CN216115372U - Sublimation instrument - Google Patents

Abstract

The utility model relates to a sublimation apparatus, comprising: a plurality of heating temperature field structures are distributed in the furnace body; wrapping a furnace tube in the furnace body; one side of the furnace tube is connected with a vacuum system through a gate valve mechanism; the master control system controls the vacuum system to perform vacuum extraction control on the furnace tube; when the vacuum degree in the furnace tube reaches a preset value, the main control system controls the heating temperature field structure in a segmented manner to heat the furnace tube, or inert gas is filled into the furnace tube; heating the furnace tube by controlling the heating temperature field structure in a segmented manner, so that the material in the furnace tube is sublimated and collected again; the furnace tube is vacuumized by a vacuum system to reach a vacuum state, or inert gas is filled into the furnace tube, so that the material to be purified is sublimated in a vacuum state or under other inert protection, the purity requirement of the organic optoelectronic materials in the fields of OLED, OPV and the like is met, and the technical problem that the loss of the purified material is very large is solved.

Description

Sublimation instrument

Technical Field

The embodiment of the utility model relates to small molecule material purification equipment, in particular to a sublimation instrument.

Background

In the application aspect of the existing small molecule luminescent material, the requirement on the purity of the small molecule luminescent material is very high, the purification is carried out only by a heating mode according to the existing purification equipment, so that the purity, yield and the like of the organic optoelectronic materials applied to the fields of OLED, OPV and the like can not meet the requirements of the organic optoelectronic materials in the fields of OLED, OPV and the like, and the loss of the purified materials is very large.

SUMMERY OF THE UTILITY MODEL

An object of an embodiment of the present invention is to provide a sublimator capable of automatically purifying equipment while ensuring the purity of a purified material while reducing the loss of a material to be purified.

In order to achieve the above object, an embodiment of the present invention provides a sublimation apparatus including:

the cabinet body is arranged below the sublimation instrument;

the furnace body is fixed above the cabinet body, and a plurality of heating temperature field structures are distributed in the furnace body;

the furnace tube is wrapped in the furnace body;

the vacuum system is connected with one side of the furnace tube through a gate valve mechanism;

the main control system controls the vacuum system to perform vacuum extraction control on the furnace tube; when the vacuum degree in the furnace tube reaches a preset value, the main control system controls the heating temperature field structure in a segmented mode to heat the furnace tube, or controls the furnace tube to be filled with inert gas; and then, the main control system controls the heating temperature field structure in a segmented manner to heat the furnace tube, so that the material in the furnace tube is sublimated and collected again.

Further, the furnace body still includes:

an upper furnace body; the upper furnace body is in a semicircular shape and is transversely arranged along a preset axis of the furnace body;

the lower furnace body is in a semicircular shape and is connected with the upper furnace body through a hinge structure;

the upper furnace body and the lower furnace body are internally provided with a plurality of heating temperature field structures along the preset axis of the furnace body, and the heating temperature field structures are transversely arranged in parallel at non-average intervals along the preset axis.

The upper furnace body is transversely arranged along the central axis of the furnace body along the unfolding direction, and a semicircular first cavity is arranged on the upper furnace body along the central axis of the furnace body;

the lower furnace body is transversely arranged along the furnace body along the unfolding direction, and a semicircular second cavity is arranged on the lower furnace body along the central axis of the furnace body.

The first cavity on the upper furnace body and the second cavity on the lower furnace body are combined up and down to form a cylindrical cavity for placing the furnace tube.

Furthermore, heating temperature field structures with different lengths are arranged in parallel on the upper furnace body and the lower furnace body along the direction of a transverse central axis; any one of the heating temperature field structure, further comprising:

the heating wire grooves are transversely arranged in parallel along the circumference of the cavity formed by the upper furnace body and the lower furnace body;

the heating wire penetrates into the heating wire groove; one end of the heating wire is led out to one side of the upper furnace body and one side of the lower furnace body.

Further, the heating temperature field structure is also respectively provided with:

the heat preservation area is arranged on one side of the upper furnace body and one side of the lower furnace body;

the sublimation area is arranged on one side of the heat preservation area;

the collecting region is provided with a plurality of collecting regions in parallel on one side of the sublimation region; the length of the sublimation area is larger than that of the heat preservation area and the collection area.

Further, heat insulating materials are arranged in the cylinders of the upper furnace body and the lower furnace body, a shell is arranged on the outer sides of the upper furnace body and the lower furnace body, and a plurality of heat dissipation holes are formed in the shell; a furnace frame is fixed below the lower furnace body; a motor opening and closing device is fixed on one side of the upper furnace body and one side of the lower furnace body; one end of the motor opening and closing device is fixed on the side surface of the upper furnace body, and the bottom of the motor opening and closing device is fixed above the cabinet body.

Further, the furnace tube still includes:

the cavity is hollow and cylindrical, and is arranged along a preset central axis of the furnace body; the edge of the chamber is smooth, and a plane seal is arranged between the chamber and the sealing device; the sealing devices are fixed at two end sides of the chamber; a sealing ring is annularly arranged on the inner side of the sealing device and is arranged between the cavity and the sealing device;

the annular cooling water hole is formed in an annular connecting block of the sealing device surrounding the cavity;

the cooling water inlet joint is connected with the annular cooling water hole after penetrating through the annular cooling water hole;

the cooling water outlet joint is also connected with the annular through hole after penetrating through; a group of cooling water is connected into the cooling water inlet joint and the cooling water outlet joint and is used for cooling the sealing ring;

the cooling water inlet joint and the cooling water outlet joint are arranged below the cavity; one side of the sealing device and one side of the connecting pipe device are fixedly connected into a whole in a ring shape to form a structure; a fixed support is fixed at the lower part of the connecting pipe device;

