CN115216747A

CN115216747A - Continuous preparation device for high-temperature superconducting material buffer layer

Info

Publication number: CN115216747A
Application number: CN202210817503.2A
Authority: CN
Inventors: 杨晨; 张学锋; 王启佳; 佟雷; 赵崇凌
Original assignee: Sky Development Co ltd Chinese Academy Of Sciences
Current assignee: Sky Development Co ltd Chinese Academy Of Sciences
Priority date: 2022-07-12
Filing date: 2022-07-12
Publication date: 2022-10-21
Anticipated expiration: 2042-07-12
Also published as: CN115216747B

Abstract

The invention belongs to the technical field of vacuum coating, and particularly relates to a continuous preparation device for a high-temperature superconducting material buffer layer. The invention adopts an integrated coating chamber structure, and a cleaning chamber, a drying chamber, a transition chamber, a coating chamber and a cooling chamber are respectively separated and sequentially communicated; the conveying parts are arranged in the drying chamber, the transition chamber and the coating chamber respectively, and the mechanical arms are arranged on the inner walls of the cleaning chamber, the cooling chamber and the coating chamber respectively, so that the conveying parts and the mechanical arms are matched for use to convey sample wafers, mechanical automation operation is facilitated, and production efficiency is improved.

Description

Continuous preparation device for high-temperature superconducting material buffer layer

Technical Field

The invention belongs to the technical field of vacuum coating, and particularly relates to a continuous preparation device for a high-temperature superconducting material buffer layer.

Background

In recent years, with the discovery of high temperature superconductors whose critical transition temperature is above the boiling point of liquid nitrogen, the use of high temperature superconducting thin films in integrated electronic and microwave devices has begun to begin, and has been rapidly developed over the last two decades. At present, YBCO and other high-temperature superconducting films are used for researching relatively hot.

In order to prepare a high-temperature superconducting coating with excellent performance, an oxide buffer layer is generally grown on a substrate. The transition function is realized between the substrate and the superconducting layer, so that impurity atoms in the substrate are prevented from entering the superconducting layer to pollute the film layer, and the texture of the substrate can be transferred to the superconducting layer. The crystal structure and the surface appearance of the superconducting thin film can directly play a decisive role in the electrical performance of the superconducting thin film.

With the currently commonly used LaMnO ₃ The oxide buffer layer is taken as an example, and the preparation method mainly comprises Physical Vapor Deposition (PVD) and Chemical Solution Deposition (CSD). The PVD method mainly adopts a pulse laser deposition method (PLD), direct current reactive magnetron sputtering and radio frequency magnetron sputtering technology, and the CSD method mainly adopts a metal organic deposition Method (MOD). However, in consideration of production cost, quality and efficiency, the surface of the film deposited by the MOD technology is rough and the density is poor, the reactive sputtering process is difficult to control, and the PLD technology cannot prepare a large-area film, which is not favorable for industrial production. Therefore, the most popular buffer layer preparation method at present is the radio frequency magnetron sputtering method.

But is limited by the vacuum environment and the device configuration, only one sheet can be produced at a time for larger size substrates. In each production process, the coating chamber of the existing preparation device needs to repeat the processes of vacuumizing, heating, ventilating, pressure controlling, sputtering, air discharging and cooling again, so that the production period of the product is longer, and the productivity and efficiency of the product are low. And for the LMO oxide film, a higher temperature needs to be maintained in the preparation process, when the temperature is lower than 800 ℃, the diffraction peak intensity is lower, and an MnO heterogeneous phase peak appears, so that the use requirement cannot be met. And the heating mode of the furnace plate and the filament used at the present stage can not maintain the sputtering of the substrate at high temperature for the production type large magnetron cavity, and the temperature difference between the surface of the substrate and the temperature of the furnace plate is more than 200 ℃ by measuring. The LMO film meeting the use standard can not be obtained, and the industrial continuous production can not be realized.

Disclosure of Invention

The invention aims to provide a continuous preparation device for a high-temperature superconducting material buffer layer, aiming at the problems that the temperature required by a high-quality LMO film is difficult to reach by a thermal field and continuous and rapid production cannot be realized in the conventional preparation of the LMO film by radio frequency magnetron sputtering.

The purpose of the invention is realized by the following technical scheme:

a continuous preparation device for a high-temperature superconducting material buffer layer comprises a cleaning chamber, a drying chamber, a transition chamber, a coating chamber and a cooling chamber which are sequentially and continuously arranged, wherein a sample injection door is arranged between the cleaning chamber and the drying chamber, a sealing door A is arranged between the drying chamber and the transition chamber, a sealing door B is arranged between the transition chamber and the coating chamber, a sealing door C is arranged between the coating chamber and the cooling chamber, and the cooling chamber is provided with a sampling door;

an ultrasonic cleaning assembly and a manipulator A are arranged in the cleaning chamber; the drying chamber is internally provided with a conveying component A and a drying heating component; a conveying component B is arranged in the transition chamber, a manipulator C and a conveying component C are arranged in the coating chamber, a cover plate is arranged at the top end of the coating chamber, a target rod is arranged on the cover plate, and the lower end of the target rod is connected with a rectangular plane magnetic control target; the cooling chamber is provided with a manipulator B, a rotary carrying part and a cooling part; photoelectric switches are respectively arranged at positions corresponding to the positions of two ends of the conveying component A in the drying chamber, positions corresponding to the positions of two ends of the conveying component B in the transition chamber, and positions corresponding to two ends and the middle position of the conveying component C in the coating chamber;

the dry chamber is provided with a dry gas outlet, the transition chamber, the coating chamber and the cooling chamber are respectively provided with a full-range gauge pipe, an exhaust port and a vacuum pumping port, the coating chamber is provided with a film gauge, an argon inlet and an oxygen inlet, and the cooling chamber is provided with a nitrogen inlet.

