CN106801223B

CN106801223B - A double heat source vertical atmosphere reaction furnace

Info

Publication number: CN106801223B
Application number: CN201710062952.XA
Authority: CN
Inventors: 徐庆宇; 张昊; 董帅
Original assignee: Southeast University
Current assignee: Southeast University
Priority date: 2017-02-01
Filing date: 2017-02-01
Publication date: 2019-04-09
Anticipated expiration: 2037-02-01
Also published as: CN106801223A

Abstract

The invention discloses a kind of double heat source vertical-type atmosphere reacting furnaces, mainly be made of controller, rotary heating base station, burner hearth three parts, purposes be heat substrate table under required reaction temperature with heating bottom stage can sublimator material generate atmosphere occur chemical reaction generate needed for film.The present invention, to placement, it is smaller to which upwards are easier to react with the substrate contact on heating substrate table to heat the gas density that material is generated by thermal decomposition on bottom stage using heating substrate table and heating bottom stage top and bottom；And the heating substrate table where substrate is can to adjust the speed rotation, and the film for reacting preparation can be more uniform, while can also adjust and heat at a distance from bottom stage；The present invention can adjust separately the material sublimation temperature T1 of heating bottom stage and the underlayer temperature T2 of heating substrate table, so that the heating process of atmosphere reactive deposition does not influence between each other using double heat source heating.

Description

A kind of double heat source vertical-type atmosphere reacting furnaces

Technical field

The present invention be it is a kind of using bottom-heated can sublimator material come the substrate for generating and being heated on atmosphere and substrate table that distils Film carries out chemical reaction at a certain temperature and generates the instrument for growing required film, belongs to processing film instrument field.

Background technique

The currently used instrument that film is prepared in relation to atmosphere or vapor phase method, there are mainly two types of: 1. to be passed through two kinds of gases anti- Should after condense and be deposited in a substrate (CVD)；2. being passed through a kind of gas into tube furnace to be reacted with the substrate in pipe.But It is that the instrument of the first seed type is only applicable to two kinds of gas reaction condensation depositions, is not particularly suited for solid film substrate specific At a temperature of the situation of film is directly prepared with atmosphere chemical reaction；Although and the instrument of second of type is applicable in, and is not suitable for In the material atmosphere easily condensed, because (can not be condensed in tracheae or glass tube walls) in access tube, and it is put into internal direct High temperature distillation can make material sublimation temperature identical as substrate reaction temperature again and more difficult completion is tested, and static in substrate reaction It places, is unfavorable for preparing uniform film.Therefore, profession is lacked in research and production and is directed to solid substrate in material gas of easily sublimating The instrument of reaction growth high-quality thin film in atmosphere.

Summary of the invention

Goal of the invention: in order to overcome the deficiencies in the prior art, the present invention provides a kind of double heat source vertical-type atmosphere Reacting furnace, the film quality which obtains is good, reaction is uniform.

Technical solution: to achieve the above object, the technical solution adopted by the present invention are as follows:

A kind of double heat source vertical-type atmosphere reacting furnaces, including controller (1), rotary heating base station (2) and burner hearth (3), The burner hearth (3) includes furnace body open at one end (35), bell (36), pressure gage (30), gas-guide tube (31), vacuum pump, heating Bottom stage (32), the heating bottom stage (32) are set in furnace body (35), and pressure gage (30) is used to measure the pressure in furnace body (35) By force, the measuring probe of the pressure gage (30) is set in furnace body (35), and the pressure gage (30) is connect with controller (1), The furnace body (35) is connected to by gas-guide tube (31) with vacuum pump；The rotary heating base station (2) includes stepper motor (4), shakes Hand (5), otating drive rod (6), threaded rod (7), connecting rod (10), fixed ring (8), support tube (81), heating substrate table (14), The bell (36) is mounted on the open end of furnace body (35), and one end and bell (36) of the threaded rod (7) are rotatablely connected, and institute State the other end of threaded rod (7) with shake the hand (5) be fixedly connected, described connecting rod (10) one end passes through screwed ring and threaded rod (7) Connection, the other end is fixedly connected with fixed ring (8), and the fixed ring (8) is fixedly mounted on support tube (81)；The stepping Motor (4) is fixedly mounted on one end of support tube (81), and the other end of support tube (81) passes through bell (36) and heating serves as a contrast Bottom stage (14) rotation connection, and the support tube (81) and bell (36) are rotatablely connected；The otating drive rod (6) is set to branch In stay tube (81), and the otating drive rod (6) one end is connect with stepper motor (4) shaft, the other end and heating substrate table (14) it is fixedly connected；What heating substrate table (14) and support tube (81) were away from each other is provided with fixed metal clips (12) on one side With fixed screw holes (13), the fixed metal clips (12) is mounted on heating substrate table (14) by fixed screw holes (13) On；The heating substrate table (14) is oppositely arranged with heating bottom stage (32).

