CN114405404A - Improved doping reaction device - Google Patents
Improved doping reaction device Download PDFInfo
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- CN114405404A CN114405404A CN202210020221.XA CN202210020221A CN114405404A CN 114405404 A CN114405404 A CN 114405404A CN 202210020221 A CN202210020221 A CN 202210020221A CN 114405404 A CN114405404 A CN 114405404A
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- crucible
- doping reaction
- upper cover
- doping
- reaction
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 143
- 238000003756 stirring Methods 0.000 claims abstract description 49
- 239000000376 reactant Substances 0.000 claims abstract description 15
- 238000007789 sealing Methods 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000010687 lubricating oil Substances 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 62
- 239000002912 waste gas Substances 0.000 abstract description 6
- 239000011261 inert gas Substances 0.000 abstract description 3
- 238000005086 pumping Methods 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses an improved doping reaction device which comprises an upper cover, a gas generation crucible and a doping reaction crucible. The gas required for the doping reaction is temporarily prepared through the gas generation crucible positioned in the doping reaction crucible, and an additional gas generation device or a storage device is not required; vacuumizing the reaction chamber or further introducing inert gas through a vacuumizing channel of the upper cover before the doping reaction so as to ensure the purity of the gas atmosphere during the doping reaction; the stirring device driven by the clockwork spring mechanism can stir the doped reactants in a high-temperature environment so as to fully perform the reaction; after the reaction is finished, the waste gas in the device can be collected through a vacuumizing channel for treatment; the device has the advantages of simple structure, lower cost and convenient use, and can be used for preparing high-purity doped reactants.
Description
Technical Field
The invention belongs to the field of chemical reaction devices, and particularly relates to an improved doping reaction device.
Background
When some doping reactions are carried out, it is often necessary to ensure that the reactions are carried out in a certain pure gas atmosphere, and a common way is to directly introduce gases required for the reactions into a reactor (such as a tube furnace) until the reactions are finished, which causes a large amount of waste gas to be discharged into the environment, so that the pollution is large, and in order to ensure the gas atmosphere of the reactions, the required gases need to be continuously prepared and introduced, so that the cost is high. In addition, the purity of the doped product is also affected in the early stage of the reaction due to the air mixed in the reactor. In order to ensure the purity of the gas atmosphere, for some reactors with good gas tightness, the reactor can be vacuumized before doping reaction, and then required gas is introduced during the reaction, but an additional gas preparation device or a storage device is still needed, and the preparation at the front stage is complicated. In order to ensure the sufficient progress of the doping reaction, the reactant needs to be stirred while ensuring the required pure gas atmosphere, in the existing method, a magnetic stirring rod can be placed at the bottom in the reactor, the stirring rod is driven by an external magnetic field to stir the reactant, but the cost of the generation and control device of the external magnetic field is higher, and if an electric-driven stirring device is directly additionally arranged on the reactor, the method is not suitable for the doping reaction needing high temperature conditions.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an improved doping reaction device which can ensure the purity of the required gas atmosphere and the sufficient doping reaction without an additional gas generation device. The invention adopts the following technical scheme:
an improved doping reaction device comprises an upper cover, a gas generation crucible and a doping reaction crucible;
the upper cover is tightly fixed with the doping reaction crucible through a fastening structure to form a reaction chamber, a sealing structure is arranged between the upper cover and the doping reaction crucible, the upper cover is also provided with a through vacuumizing channel for exhausting gas in the reaction chamber, and a control valve is arranged above the vacuumizing channel for opening or closing the vacuumizing channel;
the gas generation crucible comprises a gas generation chamber, a gas generation reaction chamber and an upper cover, wherein the gas generation chamber is used for containing reactants required during gas preparation, the gas generation crucible is placed in the doping reaction crucible during doping reaction, a certain distance is reserved between the gas generation crucible and the upper cover to ensure gas circulation in the reaction chamber, and after the doping reaction is finished, the upper cover is opened to take the gas generation crucible out of the doping reaction crucible;
the inner diameter of the lower half part of the doping reaction crucible is smaller than that of the upper half part of the doping reaction crucible, the maximum outer diameter of the gas generation crucible is larger than that of the lower half part of the doping reaction crucible, a doping reaction chamber is formed between the gas generation crucible and the bottom of the doping reaction crucible, and the doping reaction chamber is used for containing reactants required by doping reaction.