The utility model discloses a wash bowl, including wash bowl, elevating assembly, threaded rod, fixing platform, elevating assembly, water inlet and delivery port have been seted up respectively to wash bowl upper end opening, lower part, be equipped with inlet valve on the water inlet, be equipped with outlet valve on the delivery port, be equipped with the supporter in the wash bowl, it holds the chamber to be equipped with elevating assembly on the inner wall of wash bowl, elevating assembly holds the inside in chamber and is equipped with elevating assembly, elevating assembly includes elevating drive motor, threaded rod and fixed station, be equipped with on the fixed station with the nut that the threaded rod is connected, elevating drive motor drive rotate install in elevating assembly holds the threaded rod rotation in the chamber, and then through the vice drive of the spiral of nut and threaded rod formation the fixed station goes up and down along vertical direction, be equipped with the lower extreme of a plurality of parallel arrangement's inserted bar on the fixed station, each the upper end all with the upper end of supporter is connected.

The supporter holds in the palm from last to respectively a plurality of parallel arrangement's sample piece and accepts fork portion, every the sample piece holds in the palm and accepts the equal joint of fork portion and has a sample piece to hold in the palm, every the bottom periphery that the sample piece held in the palm all is seted up and is held in the palm the periphery draw-in groove of accepting fork portion and agreeing with mutually with the sample piece that corresponds.

The lowermost end of the commodity shelf is provided with a filter screen A.

Dry heater block includes dry gas holding vessel, dry gas air duct, heating rod group and fan group, the dry gas holding vessel set up in the outside of drying chamber, dry gas air duct one end with dry gas holding vessel intercommunication, the other end extend to the inner chamber top of drying chamber, the heating rod group sets up in the inner chamber top position of drying chamber, the fan group then set up in heating rod group downside in the drying chamber inner chamber.

The conveying component C is arranged in the middle of an inner cavity of the coating chamber and is divided into two conveying belt components which are arranged in parallel and have gaps between the conveying belt components, a conveying belt body of each conveying belt component is provided with an object carrying support limiting groove, the object carrying support limiting grooves on the conveying belt bodies of the two conveying belt components correspond to each other, an object carrying support is accommodated between the two object carrying support limiting grooves, and the object carrying support is uniformly provided with a plurality of sample wafer accommodating grooves;

a tantalum sheet heat-insulating layer C is arranged at the bottom of the coating chamber on the lower side of the conveying component C, a lifting platform is arranged on the lower side of the bottom of the coating chamber, the lifting end of the lifting platform penetrates through the coating chamber from the bottom, penetrates through the tantalum sheet heat-insulating layer C and is connected with a carrying tray, and the carrying tray is positioned in a gap between the two conveying belt components on the lower side of the carrying tray;

manipulator C install in the delivery unit C upside on the coating chamber inner wall, manipulator C upside install solid fixed ring on the coating chamber inner wall, gu fixed ring's last surface mounting has heat insulating ring, in the coating chamber install tantalum piece heat preservation A on the apron bottom surface, tantalum piece heat preservation A with between the heat insulating ring be equipped with tantalum piece heat preservation B on the coating chamber inner wall, install the heat-generating body on tantalum piece heat preservation B's the inner wall, tantalum piece heat preservation B's bottom reaches the bottom of heat-generating body all with the upper surface that heat insulating ring laminated mutually.

The infrared temperature measuring port is formed in the cover plate, the cover plate lifting part used for driving the cover plate to lift is installed on the outer side of the coating chamber, and the driving end of the cover plate lifting part is connected with the cover plate.

Install rotary driving motor on the bottom surface of cooling chamber, rotatory objective part includes objective table and roating seat, the top of roating seat with the bottom surface of objective table is connected, the bottom with penetrate the inside rotary driving motor output of cooling chamber is connected, seted up a plurality of thing grooves of putting on the top surface of objective table, each put and all seted up a plurality of through-holes on the bottom surface in thing groove, manipulator B install in the objective table upside on the cooling chamber inner wall.

The cooling part comprises a roots pump, a water cooler and an air outlet disc, the roots pump and the water cooler are respectively arranged on the outer side of the cooling chamber, the air outlet disc is arranged inside the cooling chamber, an air flow channel is arranged inside the air outlet disc and is communicated with the output end of the roots pump, a plurality of air holes respectively communicated with the air flow channel are formed in the bottom surface of the air outlet disc, the input end of the roots pump is communicated with one end of a spiral cooling pipe, the spiral cooling pipe penetrates through a to-be-cooled port of the water cooler, a plurality of air outlets are formed in the bottom of the cooling chamber, the lower end of each air outlet is respectively communicated with one input end of an air exhaust pipe, and the output end of the air exhaust pipe is communicated with the other end of the spiral cooling pipe.

The input end of the Roots pump is provided with filter cotton for filtering gas input from the spiral cooling pipe; and a filter screen B is arranged at the lower end of the air outlet.