one end of the connecting pipe device is fixed on the other side of the sealing device; a vacuum connecting port is penetratingly connected to the sealing device at one end along the longitudinal axis direction of the cavity; a sealing element is fixed on the vacuum connecting port; the sealing member is used for connecting the vacuum system;

a vacuum gauge connection port which is formed on one side of the vacuum connection port and is connected to the vacuum gauge connection port in a penetrating manner along the longitudinal axis direction of the cavity; a vacuum gauge is fixedly connected above the vacuum gauge connecting port;

both ends of the cavity extend into one end of a connecting pipe, and the connecting pipes are symmetrically arranged along the central axis of the cavity;

a stop ring is arranged on the connecting pipe, and the stop ring limits the connecting pipe in the direction of the transverse axis of the cavity;

the connecting pipe and the cavity are communicated with each other along the transverse axis direction of the cavity to form an integral structure;

a sealing gasket is arranged between the connecting pipe and the cavity body to seal a connecting gap between the connecting pipe and the cavity body;

a vacuum pumping hole with the same diameter as the cavity is connected to the side surface of the connecting pipe device at the other end in a penetrating way;

the other side of the connecting pipe device is movably connected with the furnace door through a hinge structure; an observation mirror is arranged on the transverse axis of the furnace door; a bracket is fixed on one side of the connecting pipe device, one end of the fixing bolt is movably connected to the bracket, and a fixing nut is arranged at the other end of the fixing bolt; a plurality of fixing nuts are evenly distributed along the circumferential edge of the connecting pipe device, and the fixing nuts and the fixing bolts are used for fixing the furnace door;

fixing a moving device below the connecting pipe device; a transverse moving sliding block is arranged at the bottom of the moving device and fixed below the fixed support;

the transverse moving slide block is embedded into the transverse moving guide rail and slides on the transverse moving guide rail;

fixing the longitudinal moving slide block at the bottom of the transverse moving guide rail;

the longitudinal moving slide block is embedded into the longitudinal moving guide rail and slides on the longitudinal moving guide rail;

the transverse moving guide rail and the longitudinal moving guide rail are fixed in a cross mode and are perpendicular to each other.

Further, the vacuum system further comprises:

the vacuum tube is arranged on one side of the furnace tube along a preset central axis; the vacuum pipe and the furnace pipe are vertically and fixedly connected to one side of the furnace pipe along the central axis, and are communicated and stopped with the furnace pipe through the gate valve mechanism;

a gate valve mechanism is fixedly connected between the vacuum tube and the furnace tube; the vacuum tube is used for controlling the on-off of the vacuum in the furnace tube and the vacuum tube; the gate valve mechanism is arranged along the longitudinal central axis of the vacuum tube; the longitudinal cross section of the vacuum tube is cut off by the inserting plate of the inserting plate valve mechanism;

the top of the gate valve mechanism is fixed with the gate valve driving device which drives the gate to move up and down; the gate valve driving device is a motor or a cylinder;

one side of the gate valve mechanism is connected to one side of the filtering device in series;

one side of a flashboard in the flashboard valve mechanism is connected with a fixed ethanol cold trap;

the other side of the ethanol cold trap is fixedly connected with one side of the liquid nitrogen cold trap;

the other end of the liquid nitrogen cold trap is connected with one side of a pneumatic gate valve, and the other side of the pneumatic gate valve is connected with a fixed molecular pump; and a mechanical pump is connected below the liquid nitrogen cold trap.

Further, the ethanol cold trap further comprises:

the first cavity is connected with one end of the gate valve;

the ethanol cooling pipe penetrates into the first cavity;

the cooling fins are penetrated through the ethanol cooling pipes in sequence and are symmetrically arranged along the central axis of the first cavity; the cooling radiating fins are fixed on the ethanol cooling pipe at intervals up and down;

the ethanol cooling pipe is U-shaped, a U shape is formed in the first cavity, and the inlet of the ethanol cooling pipe and the outlet of the ethanol cooling pipe are fixed above the first cavity; a cooling circuit is formed within the first cavity.

Further, the liquid nitrogen cold trap further comprises:

the second cavity is arranged on the central axis of the liquid nitrogen cold trap, and one side of the second cavity is connected with one side of the ethanol cold trap; the other side of the second cavity is connected with one side of the pneumatic gate valve;

the liquid nitrogen cavity is arranged in the second cavity, a liquid feeding pipe is arranged above the liquid nitrogen cavity, and one end of the liquid feeding pipe extends out of the second cavity; and the upper shell of the liquid nitrogen cavity is fixedly connected with the upper shell of the second cavity.

Further, a PLC controller is arranged in the master control system, and the input end of the PLC controller is connected with an input operation panel, a vacuum sensor, a gas flow sensor and a temperature sensor;

the operation panel is electrically connected with the input end of the PLC controller, and an input button is arranged on the operation panel and is connected to the input end of the PLC controller through a mechanical point location;

the output analog quantity of the vacuum sensor is electrically connected with a first analog quantity input end on the input end of the PLC; the digital output end of the vacuum sensor is electrically connected with the digital input end of the PLC controller;

the output analog quantity of the gas flow sensor is electrically connected with a second analog quantity input end on the input end of the PLC;

and the temperature sensors output analog quantity and are electrically connected with a temperature input module on the input end of the PLC.

