CN209027283U - A kind of tube furnace for nano material growth - Google Patents

A kind of tube furnace for nano material growth Download PDF

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Publication number
CN209027283U
CN209027283U CN201821747603.8U CN201821747603U CN209027283U CN 209027283 U CN209027283 U CN 209027283U CN 201821747603 U CN201821747603 U CN 201821747603U CN 209027283 U CN209027283 U CN 209027283U
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China
Prior art keywords
nano material
push rod
temperature
hollow push
material growth
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Expired - Fee Related
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CN201821747603.8U
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Chinese (zh)
Inventor
王红波
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Changan University
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Changan University
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Abstract

The utility model discloses a kind of tube furnaces for nano material growth, including furnace body, heating tube is provided in furnace body, furnace body is stretched out at the both ends of heating tube, the both ends of heating tube are provided with end cap, perforation is offered on one end cap, hollow push rod is provided in perforation, and hollow push rod is moved left and right along perforation;One end of hollow push rod is provided with carrying apparatus, and the other end stretches out heating tube;Temperature measuring equipment is provided in hollow push rod, the thermometric end of temperature measuring equipment stretches out the loading end of hollow push rod, for measuring the temperature of reaction mass on carrying apparatus;Bleeding point is offered on another end cap.The utility model realizes the accurate control of the real-time adjustment and nano material reaction temperature of reaction mass position, real-time temperature regulation can be achieved, the change for avoiding nano material growth behavior caused by the temperature difference of control temperature and actual temperature, improves the reproducibility of nano material growth course.

