production efficiency and increased production costs.
[0004] Therefore, it is urgent to develop a vacuum reaction chamber and a low-pressure chemical vapor deposition device to improve the above technical problems. Utility Model Content
[0005] The utility model aims to provide a vacuum reaction chamber and a low-pressure chemical vapor deposition device, wherein the vacuum reaction chamber can extend the maintenance cycle, improve the maintenance efficiency, reduce the downtime, improve the production efficiency, and reduce the production cost.
[0006] To achieve this purpose, the utility model adopts the following technical solutions:
[0007] A vacuum reaction chamber comprising:
[0008] A furnace tube, both ends of which are arranged to be openings, one of which is closed by an end cover, and the other is closed by a furnace door, so that the inner cavity of the furnace tube forms a reaction chamber; a silicon carbide lining is arranged in the furnace tube, and the inner wall of the silicon carbide lining forms the inner wall of the reaction chamber;
[0009] The heating furnace body is arranged outside the furnace tube and is used for heating the reaction chamber.
[0010] As an optional solution for the vacuum reaction chamber, a plurality of silicon carbide liners are provided, and the plurality of silicon carbide liners are arranged in sequence along the length direction of the furnace tube, and the inner walls of the plurality of silicon carbide liners are spliced to form the inner wall of the reaction chamber.
[0011] As an optional solution of the vacuum reaction chamber, the furnace tube further includes an outer furnace tube, the outer furnace tube is sleeved outside the silicon carbide lining, and the silicon carbide lining is fixed to the outer furnace tube through a support.
[0012] As an optional solution for the vacuum reaction chamber, an arc-shaped positioning groove is provided on the inner wall of the outer tube of the furnace, and the support member is arranged in an arc shape, with one end of the arc-shaped support member arranged in the arc-shaped positioning groove and the other end abutting against the silicon carbide lining.
[0013] As an optional solution for the vacuum reaction chamber, one arc-shaped support member is provided corresponding to one silicon carbide liner; or, two arc-shaped support members are provided corresponding to one silicon carbide liner, and the two arc-shaped support members are provided opposite to each other.
[0014] As an optional solution of the vacuum reaction chamber, the support member is a silicon carbide support member or a quartz support member;
[0015] And / or, the furnace outer tube is a quartz tube.
[0016] As an optional solution of the vacuum reaction chamber, the vacuum reaction chamber further includes a flange assembly and a sealing assembly, wherein two flange assemblies are provided, and the two ends of the heating furnace body are respectively connected to the two ends of the furnace tube through one flange assembly in a one-to-one correspondence, and the end cover or the furnace door is connected to the end of the flange assembly away from the furnace tube;
[0017] The sealing assembly comprises a circumferential sealing member and an end face sealing member. The circumferential sealing member is arranged between the outer wall of the furnace tube and the flange assembly, and the end face sealing member is arranged between the flange assembly and the end of the furnace tube.
[0018] As an optional solution of the vacuum reaction chamber, the flange assembly includes an annular flange and an end face flange, the annular flange is sleeved outside the furnace tube, the end face flange is sleeved at the end of the furnace tube, one end of the annular flange is connected to the heating furnace body, and the other end is abutted against the end face flange;
[0019] The circumferential seal is arranged between the annular flange and the outer wall of the furnace tube, and between the end face flange and the outer wall of the furnace tube, and the end face seal is arranged between the end face flange and the end of the furnace tube.
[0020] As an optional solution of the vacuum reaction chamber, a first cooling cavity is provided in the annular flange, and the first cooling cavity is used to cool the circumferential seal between the annular flange and the outer wall of the furnace tube; a second cooling cavity is provided in the end face flange, and the second cooling cavity is used to cool the circumferential seal between the end face flange and the outer wall of the furnace tube, and the end face seal between the end face flange and the end of the furnace tube;
[0021] The volume of the second cooling chamber is greater than that of the first cooling chamber.
[0022] A low-pressure chemical vapor deposition device comprises a vacuum reaction chamber as described in any of the above schemes.
