CN215757573U - Vacuum evaporation furnace with high collection rate for preparing silicon monoxide - Google Patents

Vacuum evaporation furnace with high collection rate for preparing silicon monoxide Download PDF

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Publication number
CN215757573U
CN215757573U CN202122126719.8U CN202122126719U CN215757573U CN 215757573 U CN215757573 U CN 215757573U CN 202122126719 U CN202122126719 U CN 202122126719U CN 215757573 U CN215757573 U CN 215757573U
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water
cooling
vacuum
vacuum evaporation
collecting barrel
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贺翔
李阁
许迪新
程晓彦
岳风树
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Shanxi Fuji New Energy Material Technology Co ltd
Beijing One Gold Amperex Technology Ltd
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Shanxi Fuji New Energy Material Technology Co ltd
Beijing One Gold Amperex Technology Ltd
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Abstract

The utility model relates to a vacuum evaporation furnace with high collection rate for preparing silicon monoxide, which comprises a vacuum evaporation chamber, an evaporation source, a collector, a vacuum device and a cooling device, wherein the evaporation source and the collector are arranged in the vacuum evaporation chamber, the air inlet end of the collector is hermetically connected with the opening end of the evaporation source, and the vacuum device is connected with the vacuum evaporation chamber through a vacuum pumping pipe; the cooling device comprises a first cooler and a second cooler, wherein the first cooler comprises a cooling sleeve sleeved outside the vacuum evaporation chamber; the second cooler comprises a water-cooling column and a cooling water tank which are connected with each other, wherein the water-cooling column is arranged inside the collector and penetrates through the axial direction of the collector.