Description

A kind of tube furnace for nano material growth
Technical field
The utility model belongs to nano material Preparation equipment technical field, grows more particularly, to one kind for nano material Tube furnace.
Background technique
In recent years, with the high speed development of nano materials research and application, tube furnace is answered field of nano material preparation With more and more.The growth mechanism that tube furnace prepares nano material is mainly VLS mechanism, i.e., gas-liquid-solid mechanism, this mechanism is first Raw material prepared by nano material are first heated to certain temperature and are evaporated gasification, then this high-temperature gasification raw material is in nanometer Condensation becomes liquid on the substrate of material preparation, and liquid is precipitated under catalyst or flux effect is changed into solid nano material Material.In this growth course, the temperature of raw material and growth substrates must be fixed, and the growth behavior of nano material is easily grown The influence of condition slight change, especially temperature condition, the nuance of temperature may result in appearance of nano material and structure Significant changes, therefore be one of the key point of controllable preparation nano material to the accurate control of growth temperature.
Tube furnace in-furnace temperature currently on the market is uneven, and tubular type furnace electric thermo-couple is generally loaded on furnace body center, if Determining the temperature that heating temperature is generally its heating tube center leads to it due to the heat loss at diamond heating pipe both ends Center temperature highest is gradually decreased along tube furnace center to both ends temperature, shows certain temperature gradient (such as Fig. 3 institute Show).
In nano material growth course, due to being manually placed into the location error of reaction mass, nano material will lead to Growth temperature generates certain error, and in nano material growth course, may lead due to being passed through gas or reaction release latent heat It causes the temperature of reaction mass to change, therefore causes the uncontrollable of nano material growth behavior, and make nano material reproducibility Difference.
Utility model content
To solve the above-mentioned problems, the purpose of this utility model is to propose a kind of tube furnace for nano material growth, The real-time adjustment of reaction mass position and the accurate control of nano material reaction temperature are realized, it can be achieved that real-time temperature tune Control avoids the change of nano material growth behavior caused by the temperature difference of control temperature and actual temperature, improves a nanometer material Expect the reproducibility of growth course.
In order to achieve the above object, the utility model is resolved using following technical scheme.
A kind of tube furnace for nano material growth, including furnace body are provided with heating tube, the heating in the furnace body The furnace body is stretched out at the both ends of pipe, and the both ends of the heating tube are provided with end cap, perforation is offered on an end cap, described Hollow push rod is provided in perforation, and the hollow push rod is moved left and right along the perforation;One end of the hollow push rod is arranged There is carrying apparatus, the other end stretches out the heating tube;Temperature measuring equipment, the survey of the temperature measuring equipment are provided in the hollow push rod The loading end of hollow push rod is stretched out at warm end, for measuring the temperature of reaction mass on carrying apparatus;On another described end cap Offer bleeding point.
In addition, the tube furnace provided by the utility model for nano material growth can also have following supplementary technology special Sign:
Preferably, the extension end of the hollow push rod is connected with driving device.
It is further preferred that the driving device includes ball-screw and stepper motor, the nut seat of the ball-screw It is connect with the extension end of the hollow push rod, the output axis connection of the end of the ball screw and the stepper motor.
Preferably, the temperature measuring equipment is connected with controller, and the input terminal of the controller is defeated with the temperature measuring equipment Outlet connection, the output end of the controller are connect with the control terminal of the stepper motor.
Preferably, the both ends of the heating tube are tightly connected with two end caps by vacuum flange.
Preferably, the hollow push rod is high temperature resistant heat insulation material.
Preferably, the hollow push rod and end cap are connected at perforation using dynamic sealing.
Preferably, the temperature measuring equipment is thermocouple.
Preferably, the carrying apparatus is specimen holder or sample table.
Preferably, vacuum meter is provided on the side wall of the heating tube.
Be compared with the prior art, the utility model has the following beneficial effects: by the side-to-side movement of hollow push rod realize to Reaction mass real-time accurate adjustment of position in tube furnace is realized in conjunction with the temperature distribution history of tube furnace to reactant Expect the real-time adjustment of reaction temperature;By the setting of the temperature measuring equipment in hollow push rod, nano material reaction temperature is realized Accurate control, avoids the temperature difference of the temperature and tube furnace control temperature at reaction mass, and then avoids control temperature The change of nano material growth behavior caused by temperature difference with actual temperature, improves the reproduction of nano material growth course Property, improve the stability of the nano material quality of preparation.
Detailed description of the invention
The utility model is described in further details in the following with reference to the drawings and specific embodiments.
Fig. 1 is a kind of structural schematic diagram of embodiment of tube furnace for nano material growth of the utility model.
Fig. 2 is the connection figure of driving device in the utility model.
Fig. 3 is the temperature distribution history of tube furnace.
In the above figure: 1 furnace body;101 bleeding points;102 vacuum meters;2 heating tubes;201 vacuum flanges;3 hollow push rods;301 Elastic seal ring;4 carrying apparatus;5 temperature measuring equipments;6 driving devices;601 stepper motors;602 ball-screws;7 controllers.
Specific embodiment
With reference to Fig. 1, a kind of tube furnace for nano material growth of the utility model, including furnace body 1 is set in furnace body 1 It is equipped with heating tube 2, furnace body 1 is stretched out at the both ends of heating tube 2, and the both ends of heating tube 2 are provided with end cap, it is used for heated sealed pipe 2, one Perforation is offered on a end cap, hollow push rod 3 is provided in perforation, and hollow push rod 3 is moved left and right along perforation, hollow push rod 3 One end be provided with carrying apparatus 4, the other end stretches out heating tube 2;Carrying apparatus 4 makes for placing reaction mass to anti- It answers material to move left and right in heating tube 2 with hollow push rod 3 along perforation, thus can adjust at any time reaction mass and exist Position in heating tube 2, while facilitating the handling of reactant, reduce the error generated in manual cargo handling process.
