CN109444331B - Ultrahigh vacuum heating device and heating method thereof - Google Patents
Ultrahigh vacuum heating device and heating method thereof Download PDFInfo
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- CN109444331B CN109444331B CN201811160088.8A CN201811160088A CN109444331B CN 109444331 B CN109444331 B CN 109444331B CN 201811160088 A CN201811160088 A CN 201811160088A CN 109444331 B CN109444331 B CN 109444331B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/0033—Heating devices using lamps
- H05B3/0038—Heating devices using lamps for industrial applications
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Abstract
The invention relates to an ultrahigh vacuum heating device and a heating method thereof, wherein the ultrahigh vacuum heating device is provided with an adapter which can be connected with a magnetic rod, and the whole sample table can be transmitted out of and into an ultrahigh vacuum system through the adapter; the sample heating device is provided with a sample slot capable of placing a sample, and the sample heating table can move simultaneously through the sample slot; the direct-current heating electric brush system is arranged, and combined with a specific sample rack, the direct-current heating electric brush can realize the directional transmission of direct current on a sample; the positioning conductive jack is arranged, and a positioning plug arranged in the cavity is inserted into the jack, so that the positioning of the sample table can be realized, and the connection with a circuit outside the cavity can be realized, and the direct current heating without damaging the vacuum can be realized; the heating table is provided with a central hollow structure, is combined with a specific sample rack, and can realize laser heating of the sample by using an infrared laser heater. The invention can realize good heating capacity to the sample while maintaining the ultrahigh vacuum environment, and has the advantages of high heating speed, high temperature, small temperature gradient and accurate temperature measurement.
Description
Technical Field
The invention belongs to the technical field of vacuum heating, and particularly relates to an ultrahigh vacuum heating device and a heating method thereof.
Background
Vacuum means sub-atmospheric pressure (10)5Pa), depending on the range of the degree of vacuum, the gas space can be generally classified into a rough vacuum (10)5-103Pa), low vacuum (10)3-10-1Pa), high vacuum (10)-1-10-6Pa), ultra-high vacuum (10)-6-10-10Pa) and very high vacuum: (<10-10Pa) is added. In the ultra-high vacuum field, the existence of gas molecules including molecules adsorbed on the wall of the vacuum container is almost negligible, and the maintenance time of the solid cleaning surface can be relatively prolonged. Vacuum technology is widely used in the fields of electronics, aerospace, accelerators, surface physics, microelectronics, material science, and the like. In particular, in a vacuum environment, research in the fields of surface science, semiconductor application, nuclear fusion devices, and the like can be carried out, and these problems play an important role in solving problems such as environment, energy, new materials, and the like currently faced by human beings. Therefore, the need to develop equipment that operates in such extreme environments in the ultra-high vacuum field becomes more urgent.
In the prior art, in order to clean the surface of a sample in ultrahigh vacuum and anneal the sample at different temperatures, a resistance wire heating or back scattering bombardment method is mostly used, the two heating methods have low heating efficiency, the resistance wire is far away from a material, the temperature gradient between the resistance wire and the material is large, the temperature measurement is inaccurate, and the sample is difficult to be heated to extremely high temperature. The direct current heating technology can directly apply current to a sample, the heating efficiency is high, the temperature gradient is small, the use in the ultrahigh vacuum field is less, the direct current heating platform is mainly used for heating semiconductor materials, the direct current heating platform in the prior art is fixed in a vacuum cavity, in order to realize the transfer of the sample position, a manipulator is required to be matched with vacuum rotating equipment, the cost of the manipulator and the vacuum rotating equipment is high, the design of the use is also a weak link of a vacuum system, and the direct current heating platform is very easy to damage after being used for many times. The electric brush of direct current heating is along with the plug of sample many times, very easily lax, can not realize good contact, and if this kind of problem appears in prior art, can only stop the vacuum state of cavity, make the cavity expose the atmosphere, demolish the maintenance, waste time and energy. Therefore, it is urgent to develop an ultra-high vacuum dc heating device in which a sample can move along with a heating stage and an electric brush can be maintained without breaking the vacuum of a chamber.