[0023] Beneficial effects of the utility model:
[0024] The vacuum reaction chamber provided by the utility model is formed by setting both ends of the furnace tube as openings, one of which is closed by an end cover, and the other opening is closed by a furnace door, so that the inner cavity of the furnace tube forms a reaction chamber. A heating furnace body is arranged outside the furnace tube for heating the reaction chamber, and a silicon carbide lining is arranged in the furnace tube, and the inner wall of the silicon carbide lining forms the inner wall of the reaction chamber. The thin film produced by the chemical reaction in the reaction chamber is deposited on the silicon carbide lining. Since silicon carbide has better stress resistance, the probability of cracking of the silicon carbide lining due to stress concentration can be reduced, thereby reducing the frequency of disassembly and cleaning and extending the maintenance cycle. At the same time, both ends of the furnace tube are set as openings, one opening is closed by an end cover, and the other opening is closed by a furnace door. When disassembling and cleaning the silicon carbide lining, it is only necessary to open the furnace door and take the silicon carbide lining out of the furnace tube, which is convenient for disassembly and assembly, improves maintenance efficiency, reduces downtime, and thus improves production efficiency; reduces the cost of replacing furnace tubes. The vacuum reaction chamber provided by the utility model can not only ensure the process quality in the vacuum reaction chamber, but also prolong the maintenance cycle, improve the maintenance efficiency, reduce the maintenance cost, and improve the production efficiency.
[0025] The low-pressure chemical vapor deposition equipment provided by the utility model comprises the above-mentioned vacuum reaction chamber. The low-pressure chemical vapor deposition equipment can not only ensure the process quality in the vacuum reaction chamber, but also improve the maintenance efficiency, reduce the maintenance cost, and improve the production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0026] Figure 1 It is a cross-sectional view of a vacuum reaction chamber provided in a specific embodiment of the utility model;
[0027] Figure 2 yes Figure 1 A partial enlarged view of point Ⅰ in the middle;
[0028] Figure 3 yes Figure 1 A partial enlarged view of point II in the middle.
[0029] In the figure:
[0030] 100, air intake pipe; 200, air exhaust pipe; 300, thermocouple;
[0031] 1. furnace tube; 11. silicon carbide lining; 12. quartz tube; 121. arc-shaped positioning groove; 122. support member;
[0032] 2. Heating the furnace body;
[0033] 3. End cap;
[0034] 4. Flange assembly; 41. annular flange; 411. first cooling cavity; 42. end face flange; 421. second cooling cavity;
[0035] 5. Sealing assembly; 51. O-ring; 52. Sealing gasket. DETAILED DESCRIPTION
[0036] In order to make the technical problems solved by the present invention, the technical solutions adopted and the technical effects achieved more clearly, the technical solutions of the present invention are further explained below with reference to the accompanying drawings and through specific implementation methods.
[0037] In the description of the present invention, unless otherwise clearly specified and limited, the terms "connected", "connected", and "fixed" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0038] like Figure 1As shown, this embodiment provides a low-pressure chemical vapor deposition device, including a vacuum reaction chamber, an air inlet pipe 100, an air extraction pipe 200 and a thermocouple 300. The air inlet pipe 100 and the air extraction pipe 200 are both connected to the reaction chamber in the vacuum reaction chamber. The air inlet pipe 100 supplies gas into the reaction chamber, and the air extraction pipe 200 is used to extract the gas after the reaction in the reaction chamber is completed. The thermocouple 300 is arranged in the reaction chamber to detect the temperature in the reaction chamber so that the temperature in the reaction chamber reaches the reaction temperature to ensure the process quality.
[0039] This embodiment also provides a vacuum reaction chamber, which is applied to the above-mentioned low-pressure chemical vapor deposition equipment to achieve the purpose of not only ensuring the process quality in the vacuum reaction chamber, but also improving maintenance efficiency, reducing maintenance costs, and improving production efficiency.
[0040] like Figure 1-Figure 3 As shown, the vacuum reaction chamber provided in this embodiment includes a furnace tube 1 and a heating furnace body 2. Both ends of the furnace tube 1 are set to be openings, one of which is closed by an end cover 3, and the other opening is closed by a furnace door, so that the inner cavity of the furnace tube 1 forms a reaction chamber. The crystal boat is used to carry the silicon substrate. The crystal boat can be pushed into the furnace tube 1 through the furnace door so that the silicon substrate deposits a thin film in the reaction chamber; after the reaction is completed, the crystal boat is pulled out of the furnace tube 1 to take out the silicon substrate after the film is deposited. The heating furnace body 2 is arranged outside the furnace tube 1 and is used to heat the reaction chamber. The vacuum reaction chamber also includes a flange assembly 4 and a sealing assembly 5. Two flange assemblies 4 are provided. The two ends of the heating furnace body 2 are connected to the two ends of the furnace tube 1 one by one through a flange assembly 4, and the end cover 3 or the furnace door is connected to the end of the flange assembly 4 away from the furnace tube 1. The flange assembly 4 is fixedly connected by fastening screws. The sealing assembly 5 includes a circumferential seal and an end face seal. The circumferential seal is arranged between the outer wall of the furnace tube 1 and the flange assembly 4, and the end face seal is arranged between the flange assembly 4 and the end of the furnace tube 1. The furnace tube 1 is fixed by press-fitting through the circumferential seal, and the furnace tube 1 is radially positioned; the furnace tube 1 is axially positioned through the end face seal, and the sealing of the reaction chamber is ensured at the same time.