Temperature measuring equipment 5 is provided in hollow push rod 3, the thermometric end of temperature measuring equipment 5 stretches out the loading end of hollow push rod 3, uses In the temperature of reaction mass on measurement carrying apparatus 4, experimenter is enable to obtain the actual response of reaction mass in real time Temperature, and then can realize the accurate control of nano material reaction temperature, while avoiding to be passed through gas or react release latent heat and lead The temperature of the reaction mass of cause changes, the temperature difference of the temperature at reaction mass and tube furnace control temperature, and then keeps away The change for having exempted from nano material growth behavior caused by controlling the temperature difference of temperature and actual temperature improves nano material growth The reproducibility of process improves the stability of the nano material quality of preparation;Bleeding point 101 is offered on another end cap.It takes out Port 101 can connect vacuum pump, to vacuumizing in heating tube 2, can also connect inertia gas cylinder, to being filled with indifferent gas in heating tube 2 Body makes the atmosphere in heating tube 2 be suitble to the growth of nano material.
The tube furnace for nano material growth of the utility model, also has following additional embodiment:
With reference to Fig. 2, one embodiment according to the present utility model, the extension end of hollow push rod 3 is connected with driving device 6.
In the embodiment above, driving device 6 is used to provide power for moving left and right for hollow push rod 3.
With reference to Fig. 2, one embodiment according to the present utility model, driving device 6 includes ball-screw 602 and stepper motor 601, the nut seat of ball-screw 602 is connect with the extension end of hollow push rod 3, end and the stepper motor 601 of ball screw Export axis connection.
In the embodiment above, the output shaft of stepper motor 601 drives ball-screw 602 to rotate, and passes through ball-screw 602 Rotary motion conversion is become to the linear motion of the nut seat on ball-screw 602, the extension end of hollow push rod 3 and ball-screw 602 nut seat connection, makes hollow push rod 3 do linear reciprocating motion with the nut seat of ball-screw 602, thus realizes Moving left and right for hollow push rod 3, makes the position real-time, tunable of the reactant on carrying apparatus 4, in conjunction with the survey in hollow push rod 3 Warm device 5 realizes the accurate control of nano material growth temperature;In addition, the structure of the driving device 6 is simple, occupied space It is small, without doing larger change to existing equipment.
With reference to Fig. 1-Fig. 3, one embodiment according to the present utility model, temperature measuring equipment 5 is connected with controller 7, controller 7 Signal input part connect with the signal output end of temperature measuring equipment 5, the control of the signal output end of controller 7 and stepper motor 601 End connection processed.
In the embodiment above, the temperature distribution history of tube furnace is stored in controller 7, before reaction starts, controller 7 The theoretical placement location that reaction mass is determined according to the curve transmits the signal to stepper motor 601, stepper motor 601 Hollow push rod 3 is pushed to be moved to the position;In reaction process, temperature measuring equipment 5 obtains the reaction temperature of nano material in real time, and leads to It crosses controller 7 to be compared with set temperature, when the two is unequal, controller 7 controls stepper motor 601 and drives hollow push rod 3 is mobile, is adjusted in real time to the position of reactant, until real reaction temperature is equal with set temperature, realizes a nanometer material Expect the real-time adjustment of growth temperature, and then avoids growth behavior change and reproducibility caused by nano material reaction temperature changes Low problem.
With reference to Fig. 1, one embodiment according to the present utility model is led to respectively between the both ends of heating tube 2 and two end caps Cross the sealing of vacuum flange 201.
In the embodiment above, it is sealed between 2 both ends of heating tube and two end caps by vacuum flange 201, guarantees heating Air-tightness in pipe 2, and then keep nanometer reaction atmosphere controllable.
With reference to Fig. 1, one embodiment according to the present utility model, hollow push rod 3 is high temperature resistant heat insulation material.
In the embodiment above, hollow push rod 3 is high temperature resistant heat insulation material, such as high-temperature resistant aluminium oxide ceramics, is made hollow Push rod 3 can not deform under the reaction temperature of nano material, and temperature measuring equipment 5 is protected to be not affected by high temperatures, and make nanometer The temperature adjustment process of the reaction of material can be gone on smoothly.
With reference to Fig. 1, one embodiment according to the present utility model, hollow push rod 3 and end cap use dynamic sealing at perforation Connection.
In the embodiment above, dynamic sealing is connected as that elastic seal ring is arranged at the perforation of hollow push rod 3 and end cap 301, in the moving process of hollow push rod 3, is compressed by the deformation of elastic seal ring 301 and realize sealing, and then guarantee heating The air-tightness of pipe 2.
With reference to Fig. 1, one embodiment according to the present utility model, temperature measuring equipment 5 is thermocouple.
In the embodiment above, the hot end of thermocouple can high temperature resistant, conducting wire is placed in hollow push rod 3, and conducting wire pass through it is outer Protective case protection in portion's damages conducting wire from high temperature, and terminals are placed in outside heating tube 2, and thermocouple temperature measurement can be done directly on to be measured On object, compared to induction temperature sensing, more acurrate convenience is measured, is surveyed more suitable for the growth temperature of thermally sensitive nano material Amount.
With reference to Fig. 1, one embodiment according to the present utility model, carrying apparatus 4 is specimen holder or sample table.
In the embodiment above, specimen holder and sample table are convenient for the handling of sample.
With reference to Fig. 1, one embodiment according to the present utility model is provided with vacuum meter 102 on the side wall of heating tube 2.
In the embodiment above, vacuum meter 102 is used to show the vacuum degree in tube furnace, and then instructs heating start-up time With check furnace in whether gas leakage, convenient for the control of reaction process.
Reaction mass in the utility model is the raw material for preparing nano material.
Obviously, it is practical without departing from this can to carry out various modification and variations to the utility model by those skilled in the art Novel spirit and scope.If in this way, these modification and variations of the utility model belong to the utility model claims and Within the scope of its equivalent technologies, then the utility model is also intended to include these modifications and variations.