The output end of the PLC controller respectively outputs and controls a heating wire, a mechanical pump, a molecular pump and a flowmeter;

connecting a plurality of heating contactors to a plurality of point positions on the output end of the PLC controller, wherein the heating contactors electrically connect a power supply with a heating coil; the temperature control device is used for controlling the temperature of the multi-section heating temperature field;

outputting at least one point position on the output end of the PLC controller to be electrically connected to a contactor for controlling the mechanical pump; the mechanical pump is started and stopped;

similarly, at least one point position is output on the output end of the PLC controller and is electrically connected to the contactor of the molecular pump; the molecular pump is used for controlling starting and stopping of the molecular pump;

controlling a contactor of the mechanical pump at the output end of the PLC; and the interlocking is carried out with a contactor which controls the molecular pump on the output end of the PLC controller.

The output analog quantity output end of the PLC controller is electrically connected with the flowmeter through the analog quantity output quantity, and the output analog quantity output end is used for controlling the flow of the flowmeter;

the PLC is in communication connection with the human-computer interaction interface; and the man-machine interaction interface is provided with a switch button, a parameter setting window and a display window for manual control, parameter input and parameter display.

Compared with the prior art, the utility model adopts the vacuum system for the furnace tube to perform vacuum extraction, so that the furnace tube reaches the vacuum state, or the inert gas is filled into the furnace tube to sublimate the material to be purified under the vacuum state or other inert protections, thereby solving the technical problems that the purity, yield and the like of the organic optoelectronic materials applied to the fields of OLED, OPV and the like can not meet the purity requirements of the organic optoelectronic materials in the fields of OLED, OPV and the like, and the loss of the purified materials is very large because the conventional purification equipment is only used for purification in a heating mode.

Drawings

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

FIG. 2 is a schematic front view in the direction of FIG. 1;

FIG. 3 is a schematic left side view of FIG. 1;

FIG. 4 is a perspective view of the furnace body of the present invention;

FIG. 5 is a schematic front view in the direction of FIG. 4;

FIG. 6 is a schematic left side view of FIG. 4;

FIG. 7 is a schematic view of the front view of the temperature field structure according to the present invention;

FIG. 8 is a left side view of the thermal field structure of the present invention;

FIG. 9 is a schematic perspective view of a furnace tube according to the present invention;

FIG. 10 is a front view in perspective of FIG. 9;

FIG. 11 is a left side view in elevation of FIG. 9;

FIG. 12 is a schematic perspective view of a vacuum system of the present invention;

FIG. 13 is a front view in perspective of FIG. 12;

FIG. 14 is a left side view in elevation of FIG. 12;

FIG. 15 is a partial schematic view of a filter apparatus;

fig. 16 is a schematic diagram of a master control system.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail below with reference to the accompanying drawings. However, it will be appreciated by those of ordinary skill in the art that numerous technical details are set forth in order to provide a better understanding of the present application in various embodiments of the present invention. However, the technical solutions claimed in the claims of the present application can be implemented without these technical details and with various changes and modifications based on the following embodiments.

A first embodiment of the present invention relates to a sublimation apparatus, as shown in fig. 1, 2, and 3, including:

the cabinet body 100 is arranged below the sublimation instrument, and is mainly used for supporting the whole sublimation instrument to play a supporting role;

a furnace body 200 is fixed above the cabinet body 100, and a plurality of heating temperature field structures 300 are distributed in the furnace body 200; wrapping a furnace tube 400 in the furnace body 200; the furnace body 200 is mainly used for supporting the furnace tube 400, and the heating temperature field structure 300 heats the furnace tube 400;

one side of the furnace tube 400 is connected with the vacuum system 500 through a gate valve mechanism 600; the vacuum system 500 is used for vacuumizing the furnace tube 400, and the gate valve mechanism 600 is used for switching between the furnace tube 400 and the vacuum system 500;

the main control system 700 controls the vacuum system 500 to perform vacuum pumping control on the furnace tube 400; when the vacuum degree in the furnace tube 400 reaches a preset value, the main control system 700 controls the heating temperature field structure 300 in a segmented manner to heat the furnace tube 400, or the main control system 700 controls the furnace tube 400 to be filled with inert gas; then, the main control system 700 controls the heating temperature field structure 300 in a segmented manner to heat the furnace tube 400, so that the material in the furnace tube 400 is sublimated and recollected. The main control system 700 is mainly used for controlling the functions of the vacuum system 500, the heating temperature field structure 300, the inert gas filling and the like.

In order to achieve the above technical effects, as shown in fig. 1, 4, 5, and 6, the furnace body 200 further includes:

the upper furnace body 210 is in a semicircular shape, and the upper furnace body 210 is transversely arranged along a preset axis of the furnace body 200;

the lower furnace body 220 is in a semicircular shape, and the lower furnace body 220 is connected with the upper furnace body 210 through a hinge structure; the upper furnace body 210 and the lower furnace body 220 constitute a basic frame of the furnace body 200.

A plurality of heating temperature field structures 300 are arranged in the upper furnace body 210 and the lower furnace body 220 along a preset axis of the furnace body 200, and the heating temperature field structures 300 are transversely arranged in parallel along the preset axis at non-average intervals.

The upper furnace body 210 is transversely arranged along the extending transverse direction along the central axis of the furnace body 200, and a semicircular first cavity 211 is arranged on the upper furnace body 210 along the central axis of the furnace body 200;

the lower furnace body 220 is arranged along the furnace body 200 in the span-wise direction, and a semicircular second cavity 221 is arranged on the lower furnace body 220 along the central axis of the furnace body 200.

The first cavity 211 on the upper furnace body 210 and the second cavity 221 on the lower furnace body 220 are combined up and down to form a cylindrical cavity for placing the furnace tube 400.