Description

Vacuum evaporation furnace with high collection rate for preparing silicon monoxide
Technical Field
The utility model belongs to the technical field of vacuum evaporation coating, and particularly relates to a vacuum evaporation furnace with high collection rate for preparing silicon monoxide.
Background
With the development of photovoltaic technology and semiconductor technology, the demand of related high-performance raw materials is increasing, wherein, silicon monoxide can be used as a fine ceramic synthesis raw material due to the high activity, such as silicon nitride, silicon carbide fine ceramic synthesis raw material, preparation of optical glass and semiconductor material, and the like. In addition, SiO is an excellent coating material that can be evaporated in vacuum and deposited on the surface of a metallic mirror for optical instruments as a protective film. In recent years, much research has been conducted on silicon monoxide as a negative electrode material for lithium ion batteries because of its high specific capacity and excellent cycle stability. The silicon monoxide is obtained by reacting silicon dioxide with simple substance silicon under high-temperature vacuum condition and rapidly cooling.
The vacuum evaporation coating technology is that a film material to be evaporated is placed in a vacuum coating chamber and is heated by an evaporation source to be evaporated, when the mean free path of evaporated molecules is larger than the line distance between the evaporation source and a substrate, evaporated particles escape from the surface of the evaporation source, and the particles are rarely hindered by collision of other particles (mainly residual gas molecules) in the process of flying to the surface of the substrate, and can directly reach the surface of the substrate to be condensed to generate a film. The vacuum evaporation coating equipment must have several important parts such as an evaporation source, a coating chamber, a substrate, a vacuum system, and the like. The thickness of the film at any point on the substrate depends on the emission characteristics of the evaporation source, the geometry of the substrate and the evaporation source, the relative positions, and the amount of material evaporated, and this phenomenon is more pronounced as the degree of vacuum increases.
In addition to coating the workpiece surface, vacuum evaporation coating techniques can also be used to prepare and purify evaporated materials, particularly materials that react at high temperatures and in vacuum to produce vapor and require condensation to deposit at low temperatures, such as silicon monoxide. The successful preparation of SiO requires rapid, efficient and uniform cooling conditions, which are critical to the optical and electrochemical properties of the SiO product, since SiO disproportionates to form Si and Si dioxide during slow condensation, thereby losing the corresponding optical and electrochemical properties. At present, the problems of uneven cooling and unsatisfactory temperature control generally exist in a collecting device of vacuum evaporation equipment for preparing the silicon monoxide in a cooling process, so that the deposition effect of the silicon monoxide is poor, and the cooling effect and the collection yield of the silicon monoxide are seriously influenced.
SUMMERY OF THE UTILITY MODEL
In order to solve the problems, the utility model provides a vacuum evaporation furnace with high collection rate for preparing silicon monoxide, which comprises a vacuum evaporation chamber, an evaporation source, a collector, a vacuum device and a cooling device, wherein the evaporation source and the collector are arranged in the vacuum evaporation chamber, the air inlet end of the collector is hermetically connected with the opening end of the evaporation source, and the vacuum device is connected with the vacuum evaporation chamber through a vacuum pumping pipe;
the cooling device comprises a first cooler and a second cooler, wherein the first cooler comprises a cooling sleeve sleeved outside the vacuum evaporation chamber;
the second cooler comprises a water-cooling column and a cooling water tank which are connected with each other, wherein the water-cooling column is arranged inside the collector and penetrates through the axial direction of the collector.
Optionally, the evaporation source is selected from one of a resistance heating type evaporation source, an electron beam heating type evaporation source, a hollow hot cathode plasma beam evaporation source, an induction heating type evaporation source, a laser heating type evaporation source, or a radiation heating type evaporation source.
Preferably, the evaporation source is a resistance heating evaporation source, and specifically comprises an aluminum oxide furnace tube and a resistance wire, wherein one end of the aluminum oxide furnace tube is closed, the other end of the aluminum oxide furnace tube is open, the aluminum oxide furnace tube is a closed end, the other end of the aluminum oxide furnace tube is an open end, raw materials can be placed in the inner cavity space of the aluminum oxide furnace tube, and the resistance wire is spirally and uniformly wound outside the aluminum oxide furnace tube to heat the furnace tube.