At present, China is far from meeting the requirements in the aspects of high-end vacuum equipment research and development and technical popularization, and even has no strength to compete directly with international opponents, and a considerable proportion of scientific research expenses invested every year in China are used for purchasing foreign scientific research equipment, so that the national scientific research is restricted by people, and original scientific research achievements are difficult to achieve. Therefore, the development of vacuum technical equipment in China is rapidly improved, and the vacuum equipment is urgent.
Disclosure of Invention
Aiming at the problems in the prior art, the invention innovatively designs the ultrahigh vacuum heating device and the heating method thereof, wherein the ultrahigh vacuum heating device has the advantages of simple structure, low cost, convenience in use, simplicity in maintenance and easiness in realizing batch industrial production.
The technical solution for realizing the purpose of the invention is as follows:
an ultrahigh vacuum heating device comprises a sample frame, a heating sample table and an intracavity positioning conductive column, wherein the sample frame can be jointed with the heating sample table, the heating sample table can be jointed with the intracavity positioning conductive column, the heating sample table comprises an adapter, a sample table main body, a sample slot, a direct current brush system, a positioning conductive jack and a connecting hole arranged on the rear end face of the sample table main body, the adapter is fixedly connected with the front end of the sample table main body, the sample slot is fixed in the middle of the sample table main body,
the direct current electric brush system comprises an electric brush, a direct current electric brush system screw rod, an insulating ceramic chip, a fastening nut and a silver wire, the bottom end of the screw rod of the direct current brush system passes through the sample slot and the sample table main body and is fixed, the electric brush penetrates through a screw rod of the direct current electric brush system and is fixed at the upper end of the screw rod of the direct current electric brush system through an insulating ceramic chip and a fastening nut, the positioning conductive jacks comprise a first positioning conductive jack and a second positioning conductive jack, the first positioning conductive jack and the second positioning conductive jack are respectively and concentrically fixed in two through holes at the rear side of the sample stage main body by using ceramic cement, the silver wire comprises a first silver wire and a second silver wire, the first silver wire is connected with the first positioning conductive jack and the electric brush insulated from the screw rod of the direct current electric brush system, the second silver wire is connected with the second positioning conductive jack and the sample stage main body,
the positioning conductive column in the cavity comprises a vacuum electrode, a support rod, a main positioning column, a positioning conductive plug and wires, wherein the support rod comprises a thin cylindrical section and a thick cylindrical section which are integrally connected, one end of the thin cylindrical section is welded on a flange of the vacuum electrode, the other end of the thin cylindrical section is integrally connected with the thick cylindrical section, the main positioning column is fixedly connected to the end face of the thick cylindrical section, the thick cylindrical section is provided with two through holes along the axial direction of the thick cylindrical section, the positioning conductive plug is concentrically positioned in the two through holes through ceramic cement so that the positioning conductive plug is insulated from the support rod, one ends of the two wires are respectively connected with the vacuum electrode, and the other ends of the two wires are respectively connected with the positioning conductive plug.
Further, the sample rack comprises a hollowed sample rack, a nut, a sample rack insulating ceramic sheet, an electric brush electrode pressing sheet, a sample rack electrode pressing sheet, a sample rack screw and a sample, wherein the hollowed sample rack comprises a through hole positioned in the center and screw holes positioned on corners, the sample rack screw respectively penetrates through the screw holes, the electric brush electrode sheet and the electric brush electrode pressing sheet penetrating through the sample rack screw on one side of the hollowed sample rack are fixed through the nut and the sample rack insulating ceramic sheet, the sample rack electrode sheet and the sample rack electrode pressing sheet penetrating through the sample rack screw on the other side of the hollowed sample rack are fixed through another nut, the sample is transversely lapped on the electric brush electrode sheet and the sample rack electrode sheet, one side of the sample is positioned between the electric brush electrode sheet and the electric brush electrode pressing sheet and is compressed and fixed, and the other side of the sample is positioned between the electrode plate of the sample receiving frame and the electrode pressing sheet of the sample receiving frame and is compressed and fixed.
