High-cleanliness high-vacuum high-pressure heat treatment device

Abstract

The high-cleanliness high-vacuum high-pressure heat treatment device comprises a furnace body and a furnace door, crystal materials needing heat treatment are placed in a furnace cavity in the middle of the furnace body, and the crystal materials in the furnace cavity are subjected to high-temperature sintering through a first heating furnace pipe, an aluminum oxide furnace pipe and a second heating furnace pipe which are arranged on the peripheral side of the furnace cavity. The furnace door and the furnace body are sealed through the fluororubber sealing ring, heat loss in the furnace cavity is avoided, the stainless steel water cooling cavity is formed in the furnace door, the furnace door is cooled, the fluororubber sealing ring is prevented from being heated and deformed, and the service life of the sealing ring is prolonged; cold water is introduced into the water cooling cavity from the water inlet to cool the furnace door, the cold water flows out from the water outlet and is recycled, continuous cooling of the furnace door is achieved, the pipe plug sewn by aluminum oxide cloth is installed between the furnace door and the furnace cavity to block heat transfer from the furnace cavity to the furnace door, and heat loss in the furnace cavity is further reduced.

Description

Technical Field

[0001] The invention belongs to the technical field of crystal growth equipment and relates to a heat treatment device, in particular to a high-cleanliness, high-vacuum and high-pressure heat treatment device. Background Art

[0002] The crystal growth heat treatment device is a process test instrument used in the field of electronics and communication technology. It is suitable for preparing oxides, photonic crystal metals, alloys, compounds and various single crystal samples, and can adjust the atmosphere during the growth process. When the crystal growth heat treatment device is in use, the crucible containing the crystal material is placed in the furnace chamber for heating and treatment. The existing box-type heat treatment device has high requirements for sealing because it needs to maintain a high temperature in the furnace. The furnace door is the main part of energy loss because it often needs to be opened, so the sealing between the furnace door and the front wall has high requirements. Under the convection of the high-temperature gas in the furnace and the heat absorption and conduction of the metal components, the front wall and the furnace door structure will undergo certain thermal deformation, causing the furnace body seal failure and heat dissipation loss. Summary of the invention

[0003] In order to solve the technical problems existing in the background technology, the present invention proposes a high-cleanliness, high-vacuum, and high-pressure heat treatment device, which reduces the heat loss in the furnace cavity by arranging a fluororubber sealing ring between the furnace door and the furnace body, and cools the furnace door by arranging a stainless steel water-cooling cavity in the furnace door to avoid the fluororubber sealing ring from being deformed by heat and extend the service life of the sealing ring.

[0004] The purpose of the present invention can be achieved through the following technical solutions:

[0005] A high-cleanliness, high-vacuum, high-pressure heat treatment device comprises a furnace body and a furnace door hinged on the furnace body, a furnace cavity is arranged in the middle of the furnace body to place crystal materials to be heat treated, and a first heating furnace is coated around the furnace cavity to sinter the crystal materials in the furnace cavity at high temperature;

[0006] The furnace door is arranged on the front side of the furnace cavity, and the furnace door and the furnace body are sealed by a fluororubber sealing ring. There is a stainless steel water-cooling cavity inside the furnace door to cool the furnace door and prevent the fluororubber sealing ring from being deformed by heat. The water-cooling cavity is respectively connected with the water inlet and water outlet arranged on both sides of the furnace door, so that when the temperature of the furnace door exceeds the preset threshold, cold water is passed from the water inlet into the water-cooling cavity to cool the furnace door, and the cold water flows out from the water outlet and is recycled.

[0007] Furthermore, a pipe plug made of alumina cloth is provided between the furnace door and the furnace cavity to block heat transfer from the furnace cavity to the furnace door and reduce the heating rate of the furnace door. The pipe plug is fixed in the furnace body by a stainless steel sheet.

[0008] Furthermore, the first heating furnace is provided with multiple temperature zones for temperature control so as to increase the length of the constant temperature zone and increase the uniformity of the entire temperature field.

[0009] Furthermore, an alumina furnace core is provided on one side of the first heating furnace core to improve the high temperature resistance of the furnace body, so that crystal materials with higher melting points can be sintered through the alumina furnace core.

[0010] Furthermore, a second heating furnace liner is provided on one side of the alumina furnace liner, and the second heating furnace liner is arranged on the back side of the furnace cavity to increase the uniformity of the temperature field.