In order to achieve the above technical problem, heating temperature field structures 300 having different lengths are arranged in parallel in the direction of the horizontal central axis between the upper furnace body 210 and the lower furnace body 220; in order to realize the heating function of the heating thermal field structure 300, as shown in fig. 7 and 8, any one of the heating thermal field structures 300 further includes:

the heating wire grooves 351 are transversely and parallelly arranged along the circumference of a cavity formed by the upper furnace body 210 and the lower furnace body 220;

a heater wire 352 penetrating the heater wire 352 in the heater wire groove 351; one end of the heating wire 352 is led out to one side of the upper furnace body 210 and the lower furnace body 220.

As shown in fig. 1, 7, and 8, in order to sublimate the material, it is necessary to provide different regions in the heating thermal field structure 300 on the furnace body 200 according to the heating thermal field structure 300, and further provide:

a heat preservation area 341 is arranged on one side of the upper furnace body 210 and the lower furnace body 220; the insulating region 341 is mainly used for temperature insulation of the sublimated material.

A sublimation zone 342 is arranged at one side of the heat preservation zone 341; the sublimation zone 342 is primarily for sublimation of material from which material is sublimated.

A plurality of collecting regions 343 are arranged in parallel at one side of the sublimation region 342; the sublimation zone 342 is longer than both the soak zone 341 and the collection zone 343, with the collection zone 343 being primarily used for material collection of the sublimated material.

In order to realize the heat preservation and opening/closing functions of the heating thermal field structure 300, as shown in fig. 1, 7 and 8, heat insulating materials 311 are arranged in the cylinders of the upper furnace body 210 and the lower furnace body 220, a shell 312 is arranged outside the upper furnace body 210 and the lower furnace body 220, and a plurality of heat dissipation holes 313 are arranged on the shell 312; a furnace frame 314 is fixed below the lower furnace body 220; a motor opening and closing device 315 is fixed on one side of the upper furnace body 210 and one side of the lower furnace body 220; one end of the motor opening and closing device 315 is fixed to the side of the upper furnace body 210, and the bottom of the motor opening and closing device 315 is fixed above the cabinet 100.

In order to realize sublimation and collection of the material, as shown in fig. 9, 10, and 11, the furnace tube 400 further includes:

a cavity 410, wherein the cavity 410 is hollow, the cavity 410 is cylindrical, and the cavity 410 is arranged along a preset central axis of the furnace body 200; the edge of the chamber 410 is smooth, and a plane seal is arranged between the chamber and the sealing device 420; the sealing means 420 is fixed to both end sides of the chamber 410; a sealing ring 421 is annularly arranged inside the sealing device 420 and is arranged between the cavity 410 and the sealing device 420;

an annular cooling water hole 422 is formed in an annular connecting block of the sealing device 420 around the cavity 410; the annular cooling water hole 422 is used for introducing cooling water to cool the sealing device 420;

the cooling water inlet joint 423 is connected with the annular cooling water hole 422 after penetrating through;

the cooling water outlet joint 424 is also connected with the annular cooling water hole 422 after penetrating through; a group of cooling water is connected into the cooling water inlet joint 423 and the cooling water outlet joint 424 to cool the sealing ring 421; the cooling water inlet joint 423 and the cooling water outlet joint 424 function to introduce cooling water.

The cooling water inlet joint 423 and the cooling water outlet joint 424 are arranged below the cavity 410; one side of the sealing device 420 and one side of the connecting pipe device 430 are fixedly connected into an integrated structure in a ring shape; a fixing support 339 is fixed at the lower part of the connection pipe means 430;

one end of the connection pipe means 430 is fixed at the other side of the sealing means 420; a vacuum connection port 436 is penetratingly connected to the sealing device 420 at one end along the longitudinal axis direction of the cavity 410; a sealing member is fixed to the vacuum connection port 436; the sealing member is used for connecting the vacuum system;

a vacuum meter connection port 436 penetrating and connected to one side of the vacuum connection port 436 along the longitudinal axis direction of the cavity 410; a vacuum gauge 437 is fixedly connected above the vacuum gauge connecting port 436;

both ends of the chamber 410 are extended into one end of a connection pipe 431, and the connection pipes 431 are symmetrically arranged along the central axis of the chamber 410;

a stop ring 432 is provided on the connection pipe 431, and the stop ring 432 limits the connection pipe 431 in the transverse axial direction of the cavity 410;

the connecting pipe 431 and the cavity 410 are communicated with each other along the transverse axial direction of the cavity 410 to form an integral structure;

a sealing gasket is arranged between the connecting pipe 431 and the cavity 410 to seal a connecting gap between the connecting pipe 431 and the cavity 410;

a vacuum hole 438 with the same diameter as the cavity 410 is connected on the side surface of the connecting pipe device 430 at the other end in a penetrating way;

the other side of the connecting pipe device 430 is movably connected with the oven door 440 through a hinge structure; a sight glass 441 is disposed on a lateral axis of the oven door 440; a bracket 443 is fixed on one side of the connection pipe device 430, one end of the fixing bolt 442 is movably connected to the bracket 443, and a fixing nut 445 is provided on the other end of the fixing bolt 442; a plurality of fixing nuts 445 are evenly distributed along the circumferential edge of the connecting pipe device 430, and the fixing nuts 445 and the fixing bolts 442 are used for fixing the oven door 440; the oven door 440 and the connecting pipe device 430 form a quick-opening door structure, which is mainly used for placing the material to be sublimated and taking out the sublimated material.

Fixing a moving means 450 under the connection pipe means 430; a transverse moving slide block 451 is arranged on the bottom of the moving device 450, and the transverse moving slide block 451 is fixed below the fixed support 439;

the lateral movement block 451 is fitted into the lateral movement guide 452, and the lateral movement block 451 slides on the lateral movement guide 452; the lateral movement block 451 and the lateral movement guide 452 constitute a guide structure that slides laterally.

