CN221052049U - Molecular beam epitaxy mercury beam source furnace metal crucible - Google Patents

Molecular beam epitaxy mercury beam source furnace metal crucible Download PDF

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Publication number
CN221052049U
CN221052049U CN202322390790.6U CN202322390790U CN221052049U CN 221052049 U CN221052049 U CN 221052049U CN 202322390790 U CN202322390790 U CN 202322390790U CN 221052049 U CN221052049 U CN 221052049U
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mercury
crucible
beam source
source furnace
molecular beam
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杨春章
孔金丞
王善力
李艳辉
陈卫业
杨晋
赵丽
姬荣斌
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Kunming Institute of Physics
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Kunming Institute of Physics
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Abstract

The utility model discloses a molecular beam epitaxial mercury beam source furnace metal crucible, which is used for heating mercury in a molecular beam epitaxial beam source furnace, wherein a protective layer is arranged on the inner wall of the crucible, and the protective layer is a high heat conduction layer formed by using pyrolysis graphite, pyrolysis boron nitride, graphene, carbon nano tubes or silicon carbide nano materials formed on the inner wall of the crucible by CVD. The crucible provided by the utility model can greatly reduce the heating influence of the crucible on mercury under the heating of the mercury beam source furnace, and is beneficial to the evaporation control of mercury particle beams.