Further, each sample frame insulating ceramic piece comprises a first sample frame insulating ceramic piece, a second sample frame insulating ceramic piece, a third sample frame insulating ceramic piece and a fourth sample frame insulating ceramic piece, wherein the first sample frame insulating ceramic piece and the second sample frame insulating ceramic piece are respectively positioned between each nut of each electric brush electrode piece and each hollow sample frame, and the third sample frame insulating ceramic piece and the fourth sample frame insulating ceramic piece are respectively positioned between each nut of each electric brush electrode pressing piece and each nut of one side of each electric brush electrode pressing piece.
Furthermore, the sample table main body is in partial contact with the sample slot, and a slot heat insulation pressing sheet is arranged in a gap which is not in contact with the sample slot.
Furthermore, the sample slot comprises a sample slot body partially in contact with the sample stage main body, a main slot vertically extending from the surface of the sample slot body, and a sample frame anti-dropping piece fixedly connected with the main slot respectively, wherein a sliding groove structure is formed between each main slot and the sample frame anti-dropping piece at the top end.
Furthermore, the conducting wire is made of silver.
Furthermore, the device also comprises a vacuum cavity, a channel extending out of the vacuum cavity is connected with the inside of the cavity, the end part of the channel comprises a connecting flange plate, the conductive column positioned in the cavity can extend into the vacuum cavity through the channel, and the flange plate of the vacuum electrode can be in butt joint with the connecting flange plate to realize sealing connection.
Further, the device also comprises a laser heater and an infrared laser thermometer, wherein the laser heater is fixedly connected with one window of the vacuum cavity, and the infrared laser thermometer is fixedly connected with the other window of the vacuum cavity.
A heating method of the ultra-high vacuum heating device as described above, comprising the steps of:
the method comprises the following steps: fixing a sample on the sample holder, and then inserting the sample holder into the sample slot, so that one end of the electric brush is lapped on an electrode plate of the electric brush of the sample holder;
step two: connecting an adapter with a magnetic rod in an atmospheric state and positioned in a sample injection cavity, vacuumizing the sample injection cavity, opening a gate valve for communicating a vacuum cavity and the sample injection cavity when the vacuum reaches a proper value, sending a heating sample table into the vacuum cavity from the sample injection cavity through the magnetic rod, inserting the heating sample table into a cavity positioning conductive column positioned in the vacuum cavity, realizing butt joint of a positioning conductive jack and a positioning conductive plug and butt joint of a connecting hole and a main positioning column, loosening the connection of the magnetic rod and the adapter, withdrawing the magnetic rod, and closing the gate valve;
step three: the direct current is applied to the vacuum electrode, so that the sample can be heated in vacuum, and the real-time temperature monitoring can be realized through the infrared thermometer.
Furthermore, laser heating can be adopted simultaneously or independently in the third step, namely, laser is irradiated on the sample through the central through hole of the hollow sample frame by a laser heating instrument to realize laser heating.
Compared with the prior art, the invention has the following remarkable advantages:
(1) the invention has simple structure and easy operation: the sample and the sample table can be combined and transmitted without using expensive and fragile mechanical arms and vacuum rotating equipment;
(2) the invention has low cost and easy maintenance: after other multidimensional vacuum operation equipment is planed, direct current heating can be realized only by manufacturing the vacuum heating device, the whole heating device can be taken out of the cavity under the condition of not damaging the vacuum of the main cavity, and each part can be easily maintained and replaced;
(3) the special electric brush design of the invention can realize direct current heating, the hollow design of the sample rack and the heating table can realize laser heating, the two heating modes can be used independently and simultaneously, the heating speed is high, the temperature gradient is small, and the sample selection range is wide;
(4) the invention has high and uniform heating efficiency: the heating unit and the sample are not blocked by vacuum or a sample rack, the heating range is concentrated on the sample, and a larger heating effect can be obtained by using smaller energy;
(5) real-time temperature feedback can be realized, and an operator is helped to control the temperature.
Drawings
Fig. 1 is a schematic view of the overall structure of the sample holder of the present invention.
FIG. 2 is a schematic view of the general structure of the heating sample stage according to the present invention.
FIG. 3 is a schematic view of a part of the heating sample stage according to the present invention.