Preferred: the heating bottom stage (32) is fixedly mounted on furnace body (35) bottom surface by fixed screw one (33), and institute It states and is provided on furnace body (35) burner hearth power outlet (34), the heating bottom stage (32) and burner hearth power outlet (34) are connected.

It is preferred: it is provided with fixing bearing one (15) on the bell (36), and the threaded rod (7) and fixing bearing one (15) inner ring is fixedly connected, so that threaded rod (7) is rotatablely connected by fixing bearing one (15) and bell (36)；The bell (36) through-hole is provided on, and the support tube (81) passes through through-hole, and is interference fitted between support tube (81) and through-hole.

It is preferred: fixing bearing two (16), the support tube (81) and fixation are provided on the heating substrate table (14) The inner ring of bearing two (16) is fixedly connected, so that support tube (81) passes through fixing bearing two (16) and heating substrate table (14) rotation Connection.

It is preferred: to be provided with scale bar (9) on the threaded rod (7).

It is preferred: to further include bellows (11), bellows limitation flange, the bellows limitation flange is fixedly mounted on branch On stay tube (81), and the bellows (11) is set between bellows limitation flange and bell (36).

Preferred: the controller (1) includes single-chip microcontroller, heating substrate table real time temperature display screen (17), heating substrate Platform real-time target temperature (18), heating substrate table control button (19), heating bottom stage real time temperature display screen (20), heating bottom stage Real-time target temperature (21), heating bottom stage control button (22), stepper motor adjust the speed knob (23), controller "ON" button (24), controller "Off" button (25), the heating substrate table real time temperature display screen (17), heating substrate table real-time target temperature Spend (18), heating substrate table control button (19), heating bottom stage real time temperature display screen (20), heating bottom stage real-time target temperature (21), bottom stage control button (22) are heated, stepper motor adjusts the speed knob (23), controller "ON" button (24), controller "Off" Button (25) is connect with single-chip microcontroller.

The present invention compared with prior art, has the advantages that

(1) using by material be placed in instrument internal heating sublimation generate the material atmosphere can make certain distillations after produce Raw gas material of easily sublimating avoids before sublimating effectively contacting with reaction substrate, these materials is allowed to be able to use vapor phase method.

(2) present invention use will heat vertical-type depositional mode of the substrate table with heating bottom stage top and bottom to placement, according to Physical thermodynamics are regular, and the gas density that material is generated by thermal decomposition on heating bottom stage is smaller to which upwards are easier to and are added Substrate contact reaction on hot substrate table, can constantly make on newly distilling the gas that floats at once with the film lining on heating substrate table Bottom is reacted, and film reaction mass is helped to improve.

(3) in atmosphere reaction process, heating substrate table can at the uniform velocity be rotated, and reaction can be made uniformly to be conducive to React obtained film quality and uniformity.

(4) the substrate disc computer heating control being separated from each other using double heat sources, compared to the double heat source vapor phase methods of common tube furnace, Can allow atmosphere reactive deposition when material sublimation temperature and substrate reaction temperature it is mutually indepedent, be independent of each other.

(5) according to the distillation severe degree of material under set temperature by rotary heating base station shake the hand adjust heating Substrate table changes the concentration for the material sublimation atmosphere that substrate is contacted at a distance from heating bottom stage and avoids the nothing of sublimating of gas Method is effectively contacted with substrate.Simultaneously when heating substrate table or heating bottom stage temperature is higher, it is next big that distance between the two can be increased Amplitude weakens mutual influence, improves film reaction mass.

(6) for different size of substrate, fixed screw holes mounting elastic sheet different on heating substrate table can be selected Substrate is fixed, has expanded the versatility of instrument.