The invention has the advantages and positive effects that:

1. the invention adopts an integrated coating chamber structure, and a cleaning chamber, a drying chamber, a transition chamber, a coating chamber and a cooling chamber are respectively separated and sequentially communicated; the conveying parts are arranged in the drying chamber, the transition chamber and the coating chamber respectively, and the mechanical arms are arranged on the inner walls of the cleaning chamber, the cooling chamber and the coating chamber respectively, so that the conveying parts and the mechanical arms are matched for use to convey sample wafers, mechanical automation operation is facilitated, and production efficiency is improved.

2. The inner wall of the upper part of the coating chamber is fixed with a multilayer tantalum sheet structure heat-insulating layer, the inner wall of the tantalum sheet heat-insulating layer is provided with an annular molybdenum heating body, and the upper part of the cover plate of the coating chamber is fixedly provided with an infrared temperature measuring system, so that the temperature in the coating chamber can be rapidly increased to more than 900 ℃, and the internal high-temperature in the coating chamber can be uniformly and accurately controlled.

3. Set up sealing door A and sealing door B respectively at the left end and the right-hand member of transition cavity, set up sealing door C at the left end of cooling chamber, set up the vacuum extraction pipeline in the upper end of coating film room, cooling chamber and transition cavity to independently adjust the atmospheric pressure of every cavity, thereby when guaranteeing production, avoid the coating film room to bleed repeatedly, heat up, cool down, reduce product production cycle, improve product production efficiency.

4. Be equipped with in the cooling chamber and have a plurality of circular objective tables of putting the thing groove, the upper end sets up nitrogen gas logical mouth and lobe pump, and the outside is provided with the cold water machine to in the while realize quick cooling to a plurality of sample wafers, greatly shortened production cycle.

Drawings

FIG. 1 is a schematic overall front view of the present invention;

FIG. 2 is a schematic top view of the present invention;

FIG. 3 is a schematic structural diagram of a sample holder according to the present invention;

FIG. 4 is a schematic view of the structure of a conveying member C of the present invention;

fig. 5 is a schematic structural diagram of the stage of the present invention.

In the figure: <xnotran> 1 , 2 , 3 , 4 , 5 , 6 , 701 A, 702 B, 703 C, 8 A, 9 B, 10 C, 11 , 12 , 13 , 14 , 15 , 16 A, 17 B, 18 , 19 , 20 , 21 , 22 , 23 , 24 A, 25 , 26 , 27 , 28 , 29 , 30 , 31 A, 32 B, 33 C, 34 , 35 , 36 , 37 , 38 , 39 , 40 , 41 , 42 , 43 , 44 B, 45 , 46 , 47 , 48 , 49 , 50 , 51 , 52 , 53 , 54 , 55 , 56 , 57 , 58 , 59 , 60 , 61 , 62 , 63 , 64 , 65 , 66 , 67 C, 68 . </xnotran>

Detailed Description

The invention is described in further detail below with reference to figures 1-5.

A continuous preparation device for a high-temperature superconducting material buffer layer is shown in figures 1-5, and comprises a cleaning chamber 6, a drying chamber 2, a transition chamber 3, a coating chamber 4 and a cooling chamber 5 which are sequentially and continuously arranged in the embodiment, wherein a sample injection door 52 is arranged between the cleaning chamber 6 and the drying chamber 2, a sealing door A8 is arranged between the drying chamber 2 and the transition chamber 3, a sealing door B9 is arranged between the transition chamber 3 and the coating chamber 4, a sealing door C10 is arranged between the coating chamber 4 and the cooling chamber 5, and the cooling chamber 5 is hinged with a sampling door 57. In the embodiment, the drying chamber 2 and the transition chamber 3 are respectively arranged on the operating platform 1, the cleaning chamber 6 is arranged on the left side of the operating platform 1, the coating chamber 4 is arranged on the right side of the operating platform 1, and the cooling chamber 5 is arranged on the right side of the coating chamber 4. The inside of the operation platform 1 is equipped with an automatic control system, and the automatic control system in the present embodiment adopts the prior art, for example, it can be an industrial automatic control system based on mass production disclosed in patent No. CN201410317572.2, or other automatic control systems matched with the present invention. The sample inlet door 52, the sealing door A8, the sealing door B9 and the sealing door C10 are all sealing doors which are longitudinally opened in the prior art, the automatic opening device can be a furnace door automatic lifting structure of a large-capacity submerged arc furnace disclosed in the patent number CN201620547462.X, or other sealing door lifting mechanisms matched with the invention, and the sealing door lifting mechanisms of all the sealing doors are electrically connected with an automatic control system.