FIG. 4 is a schematic view of a part of the heating sample stage according to the present invention.
Fig. 5 is a partial view B of fig. 4.
FIG. 6 is a schematic structural diagram of a DC brush system for heating a sample stage according to the present invention.
FIG. 7 is a schematic view of a part of the heating sample stage according to the present invention.
Fig. 8 is a partial view a of fig. 7.
FIG. 9 is a schematic view of the matching structure of the sample holder and the ultra-high vacuum heating sample stage according to the present invention.
Fig. 10 is a schematic structural view of positioning the conductive post in the cavity according to the present invention.
Fig. 11 is a schematic structural view of the present invention in which a heated sample stage is engaged with a sample holder and a positioning conductive post is engaged with a cavity.
Fig. 12 is a schematic diagram of the positions of the positioning conductive column and the heating sample stage inside the cavity, and the positions of the positioning conductive column, the laser heating instrument and the infrared thermometer outside the cavity.
Detailed Description
Referring to fig. 1-11, an ultra-high vacuum heating device comprises a sample holder 1, a heating sample stage 2, and a positioning conductive column in a cavity, wherein:
referring to fig. 1, a sample holder 1 includes a hollow sample holder 1-1, a nut 1-2, an insulating ceramic 1-3, an electrode sheet for electric brush 1-4, an electrode sheet for electric brush 1-5, an electrode sheet for sample holder 1-6, an electrode sheet for sample holder 1-7, a screw 1-8 of sample holder, and a sample 1-9 (e.g., a semiconductor). The sample rack is built according to a schematic diagram, wherein four sample rack screw rods 1-8 are screwed into screw holes of a hollow sample rack 1-1, and then four nuts 1-2 are screwed into the sample rack screw rods 1-8 until the sample rack screws are fastened on the hollow sample rack 1-1; two insulating ceramics 1-3-1 and 1-3-2 are arranged on the screw 1-8 of the sample rack on the right side with small heads upward on the nuts 1-2-1 and 1-2-2; placing electrode plates 1-4 of the electric brush on right side insulating ceramics 1-3-1 and 1-3-2 after penetrating through right side sample frame screws 1-8-1 and 1-8-2, and placing electrode plates 1-5 of the electric brush on left side sample frame screws 1-8-3 and 1-8-4 on left side nuts 1-2-3 and 1-2-4; samples 1-9 were mounted across two electrode pads; the electrode pressing sheet 1-5 of the electric connection brush is placed on the sample 1-9 through the screws 1-8-1 and 1-8-2 of the right sample frame, and the electrode pressing sheet 1-7 of the sample frame is placed on the sample 1-9 through the screws 1-8-3 and 1-8-4 of the left sample frame; placing the insulating ceramics 1-3-3 and 1-3-4 with small ends facing downwards on the electrode pressing sheet 1-5 connected with the electric brush through the right sample frame screws 1-8-1 and 1-8-2, and screwing the right sample frame screws 1-8-1 and 1-8-2 to fasten the insulating ceramics 1-3-3 and 1-3-4 by using two nuts 1-2-5 and 1-2-6; two nuts 1-2-7 and 1-2-8 are used for screwing the left sample frame screws 1-8-3 and 1-8-4 to fasten the left sample frame electrode pressing sheet 1-7.