Detailed description of the invention

Fig. 1: the whole exemplary diagram of double heat source vertical-type atmosphere reacting furnaces；

Fig. 2: rotary heating abutment structure schematic diagram；

Fig. 3: rotary heating abutment structure schematic diagram；

Fig. 4: controller positive structure schematic；

Fig. 5: controller structure schematic diagram；

Fig. 6: chamber structure schematic diagram；

The label declaration of each component in schematic diagram:

1 controller, 2 rotary heating base station, 3 burner hearth, 4 stepper motor 5 is shaken the hand

6 otating drive rod, 7 threaded rod, 8 fixed ring, 9 scale bar

10 connecting rod, 11 bellows 12 fixes metal clips

13 fixed screw holes 14 heat 15 fixing bearing of substrate table, one 16 fixing bearing two

17 heating substrate table real time temperature display screens 18 heat substrate table real-time target temperature

19 heating substrate table control buttons 20 heat bottom stage real time temperature display screen

21 heating bottom stage real-time target temperature 22 heat bottom stage control button

23 stepper motors adjust the speed 24 controller "ON" button of knob, 25 controller "Off" button

26 burner hearth wiring-connecting socket, 27 power outlet

28 29 power supply for step-by-step motor line of rotary heating base station wiring-connecting socket, 30 pressure gage

31 gas-guide tubes 32 heat 33 fixed screw of bottom stage, 34 burner hearth power outlet.

Specific embodiment

In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, it should be understood that these examples are merely to illustrate this It invents rather than limits the scope of the invention, after the present invention has been read, those skilled in the art are to of the invention various The modification of equivalent form falls within the application range as defined in the appended claims.

A kind of double heat source vertical-type atmosphere reacting furnaces, purposes be heating substrate table under required reaction temperature with heating bottom Platform can sublimator material generate atmosphere occur chemical reaction generate needed for film.As shown in Figure 1, 2, including controller 1, rotation add Hot radical platform 2 and burner hearth 3, as shown in fig. 6, the burner hearth 3 includes furnace body 35 open at one end, bell 36, pressure gage 30, air guide Pipe 31, vacuum pump, heating bottom stage 32, the heating bottom stage 32 is set in furnace body 35, and pressure gage 30 is for measuring furnace body 35 The measuring probe of interior pressure, the pressure gage 30 is set in furnace body 35, and the pressure gage 30 is connect with controller 1, institute Furnace body 35 is stated to be connected to by gas-guide tube 31 with vacuum pump；The heating bottom stage 32 is fixedly mounted on furnace body by fixed screw 1 35 bottom surfaces, and burner hearth power outlet 34 is provided on the furnace body 35, the heating bottom stage 32 is connected with burner hearth power outlet 34.

As shown in Fig. 2, the rotary heating base station 2 includes stepper motor 4,5, otating drive rod 6 of shaking the hand, threaded rod 7, connects Extension bar 10, fixed ring 8, support tube 81, heating substrate table 14, the bell 36 are mounted on the open end of furnace body 35, the screw thread One end of bar 7 and bell 36 are rotatablely connected, and the other end of the threaded rod 75 is fixedly connected with shaking the hand, the connecting rod 10 1 End is connect by screwed ring with threaded rod 7, and the other end is fixedly connected with fixed ring 8, and the fixed ring 8 is fixedly mounted on support On pipe 81；The stepper motor 4 is fixedly mounted on one end of support tube 81, and the other end of support tube 81 pass through bell 36 with It heats substrate table 14 to be rotatablely connected, and the support tube 81 and bell 36 are rotatablely connected；It is provided with through-hole on the bell 36, and The support tube 81 passes through through-hole, and is interference fitted between support tube 81 and through-hole.The otating drive rod 6 is set to support tube In 81, and 6 one end of the otating drive rod is connect with 4 shaft of stepper motor, and the other end is fixedly connected with heating substrate table 14；Institute It states heating substrate table 14 and what support tube 81 was away from each other is provided with fixed metal clips 12 and fixed screw holes 13 on one side, it is described solid Determine metal clips 12 to be mounted on heating substrate table 14 by fixed screw holes 13；The heating substrate table 14 and heating bottom stage 32 It is oppositely arranged.Scale bar 9 is provided on the threaded rod 7.It further include bellows 11, bellows limitation flange, the bellows Limitation flange is fixedly mounted on support tube 81, and the bellows 11 is set between bellows limitation flange and bell 36.

As shown in figure 3, fixing bearing 1 is provided on the bell 36, and the threaded rod 7 and fixing bearing 1 Inner ring be fixedly connected so that threaded rod 7 is rotatablely connected by fixing bearing 1 and bell 36；On the heating substrate table 14 It is provided with fixing bearing 2 16, the support tube 81 is fixedly connected with the inner ring of fixing bearing 2 16, so that support tube 81 passes through Fixing bearing 2 16 and heating substrate table 14 are rotatablely connected.