Optionally, a first thermocouple is arranged inside the alumina furnace tube, and the first thermocouple is connected with a temperature control instrument outside the vacuum evaporation chamber to accurately control the temperature inside the alumina furnace tube.
Optionally, the collector comprises a collecting barrel and a heating device, the collecting barrel is in a horizontal round table shape or a cylindrical shape and is horizontally placed, one end of the collecting barrel is a gas inlet end and is hermetically connected with the open end of the alumina furnace tube, and the other end of the collecting barrel is a sealed end; the heating device is an electromagnetic induction heating device and comprises a heater and an electromagnetic induction coil, and the electromagnetic induction coil is uniformly wound on the outer side of the collecting barrel and heats the collecting barrel.
Optionally, the water-cooling column extends into the collecting barrel from the closed end of the collecting barrel and extends to the air inlet end of the collecting barrel, and the water-cooling column is horizontally placed in the radial center of the collecting barrel.
Optionally, a first water inlet pipe and a first water outlet pipe are arranged at one end of the water-cooling column close to the closed end of the collecting barrel, and are used for inputting and outputting cooling water for the water-cooling column respectively; the water-cooling column is a U-shaped pipe, the first water inlet pipe and the first water outlet pipe are respectively connected with two ends of the U-shaped pipe, and the cooling water tank is connected with the water-cooling column through the first water inlet pipe and the first water outlet pipe and provides circulating cooling water for the water-cooling column.
Optionally, a plurality of partition plates are connected between the inner wall of the collecting barrel and the water-cooling column at the center, and the partition plates are arranged along the radial direction of the collecting barrel and equally divide the inner space of the collecting barrel.
Optionally, the heater is arranged outside the vacuum evaporation chamber, and is connected to two ends of the electromagnetic induction coil through the first heating pipe and the second heating pipe respectively, so as to provide heating current for the electromagnetic induction coil.
Optionally, the electromagnetic induction coil is formed by a hollow copper pipe and used for containing circulating cooling water, the cooling water tank is connected with the first heating pipe through a second water inlet pipe, the second water outlet pipe is connected with the second heating pipe, and cooling water is introduced into the hollow electromagnetic induction coil through the heating pipe by the connection mode.
Further optionally, cooling water tank is equipped with first water pump and second water pump, and first inlet tube is connected to first water pump for the cooling water flow of control water-cooling post, and the second inlet tube is connected to the second water pump for the cooling water flow in the control electromagnetic induction coil.
Optionally, a second thermocouple is arranged on the outer side of the collecting barrel and used for monitoring the temperature of the collecting barrel in real time, the second thermocouple is connected with the temperature control instrument, the temperature control instrument is in communication connection with the heater and a second water pump of the cooling water tank, and the temperature of the collecting barrel is controlled accurately.
Optionally, the vacuum device comprises a vacuum pump, and the vacuum pump is selected from a roots vacuum pump, a rotary vane vacuum pump or an oil diffusion pump and can provide ultimate vacuum of 0.01 Pa.
The vacuum evaporation furnace with high collection rate for preparing the silicon monoxide has the following beneficial effects:
(1) the first cooler and the second cooler of the vacuum evaporation furnace respectively cool the whole vacuum evaporation chamber and the collector, so that the cooling effect is good;
(2) the water-cooling column and the partition plate arranged in the collector can provide a larger deposition area and enable the temperature distribution in the collector to be more uniform, so that the collection efficiency and the deposition uniformity of silicon monoxide materials are improved;
(3) the outside electromagnetic induction coil of collector is except providing the heating function, in addition supplementary cooling function, with water-cooling post and baffle are to the cooperation for the holistic temperature distribution of collecting vessel is more even.
Drawings
FIG. 1 is a structural view of the vacuum evaporation furnace for producing SiO with high collection rate.
FIG. 2 is a block diagram of the collector.
Fig. 3 is a cross-sectional view of the collection bucket.
In the figure, 1-evaporation source, 101-alumina furnace tube, 2-vacuum evaporation chamber, 3-collector, 4-vacuum device, 401-vacuum tube, 5-cooling jacket, 6-heater, 7-cooling water tank, 8-collecting barrel, 9-electromagnetic induction coil, 10-water cooling column, 11-partition plate, 12-first water inlet tube, 13-first water outlet tube, 14-first heating tube, 15-second heating tube, 16-second water inlet tube, and 17-second water outlet tube.