An ultrasonic cleaning assembly and a manipulator A16 are arranged in the cleaning chamber 6; a conveying component A701 and a drying heating component are arranged in the drying chamber 2; a conveying component B702 is arranged in the transition chamber 3, a manipulator C67 and a conveying component C703 are arranged in the coating chamber 4, a cover plate 11 is arranged at the top end of the coating chamber 4, a target rod 12 is arranged on the cover plate 11, and the lower end of the target rod 12 is connected with a rectangular plane magnetic control target 13; the cooling chamber 5 is provided with a robot B17, a rotary loading member, and a cooling member. The manipulator a 16, the manipulator B17 and the manipulator C67 are all the prior art, and may be, for example, an underwater hydraulic manipulator disclosed in patent No. CN201621272518.1, or other high-temperature resistant five-axis linkage clamping manipulators compatible with the present invention, and each manipulator and the conveying component are respectively used in cooperation to convey the sample wafer. In this embodiment, the target rod 12 and the rectangular planar magnetron target 13 are both arranged in the prior art, wherein the target rod 12 is provided with a lifting adjusting device, and the lifting adjusting device can be an automatic lifting device disclosed in the patent number CN201610498114.2 or other lifting adjusting devices matched with the present invention, so as to facilitate the adjustment of the target base distance; the rectangular plane magnetic control target 13 is a rectangular plane magnetic control target product manufactured by Shenyang scientific instrument development center, ltd. The conveying component A701 and the conveying component B702 are both high-temperature resistant belt conveyors in the prior art, the belts are controlled by a servo motor to rotate, the pulse numbers of the two ends of each section of conveying component and the middle position of the conveying component in the coating chamber 4 are respectively measured, and anti-deviation grooves for preventing the sample wafers from deviating towards two sides are arranged on the belts of the conveying component A701 and the conveying component B702. Photoelectric switches for detecting and controlling the positions of the sample wafers are respectively arranged at positions corresponding to the positions of two ends of the conveying component A701 in the drying chamber 2, positions corresponding to the positions of two ends of the conveying component B702 in the transition chamber 3 and positions corresponding to two ends and the middle position of the conveying component C703 in the coating chamber 4, the photoelectric switches are all commercially available products and are respectively connected with an automatic control system, the photoelectric switches at the inlets of the chambers are used as control original points, and the photoelectric switches at the outlets play a protection role. In the belt movement process of the conveying component, the PLC of the industrial automatic control system sends out corresponding pulse numbers to realize the belt movement to the designated action, and the position precision is accurately controlled by combining the photoelectric switch and the servo motor. The ultrasonic cleaning component in the cleaning chamber 6 adopts the prior art and is the same as the ultrasonic cleaning mechanism of the existing ultrasonic cleaning machine.

The drying chamber 2 is provided with a dry gas outlet for discharging dry gas, the transition chamber 3, the coating chamber 4 and the cooling chamber 5 are respectively provided with a full-range gauge pipe 60, an exhaust port 55 and a vacuum pumping port 56, the coating chamber 4 is provided with a film gauge 64, an argon gas inlet 58 and an oxygen gas inlet 61, and the cooling chamber 5 is provided with a nitrogen gas inlet 59. Each of the exhaust ports 55 is provided with an open/close valve for discharging the gas inside each chamber. The argon inlet 58 and the oxygen inlet 61 are respectively connected with an external argon source and an oxygen source for use in film coating. Each vacuum pumping hole 56 is connected with an external vacuum pumping system through a pipeline respectively, the connected pipelines are all provided with electromagnetic valves, the external vacuum pumping system is a pumping system mainly based on a pumping pump in the prior art, and each electromagnetic valve and the pumping pump are connected with an automatic control system. The full-range gauge pipe 60 and the film gauge 64 are commercially available products, can respectively measure the vacuum degree in each chamber, are matched with each sealing door for use, are convenient for independently adjusting the pressure intensity of each chamber, are matched with an external vacuum pumping system for use, and are electrically connected with an automatic control system so as to realize automatic pressure control.

Particularly, 6 upper end openings in order to put into sample wafer and sample wafer support 26 in this embodiment, water inlet and delivery port have been seted up respectively to the lower part, be equipped with inlet valve 62 on the water inlet, be equipped with outlet valve 63 on the delivery port, be equipped with supporter 23 in the purge chamber 6, it holds chamber 18 to be equipped with lifting unit on the inner wall of purge chamber 6, lifting unit holds the inside in chamber 18 and is equipped with lifting unit, lifting unit holds chamber 18 and plays the effect of separating its inside lifting unit and the washing liquid in purge chamber 6, lifting unit includes lift driving motor 21, threaded rod 19 and fixed station 20, be equipped with the nut of being connected with threaded rod 19 on the fixed station 20, lift driving motor 21 drive rotates and installs the threaded rod 19 rotation in lifting unit holds chamber 18, and then the vice drive fixed station 20 of spiral that forms through nut and threaded rod 19 goes up and down along vertical direction, be equipped with the lower extreme of a plurality of parallel arrangement's inserted bar 22 on the fixed station 20, the upper end of each inserted bar 22 all is connected with the upper end of supporter 23. The lifting driving motor 21 is a commercially available product and is controlled to act by an automatic control system. Supporter 23 holds in the palm and accepts fork portion from last to a plurality of parallel arrangement's sample piece respectively down, and every sample piece holds in the palm and accepts the equal joint of fork portion and has a sample piece to hold in the palm 26, and every sample piece holds in the palm the bottom periphery of 26 and all offers and holds in the palm the periphery draw-in groove 25 of accepting fork portion and agreeing with mutually with the sample piece that corresponds. The filter screen A24 is installed at the lowest end of the storage rack 23, so that impurities on the surface of the sample wafer are prevented from blocking a water inlet and a water outlet, and cleaning is facilitated. The water inlet valve 62 and the water outlet valve 63 are commercially available electromagnetic valves, the water inlet valve 62 and the water outlet valve 63 are respectively controlled to be opened and closed by an automatic control system, wherein the water inlet valve 62 is communicated with an external water source, and the water outlet valve 63 is communicated with an external sewage collecting system for realizing automatic replacement of the cleaning liquid, and the cleaning liquid adopts deionized water in the prior art. Through the arrangement of the lifting component, the shelf 23 can be driven to automatically lift before and after the sample wafer is ultrasonically cleaned, so that the sample wafer can be conveniently taken out and fully immersed into the cleaning liquid in the cleaning chamber 6; the sample wafer support 26 is convenient to disassemble and can be replaced according to sample wafers with different sizes, and ultrasonic cleaning of the sample wafers with different sizes can be achieved.