As shown in Figure 4,5, the controller 1 includes single-chip microcontroller, heating substrate table real time temperature display screen 17, heating substrate Platform real-time target temperature 18, heating substrate table control button 19, heating bottom stage real time temperature display screen 20, the heating real-time mesh of bottom stage Mark temperature 21, heating bottom stage control button 22, stepper motor speed regulation knob 23, controller "ON" button 24, controller "Off" are pressed Button 25, the heating substrate table real time temperature display screen 17, heating substrate table real-time target temperature 18, heating substrate table control are pressed Key 19, heating bottom stage real time temperature display screen 20, heating bottom stage real-time target temperature 21, heating bottom stage control button 22, stepping Electric machine speed regulation knob 23, controller "ON" button 24, controller "Off" button 25 are connect with single-chip microcontroller.In the machine of controller 1 Burner hearth wiring-connecting socket 26, power outlet 27, rotary heating base station wiring-connecting socket 28, stepper motor are additionally provided on cabinet Power supply line 29.

The principle of the invention is as follows:

5 are shaken the hand by rotation, rotates threaded rod 7, and threaded rod 7 rotates, and drives screwed ring, and then mobile by connecting rod 10 Fixed ring 8 since fixed ring 8 is fixedly connected with support tube 81, and then promotes or reduces heating substrate table 14, heats substrate table 14 spacing for raising and reducing and then adjusting between heating substrate table 14 and heating bottom stage 32.In addition, at work, Ke Yitong The revolving speed that stepper motor speed regulation knob 23 controls stepper motor is crossed, the rotation of stepper motor is passed to by otating drive rod 6 to be added Hot substrate table 14, so that heating substrate table 14 rotates.

(1) present invention using heating heating bottom stage 31 on place can sublimator material come distil generate atmosphere with heating lining The substrate film heated on bottom stage 14 carries out the film needed for reaction generates at a certain temperature.

(2) this hair using heating substrate table 14 and heats 32 top and bottom of bottom stage to the vertical-type depositional mode of placement.

(3) present invention come rotary heating substrate table 14 and can adjust revolving speed by the speed regulation knob 23 on controller 1.

(4) present invention can by rotation 2 heating base stations on shake the hand 5 come adjust heating substrate table 14 and heating bottom stage 32 Distance.

(5) using double heat source separated heatings, heating substrate table 14 is separated from each other the present invention with bottom stage 32 is heated, and can be with Adjust separately temperature.

(6) the fixation metal clips 12 for being used to fix substrate on the heating substrate table 14 of rotary heating base station 2 can root Different fixed screw holes 13 are selected to be installed according to substrate size.

Case

It prepares vapor phase method methylamine bustamentite film: the lead iodide FTO glass substrate film prepared is placed on rotary heating On the heating substrate table 14 of base station 2, lead iodide FTO glass substrate is fixed with fixed metal clips 12, then by methylpyridinium iodide ammonium Powder is placed on the heating bottom stage 32 of 3 bottom of burner hearth, after instrument is installed, is adjusted and is shaken the hand 5 on rotary heating base station 2 The distance between heating substrate table 14 and heating bottom stage 31 are adjusted, the vacuum pump for opening connection gas-guide tube 31 is evacuated to pressure Meter 30 to 10^-1Pa removes air, and adjusts stepper motor speed regulation 24 rotary heating substrate table 14 of knob to make to react more uniform. Controller heating bottom stage control button 22 on operation controller 1 is heated to 200 DEG C of reaction temperature simultaneously for substrate table 14 is heated 20min is kept the temperature, then operates heating substrate table control button 19 on controller 1 and will heat bottom stage 32 and be heated to 150 DEG C and make methyl Ammonium iodide powder starts distillation and generates methylpyridinium iodide ammonium atmosphere, the lead iodide in methylpyridinium iodide ammonium atmosphere and heating substrate table 14 FTO glass substrate film issues biochemical reaction 20min at 200 DEG C and generates final product methylamine bustamentite FTO substrate film, waits When cooling closes to an end, the heating of heating bottom stage 32 is closed, instrument is opened after cooling and takes out the film that vapor phase method prepares.

In conclusion the present invention using heating substrate table and heating bottom stage top and bottom to placement, heat on bottom stage material by It is smaller to which upwards are easier to react with the substrate contact on heating substrate table to thermally decompose the gas density generated；And it serves as a contrast Heating substrate table where bottom is can to adjust the speed rotation, react preparation film can be more uniform, while can also adjust with Heat the distance of bottom stage；The present invention uses double heat sources heating, can adjust separately the material sublimation temperature T1 of heating bottom stage and add The underlayer temperature T2 of hot substrate table, so that the heating process of atmosphere reactive deposition does not influence between each other.

