A high temperature reactor and microscope combined system

Abstract

The present invention provides a high-temperature reactor and microscope combined system, belonging to the field of high-temperature reaction equipment. The combined system includes a high-temperature reactor and a microscope; the high-temperature reactor includes a reaction chamber and a high-temperature heating table located inside the reaction chamber; the reaction chamber is composed of a chamber bottom, a chamber body and a chamber cover distributed from bottom to top; a window cover is inlaid in the center of the chamber cover; the microscope is located above the window cover; the high-temperature heating table is fixed to the chamber bottom and is located directly below the window cover; an air inlet, an air outlet and an air extraction port are distributed on the reaction chamber; the high-temperature heating table is heated by resistance heating, eddy current heating or laser heating; the temperature measurement of the high-temperature heating table is achieved by a thermocouple or an infrared thermometer. The present invention has the characteristics of small size, low energy consumption, multiple temperature zones and visualization, and can especially add electric field or magnetic field conditions, and perform real-time in-situ observation of the sample morphology through a microscope.

Description

Technical Field

[0001] The invention provides a high-temperature reactor and microscope combined system, belonging to the field of high-temperature reaction equipment. Background Art

[0002] High-temperature reactors with controllable pressure and atmosphere are mainly divided into two categories, one is hot wall reactors (such as muffle furnaces), and the other is cold wall reactors (such as molecular beam epitaxy equipment). Hot wall reactors are wrapped heating, that is, the materials around the working area are first heated, and then the heat is transferred to the working area through heat conduction, heat convection and heat radiation. Therefore, the volume and power of this type of reactor are generally large, and it is difficult to achieve in-situ observation. The heating device of the cold wall reactor is small in volume and power, and mainly directly heats the target material through electron beams or lasers. However, this type of equipment is mainly used in ultra-high vacuum environments, especially in the field of molecular beam epitaxy, but there is only one heating table. At the same time, in order to open holes in the cavity and install in-situ monitoring devices such as evaporation sources (molecular beam evaporation sources, metal evaporation sources, alkali metal evaporation sources) with standard interfaces, crystal oscillators, X-ray photoelectron spectroscopy analyzers (XPS), angle-resolved photoelectron spectroscopy (ARPES), and low-energy electron diffraction (LEED), the cavity size is generally large and spherical or quasi-spherical.

[0003] The patent (application number: 201920775701.0) designs a "cold wall chemical vapor deposition device". The device concentrates a "chemical deposition reaction zone", a "sub-chamber for holding solid sources", and a "suspended catalyst device". The "chemical deposition reaction zone" designed by the patent must be composed of an "upper heater" and a "lower heater". Its structure is complex, difficult to operate, and cannot be observed in situ; there is only one "chemical deposition reaction zone", which is a typical single temperature zone design and cannot meet the experimental requirements of multiple temperature zones; the "sub-chamber" and "suspended catalyst device" are placed in the device, making its structure too complex and bloated; the "motor shaft" of the "upper heater" and the "suspended catalyst device" are directly fixed to the "upper cover", which makes it very inconvenient to operate the "upper cover", and it is also a challenge to the sealing between the "motor shaft" and the "upper cover". Similar designs also involve multiple patents, with application numbers: 201710440556.6, 201711296987.6, 201810210266.7, and 201910397618.9.

[0004] The patent (application number: 202010272658.3) designs a "microwave plasma chemical vapor deposition device". The device needs to use "microwave plasma", which severely limits its scope of application; the introduction of "microwave plasma" requires opening holes in the "growth chamber" to install magnetrons and waveguides, which makes it difficult to miniaturize the device; the introduction of "microwave plasma" results in only one heating stage in the "growth chamber", which cannot meet the requirements of multi-temperature zone experiments; the "spectrometer" installed on the top of the "growth chamber" is used to "monitor the carbon, hydrogen, nitrogen and other components in the plasma...", which cannot achieve in-situ observation of the microscopic morphology of the grown sample.