Detailed Description
The vacuum evaporation furnace with high collection rate for preparing silicon monoxide according to the embodiment, as shown in fig. 1-3, includes a vacuum evaporation chamber 2, an evaporation source 1, a collector 3, a vacuum device 4 and a cooling device, wherein the evaporation source 1 and the collector 3 are arranged inside the vacuum evaporation chamber 2, an air inlet end of the collector 3 is hermetically connected with an opening end of the evaporation source 1, and the vacuum device 4 is connected with the vacuum evaporation chamber 2 through a vacuum tube;
the cooling device comprises a first cooler and a second cooler, wherein the first cooler comprises a cooling jacket 5 sleeved outside the vacuum evaporation chamber 2;
the second cooler comprises a water-cooling column 10 and a cooling water tank 7 which are connected with each other, wherein the water-cooling column 10 is arranged inside the collector 3 and penetrates through the axial direction of the collector 3.
Alternatively, the evaporation source 1 is selected from one of a resistance heating type evaporation source, an electron beam heating type evaporation source, a hollow hot cathode plasma beam evaporation source, an induction heating type evaporation source, a laser heating type evaporation source, and a radiation heating type evaporation source.
Preferably, the evaporation source 1 is a resistance heating evaporation source, and specifically includes an alumina furnace tube 101 and a resistance wire, one end of the alumina furnace tube 101 is closed, the other end is open, the alumina furnace tube 101 is an open end, raw materials can be placed in the internal cavity space of the alumina furnace tube 101, and the resistance wire is spirally and uniformly wound outside the alumina furnace tube 101 to heat the furnace tube.
Optionally, aluminum silicate fiber blocks are arranged on the outer sides of the aluminum oxide furnace tube 101 and the resistance wire, and are filled between the resistance wire and the inner wall of the vacuum evaporation chamber 2, so that the furnace tube and the resistance wire are insulated and excessive heat loss is prevented.
Optionally, a first thermocouple is arranged inside the alumina furnace tube 101, and the first thermocouple is connected with a temperature control instrument outside the vacuum evaporation chamber 2, so that the temperature inside the alumina furnace tube 101 is accurately controlled, and the temperature inside the alumina furnace tube 101 can reach 1600 ℃.
Optionally, one end of the vacuum evaporation chamber 2 is provided with the evaporation source 1 and is communicated with a vacuum-pumping tube 401, the closed end of the alumina furnace tube 101 faces the vacuum-pumping tube 401, and the open end is hermetically connected with the air inlet end of the collector 3. The vacuum evaporation chamber 2 is a hearth of the vacuum evaporation furnace, the material of the vacuum evaporation chamber 2 is selected from high manganese steel, common carbon steel, alloy or stainless steel, the hearth is used for providing a closed environment, one end of the vacuum evaporation chamber 2, which is provided with the evaporation source 1, is closed, only an exhaust port is reserved to be connected with the vacuum-pumping pipe 401, the other end of the vacuum evaporation chamber is used for placing the collector 3, the hearth has good sealing performance, and the high vacuum environment can be maintained.
Optionally, the first cooler includes a cooling jacket 5 sleeved outside the vacuum evaporation chamber 2, and the cooling jacket 5 is provided with a water inlet and a water outlet for introducing circulating cooling water into the cooling jacket 5, for performing integral cooling and module protection on the collector 3 and the evaporation source 1, and preventing the external temperature of the device from being too high.
Optionally, the collector 3 includes a collecting barrel 8 and a heating device, the collecting barrel 8 is horizontal round table-shaped or cylindrical, and is placed horizontally, one end of the collecting barrel is a gas inlet end, and is hermetically connected with the open end of the alumina furnace tube 101, and the other end of the collecting barrel is a hermetic end; the heating device is an electromagnetic induction heating device and comprises a heater 6 and an electromagnetic induction coil 9, and the electromagnetic induction coil 9 is uniformly wound on the outer side of the collecting barrel 8 and heats the collecting barrel 8.
Optionally, the water-cooling column 10 extends into the collecting barrel 8 from the closed end of the collecting barrel 8 and extends to the air inlet end of the collecting barrel 8, and the water-cooling column 10 is horizontally placed in the radial center of the collecting barrel 8.
Optionally, one end of the water-cooling column 10 close to the closed end of the collecting barrel 8 is provided with a first water inlet pipe 12 and a first water outlet pipe 13, which are respectively used for inputting and outputting cooling water to and from the water-cooling column 10; the water-cooling column 10 is a U-shaped pipe, the first water inlet pipe 12 and the first water outlet pipe 13 are respectively connected with two ends of the U-shaped pipe, and the cooling water tank 7 is connected with the water-cooling column 10 through the first water inlet pipe 12 and the first water outlet pipe 13 to provide circulating cooling water for the water-cooling column.