The above is only a preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims

1. A dual heat source vertical atmosphere reaction furnace, characterized in that: comprising a controller (1), a rotary heating base (2) and a hearth (3), the hearth (3) comprising a furnace body (35) with an open end ), furnace cover (36), pressure gauge (30), air duct (31), vacuum pump, heating base (32), the heating base (32) is arranged in the furnace body (35), and the pressure gauge ( 30) is used to measure the pressure in the furnace body (35), the measuring probe of the pressure gauge (30) is arranged in the furnace body (35), and the pressure gauge (30) is connected with the controller (1), so The furnace body (35) is communicated with the vacuum pump through an air duct (31); the rotary heating base (2) includes a stepping motor (4), a rocker (5), a rotary transmission rod (6), and a threaded rod (7) , connecting rod (10), fixing ring (8), support pipe (81), heating substrate table (14), the furnace cover (36) is installed on the open end of the furnace body (35), the threaded rod ( One end of 7) is rotatably connected with the furnace cover (36), the other end of the threaded rod (7) is fixedly connected with the handle (5), and one end of the connecting rod (10) is connected with the threaded rod (7) through a threaded ring , the other end is fixedly connected with the fixing ring (8), and the fixing ring (8) is fixedly installed on the support tube (81); the stepper motor (4) is fixedly installed on one end of the support tube (81), The other end of the support tube (81) is rotatably connected to the heating substrate table (14) through the furnace cover (36), and the support tube (81) is rotatably connected to the furnace cover (36); the rotation transmission rod ( 6) It is arranged in the support tube (81), and one end of the rotating transmission rod (6) is connected with the rotating shaft of the stepping motor (4), and the other end is fixedly connected with the heated substrate stage (14); the heated substrate stage (14) A fixed metal dome (12) is arranged on the side away from the support tube (81); the heating substrate table (14) is arranged opposite to the heating bottom table (32).

2. The vertical atmosphere reaction furnace with dual heat sources according to claim 1, characterized in that: the heating bottom table (32) is fixedly installed on the bottom surface of the furnace body (35) through a fixing screw one (33), and the furnace body (35) is provided with a furnace power socket (34), and the heating bottom table (32) is connected to the furnace power socket (34).

3. The vertical atmosphere reaction furnace with dual heat sources according to claim 1, wherein the furnace cover (36) is provided with a fixed bearing one (15), and the threaded rod (7) and the fixed bearing one (15). 15), the inner ring is fixedly connected, so that the threaded rod (7) is rotatably connected to the furnace cover (36) through the fixed bearing one (15); the furnace cover (36) is provided with a through hole, and the support tube (81) ) pass through the through hole, and the support tube (81) and the through hole have an interference fit.

4. The vertical atmosphere reaction furnace with dual heat sources according to claim 1, characterized in that: the heating substrate table (14) is provided with two fixed bearings (16), the support pipe (81) and the second fixed bearing The inner ring of (16) is fixedly connected, so that the support tube (81) is rotatably connected to the heated substrate table (14) through the second fixed bearing (16).

5 . The vertical atmosphere reaction furnace with dual heat sources according to claim 1 , wherein a scale rod ( 9 ) is arranged on the threaded rod ( 7 ). 6 .

6. The vertical atmosphere reaction furnace with dual heat sources according to claim 1, characterized in that it further comprises a bellows (11) and a bellows limiting flange, wherein the bellows limiting flange is fixedly installed on the support pipe (81). , and the bellows (11) is arranged between the bellows limiting flange and the furnace cover (36).

7. The vertical atmosphere reaction furnace with dual heat sources according to claim 1, wherein the controller (1) comprises a single-chip microcomputer, a real-time temperature display screen (17) of the heated substrate stage, a real-time target temperature of the heated substrate stage (17). 18), heating substrate stage control key (19), heating stage real-time temperature display screen (20), heating stage real-time target temperature (21), heating stage control key (22), stepper motor speed control knob ( 23), the controller "on" button (24), the controller "off" button (25), the heated substrate stage real-time temperature display screen (17), the heated substrate stage real-time target temperature (18), the heated substrate stage Base control button (19), heating base real-time temperature display (20), heating base real-time target temperature (21), heating base control key (22), stepping motor speed control knob (23), controller The "ON" button (24) and the "OFF" button (25) of the controller are both connected to the microcontroller.