A longitudinal movement slider 453 is fixed to the bottom of the lateral movement guide 452;

the longitudinal movement slider 453 is fitted into the longitudinal movement rail 454, and the longitudinal movement slider 453 slides on the longitudinal movement rail 454;

the transverse moving guide rails 452 and the longitudinal moving guide rails 454 are fixed in a crossed and vertical manner, the transverse moving guide rails 452 and the longitudinal moving guide rails 454 can slide in four directions, namely front, back, left and right, and meanwhile, the sublimation apparatus in the embodiment is arranged on the moving device 450, so that the sublimation apparatus can slide in four directions, namely front, back, left and right, and the furnace tube 400 can move conveniently.

In order to enable the sublimation apparatus in the present embodiment to perform sublimation, it is necessary to draw a vacuum to the furnace tube 400, and for this purpose, as shown in fig. 12, 13, 14, and 15, the vacuum system 500 further includes:

the vacuum tube 510 is arranged on one side of the furnace tube 400 along a preset central axis; the vacuum tube 510 and the furnace tube 400 are vertically and fixedly connected to one side of the furnace tube 400 along the central axis, and are communicated and stopped with the furnace tube 400 through the gate valve mechanism 600;

a gate valve mechanism 600 is fixedly connected between the vacuum tube 510 and the furnace tube 400; used for controlling the on-off of the vacuum in the furnace tube 400 and the vacuum tube 510; the gate valve mechanism 600 is arranged along the longitudinal central axis of the vacuum tube 510; the inserting plate 601 of the inserting plate valve mechanism 600 cuts off the longitudinal cross section of the vacuum tube 510;

a gate valve driving device 532 is fixed at the top of the gate valve mechanism 600, and the gate valve driving device 532 drives the gate 601 to move up and down; the gate valve driving device 532 is a motor or a cylinder;

one side of the gate valve mechanism 600 is connected in series to one side of the filter device 550;

one side of the flashboard 601 in the flashboard valve mechanism 60 is connected with a fixed ethanol cold trap 551;

the other side of the ethanol cold trap 551 is fixedly connected with one side of the liquid nitrogen cold trap 552; the other end of the liquid nitrogen cold trap 552 is connected with one side of a pneumatic gate valve 553, and the other side of the pneumatic gate valve 553 is connected with a fixed molecular pump 561; a mechanical pump 562 is connected below the liquid nitrogen cold trap 552.

As shown in fig. 12, 13, 14, and 15, the ethanol cold trap 551 further includes:

one end of the gate valve 601 is connected with a first cavity 5511, and the first cavity 5511 is used for placing an ethanol cooling pipe 5512;

an ethanol cooling pipe 5512 is penetrated in the first cavity 5522; the ethanol cooling pipe 5512 is used for cooling the gaseous materials,

the cooling fins 5513 and the ethanol cooling pipes 5512 sequentially penetrate the cooling fins 5513, and the cooling fins 5513 are symmetrically arranged along the central axis of the first cavity 5511; the cooling fins 5513 are fixed on the ethanol cooling pipe 5512 at intervals from top to bottom;

the ethanol cooling pipe 5512 is U-shaped, a U-shape is formed in the first cavity 5511, and an inlet of the ethanol cooling pipe 5512 and an outlet of the ethanol cooling pipe 5512 are fixed above the first cavity 5511; forming a cooling circuit within first cavity 5511; the cooling fins 5513 are fixed on the ethanol cooling pipe 5512 at intervals from top to bottom; the cooling fins 5513 can enlarge the heat dissipation area, so that the ethanol cold trap 551 can better cool the gaseous materials, the ethanol cooling pipe 5512 is in a U-shaped design, and the cooling fins 5513 are designed on the ethanol cooling pipe 5512, so that the gas temperature is reduced, and the gas flow rate is reduced; the gas temperature can be greatly reduced, and the gas can be purified; the gas materials entering the vacuum system can be effectively separated, so that the gas entering the mechanical pump 562 and the molecular pump 561 is cleaner, and the service lives of the mechanical pump 562 and the molecular pump 561 are prolonged.

As shown in fig. 12, 13, 14 and 15, the liquid nitrogen trap 552 further includes:

a second cavity 5521 is arranged on the central axis of the liquid nitrogen cold trap 5511, and one side of the second cavity 5521 is connected with one side of the ethanol cold trap 5511; the other side of second cavity 5521 is connected to one side of pneumatic gate valve 553;

a liquid nitrogen cavity 5522 is arranged in the second cavity 5521, a liquid feeding pipe 5523 is arranged above the liquid nitrogen cavity 5522, and one end of the liquid feeding pipe 5523 extends out of the second cavity 5521; the upper shell of the liquid nitrogen cavity 5522 is fixedly connected with the upper shell of the second cavity 5521. The liquid nitrogen cavity 5522 is used for containing liquid nitrogen, the liquid nitrogen is injected into the liquid nitrogen cavity 5522 through the liquid adding pipe 5523, and a large amount of heat is absorbed in the second cavity 521 through the liquid nitrogen cavity 5522, so that the function of cooling gaseous materials is realized.

In order to control the vacuum system 500, the heating temperature field structure 300, and the inert gas filling, a main control system 700 is provided in the present embodiment, as shown in fig. 16,

a PLC (programmable logic controller) 701 is arranged in the main control system 700, and an input operation panel 711, a vacuum sensor 712, a gas flow sensor 713 and a temperature sensor 714 are connected to the input end of the PLC 701;

the operation panel 711 is electrically connected with the input end of the PLC 701, and an input button arranged on the operation panel 711 is connected to the input end of the PLC 701 through a mechanical point;

the output analog quantity of the vacuum sensor 712 is electrically connected with a first analog quantity input end on the input end of the PLC 701; the digital output end of the vacuum sensor 712 is electrically connected with the digital input end of the PLC 701;

the output analog quantity of the gas flow sensor 713 is electrically connected with a second analog quantity input end on the input end of the PLC 701;

the temperature sensors 714 output analog quantity and are electrically connected with a temperature input module on the input end of the PLC 701.