Referring to fig. 2-9, the heating sample stage 2 includes an adaptor 2-1, a sample stage main body 2-2, a sample slot 2-3, a dc brush system 2-4, a positioning conductive jack 2-5, and a connection hole 2-17 disposed on a rear end surface of the sample stage main body 2-2. The joint head 2-1 is connected with the sample table main body 2-2 by a screw 2-6 to form a whole and is connected with the magnetic rod through the joint head 2-1; the sample slot 2-3 comprises a main slot 2-7, a slot heat insulation pressing sheet 2-8 and a sample frame anti-dropping sheet 2-9, wherein the main slot 2-7 and the slot heat insulation pressing sheet are simultaneously connected with the sample table main body 2-2 by screws 2-10, and the sample frame anti-dropping sheet 2-9 is connected with the main slot 2-7 by screws 2-11; the direct current brush system 2-4 comprises electric brushes 2-12, direct current brush system screw rods 2-13, insulating ceramics 2-14, fastening nuts 2-15 and silver wires 2-16, the fastening nuts 2-15-1 are screwed into one ends of the direct current brush system screw rods 2-13, the insulating ceramics 2-14-1 are placed on the fastening nuts 2-15-1 with small ends upwards penetrating through the direct current brush system screw rods 2-13, the electric brushes 2-12 are placed on the insulating ceramics 2-14-1 with penetrating through the direct current brush system screw rods 2-13, the electric brushes 2-12 and the direct current brush system screw rods 2-13 are insulated and fixed by using the insulating ceramics 2-14-2 and the fastening nuts 2-15-2 to form a whole, and the other ends of the direct current brush system screw rods 2-13 are connected with the sample platform main body 2-2 and the sample slot 2-13 3, connecting; the positioning conductive jack 2-5 is concentrically fixed in a through hole at the rear side of the sample stage main body 2-2 by using ceramic cement; silver wires 2-16-1 and 2-16-2 are used for connecting two positioning conductive jacks 2-5-1 and 2-5-2 respectively, the other ends of the silver wires 2-16 are connected with an electric brush 2-12 insulated from a screw rod 2-13 of a direct current electric brush system and a sample platform main body 2-2 respectively, and the silver wires 2-16 can be connected by screws or can be directly wound.
Referring to fig. 10-11, the positioning conductive column 3 in the chamber includes a vacuum electrode 3-1, a support rod 3-2, a main positioning column 3-3, a positioning conductive plug 3-4, and a silver wire 3-5. Wherein the support rod 3-2 is welded on the flange of the vacuum electrode 3-1; the main positioning column 3-3 is welded on the end face of the supporting rod 3-2; fixing the positioning conductive plug 3-4 in the through hole of the support rod 3-2 by using insulating ceramic glue, so that the positioning conductive plug 3-4 is insulated from the support rod 3-2; one end of each silver wire 3-5 is connected to the vacuum electrode 3-1 in the cavity, the other end is connected to the positioning conductive plug 3-4, and the silver wires 3-5 can be connected by screws or directly wound.
With reference to fig. 9, the sample holder 1 is inserted into the sample slot 2-3, one end of the electric brush 2-12 is lapped on the electrode plate 1-4 of the electric brush of the sample holder 1, the joint 2-1 of the sample stage is connected with the magnetic pole under the atmospheric condition, the sample injection cavity is vacuumized, when the vacuum reaches a proper value, the gate valve is opened to communicate the sample injection cavity with the sample preparation cavity, the direct current heating stage is inserted into the cavity to position the conductive pole 3, the connection between the magnetic pole and the joint 1 is released, the magnetic pole is withdrawn, and the gate valve is closed. At the moment, the electrode outside the conductive column is electrified, so that the vacuum sample injection and the sample direct-current heating are not damaged.
With reference to fig. 12, the device further includes a vacuum cavity, a channel extending from the vacuum cavity is connected to the inside of the vacuum cavity, the end of the channel includes a connecting flange, the positioning conductive column 3 in the cavity can extend into the vacuum cavity through the channel, and the flange of the vacuum electrode 3-1 can be in butt joint with the connecting flange to realize sealing connection.
The device further comprises a laser heater 4 and an infrared laser thermometer 5, wherein the laser heater 4 is fixedly connected with one window of the vacuum cavity, and the infrared laser thermometer 5 is fixedly connected with the other window of the vacuum cavity.
The heating method of the ultrahigh vacuum heating device of the embodiment comprises the following steps:
the method comprises the following steps: referring to fig. 9, after fixing the samples 1 to 9 on the sample holder 1, inserting the sample holder 1 into the sample slots 2 to 3, so that one end of the brush 2 to 12 is lapped on the electrode plate 1 to 4 of the sample holder 1;
step two: connecting an adapter 2-1 with a magnetic rod in an atmospheric state and positioned in a sample injection cavity, vacuumizing the sample injection cavity, opening a gate valve for communicating a vacuum cavity and the sample injection cavity when the vacuum reaches a proper value, sending a heating sample table 2 from the sample injection cavity into the vacuum cavity through the magnetic rod, inserting the heating sample table 2 into a cavity positioning conductive column 3 positioned in the vacuum cavity, realizing butt joint of a positioning conductive jack 2-5 and a positioning conductive plug 3-4 and butt joint of a connecting hole 2-17 and a main positioning column 3-3, loosening the connection of the magnetic rod and the adapter 2-1, withdrawing the magnetic rod, and closing the gate valve;
step three: direct current is applied to the vacuum electrode 3-1, so that the sample 1-9 can be heated in vacuum, and real-time temperature monitoring can be realized through the infrared thermometer 5.