[0005] The patent (application number: 201920851656.2) designs a "small high-temperature heating stage". The device has no air inlet and can only be used in the atmosphere or in a vacuum state. It can generally only be used as a heat treatment platform and cannot achieve reactions controlled by a specific atmosphere; there is only one "heating plate", which cannot meet the requirements of multi-temperature zone experiments; the "heating plate" is made of "silicon nitride", which severely limits the introduction of other heating materials and heating methods; the "heating plate" and "sample carrier" are not designed with "thermal insulation materials", so that both are completely exposed to the cavity space, resulting in a large amount of heat dissipation, and greatly increasing the difficulty of heating the "sample carrier" to a high temperature.

[0006] The paper (Rare Metal Materials and Engineering, 2012, 41(011):2037-2040) mentioned a "schematic diagram of CVD tantalum deposition device". In the device, a "chlorination chamber" heated by resistance is suspended above a "molybdenum substrate" heated by "thyristor eddy current". The design of the upper and lower structures makes the assembly and operation of the equipment more complicated; "eddy current heating" generally means that the material of the "substrate" can only be metal, which seriously limits the use of non-metallic "substrates"; one "molybdenum substrate", that is, only one substrate heating stage, cannot meet the requirements of multi-temperature zone reactions; and in-situ observation cannot be achieved. The paper (Material Guide, 2005, 19(F11):78-80) mentioned a cold wall chemical vapor deposition device, but the device has a complex appearance and structure, no insulation material, and only one heating stage, so in-situ observation cannot be achieved.

[0007] In summary, the cold wall reactors currently designed cannot combine the characteristics of small volume, multiple temperature zones and in-situ observation, and cannot meet the requirements of experiments with electric or magnetic fields. Therefore, it is of great significance to develop a device that can simultaneously possess the above characteristics. Summary of the invention

[0008] In view of the shortcomings of the above-mentioned background technology, the present invention provides a high-temperature reactor and microscope combination system, which is mainly achieved through the following technical solutions.

[0009] The combined system comprises a high-temperature reactor and a microscope 1; the high-temperature reactor comprises a reaction chamber and a high-temperature heating platform located inside the reaction chamber; the reaction chamber consists of a chamber bottom 10, a chamber body 7 and a chamber cover 2 which are arranged from bottom to top; a window cover plate 3 is inlaid at the central position of the chamber cover 2; the microscope 1 is located above the window cover plate 3; the high-temperature heating platform is fixed to the chamber bottom 10 and is located directly below the window cover plate 3; an air inlet 11, an air outlet 8 and an air extraction port 9 are distributed on the reaction chamber; the high-temperature heating platform is heated by resistance heating, eddy current heating or laser heating; and the temperature measurement of the high-temperature heating platform is achieved by a thermocouple or an infrared temperature detector.

[0010] The operating temperature of the high temperature reactor is room temperature to 2000°C.

[0011] The light transmittance of the window cover plate 3 is 0-100%.

[0012] There are one or more high-temperature heating platforms on the cavity bottom 10 .

[0013] When the high-temperature heating platform is heated by resistance heating, its structure includes a heating element 12, a stage 4 close to the upper surface of the heating element, a bottom insulation layer 16 close to the lower surface of the heating element, a radial insulation layer 6 radially wrapping the heating element 12 and the stage 4, an insulation layer fixing ring 5 surrounding and fixing the radial insulation layer 6 and the bottom insulation layer 16, a power supply rod 14 and a temperature measuring component 15 passing through the bottom insulation layer 16 for supplying power to the heating element 12 and measuring the temperature respectively, and a high-temperature heating platform base 13 for introducing the power supply rod 14 and the temperature measuring component 15 into the reaction chamber.

[0014] The high temperature heating stage can add electric field or magnetic field conditions.

[0015] The high temperature reactor can be used independently.