Specifically, the drying heating component in this embodiment includes a dry air storage tank 30, a dry air duct 29, a heating rod set 27 and a fan set 28, the dry air storage tank 30 is disposed outside the drying chamber 2, one end of the dry air duct 29 is communicated with the dry air storage tank 30, the other end extends to the top of the inner cavity of the drying chamber 2, the heating rod set 27 is disposed on the top of the inner cavity of the drying chamber 2, and the fan set 28 is disposed in the inner cavity of the drying chamber 2 below the heating rod set 27. In this embodiment, the heating rod group 27 includes a plurality of heating rods arranged in parallel at the same height, and the fan group 28 includes a plurality of fans arranged in parallel at the same height, and each of the heating rods and the fans is a commercially available product. The drying gas may be compressed inert gas or nitrogen. The dry gas guide pipe 29 is provided with an electromagnetic valve which is controlled to open by an automatic control system and can control the flow; the solenoid valve is opened and compressed inert gas or nitrogen is introduced into the drying chamber 2. Through the setting of dry heating part, can carry out abundant drying to the sample piece earlier before carrying out the coating film, let in dry gas simultaneously when through the drying, increase gaseous flow to take away the volatile water in sample piece surface fully, unnecessary gas is followed the dry gas discharge port and is discharged in drying chamber 2.

Particularly, conveying part C703 installs in coating chamber 4's inner chamber middle part in this embodiment, conveying part C703 divide into two parallel arrangement and have gapped conveyer belt assembly between, the conveyer belt body of every conveyer belt assembly has all been seted up and has been carried thing support spacing groove 65, and carry on the conveyer belt body of two conveyer belt assemblies and hold in the palm mutual correspondence between the spacing groove 65, two carry and hold in the palm the thing support 66 between the thing support spacing groove 65, carry and evenly seted up four appearance piece holding grooves on the thing support 66. The drive structure of every conveyer belt subassembly in this embodiment is current high temperature resistant band conveyer technique also, adopts servo motor control belt reciprocating rotation, and then drives and carry the reciprocating rotation of thing support 66. A plurality of sample wafers can be simultaneously carried for film coating through the arrangement of the object carrying support 66, and the object carrying support 66 can be replaced according to the size of the sample wafers.

A tantalum sheet heat-insulating layer C33 is arranged at the bottom of the coating chamber 4 on the lower side of the conveying component C703, a lifting table 14 is arranged on the lower side of the bottom of the coating chamber 4, the lifting end of the lifting table 14 penetrates through the coating chamber 4 from the bottom, penetrates through the tantalum sheet heat-insulating layer C33 and is connected with a carrying tray 15, and the carrying tray 15 is positioned in a gap between the two conveying belt components on the lower side of the carrying tray 66. The lifting platform 14 is a conventional technology, and is controlled to lift by an automatic control system, the lifting end of the lifting platform 14 is lifted, so that the carrying tray 15 can support the carrying tray 66 on the conveying component C703, and the rectangular plane magnetron target 13 can coat the sample wafer on the lifted carrying tray 66.

The manipulator C67 is installed on the coating chamber 4 inner wall of the upside of the conveying component C703, the fixing ring 34 is installed on the coating chamber 4 inner wall of the upside of the manipulator C67, the heat insulation ring 34 is installed on the upper surface of the fixing ring 34, the tantalum sheet heat insulation layer A31 is installed on the bottom surface of the cover plate 11 in the coating chamber 4, the tantalum sheet heat insulation layer B32 is arranged on the coating chamber 4 inner wall between the tantalum sheet heat insulation layer A31 and the heat insulation ring 34, the heating body 36 is installed on the inner wall of the tantalum sheet heat insulation layer B32, and the bottom end of the tantalum sheet heat insulation layer B32 and the bottom end of the heating body 36 are attached to the upper surface of the heat insulation ring 34. The heat insulating ring 34 is made of glass fiber. The heating element 36 is a ring-shaped molybdenum heating element in the prior art, is powered by an external power supply and is controlled to be opened and closed by an automatic control system. The space surrounded by the tantalum sheet heat-insulating layer A31 and the tantalum sheet heat-insulating layer B32 on the upper side of the fixing ring 34 is a heating film coating area, and the carrying tray 15 supports the carrying tray 66 to the heating film coating area so as to coat the sample wafer.

An infrared temperature measuring port 54 is formed in the cover plate 11, a cover plate lifting member 53 for driving the cover plate 11 to lift is installed on the outer side of the film coating chamber 4, and the driving end of the cover plate lifting member 53 is connected with the cover plate 11. The cover plate lifting member 53 in this embodiment is a cylinder or an electric support rod in the prior art, and is controlled by an automatic control system. The cover plate lifting piece 53 is arranged to facilitate the environmental cleaning of the coating chamber 4 inside by the cover plate 11. The infrared temperature measuring port 54 is used for connecting an external infrared temperature measuring device to measure the surface temperature of the sample wafer, and the external infrared temperature measuring device can be an infrared temperature measuring device disclosed in the patent number CN201910216384.3 or other infrared temperature measuring devices matched with the invention.