The output end of the PLC 701 respectively outputs a control heating wire 352, a mechanical pump 562, a molecular pump 561 and a flow meter 705;

a plurality of heating contactors 702 are connected to a plurality of point positions on the output end of the PLC controller 701, and the heating contactors 702 electrically connect a power supply to the heating coils; the temperature control device is used for controlling the temperature of the multi-section heating temperature field;

outputting at least one point position on the output end of the PLC 701 to be electrically connected to a contactor 703 for controlling the mechanical pump; start-stop mechanical pump 562;

similarly, at least one point is output at the output end of the PLC controller 701 and electrically connected to the contactor 704 of the molecular pump; is used for controlling the start-stop molecular pump 561;

controlling a contactor 703 of the mechanical pump at an output terminal 701 of the PLC controller; the interlocking with the contactor 704 for controlling the molecular pump on the output end of the PLC controller 701 ensures that the molecular pump 561 is started only after the mechanical pump 562 stops after the preset vacuum of the mechanical pump 562 is reached, mainly to protect the molecular pump 561 from being damaged.

The output analog quantity output end of the PLC 701 is electrically connected with the flow meter 705 through the analog quantity output quantity, and is used for controlling the flow of the flow meter 705;

the PLC 701 is in communication connection with a human-computer interaction interface 706; the man-machine interaction interface 706 is provided with a switch button, a parameter setting window and a display window for manual control, parameter input and parameter display.

The using method of the sublimation instrument specifically comprises the following steps:

step S10: placing raw materials to be sublimated, opening the furnace door 440, placing the raw materials to be sublimated in the furnace tube 400, closing the furnace door 440, screwing the fixing bolt 442, and sealing the space between the furnace door 440 and the chamber 410; proceeding to step S20;

step S10: starting up to set parameters: after the power supply is started on the operation panel 711, starting the sublimation instrument, and after the PLC 701 and the human-computer interaction interface 706 are started, respectively setting target temperature values, heating times and material sublimation times of the heat preservation area 341, the collection area 343 and the sublimation area 342 on the human-computer interaction interface 706; setting a preset vacuum value of the mechanical pump 562, the pumping time of the mechanical pump 562, a preset vacuum value for starting the molecular pump 561, the pumping time of the molecular pump 561 and the vacuum maintaining time; compiling a temperature rise and drop curve on the human-computer interaction interface 706; proceeding to step S30;

step S30: selecting an automatic operation mode, electrifying the main control system 700 to open the electromagnetic valve of the gate valve mechanism 600 or electrifying the motor of the gate valve mechanism 600, opening the gate 601, communicating the furnace tube 400 with the mechanical pump 562, starting to pump vacuum until the preset vacuum value of the mechanical pump 562 is reached, and entering step S40; if the preset vacuum value of the mechanical pump 562 cannot be reached within the pumping time of the mechanical pump 562, the main control system 700 outputs an alarm and the process goes to step S50;

step S40: switching the molecular pump 561: after the preset vacuum value of the mechanical pump 562 is reached, the main control system 700 outputs a solenoid valve for controlling the pneumatic gate valve 553, opens the pneumatic gate valve 553, closes the mechanical pump 562, and then the main control system 700 outputs a control for opening the molecular pump 561 until the preset vacuum value of the molecular pump 561 is reached, and the process goes to step S60; if the option of injecting the inert gas is selected on the human-computer interaction interface 706, the step S70 is entered; if the preset vacuum value of the molecular pump 561 cannot be reached within the pumping time of the molecular pump 561, the main control system 700 outputs an alarm, and the process goes to step S50;

step S50: the system is restarted, the main control system 700 outputs alarm information, the alarm lamp 707 is lightened, the main control system 700 is automatically switched to a manual state, a blank valve opening button is pressed in the manual state, the main control system 700 controls a blank electromagnetic valve to connect the furnace tube 400 with the atmosphere, and the vacuum in the furnace tube 400 is damaged; after the sealing failure which breaks the vacuum is eliminated, the alarm is released, and the step returns to the step S30;

step S60: and (3) vacuum maintenance: after the preset vacuum value of the molecular pump 561 is reached and the vacuum maintaining time returns to zero, the step S80 is executed;

step S70: inert gas injection: the main control system 700 controls the inert gas injection control valve, automatically opens the inert gas injection control valve, which is marked in the figure, and injects the inert gas into the furnace tube 400, and closes the inert gas injection control valve after the vacuum value is greater than or equal to the atmospheric pressure value, which is marked in the figure; step S80:

step S80: heating in a temperature field, wherein the main control system 700 controls different temperature controllers of the heat preservation area 341, the collection area 343 and the sublimation area 342, heats the temperature according to a preset heating curve until the temperature values of the heat preservation area 341, the collection area 343 and the sublimation area 342 reach target temperature values, and then the step S100 is performed; if the temperature values of the heat preservation region 341, the collection region 343, and the sublimation region 342 do not reach the target temperature values within the heating time, the process proceeds to step S90;

step S90: stopping heating, stopping outputting the different temperature controllers of the heat preservation area 341, the collection area 343, and the sublimation area 342 by the main control system 700, starting the cooling fan 708, cooling until the temperature is reduced to normal temperature, and entering step S50;

step S100: sublimation of the material: the master control system 700 calculates the sublimation time of the material until the material is completely sublimated until the sublimation time of the material is zero; proceeding to step S90; after step S90 is completed, the main control system 700 controls the vacuum-breaking solenoid valve to connect the furnace tube 400 with the atmosphere, and opens the furnace door 440 after breaking the vacuum in the furnace tube 400, and collects the sublimated small molecule material.