Description

Molecular beam epitaxy mercury beam source furnace metal crucible
Technical Field
The utility model belongs to the technical field of molecular beam epitaxy equipment, and relates to a molecular beam epitaxy mercury beam source furnace metal crucible.
Background
The tellurium-cadmium-mercury film material prepared by the molecular beam epitaxy technology has great advantages in the aspects of material structure control, electrical parameter control and the like, particularly in the fields of multiband detection and high-temperature detection application of tellurium-cadmium-mercury, multiple layers of tellurium-cadmium-mercury film materials with different components and different electrical parameters need to be accurately prepared, and the molecular beam epitaxy technology plays an important role.
In the epitaxial growth process of the tellurium-cadmium-mercury molecular beam, the proportion of three element components in the material determines the corresponding wave band of the tellurium-cadmium-mercury material, and as the ratio of cadmium atoms in the tellurium-cadmium-mercury material increases, the ratio of mercury atoms decreases, the corresponding wave band of the tellurium-cadmium-mercury material gradually changes towards the direction of shortening the wavelength. The Te-Cd-Hg film material with three kinds of grains combined into one component has no relation to the beam current of three kinds of elements, no relation to the structure and temperature of the substrate surface, and the thermodynamic process of forming film with three kinds of grains is involved. Experiments and theoretical researches show that under the condition that the temperature of the substrate is kept at 180 ℃, the mercury beam is 2 orders of magnitude higher than that of tellurium, and a good tellurium-cadmium-mercury film can be obtained, which means that mercury needs a large amount of mercury atoms in the film forming process. At present, liquid metal mercury is generally adopted as an evaporation source material for a molecular beam epitaxy tellurium-cadmium-mercury film material, the liquid metal mercury is led into a mercury beam source furnace in a cavity, and the required mercury beam is obtained by controlling the heating power of the beam source furnace.
The crystal structure, surface defect control and photoelectric property of the material in the tellurium-cadmium-mercury molecular beam epitaxy process are closely related to mercury atoms in the material. Research shows that macroscopic defects on the surface of a molecular beam epitaxial tellurium-cadmium-mercury film have close relation with the loss of mercury in the material, and the position of mercury atoms in a material lattice has great influence on the electrical property of the material. For tellurium-cadmium-mercury materials needed for multiband detection, not only is a multi-component multi-layer tellurium-cadmium-mercury material needed to be grown, but also the electrical parameters are controlled, so that a beam source furnace configured by equipment is needed to be capable of quickly changing the beam current and keeping stable.
The general structure of the conventional beam source furnace comprises a crucible for loading source, a heater, a thermocouple, a heat insulation sleeve and the like. At present, a cracking boron nitride material is generally adopted as a crucible, and the crucible has the characteristics of high temperature resistance, high heat conduction, stable performance and the like, but is relatively complex in processing, relatively poor in mechanical strength, difficult to combine with metal, and is generally used for preparing a crucible of a solid beam source furnace. The conventional solid-state beam source furnace relates to the sublimation process of source material particles from solid state to gas state in the use process, the thermal kinetic energy and the surface condition of the source material particles heated to a certain temperature are generally considered, and the high-heat-conductivity cracking boron nitride crucible has little influence on heat in the heating process. The mercury atoms evaporated from the liquid mercury beam source furnace mainly come from a diffusion process from the liquid level of the liquid mercury to vacuum, and the evaporated mercury particles are related to the liquid level of the mercury and the thermal kinetic energy. In the evaporation process of the solid-state beam source furnace and the liquid-state mercury beam source furnace, the liquid level area of the liquid-state mercury in the crucible is relatively fixed, so that the liquid-state mercury is much smaller than the surface area of the solid-state source, the mercury beam is easier to control, however, in the actual use process, the mercury beam can be found to be stable in a long time when the temperature is changed, which is very unfavorable for changing the growth of the mercury beam.
Disclosure of utility model
The utility model aims to solve the technical problems that: the mercury atoms evaporated from the liquid mercury beam source furnace mainly come from a diffusion process from the liquid level of the liquid mercury to vacuum, and in the actual use process, the mercury beam can be found to be stable in a long time when the temperature of the mercury beam is changed, which is very unfavorable for changing the growth of the mercury beam. Therefore, the structure and the using process of the conventional mercury beam source furnace are analyzed, a metal material with heat conductivity and specific heat capacity close to those of mercury materials is adopted, the metal material is processed into a necessary crucible shape through a precise machining means, and a protective layer with high heat conductivity is formed on the inner wall of the crucible by using a CVD (chemical vapor deposition) method and the like, so that the novel crucible is designed to meet the requirement of rapid beam current stabilization.
Mercury cadmium telluride is an important infrared detector material, and the molecular beam epitaxy technology plays an important role in preparing a mercury cadmium telluride thin film material. In the tellurium-cadmium-mercury molecular beam epitaxial growth process, the proportion of three element components in the material determines the corresponding wave bands of the tellurium-cadmium-mercury material, and the three element components control the change of particle beams by changing the temperature of a beam source furnace, so that the required material is obtained by deposition. In addition, experiments and theoretical researches show that the deposition result is closely related to the surface structure and the temperature of the substrate, and a good tellurium-cadmium-mercury film can be obtained under the condition that the temperature of the substrate is 180 ℃ and the beam current of mercury is 2 orders of magnitude higher than that of tellurium, namely a large quantity of mercury atoms are needed in the film forming process. In the current preparation process of molecular beam epitaxy tellurium-cadmium-mercury film materials, liquid metal mercury is generally adopted to heat in a mercury beam source furnace to obtain required mercury beam current. In use, the heating source heats liquid metal mercury through the crucible, and the required mercury beam is stable, so the heating process has high requirements on a temperature interval and a temperature change process, the heating of the crucible has great influence on the heating of mercury materials, the crucible is processed by materials with similar specific heat capacity to mercury, and the surface is treated to avoid generating impurities by reaction.
The technical scheme adopted for solving the technical problems is as follows: a molecular beam epitaxial mercury beam source furnace metal crucible for use in a molecular beam epitaxial source furnace for heating mercury; the preparation method adopts a metal material with heat conductivity and specific heat capacity close to those of mercury materials, the metal material is processed into a necessary crucible shape by a precise machining means, and a protective layer with high heat conductivity is formed on the inner wall of the crucible by using a CVD (chemical vapor deposition) method and the like, so that the thermal influence of the crucible structure on a mercury beam source furnace is minimized.
The processing material employs a metallic material having a thermal conductivity and specific heat capacity close to those of mercury materials, including but not limited to tantalum, platinum, titanium, lead, iron, stainless steel, and the like.
The bottom of the crucible of the mercury beam source furnace is conical or arc-shaped.
The precise machining means comprise pressing, welding, machine milling and the like.
The method for preparing the protective layer with high heat conductivity by using CVD and the like forms a protective layer with high heat conductivity on the inner wall of the crucible, and the preparation method comprises, but is not limited to, chemical Vapor Deposition (CVD), atomic force deposition (ALD), plasma-assisted vapor deposition (PECVD) and the like.