Specifically, install rotary driving motor 51 on the bottom surface of cooling chamber 5 in this embodiment, the rotary object carrying part includes objective table 48 and roating seat 47, objective table 48 is circular, the top of roating seat 47 is connected with objective table 48's bottom surface, the bottom is connected with the rotary driving motor 51 output that penetrates cooling chamber 5 inside, a plurality of thing grooves 49 have evenly been seted up on objective table 48's the top surface, can place the sample piece after a plurality of coating films and cool off simultaneously, all seted up a plurality of through-holes 50 that are used for passing through gas on each thing groove 49's the bottom surface, manipulator B17 installs on the cooling chamber 5 inner wall of objective table 48 upside. The number of the storage slots 49 corresponds to the number of the specimen accommodation grooves. The rotary drive motor 51 is a commercially available product and is controlled by an automatic control system. The rotary driving motor 51 drives the object stage 48 connected with the rotary seat 47 to rotate, so that various sheets can be uniformly cooled; the through holes 50 are provided to enhance the cooling effect of the coupon.

Specifically, in the present embodiment, the cooling unit includes the roots pump 37, the water chiller 42, and the gas outlet disk 40, the roots pump 37 and the water chiller 42 are respectively installed outside the cooling chamber 5, and the roots pump 37 and the water chiller 42 are commercially available products and are controlled to operate by an automatic control system. The air outlet disc 40 is arranged inside the cooling chamber 5, an air flow channel is arranged inside the air outlet disc 40, the air flow channel is communicated with the output end of the Roots pump 37 through an air conveying pipe 39, a plurality of air holes 41 respectively communicated with the air flow channel are formed in the bottom surface of the air outlet disc 40, the input end of the Roots pump 37 is communicated with one end of a spiral cooling pipe 68, the spiral cooling pipe 68 penetrates through a to-be-cooled port of the water cooler 42, a plurality of air outlets 43 are formed in the bottom of the cooling chamber 5, the lower end of each air outlet 43 is respectively communicated with one input end of an air extraction pipe 46, the lower end of each air outlet 43 is connected with one input end of the air extraction pipe 46 through a quick-release clamp 45, and the output end of the air extraction pipe 46 is communicated with the other end of the spiral cooling pipe 68. The spiral cooling pipe 68 is provided so that the nitrogen gas can be sufficiently cooled in the spiral cooling pipe 68 by the water chiller 42. The input end of the roots pump 37 is provided with filter cotton 38 for filtering the gas input from the spiral cooling pipe 68, and the arrangement of the filter cotton 38 is the prior art, so that the nitrogen gas is prevented from entering the cavity of the roots pump 37 in a liquid form in the circulation. The lower end of the air outlet 43 is provided with a filter screen B44, the filter screen B44 is arranged between the lower end of the air outlet 43 on the inner side of the quick-release clamp 45 and the input end of the exhaust tube 46, and the filter screen B44 is 350-600 meshes and has the aperture of 0.0395-0.023 mm so as to prevent impurity blockage. Through the cooperation setting of lobe pump 37, gas outlet disk 40, exhaust tube 46 and water chiller 42, can realize that nitrogen gas constantly circulates in cooling chamber 5 and cools off the sample wafer, reduces the energy consumption. A plurality of uniformly distributed air holes 41 are formed in the bottom surface of the air outlet disc 40, so that nitrogen is discharged through the uniformly distributed air holes 41 in the air outlet disc 40, and the sample wafer can be rapidly cooled.

The working principle is as follows:

when the sample wafer cleaning device is used, sample wafers are respectively placed in sample wafer supports 26 with corresponding sizes, the sample wafer supports 26 are sequentially placed on the storage rack 23, the lifting driving motor 21 drives the threaded rod 19 vertically arranged in the lifting component accommodating cavity 18 to rotate, and then the storage rack 23 can be driven to automatically lift before and after the sample wafers are subjected to ultrasonic cleaning, so that the sample wafers can be conveniently taken out and fully immersed into cleaning liquid in the cleaning chamber 6; the arrangement of the water inlet and the water outlet is convenient for realizing automatic cleaning liquid replacement.

After the cleaning, the sample introduction door 52 is opened, the manipulator a 16 is matched with the conveying component a 701 in the drying chamber 2, and the sample wafer is transferred to the conveying component a 701, in this embodiment, the conveying component a 701 can move four sample wafers at a time, and the conveying component a 701 is electrically connected with an automatic control system to control the running speed and time of the conveyor belt of the conveying component a 701 through a program so as to achieve the purpose of controlling the drying time.

Subsequently, the sample introduction door 52 is closed, the flow of inert gas or nitrogen gas in the drying chamber 2 is increased by heating the sample by the heater bar group 27 and the fan group 28, and the sample drying time controls the movement of the sample and whether to start heating by the setting and conveying part a 701 of the operation table 1. After drying is finished, the sample wafer is conveyed to the conveying component B702 by the conveying component A701 and enters the transition chamber 3, the sealing door A8 and the exhaust port 55 of the transition chamber 3 are closed, vacuumizing is performed through an external vacuum pumping system, and when the reading number of the full-range gauge pipe 60 reaches below 8E-4, the air pressure of the transition chamber 3 is the same as that of the coating chamber 4; then, the sealing door B9 is opened, the carrier 66 on which the sample can be placed is fixed to the transfer unit C703 in the coating chamber 4, the sample on the transfer unit B702 is placed on the carrier 66 in the coating chamber 4 by the robot C67, and then the sealing door B9 is closed.