Further, laser heating can be adopted simultaneously or independently in the third step, namely, laser is irradiated on the sample 1-9 through the central through hole of the hollow sample frame 1-1 by the laser heating instrument 4 to realize laser heating.
After the heating sample table 2 is placed in the vacuum cavity, samples 1-9 on the sample frame 1 are located at growth positions, the front faces of the samples are horizontally downward, a glass window is arranged right below the samples, and an infrared thermometer 5 is fixed outside the glass window, so that the temperatures of the samples 1-9 can be observed in real time, and accurate temperature feedback can be realized no matter direct current heating or laser heating is adopted, or the direct current heating or the laser heating and the laser heating are adopted together.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. An ultrahigh vacuum heating device comprises a sample frame (1), a heating sample table (2) and an intracavity positioning conductive column (3), wherein the sample frame (1) can be jointed with the heating sample table (2), the heating sample table (2) can be jointed with the intracavity positioning conductive column (3), and the ultrahigh vacuum heating device is characterized in that the heating sample table (2) comprises an adapter (2-1), a sample table main body (2-2), a sample slot (2-3), a direct current brush system (2-4), a positioning conductive jack (2-5) and a connecting hole (2-17) arranged on the rear end face of the sample table main body (2-2), the adapter (2-1) is fixedly connected with the front end of the sample table main body (2-2), the sample slot (2-3) is fixed in the middle of the sample table main body (2-2),
the direct current brush system (2-4) comprises electric brushes (2-12), direct current brush system screw rods (2-13), insulating ceramic plates (2-14), fastening nuts (2-15) and silver conducting wires (2-16), the bottom ends of the direct current brush system screw rods (2-13) penetrate through the sample slot (2-3) and the sample table main body (2-2) and are fixed, the electric brushes (2-12) penetrate through the direct current brush system screw rods (2-13) and are fixed at the upper end positions of the direct current brush system screw rods (2-13) through the insulating ceramic plates (2-14) and the fastening nuts (2-15), the positioning conducting insertion holes (2-5) comprise first positioning conducting insertion holes (2-5-1) and second positioning conducting insertion holes (2-5-2), the first positioning conductive jack (2-5-1) and the second positioning conductive jack (2-5-2) are concentrically fixed in two through holes on the rear side of the sample stage main body (2-2) by ceramic cement respectively, the silver wires (2-16) comprise a first silver wire (2-16-1) and a second silver wire (2-16-2), the first silver wire (2-16-1) is connected with the first positioning conductive jack (2-5-1) and an electric brush (2-12) insulated from a screw rod (2-13) of a direct current electric brush system, the second silver wire (2-16-2) is connected with the second positioning conductive jack (2-5-2) and the sample stage main body (2-2),
the intracavity positioning conductive column (3) comprises a vacuum electrode (3-1), a support rod (3-2), a main positioning column (3-3), a positioning conductive plug (3-4) and a lead (3-5), wherein the support rod (3-2) comprises a thin cylindrical section and a thick cylindrical section which are integrally connected, one end of the thin cylindrical section is welded on a flange of the vacuum electrode (3-1), the other end of the thin cylindrical section is integrally connected with the thick cylindrical section, the end surface of the thick cylindrical section is fixedly connected with the main positioning column (3-3), the thick cylindrical section is provided with two through holes along the axial direction of the thick cylindrical section, the positioning conductive plug (3-4) is concentrically positioned in the two through holes through ceramic cement so as to enable the positioning conductive plug (3-4) to be insulated from the support rod (3-2), one end of each of the two leads (3-5) is respectively connected with the vacuum electrode (3-1), the other end is respectively connected with the positioning conductive plug (3-4),