Optionally, a plurality of partition plates 11 are connected between the inner wall of the collecting barrel 8 and the water-cooling column 10 at the center, the partition plates 11 are arranged along the radial direction of the collecting barrel 8 and divide the inner space of the collecting barrel 8 equally, preferably, 3-12 partition plates 11 are arranged in the collecting barrel 8 and divide the inner space of the collecting barrel 8 equally 3-12. The separator 11 is a molybdenum separator. The baffle can effectively improve the deposition area of collecting vessel, and simultaneously, the molybdenum baffle also can promote the cooling effect of water-cooling post, and other positions inside the collecting vessel are evenly conducted to the cold volume, especially guarantees that the temperature of the baffle as the deposition face is even, maintains the inside and outside constancy of temperature of collecting vessel.
Optionally, the heater 6 is disposed outside the vacuum evaporation chamber 2, and is connected to two ends of the electromagnetic induction coil 9 through a first heating pipe 14 and a second heating pipe 15, respectively, so as to provide heating current for the electromagnetic induction coil 9.
Optionally, the electromagnetic induction coil 9 is formed by a hollow copper pipe and is used for accommodating circulating cooling water, the cooling water tank 7 is connected to the first heating pipe 14 through a second water inlet pipe 16, a second water outlet pipe 17 is connected to the second heating pipe 15, and through this connection, the cooling water is introduced into the hollow electromagnetic induction coil 9 through the heating pipes.
Further optionally, the cooling water tank 7 is provided with a first water pump and a second water pump, the first water pump is connected with the first water inlet pipe 12 and used for controlling the cooling water flow of the water-cooling column 10, and the second water pump is connected with the second water inlet pipe 16 and used for controlling the cooling water flow in the electromagnetic induction coil 9.
Optionally, the cooling jacket 5 of the first cooler may be connected to the cooling water tank 7 of the second cooler through a water pipe, and shares circulating cooling water with the electromagnetic induction coil 9 and the water-cooling column 10, at this time, the cooling water tank 7 is provided with a third water pump for controlling the flow rate of cooling water of the cooling jacket 5; and can also be connected with a water cooler arranged additionally.
Optionally, a second thermocouple is arranged on the outer side of the collecting barrel 8 and used for monitoring the temperature of the collecting barrel 8 in real time, the second thermocouple is connected with the temperature control instrument, and the temperature control instrument is in communication connection with the second water pump of the heater 6 and the cooling water tank 7 and used for controlling the temperature of the collecting barrel 8 accurately; the second thermocouple is preferably a patch thermocouple.
When the temperature control device is used, when the second thermocouple detects that the temperature of the collecting barrel 8 is lower, the temperature control device can feed back the temperature control device, and the heat production quantity of the collecting barrel is increased by increasing the current on the electromagnetic induction coil 9; on the contrary, when the second thermocouple detects that the temperature of the collecting barrel 8 is higher, the temperature control instrument increases the flow of cooling water in the water cooling column 10 and the electromagnetic induction coil 9 by controlling the first water pump and the second water pump of the cooling water tank 7, and reduces the temperature of the collecting barrel 8; therefore, the collector 3 can maintain the temperature of the collecting barrel 8 constant by controlling the current of the electromagnetic induction coil 9 and the internal water flow.
Preferably, the material of the collecting barrel 8 is a high temperature resistant metal or alloy, such as tungsten, tantalum, molybdenum, niobium, vanadium, chromium, titanium, zirconium, nickel, stainless steel, chromium-molybdenum alloy, nickel-chromium-iron alloy, and tungsten-chromium-molybdenum alloy.
Optionally, the vacuum device 4 comprises a vacuum pump, and the vacuum pump is selected from a roots vacuum pump, a rotary vane vacuum pump or an oil diffusion pump, and can provide ultimate vacuum of 0.01 Pa.
Raw material powder capable of generating silicon monoxide gas is added into a crucible of the evaporation source 1, and the vacuum device 4 vacuumizes the vacuum evaporation chamber 2; heating the evaporation source 1, and reacting to generate silicon monoxide gas; the collector 3 is heated to a temperature lower than that of the evaporation source 1, and the SiO gas enters the collection barrel 8 and is deposited in the collection barrel 8 to obtain the SiO material.

