CN215087043U - Integrated transient joule heating system for preparing nano material - Google Patents

Integrated transient joule heating system for preparing nano material Download PDF

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Publication number
CN215087043U
CN215087043U CN202120757990.9U CN202120757990U CN215087043U CN 215087043 U CN215087043 U CN 215087043U CN 202120757990 U CN202120757990 U CN 202120757990U CN 215087043 U CN215087043 U CN 215087043U
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capacitor
joule heating
transient
heating system
shell
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陈浩冬
秦海英
魏瑾杨
倪华良
韩旭斌
褚雯
肖学章
刘嘉斌
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Hangzhou Dianzi University
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Hangzhou Dianzi University
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Abstract

The utility model discloses an integrated transient joule heating system for preparing nano materials, which comprises a joule heating device and a sample clamping mechanism; the joule heating device comprises a direct current power supply, a capacitor and a bidirectional switch; the direct current power supply is closed through the bidirectional switch and is connected with the capacitor in series to form a charging loop of the capacitor; and the sample clamping mechanism and the capacitor are closed through the bidirectional switch to form a capacitor discharge loop. The system also comprises a shell, wherein the sample clamping mechanism is sealed in the shell to form a closed reaction cavity; the device also comprises an atmosphere control device which supplies atmosphere to the closed reaction cavity and controls the air pressure. When the device works, the direct-current power supply and the capacitor are switched on, the capacitor is instantaneously discharged after the capacitor is charged, high-energy electron current acts on a sample to form transient joule heat, and the sample is instantaneously heated, decomposed and rapidly cooled under the transient joule heat to obtain the highly dispersed nano material.