[0041] When the chemical reaction is carried out in the reaction chamber, the reaction products not only grow on the silicon substrate, but also deposit on the inner wall of the furnace tube 1 to form a polysilicon film. In order to ensure the process quality, the polysilicon film on the inner wall of the furnace tube 1 needs to be cleaned and maintained.
[0042] In order to improve maintenance efficiency and reduce maintenance costs, a silicon carbide lining 11 is provided in the furnace tube 1, and the inner wall of the silicon carbide lining 11 forms the inner wall of the reaction chamber. The thin film produced by the chemical reaction in the reaction chamber is deposited on the silicon carbide lining 11. Since silicon carbide has better stress resistance, the probability of cracking of the silicon carbide lining 11 due to stress concentration can be reduced, thereby reducing the frequency of disassembly and cleaning and extending the maintenance cycle. In addition, both ends of the furnace tube 1 are set to be openings. When disassembling and cleaning the silicon carbide lining 11, it is only necessary to open the furnace door and take the silicon carbide lining 11 out of the furnace tube 1, which is convenient for disassembly and assembly, improves maintenance efficiency, reduces downtime, and thus improves production efficiency; reduces the cost of replacing the furnace tube 1. The vacuum reaction chamber can not only ensure the process quality in the vacuum reaction chamber; but also extend the maintenance cycle, improve maintenance efficiency, reduce maintenance costs, and improve production efficiency.
[0043] Specifically, a plurality of silicon carbide liners 11 are provided, and the plurality of silicon carbide liners 11 are sequentially arranged along the length direction of the furnace tube 1, and the inner walls of the plurality of silicon carbide liners 11 are spliced to form the inner wall of the reaction chamber. That is, a plurality of silicon carbide liners 11 are spliced to form the furnace inner tube, and the furnace inner tube is arranged in sections, which is easier to disassemble and assemble during maintenance, further improving the maintenance efficiency. In the present embodiment, four silicon carbide liners 11 are provided, and the four silicon carbide liners 11 are sequentially spliced to form the furnace inner tube, and the space formed by each silicon carbide liner 11 represents a temperature zone of the reaction chamber. Of course, in other embodiments, the silicon carbide liners 11 are not limited to four, and the specific number can be specifically designed according to the length of the furnace tube 1.
[0044] The furnace tube 1 also includes an outer furnace tube, which is sleeved outside the silicon carbide lining 11, and the silicon carbide lining 11 is fixed to the outer furnace tube through a support member 122. The two ends of the furnace tube are axially positioned by two flange assemblies 4. At the same time, an arc-shaped positioning groove 121 is opened on the inner wall of the outer furnace tube, and the support member 122 is arranged in an arc shape. One end of the arc-shaped support member 122 is arranged in the arc-shaped positioning groove 121, and the other end is abutted against the silicon carbide lining 11. The silicon carbide lining 11 is supported by the arc-shaped support member 122, and the inner furnace tube is radially positioned to prevent the inner furnace tube from moving in the radial direction. At the same time, when the support member 122 is produced, the height of the support member 122 is adjusted according to the diameter of the silicon carbide lining 11, so that the silicon carbide lining 11 is coaxially arranged with the furnace tube 1, and the arc-shaped support member 122 does not affect the disassembly and assembly of the silicon carbide lining 11, further improving the maintenance efficiency.
[0045] In addition, the furnace tube 1 is a double-layer tube, the silicon carbide lining 11 is used as the furnace inner tube, and the furnace outer tube is vacuum sealed. The furnace outer tube is a quartz tube 12. If the silicon carbide lining 11 is damaged during the reaction, there is no need to immediately stop the machine for maintenance. The inner cavity of the quartz tube 12 can also be used as a reaction chamber to continue the reaction.