The high thermal conductivity protective layer includes, but is not limited to, pyrolytic graphite, pyrolytic boron nitride, graphene, carbon nanotubes, silicon carbide nanomaterials, and the like.
The principle of the utility model comprises:
The conventional beam source furnace structure comprises a crucible for containing a source, a heater, a thermocouple, a heat insulation sleeve and the like. The mercury beam source furnace crucible is generally processed by adopting quartz materials, mainly considering the characteristics of high temperature resistance, high strength, easiness in processing and the like of quartz, however, the two parameters of the thermal conductivity and the specific heat capacity of the quartz materials are very different from those of the metal mercury materials, and the influence of the quartz crucible on heating power needs to be considered. For example, the thermal conductivity of mercury is 8.36W/mK at normal temperature, whereas quartz glass is 1.38W/mK, which differs by approximately 7 times, meaning that the thermal conductivity of quartz glass is 7 times worse than that of mercury. Another specific heat parameter, mercury, is 140J/kgK and quartz glass is 840J/kgK, which also differs 7 times, meaning that the quartz glass to metallic mercury ratio, 7 times the heat is needed to raise the same temperature, and it can be seen that quartz glass is much worse than metallic mercury in terms of heat conduction and rapid heat balance, heat has a significant portion of the variation in the temperature of the quartz crucible in the mercury beam source furnace of the quartz crucible, and to reduce the negative effects of the crucible, materials with higher thermal conductivity than metallic mercury and lower thermal conductivity than metallic mercury must be selected. Most solid metals have better thermal conductivity than liquid metal mercury from the above two parameters, however, in solid metals with only a small specific heat capacity, including platinum, gold, lead, etc., tantalum has a specific heat capacity close to that of mercury and stainless steel has a3 times greater specific heat capacity than mercury. Since the weight of mercury in the mercury crucible is several times higher than that of the crucible in practical use, a metal material slightly higher than mercury can be selected from the consideration of specific heat capacity, but the heat conduction performance is better than that of mercury, such as stainless steel, tantalum and the like.
In addition, mercury is characterized in that mercury can react with most metals except iron to form amalgam, metals such as gold, silver, aluminum and the like are easy to dissolve in liquid mercury, while stainless steel is mainly made of iron, part of the metals are chromium, elements such as Ni, ti, mn, N, nb, mo, si, cu and the like are also contained, the metal materials are adopted to form a crucible of the mercury furnace, the amalgam reaction of the mercury and the metal materials is required to be prevented, and a compact protective layer with high thermal conductivity and low specific heat capacity is arranged on the surface of the mercury contacted with the metal in a relatively effective method, so that the small thermal influence of the crucible in the heating process of the mercury beam source furnace can be ensured, and the influence of impurities in the metal crucible material on a growth material is prevented.
According to the description, the preparation process of the mercury beam source furnace crucible comprises the steps of selecting materials close to the thermal conductivity and specific heat capacity of mercury, forming the crucible with a certain shape through certain mechanical processing, then carrying out strict degreasing cleaning and surface cleaning corrosion on the crucible to obtain a clean metal surface, and then forming a high-thermal-conductivity protective layer on the metal surface of the crucible by utilizing a plurality of physical and chemical methods.
The beneficial effects of the utility model are as follows:
The material with the heat conductivity and the specific heat capacity close to those of the metal mercury is selected, so that the heat influence of the crucible in the heating process of the mercury beam source furnace is reduced; the necessary crucible shape is processed by adopting a precise machining means so as to meet the requirements of a mercury beam source furnace; the surface of the crucible is coated by adopting methods such as vapor deposition (CVD), so that the chemical reaction between the metal material crucible and mercury material is avoided, and the durability of the crucible is improved; the crucible provided by the utility model can greatly reduce the heating influence of the crucible on mercury under the heating of the mercury beam source furnace, and is beneficial to the evaporation control of mercury particle beams.
Drawings
Fig. 1: the utility model discloses a molecular beam epitaxy mercury beam source furnace mercury crucible installation position schematic diagram.
Fig. 2: the metal crucible of the utility model is a whole drawing.
Fig. 3: the utility model provides a schematic crucible with a protective layer with high heat conductivity.
In the figure: 1-a beam guide cap; a 2-mercury beam source furnace heating section; 3-mercury beam source furnace metal crucible; 4-VCR joint; 5-installing a knife edge flange; 6-controlling the valve.
Detailed Description
The method mainly comprises the steps of machining a crucible blank according to the requirements of an actual mercury beam source furnace, machining the crucible blank by using a reasonable precision machining method according to the design size, and coating a film on the crucible blank by combining the requirements of an actual film coating process after cleaning treatment so as to finish the machining and preparation of the crucible of the mercury beam source furnace. The process for preparing the crucible is described below by way of three examples.
Example 1
A316L stainless steel pipe with a smooth inner wall and a wall thickness of 0.5-1 mm and an inner diameter of 25mm is selected, the shape of a required crucible is processed by a numerical control machine tool, the length of the crucible is determined according to actual needs, a connecting port of the lower part of the crucible and a pipeline for conveying mercury sources can be processed into a conical port, the aperture of the conical port is consistent with that of the pipeline for conveying mercury below, the inner diameter of the pipeline for conveying mercury sources can be selected to be less than about 10mm, the pipeline for conveying mercury sources is also selected to be a 316L stainless steel pipe, and the two are welded into a mercury crucible blank with a conveying pipeline through an argon arc welding technology after cleaning treatment. After the mercury crucible blank is subjected to a strict ultrasonic oil stain cleaning process by using an organic solvent of acetone and methanol, the mercury crucible blank is cleaned by using a large amount of high-resistance deionized water, and then is dried in an oven. Placing the dried crucible blank into a high-temperature cracking furnace, vacuumizing the furnace to 10 -8 torr, then introducing high-purity methane or high-purity acetone for cracking and other gases, controlling the pressure in the furnace to be 1-10torr, then raising the temperature of the furnace to above 1800 ℃ for a period of time to obtain a cracking graphite passivation layer (figure 3) with a required thickness.
Example 2
The high-purity tantalum rod with the diameter of 30mm is selected, the rod is processed into the shape of a required crucible by utilizing a numerical control machine tool, the length of the crucible is determined according to actual needs, the lower part of the crucible is processed into a cone shape and is transited to a pipe with the inner diameter of about 10mm, and the conical shape is beneficial to being connected with the lower stainless steel pipe for conveying mercury sources with the same caliber, and the conical shape and the pipe can be connected through a VCR (figure 1). And (3) carrying out an ultrasonic oil stain cleaning process on the tantalum crucible which is processed independently by using a strict acetone and methanol organic solvent, cleaning by using a large amount of high-resistance deionized water, and then drying in an oven. The dried tantalum crucible blank was subjected to a graphite thermal cracking process similar to that of example 1 to deposit a layer of cracked graphite on the surface (fig. 3).
Example 3
The crucible blank made of metal material is prepared by the method of the embodiment 1 or the embodiment 2, and is put into a special vapor deposition (CVD) system after being cleaned and dried, the cavity is vacuumized to be below 1e -8 torr by an air pumping system, high-purity ammonia gas and high-purity boron trichloride are introduced into the crucible blank according to the proportion of 2:1, the vacuum degree is regulated to be in the range of 1-10torr, the reaction temperature can be set to be about 1800-2000 ℃, and the cracking boron nitride with the deposition time controlled to be tens of micrometers to hundreds of micrometers can be obtained (figure 3).