Description

Integrated transient joule heating system for preparing nano material
Technical Field
The utility model belongs to the technical field of nanometer preparation, concretely relates to instantaneous joule heating system of preparation nano-material in the industrial production process.
Background
The preparation method of the nano material mainly comprises two ways from bottom to top and from top to bottom, and the specific methods comprise a chemical vapor deposition method, a sol-gel method, a molecular beam epitaxy method and the like. The existing methods have characteristics and specific application categories, such as the chemical vapor deposition method has overhigh substrate temperature and expensive equipment; the raw material cost required by the sol-gel method is high, and the product is difficult to separate; the molecular beam epitaxy method has expensive equipment, complex operation process, high requirement on environment during preparation and high maintenance cost. Technically, the prior art is difficult to realize low cost, high efficiency and wide material range at the same time.
Therefore, a nanomaterial preparation system with simple and safe operation, high efficiency, low cost and wide application range needs to be found.
SUMMERY OF THE UTILITY MODEL
To the above-mentioned problem that prior art exists, the utility model aims to provide a convenient transient state joule heating system realizes low-cost, high efficiency, wide range's preparation nano-material.
The purpose of the utility model is realized by the following technical scheme.
An integrated transient joule heating system for preparing nano material is composed of joule heating unit and reactor. Wherein the reaction device at least comprises a sample clamping mechanism; the joule heating device at least comprises a direct current power supply, a capacitor and a bidirectional switch; the direct current power supply is closed through the bidirectional switch and is connected with the capacitor in series to form a charging loop of the capacitor; the sample clamping mechanism and the capacitor are closed through the bidirectional switch to form a capacitor discharging loop. The joule heating device further includes a circuit control center, and the circuit control center is configured to control the closing of the bidirectional switch, the output voltage of the dc power supply, that is, the charging voltage of the capacitor, and electrical parameters such as the discharging current and the discharging time of the capacitor.
When the device works, a raw material prepared from a conductive nano material, such as metal salt arranged on a conductive substrate, is fixed by a sample clamping mechanism, the charging voltage of a capacitor is set through a circuit control center, and the capacitor is charged by controlling to switch on a direct current power supply and the capacitor; then the circuit control center disconnects the direct current power supply and the capacitor, connects the capacitor and the sample clamping mechanism, the capacitor carries out instantaneous discharge, the high-energy electron current acts on the sample such as metal salt to form transient Joule heat, and the sample is instantaneously heated, decomposed and rapidly cooled under the transient Joule heat to obtain the highly dispersed nano material.
Furthermore, the reaction device also comprises a shell, and the shell seals the sample clamping mechanism in the shell to form a closed reaction cavity; the shell is detachably mounted.
Further, transient state joule heating system still includes atmosphere control device, atmosphere control device includes air supply, gas circuit and vacuum pump, atmosphere control device connects the casing is right the airtight reaction chamber that the casing seals and forms supplies with atmosphere, control atmospheric pressure.
The utility model provides an integration transient state joule heating system for nanomaterial's preparation, its principle is for adopting transient state joule heating, utilizes the high energy electron current to act on metal salt promptly and forms joule heating, makes its decomposition and quick cooling with metal salt instantaneous heating, makes the particle tend to the high dispersion in order to reach the nanometer yardstick. The utility model discloses carry out the integrated design with reaction unit and atmosphere controlling means, can realize low-cost transient state joule heating system. And the circuit control device is independent of the atmosphere control device and the reaction cavity, so that the flexible setting and the flexible change of the power-on parameters are facilitated, and the operation is more flexible. The shell of the reaction cavity can be detached, so that the preparation atmosphere can be further expanded, and the requirements of air and special atmosphere are met.
The utility model discloses a regulation and control a plurality of factors (input electric energy size and speed, metal precursor's load form and kind, atmosphere), combine carrier and precursor to improve nano-catalyst's microstructure, catalytic performance and productivity effect. The utility model provides an equipment can accomplish to use each particle with the electric energy of input in the middle of as far as, compares other nano-catalyst preparation methods simple high-efficient, can be used to industrial production.
Drawings
In order to more clearly illustrate the embodiments and technical solutions of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is the structural schematic diagram of the integrated transient joule heating system of the present invention. Wherein, 1 is a direct current power supply, 2 is a circuit control center, 3 is a capacitor, 4 is a sample clamping mechanism, 5 is a vacuum pump, 6 is an air source, and 7 is a shell of a closed reaction cavity.
FIG. 2 is a schematic diagram of a circuit control center, 21 being a power indicator; 22 is a capacitor charging switch; and 23 is a capacitor discharge switch.
Fig. 3 is a dc power control device, 11 is a dc power display screen; 12 is a DC power main switch; 13 is an output switch; 14 is a current output negative interface; 15 is a ground wire interface; 16 is a current output positive interface; 17 is a voltage coarse tuning knob; 18 is a voltage fine adjustment knob; 19 is a current coarse adjustment knob; and 10 is a current fine adjustment knob.
Fig. 4 is a diagram of a sample holder mechanism. Of which 41 is a sample holder.
FIG. 5 is a view of the closed reaction chamber formed after the housing is installed. Wherein 71 is the sealed housing of example 2.
Detailed Description
In order to clarify the technical solution of the present invention, the following further describes the present invention with reference to the accompanying drawings and specific embodiments.
The utility model discloses an integration transient state joule heating system is shown as attached figure 1, the utility model discloses integration transient state joule heating system's schematic structure diagram. The circuit control center is internally provided with a bidirectional switch for controlling the on-off of the electric connection between the capacitor and the DC power supply and the sample clamping mechanism, and an operation knob connected with the internal bidirectional switch is provided with a charging switch and a discharging switch as shown in figure 2. When the device works, the sample clamping mechanism fixes raw materials for preparing the nano material, a direct current power supply and the capacitor are firstly switched on, the power supply is switched on, the power supply indicator lamp in the figure 2 is turned on, and the capacitor starts to be charged; the capacitance and the working voltage of the capacitor can be adjusted according to the requirement of a sample through a circuit control center; after the charging is finished, the capacitor and the direct-current power supply are disconnected, the bidirectional switch is connected with the capacitor and the sample clamping structure, the capacitor carries out instantaneous discharge, and the discharge current and the discharge time of the capacitor are set and controlled through the circuit control center; in the discharging process, a sample on the clamping mechanism generates transient Joule heat, is instantaneously heated and simultaneously decomposed, and forms nano particles under the condition of quick cooling after discharging. Under the condition that a certain working atmosphere is needed, before the circuit control center is started, the shell is installed, the sample clamping mechanism is sealed in the shell, a closed reaction cavity is formed for the sample, and the air pressure in the closed reaction cavity is controlled through the vacuum pump and the external air source. The instant current of the device can reach 10-300A and the minimum discharge time of 10ms according to different samples.
In the embodiments of the present invention, the dc power supply is controlled by a power control device, as shown in fig. 3, a dc power supply main switch and an output switch are provided, and are electrically connected to the capacitor and the sample clamping mechanism through the current output negative electrode interface and the current output positive electrode interface; the power supply control device is also provided with a voltage coarse adjustment knob, a voltage fine adjustment knob, a current coarse adjustment knob and a current fine adjustment knob, so that the power supply and the current can be controlled more accurately, and the output condition of the direct-current power supply can be visually observed through a direct-current power supply display screen.
Example 1:
sample preparation in air: the atmosphere casing of sealed sample fixture is dismantled, fixes the slice sample on sample clamping structure, and the sample fixture that this embodiment used is specific, through the electrode clamp plate with the screw fixation sample, then circuit control center sets up the required load voltage of condenser and charging current, opens the charge switch on the circuit control center of fig. 2, lets the condenser full of voltage in the control circuit until DC power supply output current is 0A, closes the charge switch after the completion of charging. The discharge switch is then opened to allow current to be rapidly applied to the sample across the clamp.
Example 2:
unlike example 1, the product was prepared in a specific atmosphere. Sample preparation in a specific atmosphere: by adopting the same sample clamping method as in example 1, as shown in fig. 4, after the sample is placed, the sealed shell is installed and fixed, and is sealed and fixed by the sealing ring, the flange and the screw, so as to form a sealed reaction chamber, as shown in fig. 5, the sealed reaction chamber is formed by the sealed connection between the sealed shell and the base of the sample clamp in this embodiment. And opening a vacuum pump to exhaust the closed reaction cavity in sequence, observing that the air pressure in a barometer reactor is less than-0.1 MPa, then closing the vacuum pump, opening an air source, observing the barometer to enable a reaction sample to be in a certain protective atmosphere, setting charging parameters, charging a capacitor, then discharging the sample to enable the sample to be heated in a transient state, and preparing the required final product. And (5) closing the air source after all the samples are prepared.
The above embodiments show and describe the basic principles and main features of the technical solution of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the embodiments and descriptions are only illustrative of the principles of the present invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention, and the changes and modifications are within the scope of the invention as claimed.