the sample holder (1) comprises a hollowed sample holder (1-1), 8 nuts (1-2), 4 sample holder insulating ceramic sheets (1-3), an electric brush electrode sheet (1-4), an electric brush electrode pressing sheet (1-5), a sample holder electrode sheet (1-6), a sample holder electrode pressing sheet (1-7), 4 sample holder screw rods (1-8) and samples (1-9), wherein the hollowed sample holder (1-1) comprises a through hole positioned in the center and screw holes positioned on 4 corners, the 4 sample holder screw rods (1-8) respectively penetrate through the 4 screw holes, and the electric brush electrode sheet (1-4) and the electric brush electrode pressing sheet (1-3) penetrating through the 2 sample holder screw rods (1-8) on the side of the hollowed sample holder (1-1) are respectively penetrated through the 4 screw holes through the 4 nuts (1-2) and the 4 sample holder insulating ceramic sheets (1-3) (1-5) fixing, fixing a sample rack electrode plate (1-6) and a sample rack electrode pressing sheet (1-7) of 2 sample rack screws (1-8) penetrating through the other side on the other side of the hollowed sample rack (1-1) through another 4 nuts (1-2), wherein the sample (1-9) is transversely lapped on the electric brush electrode plate (1-4) and the sample rack electrode plate (1-6), one side of the sample (1-9) is positioned between the electric brush electrode plate (1-4) and the electric brush electrode pressing sheet (1-5) and is pressed and fixed, the other side of the sample (1-9) is positioned between the sample rack electrode plate (1-6) and the sample rack electrode pressing sheet (1-7) and is pressed and fixed,
the 4 sample rack insulating ceramic sheets (1-3) comprise a first sample rack insulating ceramic sheet (1-3-1), a second sample rack insulating ceramic sheet (1-3-2), a third sample rack insulating ceramic sheet (1-3-3) and a fourth sample rack insulating ceramic sheet (1-3-4), the first sample rack insulating ceramic sheet (1-3-1) and the second sample rack insulating ceramic sheet (1-3-2) are respectively positioned between the electric brush electrode sheet (1-4) and 2 nuts (1-2) between the electric brush electrode sheet (1-4) and the hollow sample rack (1-1), and the third sample rack insulating ceramic sheet (1-3-3) and the fourth sample rack insulating ceramic sheet (1-3-4) are respectively positioned between the electric brush electrode pressing sheet (1-5) and the electric brush electrode pressing sheet (1-3-4) -5) between 2 nuts (1-2) on one side,
the device also comprises a vacuum cavity, a channel extending out of the vacuum cavity is connected with the interior of the cavity, the end part of the channel comprises a connecting flange plate, the positioning conductive column (3) in the cavity can extend into the vacuum cavity through the channel, the flange plate of the vacuum electrode (3-1) can be in butt joint with the connecting flange plate to realize sealing connection,
the device further comprises a laser heater (4) and an infrared laser thermometer (5), wherein the laser heater (4) is fixedly connected with one window of the vacuum cavity, and the infrared laser thermometer (5) is fixedly connected with the other window of the vacuum cavity.
2. The ultra-high vacuum heating device as claimed in claim 1, wherein the sample stage body (2-2) is in partial contact with the sample slot (2-3), and a slot thermal insulation pressing sheet (2-8) is arranged in a gap between the sample stage body (2-2) and the sample slot (2-3) which is not in contact with each other.
3. The ultra-high vacuum heating apparatus according to claim 2, wherein the sample insertion groove (2-3) comprises a sample insertion groove (2-3) body partially contacting with the sample stage main body (2-2), 2 main insertion grooves (2-7) vertically extending from a surface of the sample insertion groove (2-3) body, and 2 sample holder drop prevention pieces (2-9) fixedly connected with the 2 main insertion grooves (2-7), and a sliding groove structure is formed between each main insertion groove (2-7) and the sample holder drop prevention piece (2-9) at a top end portion.