Claims (10)

1. A vacuum evaporation furnace with high collection rate for preparing silicon monoxide is characterized by comprising a vacuum evaporation chamber, an evaporation source, a collector, a vacuum device and a cooling device, wherein the evaporation source and the collector are arranged in the vacuum evaporation chamber, the air inlet end of the collector is hermetically connected with the opening end of the evaporation source, and the vacuum device is connected with the vacuum evaporation chamber through a vacuum-pumping tube;
the cooling device comprises a first cooler and a second cooler, wherein the first cooler comprises a cooling sleeve sleeved outside the vacuum evaporation chamber;
the second cooler comprises a water-cooling column and a cooling water tank which are connected with each other, wherein the water-cooling column is arranged inside the collector and penetrates through the axial direction of the collector.
2. The vacuum evaporation furnace according to claim 1, wherein the evaporation source is a resistance heating evaporation source, and comprises an alumina furnace tube and a resistance wire, one end of the alumina furnace tube is closed, the other end of the alumina furnace tube is open, the resistance wire is wound outside the alumina furnace tube in a spiral and uniform manner, and the resistance wire is used for heating the furnace tube.
3. The vacuum evaporation furnace according to claim 2, wherein a first thermocouple is arranged inside the alumina furnace tube, and the first thermocouple is connected with a temperature control instrument outside the vacuum evaporation chamber to accurately control the temperature inside the alumina furnace tube.
4. The vacuum evaporation furnace according to claim 3, wherein the collector comprises a collecting barrel and a heating device, the collecting barrel is horizontal truncated cone-shaped or cylindrical and is horizontally arranged, one end of the collecting barrel is a gas inlet end and is hermetically connected with the open end of the alumina furnace tube, and the other end of the collecting barrel is a closed end;
the heating device is an electromagnetic induction heating device and comprises a heater and an electromagnetic induction coil, and the electromagnetic induction coil is uniformly wound on the outer side of the collecting barrel and heats the collecting barrel.
5. The vacuum evaporation furnace according to claim 4, wherein the water-cooling column extends into the collecting barrel from the closed end of the collecting barrel and extends to the air inlet end of the collecting barrel, and the water-cooling column is horizontally arranged at the radial center of the collecting barrel;
a first water inlet pipe and a first water outlet pipe are arranged at one end of the water-cooling column close to the closed end of the collecting barrel and are used for inputting and outputting cooling water for the water-cooling column respectively;
the water-cooling column is a U-shaped pipe, the first water inlet pipe and the first water outlet pipe are respectively connected with two ends of the U-shaped pipe, and the cooling water tank is connected with the water-cooling column through the first water inlet pipe and the first water outlet pipe and provides circulating cooling water for the water-cooling column.
6. The vacuum evaporation furnace according to claim 5, wherein a plurality of partition plates are connected between the inner wall of the collecting barrel and the central water-cooling column, and the partition plates are arranged along the radial direction of the collecting barrel and equally divide the inner space of the collecting barrel.
7. The vacuum evaporation furnace according to claim 5, wherein the heater is disposed outside the vacuum evaporation chamber and is connected to two ends of the electromagnetic induction coil through a first heating pipe and a second heating pipe, respectively, for supplying heating current to the electromagnetic induction coil;
the electromagnetic induction coil is composed of a hollow copper pipe and used for containing circulating cooling water, the cooling water tank is connected with the first heating pipe through a second water inlet pipe, the second water outlet pipe is connected with the second heating pipe, and through the connection mode, the cooling water is introduced into the hollow electromagnetic induction coil through the heating pipe.
8. The vacuum evaporation furnace according to claim 7, wherein the cooling water tank is provided with a first water pump and a second water pump, the first water pump is connected with the first water inlet pipe and used for controlling the flow of cooling water of the water cooling column, and the second water pump is connected with the second water inlet pipe and used for controlling the flow of cooling water in the electromagnetic induction coil.
9. The vacuum evaporation furnace according to claim 8, wherein a second thermocouple is disposed outside the collection barrel for real-time monitoring of the temperature of the collection barrel, the second thermocouple is connected to the temperature control instrument, and the temperature control instrument is in communication connection with the second water pump of the heater and the cooling water tank for controlling the temperature of the collection barrel accurately.
10. The vacuum evaporation furnace according to claim 1, wherein the vacuum device comprises a vacuum pump selected from a roots vacuum pump, a rotary vane vacuum pump, and an oil diffusion pump.
CN202122126719.8U 2021-09-06 2021-09-06 Vacuum evaporation furnace with high collection rate for preparing silicon monoxide Active CN215757573U (en)

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Application Number Priority Date Filing Date Title
CN202122126719.8U CN215757573U (en) 2021-09-06 2021-09-06 Vacuum evaporation furnace with high collection rate for preparing silicon monoxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202122126719.8U CN215757573U (en) 2021-09-06 2021-09-06 Vacuum evaporation furnace with high collection rate for preparing silicon monoxide

Publications (1)

Publication Number Publication Date
CN215757573U true CN215757573U (en) 2022-02-08

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