[0016] The beneficial effects of the present invention are: a. The miniaturization of the high-temperature reactor sharply reduces the floor space of the equipment; b. The miniaturization of the high-temperature heating stage greatly reduces the energy consumption of the equipment; c. The design of multiple high-temperature heating stages meets the requirements of multi-temperature zone experiments; d. The combination with a microscope realizes in-situ observation of the reaction; e. The electric field or magnetic field conditions can be added to meet the requirements of the reaction for special fields. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a front view of the schematic diagram of the high temperature reactor and microscope coupling system.

[0018] Figure 2 It is an isometric view of a schematic diagram of a high temperature reactor coupled to a microscope system.

[0019] Figure 3 yes Figure 2 The middle window cover 3 is in a cross-sectional view.

[0020] Figure 4 yes Figure 3 Cross-sectional view of the medium and high temperature reactor (AA).

[0021] Figure 5 It is an isometric view of the laser high temperature heating stage.

[0022] Figure 6 yes Figure 5 Cross-sectional view (BB).

[0023] In the figure: 1-microscope; 2-cavity cover; 3-window cover; 4-stage; 5-insulation fixing ring; 6-radial insulation layer; 7-cavity body; 8-air outlet; 9-exhaust port; 10-cavity bottom; 11-air inlet; 12-heating element; 13-high temperature heating table base; 14-power supply rod; 15-temperature measuring element; 16-bottom insulation layer; 17-insulating sealing layer; 18-laser heating element; 19-support ring; 20-insulation layer inside the ring; 21-laser heating table base; 22-insulation layer at the bottom of the support ring; 23-laser window. DETAILED DESCRIPTION

[0024] The present invention will be further described below in conjunction with the embodiments and drawings.

[0025] Example 1

[0026] like Figure 1-4As shown in the figure, the combined system includes a circular high-temperature reactor with an operating temperature of up to 1200 °C and a telephoto optical microscope 1; the high-temperature reactor includes a reaction chamber with an outer diameter of 100.0 mm and three high-temperature heating stages with an outer diameter of 20.0 mm located inside the reaction chamber and distributed in a straight line at an equal distance (5.0 mm) in the center of the chamber bottom; the reaction chamber is composed of a chamber bottom 10, a chamber body 7 and a chamber cover 2 distributed from bottom to top, which are made of titanium alloy; a window cover plate 3 with a diameter of 80.0 mm, a material of calcium fluoride glass and a transmittance of more than 85% is inlaid in the center of the chamber cover; the microscope 1 is located 50.0 mm above the window cover plate 3; the chamber bottom 10 and the chamber body 7 are integrally formed; the chamber body 7 and the chamber cover 2 are sealed with threads; the seal between the window cover plate 3 and the chamber cover 2 is a rubber O-ring seal; the chamber body 7 is distributed with an outer diameter of 5.0 mm. The high temperature heating platform is heated by resistance heating, and its structure includes a silicon carbide heating element 12 with a diameter of 12.0 mm and a height of 10.0 mm, a silicon carbide loading platform 4 with a diameter of 12.0 mm, a height of 1.0 mm and a square loading hole with a side length of 6.0 mm on the surface, which is close to the upper surface of the heating element, a bottom thermal insulation layer 16 of aluminum silicate fiber with a diameter of 12.0 mm and a thickness of 5.0 mm, which is close to the lower surface of the heating element, a radial thermal insulation layer 6 of aluminum silicate fiber with a height of 11.0 mm and a thickness of 3 mm, which radially wraps the heating element 12 and the loading platform 4, a corundum thermal insulation layer fixing ring 5 with a height of 16.0 mm and a thickness of 1.0 mm that surrounds and fixes the radial thermal insulation layer 6 and the bottom thermal insulation layer 16, and a high-purity tantalum power supply rod 14 with a diameter of 1.5 mm and a high-purity tantalum power supply rod 14 with a diameter of 1.5 mm and a high-purity tantalum power supply rod 15 with a diameter of 1.5 mm that pass through the bottom thermal insulation layer 16 for power supply and temperature measurement of the heating element 12 respectively. The power supply rod 14 and the temperature measuring component 15 are introduced into the titanium alloy high-temperature heating platform base 13 with a diameter of 18.0 mm in the reaction chamber; the high-temperature heating platform base 13 is connected to the chamber bottom 10 by a flange connection and a metal flat gasket seal; the stage 4 and the heating element 12 are designed as an integrated whole; a ring neodymium magnet with an inner diameter of 80.0 mm, an outer diameter of 100.0 mm, a thickness of 5.0 mm, and a magnetic field strength of 0.3 T is placed on the window cover (directly above the heating platform); the reaction chamber is naturally cooled.