When the carrier tray 66 is conveyed to the middle position of the conveying component C703, the conveying component C703 stops moving, and the lifting platform 14 drives the carrier tray 15 to lift up the carrier tray 66 with the sample wafer placed thereon and slowly lift up to enter the heating coating area; after the surface of the sample wafer reaches 900 ℃ measured by an external infrared temperature measuring device, argon and oxygen are respectively introduced into an argon inlet 58 and an oxygen inlet 61 of the film coating chamber 4, the oxygen flow is controlled to be 10-35sccm, the argon gas flow is controlled to be 50-100 sccm, the air pressure is 0.5-3Pa, the rectangular plane magnetic control target 13 starts sputtering, and the target material uses high-purity LaMnO ₃ A target material; after 5-10h, the film growth is finished, the lifting platform 14 is controlled to shrink and reset, the carrying tray 15 slowly descends, and the carrying tray 66 falls into the carrying tray limiting groove 65 and continues to move along with the conveying component C703; when the carrying tray 66 is conveyed to the right-side junction, the conveying is stopped; adjusting the pressure in the cooling chamber 5 in the same manner as the pressure adjustment of the transition chamber 3, opening the sealing door C10, taking out the sample wafer by the manipulator B17, placing the sample wafer in the storage groove 49 on the storage table 48 in the cooling chamber 5, and closing the sealing door C10; the conveying component C703 in the coating chamber 4 moves reversely, and the carrying support 66 returns to the left side delivery position to wait for transferring the next batch of sample wafers; the shape of the inner groove of the carrying tray can be square or round and is determined by the size and the shape of the sample wafer.

After the nitrogen inlet 59 is opened in the cooling chamber 5 and a certain content of nitrogen is introduced, the nitrogen inlet 59 is closed; starting the roots pump 37 and the water chiller 42, and circulating nitrogen in the cooling chamber to cool the surface of the sample wafer; then, the exhaust port 55 of the cooling chamber 5 is opened, and the sampling gate 57 is opened to sample; the sampling door 57 is closed after sampling, so that in the automatic production process, the coating chamber 4 is stable at high temperature, the air pressure and temperature in the coating chamber 4 are prevented from being repeatedly adjusted, the sample wafer is rapidly cooled, the production period of the product is shortened, and the product quality and the production efficiency are improved.

Claims

1. A continuous preparation device for a high-temperature superconducting material buffer layer is characterized in that: the device comprises a cleaning chamber (6), a drying chamber (2), a transition chamber (3), a coating chamber (4) and a cooling chamber (5) which are sequentially and continuously arranged, wherein a sample introduction door (52) is arranged between the cleaning chamber (6) and the drying chamber (2), a sealing door A (8) is arranged between the drying chamber (2) and the transition chamber (3), a sealing door B (9) is arranged between the transition chamber (3) and the coating chamber (4), a sealing door C (10) is arranged between the coating chamber (4) and the cooling chamber (5), and the cooling chamber (5) is provided with a sampling door (57);

an ultrasonic cleaning assembly and a manipulator A (16) are arranged in the cleaning chamber (6); a conveying component A (701) and a drying heating component are arranged in the drying chamber (2); a conveying component B (702) is arranged in the transition chamber (3), a manipulator C (67) and a conveying component C (703) are arranged in the coating chamber (4), a cover plate (11) is arranged at the top end of the coating chamber (4), a target rod (12) is arranged on the cover plate (11), and the lower end of the target rod (12) is connected with a rectangular plane magnetic control target (13); the cooling chamber (5) is provided with a manipulator B (17), a rotary carrying part and a cooling part; photoelectric switches are respectively arranged at positions corresponding to the positions of two ends of the conveying component A (701) in the drying chamber (2), positions corresponding to the positions of two ends of the conveying component B (702) in the transition chamber (3), and positions corresponding to two ends and the middle position of the conveying component C (703) in the coating chamber (4);

be equipped with the dry gas discharge port on drying chamber (2), all be equipped with full range rule pipe (60), gas vent (55) and vacuum extraction opening (56) on transition cavity (3), coating chamber (4) and cooling chamber (5), be equipped with film rule (64), argon gas logical opening (58) and oxygen logical opening (61) on coating chamber (4), be equipped with nitrogen gas logical opening (59) on cooling chamber (5).

2. The continuous fabrication apparatus for a high-temperature superconducting material buffer layer according to claim 1, wherein: water inlet and delivery port have been seted up respectively to purge chamber (6) upper end opening, lower part, be equipped with inlet valve (62) on the water inlet, be equipped with outlet valve door (63) on the delivery port, be equipped with supporter (23) in purge chamber (6), be equipped with lifting unit on the inner wall of purge chamber (6) and hold chamber (18), lifting unit holds the inside in chamber (18) and is equipped with lifting unit, lifting unit includes lift driving motor (21), threaded rod (19) and fixed station (20), be equipped with on fixed station (20) with the nut that threaded rod (19) are connected, lift driving motor (21) drive rotate install in lifting unit holds threaded rod (19) rotation in chamber (18), and then through the vice drive of the spiral that nut and threaded rod (19) formed fixed station (20) go up and down along vertical direction, be equipped with the lower extreme of a plurality of parallel arrangement's inserted bar (22) on fixed station (20), each the upper end of inserted bar (22) all with the upper end of supporter (23) is connected.