[0011] Furthermore, a vacuum port is connected to the bottom of the furnace chamber through a pipeline, so that the air inside the furnace chamber can be evacuated before the furnace chamber is heated, thereby achieving high-vacuum sintering of the crystal material in the furnace chamber.

[0012] Furthermore, a vacuum gauge is connected to the top of the furnace chamber through a pipeline to measure the vacuum degree in the furnace chamber after the air inside the furnace chamber is evacuated.

[0013] Furthermore, the top of the furnace chamber is connected to an inlet / outlet solenoid valve through a pipeline, so that before heating the furnace chamber, protective gas is circulated into the furnace chamber to achieve flowing atmosphere sintering of the crystal material in the furnace chamber.

[0014] Furthermore, a pressure transmitter is connected to the top of the furnace chamber through a pipeline, so as to monitor and adjust the gas pressure in the furnace chamber in real time when the furnace chamber is heated, thereby achieving high-pressure sintering of the crystal material in the furnace chamber.

[0015] Beneficial effects of the present invention: The high-cleanliness, high-vacuum, and high-pressure heat treatment device provided by the present invention comprises a furnace body and a furnace door. Crystal materials that need to be heat treated are placed in the furnace cavity in the middle of the furnace body. The crystal materials in the furnace cavity are sintered at high temperature by a first heating furnace core, an alumina furnace core, and a second heating furnace core arranged on the periphery of the furnace cavity. The furnace door and the furnace body are sealed by a fluororubber sealing ring to avoid heat loss in the furnace cavity. A stainless steel water-cooling cavity is arranged in the furnace door to cool the furnace door, to avoid deformation of the fluororubber sealing ring due to heat, and to extend the service life of the sealing ring. A water inlet and a water outlet are arranged on both sides of the water-cooling cavity to connect, so that when the temperature of the furnace door exceeds a preset threshold, cold water is introduced from the water inlet into the water-cooling cavity to cool the furnace door, and the cold water flows out from the water outlet and is recycled to achieve continuous cooling of the furnace door. A pipe plug made of alumina cloth is installed between the furnace door and the furnace cavity to block heat transfer from the furnace cavity to the furnace door, to reduce the heating rate of the furnace door, and to further reduce heat loss in the furnace cavity. By setting a vacuum port at the bottom of the furnace chamber to evacuate the air inside the furnace chamber, high vacuum sintering of the crystal material in the furnace chamber is achieved, and a vacuum gauge is installed on the top of the furnace chamber to measure the vacuum degree in the furnace chamber. By setting an inlet / outlet solenoid valve on the top of the furnace chamber to circulate protective gas into the furnace chamber, flowing atmosphere sintering of the crystal material in the furnace chamber is achieved. By installing a pressure transmitter on the top of the furnace chamber to monitor and adjust the gas pressure in the furnace chamber in real time, high pressure sintering of the crystal material in the furnace chamber is achieved. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention.

[0017] Figure 2 It is a schematic diagram of the cross-sectional structure of the present invention. DETAILED DESCRIPTION

[0018] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] like Figure 1-2 As shown, the present invention provides a high-cleanliness, high-vacuum, and high-pressure heat treatment device, comprising a furnace body 1 and a furnace door 2 hinged on the furnace body 1, a furnace chamber 11 is provided in the middle of the furnace body 1 to place crystal materials that need to be heat treated, and a first heating furnace core 12 is coated around the furnace chamber 11 to sinter the crystal materials in the furnace chamber 11 at high temperature.

[0020] The furnace door 2 is arranged on the front of the furnace cavity 11, and the furnace door 2 and the furnace body 1 are sealed by a fluororubber sealing ring 21. The furnace door 2 has a stainless steel water-cooling cavity 22 to cool the furnace door 2 and prevent the fluororubber sealing ring 21 from being deformed by heat. The water-cooling cavity 22 is respectively connected with a water inlet 23 and a water outlet 24 arranged on both sides of the furnace door 2, so that when the temperature of the furnace door exceeds a preset threshold, cold water is introduced from the water inlet 23 into the water-cooling cavity 22 to cool the furnace door 2, and the cold water flows out from the water outlet 24 and is recycled. A pipe plug 13 made of alumina cloth is arranged between the furnace door 2 and the furnace cavity 11 to block the heat transfer from the furnace cavity 11 to the furnace door 2 and reduce the heating rate of the furnace door 2. The pipe plug 13 is fixedly installed in the furnace body 1 through a stainless steel sheet 14.