[0027] Example 2

[0028] like Figure 1-3As shown in FIG. 1 , the combined system includes a circular high-temperature reactor with a working temperature of up to 1500° C. and a telephoto optical microscope 1; the high-temperature reactor includes a reaction chamber with an outer diameter of 360.0 mm and 16 high-temperature heating stages with an outer diameter of 30.0 mm located inside the reaction chamber and distributed in a ring shape in the center of the chamber bottom (one in the center, five evenly distributed on a ring belt with a radius of 60.0 mm, and ten distributed on a ring belt with a radius of 120.0 mm); the reaction chamber is composed of a chamber bottom 10, a chamber body 7, and a chamber cover 2 made of 316 stainless steel distributed from bottom to top; a window cover 3 with a diameter of 300.0 mm, a material of quartz glass, and a transmittance of more than 90% is inlaid in the center of the chamber cover; the microscope 1 is located 10.0 mm above the window cover 3. mm; the cavity bottom 10 and the cavity body 7 are sealed by a snap-on rubber O-ring; the cavity body 7 and the cavity cover 2 are flange-connected and sealed with a metal flat gasket; the seal between the window cover 3 and the cavity cover 2 is a threaded seal; the cavity bottom 10 is provided with an air inlet 11, an air outlet 8 and an exhaust port 9 with an outer diameter of 7.0 mm; the high-temperature heating platform is heated by resistance heating, and its structure includes a silicon carbide heating element 12 with a diameter of 20.0 mm and a height of 15.0 mm with multiple turns of electric heating platinum wire wrapped around the surface, a boron nitride stage 4 with a diameter of 20.0 mm, a height of 2.0 mm and a square loading hole with a side length of 10.0 mm on the surface, which is close to the upper surface of the heating element, and an aluminum silicate fiber bottom insulation layer 16 with a diameter of 30.0 mm and a thickness of 10.0 mm, which is close to the lower surface of the heating element, and a 15.0 mm high and 5.0 thick layer radially wrapping the heating element 12 and the stage 4. The microstructure of the microstructure is a porous silica aerogel radial insulation layer 6. A quartz insulation layer fixing ring 5 with a height of 25.0 mm and a thickness of 1.0 mm surrounds and fixes the radial insulation layer 6 and the bottom insulation layer 16. A high-purity tungsten power supply rod 14 with a diameter of 1.0 mm and a tungsten-rhenium thermocouple temperature measuring component 15 with a diameter of 2.0 mm and a corundum-armored tungsten-rhenium thermocouple temperature measuring component 15 with a diameter of 2.0 mm pass through the bottom insulation layer 16 to supply power and measure the temperature of the heating element 12. The power supply rod 14 and the temperature measuring component 15 are introduced into a 316 stainless steel high-temperature heating table base 13 in the reaction chamber; the high-temperature heating table base 13 is integrally formed with the chamber bottom 10; a ring-shaped copper sheet with an inner diameter of 20.0 mm, an outer diameter of 25.0 mm, and a thickness of 1.0 mm is introduced into the chamber bottom 10 through Feedthrough, which is located directly above the central heating table / below the window cover 3. The ring-shaped copper sheet is used as the positive electrode and the central heating table is used as the negative electrode. A load of 1000 V electric field; the cavity bottom 10, cavity body 7 and cavity cover 2 are cooled by forced air outside the equipment.