Claims (3)

1. A molecular beam epitaxy mercury beam source furnace metal crucible, which is used for heating mercury in a molecular beam epitaxy beam source furnace, and is characterized in that the crucible is processed into a required shape by adopting tantalum, platinum, titanium, lead, iron or stainless steel materials with heat conductivity and specific heat capacity close to those of mercury materials through a precise mechanical processing means, the inner wall of the crucible is provided with a protective layer, and the protective layer is a high heat conducting layer formed on the inner wall of the crucible by CVD; the material of the high heat conduction layer comprises pyrolytic graphite, pyrolytic boron nitride, graphene, carbon nano tube or silicon carbide nano material.
2. The molecular beam epitaxy mercury beam source furnace metal crucible of claim 1, wherein the bottom shape of the crucible is tapered or arc shaped.
3. The molecular beam epitaxy mercury beam source furnace metal crucible of claim 1 or 2, wherein forming a high thermal conductivity layer on an inner wall of the crucible by CVD comprises atomic force deposition or plasma-assisted vapor deposition.
CN202322390790.6U 2023-09-04 2023-09-04 Molecular beam epitaxy mercury beam source furnace metal crucible Active CN221052049U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202322390790.6U CN221052049U (en) 2023-09-04 2023-09-04 Molecular beam epitaxy mercury beam source furnace metal crucible

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202322390790.6U CN221052049U (en) 2023-09-04 2023-09-04 Molecular beam epitaxy mercury beam source furnace metal crucible

Publications (1)

Publication Number Publication Date
CN221052049U true CN221052049U (en) 2024-05-31

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