[0021] The first heating furnace 12 is provided with multiple temperature zones to increase the length of the constant temperature zone and increase the uniformity of the entire temperature field. An alumina furnace 14 is provided on one side of the first heating furnace 12 to improve the high temperature resistance of the furnace body 1 so that crystal materials with higher melting points can be sintered through the alumina furnace 14. A second heating furnace 15 is provided on one side of the alumina furnace 14, and the second heating furnace 15 is arranged on the back of the furnace cavity 11 to increase the uniformity of the temperature field.

[0022] The bottom of the furnace chamber 11 is connected to a vacuum port 19 through a pipeline, which is used to connect a vacuum pump to evacuate the air inside the furnace chamber 11 before heating the furnace chamber 11, so as to achieve high vacuum sintering of the crystal material in the furnace chamber 11. The top of the furnace chamber 11 is connected to a vacuum gauge 17 through a pipeline to measure the vacuum degree in the furnace chamber 11 after the air inside the furnace chamber 11 is evacuated. The top of the furnace chamber 11 is connected to an inlet / outlet solenoid valve through pipelines, respectively, so as to circulate and fill the protective gas into the furnace chamber 11 before heating the furnace chamber 11, so as to achieve flowing atmosphere sintering of the crystal material in the furnace chamber 11. The top of the furnace chamber 11 is connected to a pressure transmitter 18 through a pipeline, so as to monitor and adjust the gas pressure in the furnace chamber 11 in real time when heating the furnace chamber 11, so as to achieve high pressure sintering of the crystal material in the furnace chamber 11.

[0023] A touch screen 3 is also installed on the furnace body 1. The touch screen 3 is arranged on one side of the furnace door 2. The touch screen 3 is connected to the first heating furnace 12, the alumina furnace 14, the second heating furnace 15, the vacuum pump, the vacuum gauge 17, the inlet and outlet solenoid valves, and the pressure transmitter 18 through the controller, so that the rising-constant-lowering curve can be set through the touch screen 3. The pressure, vacuum degree, and temperature in the furnace chamber 11 can be displayed in real time on the touch screen 3. The parameters can also be set through the touch screen 3 for constant pressure control. The constant pressure range is 0.01MPa-0.2MPa. The experimental data can be saved, recorded, and downloaded, and the process curve can also be generated and saved for easy retrieval when needed.

[0024] The heat treatment device provided by the present invention has a maximum heating temperature of 800 degrees Celsius, adopts a 310S stainless steel cavity with a volume of 366L, can be sintered at positive pressure, has a pressure resistance of 0.25MPa at 750 degrees Celsius, can be vacuum sintered, has a maximum vacuum degree of 5.0X10-3pa, can be sintered in a flowing atmosphere, adopts British Continental instruments, internal and external cascade control, and a temperature control accuracy of plus or minus 5 degrees Celsius. It can be used for sintering treatment under vacuum / high pressure / atmosphere, such as heat treatment of superconducting materials (YBCO) under a high-pressure oxygen environment. The rise-constant-falling temperature curve can be set through the touch screen, and the pressure, vacuum degree, and temperature in the cavity can be displayed in real time on the touch screen. The parameters can also be set through the touch screen for constant pressure control. The constant pressure range is 0.01MPa-0.2MPa. The experimental data can be saved, recorded, and downloaded, and a process curve can also be generated and saved for easy retrieval when needed.

[0025] The high-cleanliness, high-vacuum, and high-pressure heat treatment device provided by the present invention comprises a furnace body and a furnace door. Crystal materials that need to be heat treated are placed in a furnace cavity in the middle of the furnace body. The crystal materials in the furnace cavity are sintered at high temperature by a first heating furnace core, an alumina furnace core, and a second heating furnace core arranged on the periphery of the furnace cavity. The furnace door and the furnace body are sealed by a fluororubber sealing ring to avoid heat loss in the furnace cavity. A stainless steel water-cooling cavity is arranged in the furnace door to cool the furnace door, to avoid deformation of the fluororubber sealing ring due to heat, and to extend the service life of the sealing ring. A water inlet and a water outlet are arranged on both sides of the water-cooling cavity to communicate with each other, so that when the temperature of the furnace door exceeds a preset threshold, cold water is introduced from the water inlet into the water-cooling cavity to cool the furnace door, and the cold water flows out from the water outlet and is recycled to achieve continuous cooling of the furnace door. A pipe plug made of alumina cloth is installed between the furnace door and the furnace cavity to block heat transfer from the furnace cavity to the furnace door, to reduce the heating rate of the furnace door, and to further reduce heat loss in the furnace cavity. By setting a vacuum port at the bottom of the furnace chamber to evacuate the air inside the furnace chamber, high vacuum sintering of the crystal material in the furnace chamber is achieved, and a vacuum gauge is installed on the top of the furnace chamber to measure the vacuum degree in the furnace chamber. By setting an inlet / outlet solenoid valve on the top of the furnace chamber to circulate protective gas into the furnace chamber, flowing atmosphere sintering of the crystal material in the furnace chamber is achieved. By installing a pressure transmitter on the top of the furnace chamber to monitor and adjust the gas pressure in the furnace chamber in real time, high pressure sintering of the crystal material in the furnace chamber is achieved.