[0029] Example 3

[0030] like Figure 1-3As shown in the figure, the combined system includes a circular high-temperature reactor with a working temperature of up to 1700 °C and an optical microscope 1 with a CCD camera; the high-temperature reactor includes a reaction chamber with an outer diameter of 70.0 mm and three high-temperature heating stages with an outer diameter of 20.0 mm located inside the reaction chamber and distributed in the center of the chamber bottom in an equilateral triangle shape (side length 25.0 mm); the reaction chamber is composed of a chamber bottom 10, a chamber body 7 and a chamber cover 2 made of 304 stainless steel distributed from bottom to top; a window cover plate 3 with a diameter of 50.0 mm, made of sapphire and a transmittance of more than 99% is inlaid in the center of the chamber cover; the microscope 1 is located 5.0 mm above the window cover plate 3; the chamber bottom 10 and the chamber body 7 are integrally formed; the chamber body 7 and the chamber cover 2 are sealed with a metal flat gasket; the seal between the window cover plate 3 and the chamber cover 2 is a rubber O-ring seal; the chamber body 7 is distributed with a 5.0 mm outer diameter gasket. The high temperature heating platform is heated by eddy current heating, and its structure includes a metal tungsten column heating element 12 with a diameter of 10.0 mm and a height of 10.0 mm, a hexagonal boron nitride stage 4 with a diameter of 10.0 mm, a height of 1.0 mm and a square loading hole with a side length of 6.0 mm on the surface, which is close to the upper surface of the heating element, a bottom thermal insulation layer 16 of aluminum silicate fiber with a diameter of 10.0 mm and a thickness of 5.0 mm, which is close to the lower surface of the heating element, a radial thermal insulation layer 6 of silica aerogel with a height of 11.0 mm and a thickness of 5.0 mm and having a porous microstructure, which radially wraps the heating element 12 and the stage 4, a magnesium oxide ceramic thermal insulation layer fixing ring 5 with a height of 16.0 mm and a thickness of 1.0 mm, which surrounds and fixes the radial thermal insulation layer 6 and the bottom thermal insulation layer 16, and passes through the bottom thermal insulation layer 16 to generate an eddy current electromotive force inside the heating element - the eddy current is wrapped around the outer surface of the thermal insulation layer fixing ring 5 with an inner diameter of 1.0 mm. The copper tube coil is 0.5 mm thick and has cooling water flowing inside, and the copper tube coil is introduced into the 304 stainless steel high-temperature heating table base 13 in the reaction chamber; the high-temperature heating table base 13 and the chamber bottom 10 are connected by flanges and sealed with metal flat gaskets; the temperature of the high-temperature heating table is measured by an infrared temperature sensor arranged on the upper part of the chamber cover 2 and capable of passing through the window cover 3; the chamber bottom 10 and the chamber body 7 are water-cooled, and the chamber cover 2 is air-cooled.