Claims (10)

1. a kind of tube furnace for nano material growth, which is characterized in that including furnace body (1), be provided in the furnace body (1) The furnace body (1) is stretched out at the both ends of heating tube (2), the heating tube (2);The both ends of the heating tube (2) are provided with end cap, and one Perforation is offered on a end cap, is provided in the perforation hollow push rod (3), and the hollow push rod (3) is worn along described Hole moves left and right;
One end of the hollow push rod (3) is provided with carrying apparatus (4), and the other end stretches out the heating tube (2);It is described hollow to push away It is provided with temperature measuring equipment (5) in bar (3), the thermometric end of the temperature measuring equipment (5) stretches out the loading end of hollow push rod (3), is used for Measure the temperature of reaction mass on carrying apparatus (4);Bleeding point (101) are offered on another described end cap.
2. the tube furnace according to claim 1 for nano material growth, which is characterized in that the hollow push rod (3) Extension end be connected with driving device (6).
3. the tube furnace according to claim 2 for nano material growth, which is characterized in that the driving device (6) Comprising ball-screw (602) and stepper motor (601), nut seat and the hollow push rod (3) of the ball-screw (602) Extension end connection, the output axis connection of the end of the ball screw and the stepper motor (601).
4. the tube furnace according to claim 3 for nano material growth, which is characterized in that the temperature measuring equipment (5) It is connected with controller (7), the signal input part of the controller (7) is connect with the signal output end of the temperature measuring equipment (5), institute The signal output end for stating controller (7) is connect with the control terminal of the stepper motor (601).
5. the tube furnace according to claim 1 for nano material growth, which is characterized in that the heating tube (2) Both ends are tightly connected with two end caps by vacuum flange (201).
6. the tube furnace according to claim 1 for nano material growth, which is characterized in that the hollow push rod (3) For high temperature resistant heat insulation material.
7. the tube furnace according to claim 1 for nano material growth, which is characterized in that the hollow push rod (3) It is connect at perforation using dynamic sealing with end cap.
8. the tube furnace according to claim 1 for nano material growth, which is characterized in that the temperature measuring equipment (5) For thermocouple.
9. the tube furnace according to claim 1 for nano material growth, which is characterized in that the carrying apparatus (4) For specimen holder or sample table.
10. the tube furnace according to claim 1 for nano material growth, which is characterized in that the heating tube (2) Vacuum meter (102) are provided on side wall.
CN201821747603.8U 2018-10-26 2018-10-26 A kind of tube furnace for nano material growth Expired - Fee Related CN209027283U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201821747603.8U CN209027283U (en) 2018-10-26 2018-10-26 A kind of tube furnace for nano material growth

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201821747603.8U CN209027283U (en) 2018-10-26 2018-10-26 A kind of tube furnace for nano material growth

Publications (1)

Publication Number Publication Date
CN209027283U true CN209027283U (en) 2019-06-25

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114288956A (en) * 2021-12-31 2022-04-08 浙江中控技术股份有限公司 Reactor temperature control method and device and computer equipment

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114288956A (en) * 2021-12-31 2022-04-08 浙江中控技术股份有限公司 Reactor temperature control method and device and computer equipment

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Granted publication date: 20190625

Termination date: 20191026