4. The ultra-high vacuum heating device as claimed in claim 1, wherein the wire (3-5) is made of silver.
5. A heating method of the ultra-high vacuum heating apparatus according to claim 1, comprising the steps of:
the method comprises the following steps: fixing a sample (1-9) on the sample holder (1), and then inserting the sample holder (1) into a sample slot (2-3) to enable one end of the electric brush (2-12) to be lapped on an electric brush electrode plate (1-4) of the sample holder (1);
step two: connecting an adapter (2-1) with a magnetic rod which is positioned in a sample injection cavity in an atmospheric state, vacuumizing the sample injection cavity, opening a gate valve for communicating the vacuum cavity with the sample injection cavity when the vacuum reaches a proper value, sending a heating sample table (2) into the vacuum cavity from the sample injection cavity through the magnetic rod, inserting the heating sample table (2) into an intracavity positioning conductive column (3) positioned in the vacuum cavity, realizing butt joint of a positioning conductive jack (2-5) and a positioning conductive plug (3-4) and butt joint of a connecting hole (2-17) and a main positioning column (3-3), loosening the connection of the magnetic rod and the adapter (2-1), withdrawing the magnetic rod, and closing the gate valve;
step three: direct current is applied to the vacuum electrode (3-1), so that the sample (1-9) can be heated in vacuum, and real-time temperature monitoring can be realized through the infrared laser thermometer (5).
6. The method according to claim 5, characterized in that laser heating can be simultaneously or separately adopted in the third step, namely laser heating is realized by irradiating laser to the sample (1-9) through the central through hole of the hollow sample rack (1-1) by a laser heating instrument (4).
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| CN111139530A (en) * | 2020-01-20 | 2020-05-12 | 北京科技大学 | Rutile TiO2Single crystal ultrahigh vacuum treatment process |
| CN111710628B (en) * | 2020-06-03 | 2023-04-28 | 西安交通大学 | Multifunctional sample stage in ultrahigh vacuum environment and sample in-situ patterning method |
| CN114904592B (en) * | 2021-02-10 | 2024-05-07 | 中国科学院物理研究所 | Sample transfer device under ultrahigh vacuum condition |
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| NL260906A (en) * | 1960-02-12 | |||
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| DE1289829B (en) * | 1963-05-09 | 1969-02-27 | Siemens Ag | Process for producing a monocrystalline semiconductor layer by deposition from a reaction gas |
| US3915765A (en) * | 1973-06-25 | 1975-10-28 | Bell Telephone Labor Inc | MBE technique for fabricating semiconductor devices having low series resistance |
| DE3485738D1 (en) * | 1983-11-10 | 1992-06-25 | Texas Instruments Inc | MBE SYSTEM WITHOUT WELDING. |
| CN2458615Y (en) * | 2001-01-05 | 2001-11-07 | 中国科学院大连化学物理研究所 | Fast linear hyperthermic device for conductive sampler |
| CN1700017B (en) * | 2005-06-29 | 2010-05-05 | 中国科学院物理研究所 | Super high vacuum system sample feeding apparatus |
| CN2879192Y (en) * | 2005-06-30 | 2007-03-14 | 中国科学院物理研究所 | Sample receiving desk for new type super-high vacuum system sample transferring device |
| CN2837850Y (en) * | 2005-06-30 | 2006-11-15 | 中国科学院物理研究所 | Sample tray for sample conveying device of ultra-high vacuum system |
| CN2837847Y (en) * | 2005-09-27 | 2006-11-15 | 中国科学院物理研究所 | Five-dimensional low-temperature sample operating bench tray for ultra-high vacuum system |
| CN2837831Y (en) * | 2005-11-11 | 2006-11-15 | 中国科学院物理研究所 | Ultra-high vacuum in-situ growth, characterization and test system |
| JP5764246B1 (en) * | 2014-09-24 | 2015-08-19 | 株式会社日立国際電気 | Substrate processing apparatus, gas introduction shaft and gas supply plate |
| CN104711670B (en) * | 2015-04-02 | 2017-12-29 | 中国科学院上海微系统与信息技术研究所 | The sample carrier tested for molecular beam epitaxial growth and angle resolved photoelectron spectroscope |
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