[0031] Example 4

[0032] like Figure 1 , 2, 5 and 6, the system includes a circular high-temperature reactor with an operating temperature of up to 2000 °C and an optical microscope 1 with a CCD camera; the high-temperature reactor includes a reaction chamber with an outer diameter of 50.0 mm and a high-temperature heating stage with an outer diameter of 20.0 mm located inside the reaction chamber and fixed at the center of the chamber bottom; the reaction chamber is composed of a chamber bottom 10, a chamber body 7 and a chamber cover 2 made of 304 stainless steel distributed from bottom to top; a window cover 3 with a diameter of 50.0 mm, a material of single crystal germanium wafer and a transmittance of 1% is inlaid in the center of the chamber cover; the microscope 1 is located 5.0 mm above the window cover 3; the chamber bottom 10 and the chamber body 7 are integrally formed; the chamber body 7 and the chamber cover 2 are sealed with a metal flat gasket; the seal between the window cover 3 and the chamber cover 2 is a rubber O-ring seal; the chamber body 7 is distributed with an outer diameter of 5.0 The high temperature heating platform is heated by laser heating, and its structure includes a corundum support ring 19 with an inner diameter of 14.0 mm, a wall thickness of 1.0 mm, a height of 17.0 mm, and four notches with a depth of 2.0 mm at the upper end; a square silicon carbide laser heating body 18 with a side length of 11.3 mm, a thickness of 2.0 mm, and square loading holes on the surface is mounted on the four notches at the upper end of the support ring 19; the lower part of the laser heating body 18 has an aluminum oxide aerogel ring inner insulation layer 20 with a thickness of 2.0 mm and a height of 8.0 mm and a porous microstructure, which is close to the inner wall of the support ring; the lower part of the ring inner insulation layer 20 has an aluminum oxide aerogel support ring bottom insulation layer 22 with an outer diameter of 14.0 mm, an inner diameter of 4.0 mm, and a height of 5.0 mm; and the central position has a diameter of 4.0 mm. The laser heating table base 21 has a hole of 0.1 mm and is inlaid with a laser window 23; the support ring 19 is embedded in a corresponding annular groove on the upper surface of the laser heating table base 21 that is concentric with the laser window 23; the laser heating table base 21 and the cavity bottom 10 are connected by flanges and sealed with metal flat gaskets; the temperature of the laser heated body 18 is measured by an infrared temperature sensor arranged on the upper part of the cavity cover 2 and capable of penetrating the window cover 3; the cavity body 7 is naturally cooled, and the cavity bottom 10 and the cavity cover 2 are water cooled.

Claims

1. A high temperature reactor and microscope combined system, characterized in that: The combined system comprises a high-temperature reactor and a microscope (1); the high-temperature reactor comprises a reaction chamber and a high-temperature heating platform located inside the reaction chamber; the reaction chamber is composed of a chamber bottom (10), a chamber body (7) and a chamber cover (2) arranged from bottom to top; a window cover plate (3) is inlaid at the center of the chamber cover (2); the microscope (1) is located above the window cover plate (3); the high-temperature heating platform is fixed to the chamber bottom (10) and is located directly below the window cover plate (3); an air inlet (11), an air outlet (8) and an air extraction port (9) are distributed on the reaction chamber; the high-temperature heating platform is heated by resistance heating, eddy current heating or laser heating; the temperature measurement of the high-temperature heating platform is achieved by using a thermocouple or an infrared temperature detector; there are multiple high-temperature heating platforms on the chamber bottom (10); and each high-temperature heating platform is independently heated.

2. The high temperature reactor and microscope combination system according to claim 1, characterized in that: The operating temperature of the high temperature reactor is room temperature to 2000°C.

3. The high temperature reactor and microscope combination system according to claim 1, characterized in that: The light transmittance of the window cover plate (3) is 0-100%.

4. The high temperature reactor and microscope combined system according to claim 1, characterized in that: When the high-temperature heating platform is heated by resistance heating, its structure includes a heating element (12), a loading platform (4) closely attached to the upper surface of the heating element, a bottom heat insulation layer (16) closely attached to the lower surface of the heating element, a radial heat insulation layer (6) radially wrapping the heating element (12) and the loading platform (4), a heat insulation layer fixing ring (5) surrounding and fixing the radial heat insulation layer (6) and the bottom heat insulation layer (16), a power supply rod (14) and a temperature measuring element (15) passing through the bottom heat insulation layer (16) to respectively supply power to the heating element (12) and measure the temperature, and the power supply rod (14) and the temperature measuring element (15) are introduced into a high-temperature heating platform base (13) in a reaction chamber.

5. The high temperature reactor and microscope combined system according to claim 1, characterized in that: The high temperature heating stage is equipped with electric or magnetic field conditions.

6. The high temperature reactor and microscope combined system according to claim 1, characterized in that: The high temperature reactor can be used independently.

Images