Claims (5)

1. An integrated transient joule heating system for preparing nano materials is characterized in that: the transient Joule heating system at least comprises a Joule heating device and a reaction device; wherein the reaction device at least comprises a sample clamping mechanism; the joule heating device at least comprises a direct current power supply, a capacitor and a bidirectional switch; the direct current power supply is closed through the bidirectional switch and is connected with the capacitor in series to form a charging loop of the capacitor; the sample clamping mechanism and the capacitor are closed through the bidirectional switch to form a capacitor discharging loop; the joule heating device further includes a circuit control center, and the circuit control center is configured to control the closing of the bidirectional switch, the output voltage of the dc power supply, that is, the charging voltage of the capacitor, and electrical parameters such as the discharging current and the discharging time of the capacitor.
2. The integrated transient joule heating system for nanomaterial fabrication according to claim 1, wherein: the reaction device also comprises a shell, and the sample clamping mechanism is sealed in the shell by the shell to form a closed reaction cavity.
3. The integrated transient joule heating system for nanomaterial fabrication according to claim 1, wherein: the shell is detachably mounted.
4. The integrated transient joule heating system for nanomaterial fabrication according to claim 2, wherein: the transient joule heating system further comprises an atmosphere control device, wherein the atmosphere control device comprises an air source, an air path and a vacuum pump, and the atmosphere control device is connected with the shell and is used for supplying atmosphere and controlling air pressure to the sealed reaction cavity formed by sealing the shell.
5. The integrated transient joule heating system for nanomaterial fabrication according to claim 1, wherein: the transient joule heating system can provide instantaneous current of at least 10-300A and minimum discharge time of 10 ms.
CN202120757990.9U 2021-04-14 2021-04-14 Integrated transient joule heating system for preparing nano material Active CN215087043U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113578222A (en) * 2021-07-12 2021-11-02 浙江大学 Nanocomposite synthesis device based on instantaneous high-temperature Joule heating method, preparation method and application
CN115318219A (en) * 2022-10-12 2022-11-11 常州烯聚新材料科技有限公司 Needle electrode discharge tube suitable for flash joule heating process and joule heating equipment

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113578222A (en) * 2021-07-12 2021-11-02 浙江大学 Nanocomposite synthesis device based on instantaneous high-temperature Joule heating method, preparation method and application
CN115318219A (en) * 2022-10-12 2022-11-11 常州烯聚新材料科技有限公司 Needle electrode discharge tube suitable for flash joule heating process and joule heating equipment
CN115318219B (en) * 2022-10-12 2023-08-18 常州烯聚新材料科技有限公司 Needle electrode discharge tube suitable for flash Joule heating process and Joule heating equipment

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