3. The continuous fabrication apparatus for a high-temperature superconducting material buffer layer according to claim 2, wherein: supporter (23) are from last to holding in the palm of respectively a plurality of parallel arrangement's sample piece and accept fork portion, every the sample piece holds in the palm and accepts the equal joint of fork portion and has a sample piece to hold in the palm (26), every the bottom periphery that sample piece held in the palm (26) all is seted up and is held in the palm the periphery draw-in groove (25) of accepting fork portion agreeing with the sample piece that corresponds.

4. The continuous fabricating apparatus for a buffer layer of high temperature superconducting material according to claim 3, wherein: and a filter screen A (24) is arranged at the lowest end of the article placing rack (23).

5. The continuous fabricating apparatus for a buffer layer of high temperature superconducting material according to claim 1, wherein: dry heater block includes dry gas holding vessel (30), dry gas air duct (29), heater rod group (27) and fan group (28), dry gas holding vessel (30) set up in the outside of drying chamber (2), dry gas air duct (29) one end with dry gas holding vessel (30) intercommunication, the other end extend to the inner chamber top of drying chamber (2), heater rod group (27) set up in the inner chamber top position of drying chamber (2), fan group (28) then set up in heater rod group (27) downside in drying chamber (2) the inner chamber.

6. The continuous fabricating apparatus for a buffer layer of high temperature superconducting material according to claim 1, wherein: the conveying component C (703) is arranged in the middle of an inner cavity of the coating chamber (4), the conveying component C (703) is divided into two conveying belt components which are arranged in parallel and have gaps between the conveying belt components, a conveying belt body of each conveying belt component is provided with an object carrying support limiting groove (65), the object carrying support limiting grooves (65) on the conveying belt bodies of the two conveying belt components correspond to each other, an object carrying support (66) is accommodated between the two object carrying support limiting grooves (65), and a plurality of sample wafer accommodating grooves are uniformly formed in the object carrying support (66);

a tantalum sheet heat-insulating layer C (33) is arranged at the bottom of the coating chamber (4) on the lower side of the conveying component C (703), a lifting table (14) is arranged on the lower side of the bottom of the coating chamber (4), the lifting end of the lifting table (14) penetrates from the bottom of the coating chamber (4), penetrates through the tantalum sheet heat-insulating layer C (33) and is connected with a carrying disc (15), and the carrying disc (15) is positioned in a gap between the two conveying belt components on the lower side of the carrying tray (66);

manipulator C (67) install in carry part C (703) upside on coating film room (4) inner wall, manipulator C (67) upside install solid fixed ring (34) on coating film room (4) inner wall, the last surface mounting of solid fixed ring (34) has heat insulating ring (34), in coating film room (4) install tantalum piece heat preservation A (31) on apron (11) bottom surface, tantalum piece heat preservation A (31) with between heat insulating ring (34) be equipped with tantalum piece heat preservation B (32) on coating film room (4) inner wall, install heat-generating body (36) on the inner wall of tantalum piece heat preservation B (32), the bottom of tantalum piece heat preservation B (32) reaches the bottom of heat-generating body (36) all with the upper surface of heat insulating ring (34) is laminated mutually.

7. The continuous fabrication apparatus for a high-temperature superconducting material buffer layer according to claim 6, wherein: the coating device is characterized in that an infrared temperature measuring port (54) is formed in the cover plate (11), a cover plate lifting piece (53) used for driving the cover plate (11) to lift is installed on the outer side of the coating chamber (4), and the driving end of the cover plate lifting piece (53) is connected with the cover plate (11).

8. The continuous fabricating apparatus for a buffer layer of high temperature superconducting material according to claim 1, wherein: install rotation driving motor (51) on the bottom surface of cooling chamber (5), rotatory thing parts of carrying include objective table (48) and roating seat (47), the top of roating seat (47) with the bottom surface of objective table (48) is connected, the bottom with penetrate the inside rotation driving motor (51) output of cooling chamber (5) is connected, a plurality of thing grooves (49) of putting have been seted up on the top surface of objective table (48), each put and all seted up a plurality of through-holes (50) on the bottom surface of thing groove (49), manipulator B (17) install in objective table (48) upside on cooling chamber (5) inner wall.

9. The continuous fabrication apparatus for a high-temperature superconducting material buffer layer according to claim 1, wherein: the cooling part comprises a roots pump (37), a water cooler (42) and an air outlet disc (40), the roots pump (37) and the water cooler (42) are respectively installed on the outer side of the cooling chamber (5), the air outlet disc (40) is arranged inside the cooling chamber (5), an air flow channel is arranged inside the air outlet disc (40), the air flow channel is communicated with the output end of the roots pump (37), a plurality of air holes (41) respectively communicated with the air flow channel are formed in the bottom surface of the air outlet disc (40), the input end of the roots pump (37) is communicated with one end of a spiral cooling pipe (68), the spiral cooling pipe (68) penetrates through a to-be-cooled port of the water cooler (42), a plurality of air outlets (43) are formed in the bottom of the cooling chamber (5), the lower end of each air outlet (43) is respectively communicated with one input end of an air extraction pipe (46), and the output end of the air extraction pipe (46) is communicated with the other end of the spiral cooling pipe (68).

10. The continuous fabrication apparatus for a high temperature superconducting material buffer layer according to claim 9, wherein: the input end of the roots pump (37) is provided with filter cotton (38) for filtering the gas input from the spiral cooling pipe (68); and a filter screen B (44) is arranged at the lower end of the air outlet (43).