[0046] The fewer the number of supports 122, the easier it is to disassemble and assemble the silicon carbide liner 11 during maintenance. In the present embodiment, the vacuum reaction chamber is placed horizontally, and one arc-shaped support member 122 is provided for each silicon carbide liner 11. When the furnace tube 1 is placed horizontally, only one arc-shaped support member 122 needs to be provided at the bottom of the silicon carbide liner 11 to support the weight of the silicon carbide liner 11. In other embodiments, when the vacuum reaction chamber is placed vertically, two arc-shaped supports 122 are provided for each silicon carbide liner 11, and the two arc-shaped supports 122 are arranged opposite to each other. The silicon carbide liner 11 is supported by two arc-shaped supports 122, so that the silicon carbide liner 11 is coaxially arranged with the furnace tube 1.
[0047] Furthermore, the support member 122 is a silicon carbide support member or a quartz support member. The silicon carbide support member and the quartz support member have excellent thermal conductivity and will not affect the heat transfer from the heating furnace body 2 to the reaction chamber.
[0048] Specifically, Figure 3 As shown, the flange assembly 4 includes an annular flange 41 and an end face flange 42. The annular flange 41 is sleeved outside the furnace tube 1, and the end face flange 42 is sleeved at the end of the furnace tube 1. One end of the annular flange 41 is connected to the heating furnace body 2, and the other end is abutted against the end face flange 42. In this embodiment, the length of the heating furnace body 2 is less than the length of the furnace tube 1. The flange assembly 4 includes two annular flanges 41 and an end face flange 42, one of the annular flanges 41 is fixedly connected to the heating furnace body 2 by fastening screws, and the other annular flange 41 is arranged between the end face flange 42 and the annular flange 41. A countersunk hole is provided at one end of the end face flange 42 close to the annular flange 41. The end of the furnace tube 1 is placed in the countersunk hole and abuts against the bottom of the countersunk hole. The furnace tube is axially positioned by the bottom of the countersunk holes of the two flange assemblies 4.
[0049] The circumferential seal is arranged between the annular flange 41 and the outer wall of the furnace tube 1, and between the end face flange 42 and the outer wall of the furnace tube 1, and the end face seal is arranged between the end face flange 42 and the end of the furnace tube 1. A circumferential seal is arranged between the two annular flanges 41 and the outer wall of the furnace outer tube, and the circumferential seal is arranged as an O-shaped sealing ring 51. A first sealing groove is arranged on the annular flange 41, and the O-shaped sealing ring 51 is arranged in the first sealing groove. A second sealing groove is arranged on the end face flange 42 corresponding to the end of the furnace outer tube and the end of the furnace inner tube, and the end face seal is a sealing gasket 52. A sealing gasket 52 is arranged in each second sealing groove. The two ends of the furnace inner tube are axially positioned by the two sealing gaskets 52, and the sealing gasket 52 also plays the role of sealing the reaction chamber. In this embodiment, an O-ring 51 is also provided between the end cover 3 and the end face flange 42. A third sealing groove is provided on the side of the end cover 3 close to the end face flange 42, and the O-ring 51 is provided in the third sealing groove. The cross section of the third sealing groove is provided as a trapezoidal cross section, so that the opening of the third sealing groove is a constricted opening to prevent the O-ring 51 from falling out.
[0050] Furthermore, in order to prevent the sealing assembly 5 from failing due to high temperature, affecting the stability of the silicon carbide liner 11 and the sealing of the reaction chamber, a first cooling chamber 411 is provided in the annular flange 41, and the first cooling chamber 411 is used to cool the circumferential seal between the annular flange 41 and the outer wall of the furnace tube 1; a second cooling chamber 421 is provided in the end face flange 42, and the second cooling chamber 421 is used to cool the circumferential seal between the end face flange 42 and the outer wall of the furnace tube 1, and the end face seal between the end face flange 42 and the end of the furnace tube 1. By passing cooling water into the first cooling chamber 411 and the second cooling chamber 421, the heat of the circumferential seal and the end face seal is dissipated.
[0051] Since the silicon carbide liner 11 and the sealing assembly 5 are added to the furnace tube 1, higher requirements are placed on the heating and heat dissipation capabilities of the vacuum reaction chamber, and it is necessary to increase the heating efficiency of the heating furnace body 2, and increase the volume of the cooling cavity inside the flange assembly 4 to increase the cooling water flow. Furthermore, since the end face flange 42 needs to dissipate heat for a circumferential seal and two end face seals, the volume of the second cooling cavity 421 is set to be larger than the volume of the first cooling cavity 411, so as to increase the cooling water flow in the end face flange 42 and improve the cooling efficiency.