It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples for carrying out the utility model, and that various changes in form and details may be made therein without departing from the spirit and scope of the utility model in practice.

Claims (10)

1. A sublimation meter, comprising:

the cabinet body is arranged below the sublimation instrument;

the furnace body is fixed above the cabinet body, and a plurality of heating temperature field structures are distributed in the furnace body;

the furnace tube is wrapped in the furnace body;

the vacuum system is connected with one side of the furnace tube through a gate valve mechanism;

the main control system controls the vacuum system to perform vacuum extraction control on the furnace tube; when the vacuum degree in the furnace tube reaches a preset value, the main control system controls the heating temperature field structure in a segmented mode to heat the furnace tube, or controls the furnace tube to be filled with inert gas; and then, the main control system controls the heating temperature field structure in a segmented manner to heat the furnace tube, so that the material in the furnace tube is sublimated and collected again.

2. The sublimation apparatus of claim 1, wherein the furnace body further comprises:

an upper furnace body; the upper furnace body is in a semicircular shape and is transversely arranged along a preset axis of the furnace body;

the lower furnace body is in a semicircular shape and is connected with the upper furnace body through a hinge structure;

a plurality of heating temperature field structures are arranged in the upper furnace body and the lower furnace body along a preset axis of the furnace body, and the heating temperature field structures are transversely arranged in parallel at non-average intervals along the preset axis;

the upper furnace body is transversely arranged along the central axis of the furnace body along the unfolding direction, and a semicircular first cavity is arranged on the upper furnace body along the central axis of the furnace body;

the lower furnace body is transversely arranged along the furnace body in the unfolding direction, and a semicircular second cavity is arranged on the lower furnace body along the central axis of the furnace body;

the first cavity on the upper furnace body and the second cavity on the lower furnace body are combined up and down to form a cylindrical cavity for placing the furnace tube.

3. The sublimation apparatus according to claim 2, wherein heating temperature field structures of different lengths are juxtaposed in the direction of the transverse central axis between the upper furnace body and the lower furnace body; any one of the heating temperature field structure, further comprising:

the heating wire grooves are transversely arranged in parallel along the circumference of the cavity formed by the upper furnace body and the lower furnace body;

the heating wire penetrates into the heating wire groove; one end of the heating wire is led out to one side of the upper furnace body and one side of the lower furnace body.

4. The sublimation apparatus according to claim 3, wherein the heating temperature field structure is further provided with:

the heat preservation area is arranged on one side of the upper furnace body and one side of the lower furnace body;

the sublimation area is arranged on one side of the heat preservation area;

the collecting region is provided with a plurality of collecting regions in parallel on one side of the sublimation region; the length of the sublimation area is larger than that of the heat preservation area and the collection area.

5. The sublimation apparatus according to claim 3, wherein heat insulating material is provided in the cylindrical bodies of the upper furnace body and the lower furnace body, a housing is provided outside the upper furnace body and the lower furnace body, and a plurality of heat dissipation holes are provided in the housing; a furnace frame is fixed below the lower furnace body; a motor opening and closing device is fixed on one side of the upper furnace body and one side of the lower furnace body; one end of the motor opening and closing device is fixed on the side surface of the upper furnace body, and the bottom of the motor opening and closing device is fixed above the cabinet body.

6. The sublimation meter of claim 1, wherein the furnace tube further comprises:

the cavity is hollow and cylindrical, and is arranged along a preset central axis of the furnace body; the edge of the chamber is smooth, and a plane seal is arranged between the chamber and the sealing device; the sealing devices are fixed at two end sides of the chamber; a sealing ring is annularly arranged on the inner side of the sealing device and is arranged between the cavity and the sealing device;

the annular cooling water hole is formed in an annular connecting block of the sealing device surrounding the cavity;

the cooling water inlet joint is connected with the annular cooling water hole after penetrating through the annular cooling water hole;

the cooling water outlet joint is also connected with the annular through hole after penetrating through; a group of cooling water is connected into the cooling water inlet joint and the cooling water outlet joint and is used for cooling the sealing ring;

the cooling water inlet joint and the cooling water outlet joint are arranged below the cavity; one side of the sealing device and one side of the connecting pipe device are fixedly connected into an integrated structure in an annular mode; a fixed support is fixed at the lower part of the connecting pipe device;

one end of the connecting pipe device is fixed on the other side of the sealing device; a vacuum connecting port is penetratingly connected to the sealing device at one end along the longitudinal axis direction of the cavity; a sealing element is fixed on the vacuum connecting port; the sealing member is used for connecting the vacuum system;

a vacuum gauge connection port which is formed on one side of the vacuum connection port and is connected to the vacuum gauge connection port in a penetrating manner along the longitudinal axis direction of the cavity; a vacuum gauge is fixedly connected above the vacuum gauge connecting port;

both ends of the cavity extend into one end of a connecting pipe, and the connecting pipes are symmetrically arranged along the central axis of the cavity;

a stop ring is arranged on the connecting pipe, and the stop ring limits the connecting pipe in the direction of the transverse axis of the cavity;

the connecting pipe and the cavity are communicated with each other along the transverse axis direction of the cavity to form an integral structure;

a sealing gasket is arranged between the connecting pipe and the cavity body to seal a connecting gap between the connecting pipe and the cavity body;