[0026] The above contents are merely examples and explanations of the structure of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the structure of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.

Claims

1. A high-purity, high-vacuum, high-pressure heat treatment device, characterized in that: The invention comprises a furnace body (1) and a furnace door (2) hinged on the furnace body (1); a furnace chamber (11) is provided in the middle of the furnace body (1) for placing crystal materials to be heat treated; and a first heating furnace core (12) is coated around the furnace chamber (11) for sintering the crystal materials in the furnace chamber (11) at high temperature; The furnace door (2) is arranged on the front side of the furnace cavity (11), and the furnace door (2) and the furnace body (1) are sealed by a fluororubber sealing ring (21). A stainless steel water cooling cavity (22) is provided inside the furnace door (2) to cool the furnace door (2) and prevent the fluororubber sealing ring (21) from being deformed by heat. The water cooling cavity (22) is respectively connected to a water inlet (23) and a water outlet (24) arranged on both sides of the furnace door (2), so that when the temperature of the furnace door exceeds a preset threshold, cold water is introduced from the water inlet (23) into the water cooling cavity (22) to cool the furnace door (2), and the cold water flows out from the water outlet (24) and is circulated.

2. The heat treatment device according to claim 1, characterized in that A pipe plug (13) made of aluminum oxide cloth is provided between the furnace door (2) and the furnace cavity (11) to block heat transfer from the furnace cavity (11) to the furnace door (2) and reduce the temperature rise rate of the furnace door (2). The pipe plug (13) is fixedly installed in the furnace body (1) through a stainless steel sheet (14).

3. The heat treatment device according to claim 1, characterized in that The first heating furnace (12) is provided with a plurality of temperature zones for temperature control so as to increase the length of the constant temperature zone and increase the uniformity of the entire temperature field.

4. The heat treatment device according to claim 3, characterized in that: An alumina furnace core (14) is provided on one side of the first heating furnace core (12) to improve the high temperature resistance of the furnace body (1) and enable crystalline materials with a higher melting point to be sintered through the alumina furnace core (14).

5. The heat treatment device according to claim 4, characterized in that: A second heating furnace liner (15) is provided on one side of the alumina furnace liner (14), and the second heating furnace liner (15) is arranged on the back side of the furnace cavity (11) to increase the uniformity of the temperature field.

6. The heat treatment device according to claim 1, characterized in that: The bottom of the furnace chamber (11) is connected to a vacuum port (19) via a pipeline, so that the air inside the furnace chamber (11) can be evacuated before the furnace chamber (11) is heated, thereby achieving high-vacuum sintering of the crystal material in the furnace chamber (11).

7. The heat treatment device according to claim 6, characterized in that The top of the furnace chamber (11) is connected to a vacuum gauge (17) via a pipeline so as to measure the vacuum degree in the furnace chamber (11) after the air inside the furnace chamber (11) is evacuated.

8. The heat treatment device according to claim 1, characterized in that: The top of the furnace chamber (11) is connected to gas inlet / outlet electromagnetic valves through pipelines, so that protective gas is circulated into the furnace chamber (11) before the furnace chamber (11) is heated, thereby achieving flowing atmosphere sintering of the crystal material in the furnace chamber (11).

9. The heat treatment device according to claim 1, characterized in that: The top of the furnace chamber (11) is connected to a pressure transmitter (18) via a pipeline so as to monitor and adjust the gas pressure in the furnace chamber (11) in real time when the furnace chamber (11) is heated, thereby achieving high-pressure sintering of the crystal material in the furnace chamber (11).

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