[0052] The above contents are only preferred embodiments of the present invention. For ordinary technicians in this field, according to the concept of the present invention, there will be changes in the specific implementation methods and application scopes. The contents of this specification should not be understood as limiting the present invention.
Claims
1. A vacuum reaction chamber, characterized in that: include: A furnace tube (1), both ends of the furnace tube (1) are arranged to be openings, one of the openings is closed by an end cover (3), and the other opening is closed by a furnace door, so that the inner cavity of the furnace tube (1) forms a reaction chamber; a silicon carbide lining (11) is arranged in the furnace tube (1), and the inner wall of the silicon carbide lining (11) forms the inner wall of the reaction chamber; A heating furnace body (2) is arranged outside the furnace tube (1) and is used for heating the reaction chamber.
2. The vacuum reaction chamber according to claim 1, characterized in that: A plurality of the silicon carbide liners (11) are provided, and the plurality of the silicon carbide liners (11) are arranged in sequence along the length direction of the furnace tube (1), and the inner walls of the plurality of the silicon carbide liners (11) are spliced to form the inner wall of the reaction chamber.
3. The vacuum reaction chamber according to claim 2, characterized in that: The furnace tube (1) further comprises an outer furnace tube, the outer furnace tube being sleeved outside the silicon carbide lining (11), and the silicon carbide lining (11) being fixed to the outer furnace tube via a support member (122).
4. The vacuum reaction chamber according to claim 3, characterized in that: An arc-shaped positioning groove (121) is provided on the inner wall of the furnace outer tube, and the support member (122) is arranged in an arc shape, with one end of the arc-shaped support member (122) being arranged in the arc-shaped positioning groove (121) and the other end being in contact with the silicon carbide liner (11).
5. The vacuum reaction chamber according to claim 4, characterized in that: One of the silicon carbide linings (11) is provided with one arc-shaped support member (122); or, one of the silicon carbide linings (11) is provided with two arc-shaped support members (122), and the two arc-shaped support members (122) are arranged opposite to each other.
6. The vacuum reaction chamber according to claim 3, characterized in that: The support member (122) is a silicon carbide support member or a quartz support member; And / or, the furnace outer tube is a quartz tube (12).
7. The vacuum reaction chamber according to any one of claims 1 to 6, characterized in that: The vacuum reaction chamber further comprises a flange assembly (4) and a sealing assembly (5), wherein two flange assemblies (4) are provided, and the two ends of the heating furnace body (2) are respectively connected to the two ends of the furnace tube (1) in a one-to-one correspondence through one of the flange assemblies (4), and the end cover (3) or the furnace door is connected to the end of the flange assembly (4) away from the furnace tube (1); The sealing assembly (5) comprises a circumferential seal and an end face seal, wherein the circumferential seal is arranged between the outer wall of the furnace tube (1) and the flange assembly (4), and the end face seal is arranged between the flange assembly (4) and the end of the furnace tube (1).
8. The vacuum reaction chamber according to claim 7, characterized in that: The flange assembly (4) comprises an annular flange (41) and an end face flange (42); the annular flange (41) is sleeved on the outside of the furnace tube (1); the end face flange (42) is sleeved on the end of the furnace tube (1); one end of the annular flange (41) is connected to the heating furnace body (2), and the other end is in contact with the end face flange (42); The circumferential seal is arranged between the annular flange (41) and the outer wall of the furnace tube (1), and between the end face flange (42) and the outer wall of the furnace tube (1), and the end face seal is arranged between the end face flange (42) and the end of the furnace tube (1).
9. The vacuum reaction chamber according to claim 8, characterized in that: A first cooling cavity (411) is provided in the annular flange (41), and the first cooling cavity (411) is used to cool the circumferential seal between the annular flange (41) and the outer wall of the furnace tube (1); a second cooling cavity (421) is provided in the end face flange (42), and the second cooling cavity (421) is used to cool the circumferential seal between the end face flange (42) and the outer wall of the furnace tube (1), and the end face seal between the end face flange (42) and the end of the furnace tube (1); The volume of the second cooling chamber (421) is greater than the volume of the first cooling chamber (411).
10. Low pressure chemical vapor deposition equipment, characterized in that Comprising the vacuum reaction chamber as described in any one of claims 1-9.