a vacuum pumping hole with the same diameter as the cavity is connected to the side surface of the connecting pipe device at the other end in a penetrating way;

the other side of the connecting pipe device is movably connected with the furnace door through a hinge structure; an observation mirror is arranged on the transverse axis of the furnace door; a bracket is fixed on one side of the connecting pipe device, one end of a fixing bolt is movably connected on the bracket, and a fixing nut is arranged on the other end of the fixing bolt; a plurality of fixing nuts are evenly distributed along the circumferential edge of the connecting pipe device, and the fixing nuts and the fixing bolts are used for fixing the furnace door;

fixing a moving device below the connecting pipe device; a transverse moving sliding block is arranged at the bottom of the moving device and fixed below the fixed support;

the transverse moving slide block is embedded into the transverse moving guide rail and slides on the transverse moving guide rail;

a longitudinal moving slide block is fixed at the bottom of the transverse moving guide rail;

the longitudinal moving slide block is embedded into the longitudinal moving guide rail and slides on the longitudinal moving guide rail;

the transverse moving guide rail and the longitudinal moving guide rail are fixed in a cross mode and are perpendicular to each other.

7. The sublimation meter of claim 1, wherein the vacuum system further comprises:

the vacuum tube is arranged on one side of the furnace tube along a preset central axis; the vacuum pipe and the furnace pipe are vertically and fixedly connected to one side of the furnace pipe along the central axis, and are communicated and stopped with the furnace pipe through the gate valve mechanism;

the gate valve mechanism is fixedly connected between the vacuum tube and the furnace tube; the vacuum tube is used for controlling the on-off of the vacuum in the furnace tube and the vacuum tube; the gate valve mechanism is arranged along the longitudinal central axis of the vacuum tube; the longitudinal cross section of the vacuum tube is cut off by the inserting plate of the inserting plate valve mechanism;

the top of the gate valve mechanism is fixed with the gate valve driving device which drives the gate to move up and down; the gate valve driving device is a motor or a cylinder;

one side of the gate valve mechanism is connected to one side of the filtering device in series;

one side of a flashboard in the flashboard valve mechanism is connected with a fixed ethanol cold trap;

the other side of the ethanol cold trap is fixedly connected with one side of the liquid nitrogen cold trap; the other end of the liquid nitrogen cold trap is connected with one side of a pneumatic gate valve, and the other side of the pneumatic gate valve is connected with a fixed molecular pump; and a mechanical pump is connected below the liquid nitrogen cold trap.

8. The sublimation meter of claim 7, wherein the ethanol cold trap further comprises:

the first cavity is connected with one end of the gate valve;

the ethanol cooling pipe penetrates into the first cavity;

the cooling fins are penetrated through the ethanol cooling pipes in sequence and are symmetrically arranged along the central axis of the first cavity; the cooling radiating fins are fixed on the ethanol cooling pipe at intervals up and down;

the ethanol cooling pipe is U-shaped, a U shape is formed in the first cavity, and the inlet of the ethanol cooling pipe and the outlet of the ethanol cooling pipe are fixed above the first cavity; a cooling circuit is formed within the first cavity.

9. The sublimation meter of claim 7, wherein the liquid nitrogen-cooled trap further comprises:

the second cavity is arranged on the central axis of the liquid nitrogen cold trap, and one side of the second cavity is connected with one side of the ethanol cold trap; the other side of the second cavity is connected with one side of the pneumatic gate valve;

the liquid nitrogen cavity is arranged in the second cavity, a liquid feeding pipe is arranged above the liquid nitrogen cavity, and one end of the liquid feeding pipe extends out of the second cavity; and the upper shell of the liquid nitrogen cavity is fixedly connected with the upper shell of the second cavity.

10. The sublimation apparatus according to claim 1, wherein a PLC controller is provided in the main control system, and an input operation panel, a vacuum sensor, a gas flow sensor, and a temperature sensor are connected to an input end of the PLC controller;

the operation panel is electrically connected with the input end of the PLC controller, and an input button is arranged on the operation panel and is connected to the input end of the PLC controller through a mechanical point location;

the output analog quantity of the vacuum sensor is electrically connected with a first analog quantity input end on the input end of the PLC; the digital output end of the vacuum sensor is electrically connected with the digital input end of the PLC controller;

the output analog quantity of the gas flow sensor is electrically connected with a second analog quantity input end on the input end of the PLC;

the temperature sensors output analog quantity and are electrically connected with a temperature input module on the input end of the PLC;

the output end of the PLC controller respectively outputs and controls a heating wire, a mechanical pump, a molecular pump and a flowmeter;

connecting a plurality of heating contactors to a plurality of point positions on the output end of the PLC controller, wherein the heating contactors electrically connect a power supply with a heating coil; the temperature control device is used for controlling the temperature of the multi-section heating temperature field;

outputting at least one point position on the output end of the PLC controller to be electrically connected to a contactor for controlling the mechanical pump; the mechanical pump is started and stopped;

similarly, at least one point position is output on the output end of the PLC controller and is electrically connected to the contactor of the molecular pump; the molecular pump is used for controlling starting and stopping of the molecular pump;

controlling a contactor of the mechanical pump at the output end of the PLC; the interlocking device is interlocked with a contactor which controls the molecular pump on the output end of the PLC controller;

the output analog quantity output end of the PLC controller is electrically connected with the flowmeter through the analog quantity output quantity, and the output analog quantity output end is used for controlling the flow of the flowmeter;

the PLC is in communication connection with the human-computer interaction interface; and the man-machine interaction interface is provided with a switch button, a parameter setting window and a display window for manual control, parameter input and parameter display.

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