Further, the fastening structure is: the edge parts of the upper cover and the doping reaction crucible are separately provided with a plurality of corresponding threaded holes, and the upper cover and the doping reaction crucible are tightly fixed through bolts.
Further, the sealing structure is: corresponding surrounding grooves are formed in the edge portions of the upper cover and the doping reaction crucible, protruding sealing rubber strips are embedded in the surrounding grooves of the upper cover or the doping reaction crucible, and when the upper cover and the doping reaction crucible are closed, the sealing rubber strips fill surrounding channels formed by the surrounding grooves of the upper cover and the doping reaction crucible.
Furthermore, a stirring connecting rod penetrating through the upper cover is arranged in the center of the upper cover, the stirring connecting rod is connected with a clockwork mechanism through a gear fixed at the upper end of the stirring connecting rod, the clockwork mechanism drives the stirring connecting rod to rotate through the gear, the clockwork mechanism is fixed on the upper surface of the upper cover, and a clockwork is wound on the clockwork mechanism through a clockwork hole;
when the upper cover and the doping reaction crucible are closed, the lower end of the stirring connecting rod is inserted into a bearing fixed at the bottom of the doping reaction crucible, the inner ring structure of the bearing is matched with the shape of the lower end of the stirring connecting rod, the inner ring of the bearing also rotates along with the connecting rod when the connecting rod rotates, a plurality of stirring blades are further arranged at the bottom of the doping reaction crucible, the stirring blades are fixedly connected with the inner ring of the bearing, and the inner ring of the bearing rotates to drive the stirring blades to rotate so as to stir reactants.
Further, the stirring connecting rod penetrates through the upper cover after passing through the airtight bearing, the airtight bearing is located on the upper surface of the upper cover, and the contact surface of the airtight bearing and the upper cover is identical in smoothness and coated with lubricating oil to form an air isolation layer.
Furthermore, the middle part of the gas generation crucible is a through connecting rod channel, the outer wall of the connecting rod channel and the inner wall of the gas generation crucible form a gas generation chamber, and a certain gap is reserved between the stirring connecting rod and the connecting rod channel when the stirring connecting rod passes through the connecting rod channel so as to ensure the gas circulation in the reaction chamber.
The invention has the beneficial effects that: the invention simplifies the preparation flow of the doping reaction, and the gas required by the doping reaction is temporarily prepared by the gas generation crucible positioned in the doping reaction crucible without an additional gas generation device or a storage device; vacuumizing the reaction chamber or further introducing inert gas through a vacuumizing channel of the upper cover before the doping reaction so as to ensure the purity of the gas atmosphere during the doping reaction; the stirring device driven by the clockwork spring mechanism can stir the doped reactants in a high-temperature environment so as to fully perform the reaction; after the reaction is finished, the waste gas in the device can be collected through a vacuumizing channel for treatment; the device has the advantages of simple structure, lower cost and convenient use, and can be used for preparing high-purity doped reactants.
Drawings
FIG. 1 is a sectional view showing the overall structure of the apparatus of the present invention;
FIG. 2 is a top view of the upper cover of the apparatus of the present invention;
FIG. 3 is a schematic view of a gas generating crucible in the apparatus of the present invention;
FIG. 4 is a top view of a doping reaction crucible in the apparatus of the present invention;
FIG. 5 is a schematic view of the connection between the stirring rod and the airtight bearing in the apparatus of the present invention;
the device comprises a threaded hole 1, an upper cover 2, a vacuum pumping channel 3, a surrounding groove 4, a bearing 5, a doping reaction crucible 6, a gas generation crucible 7, a doping reaction chamber 8, a gas generation chamber 9, a clockwork spring mechanism 10, a gear 11, a stirring connecting rod 12, a connecting rod inserting hole 13, a stirring blade 14, a spring hole 15, an airtight bearing 16, a bearing ball 17 and an airtight surface 18.
Detailed Description
The present invention will now be described in further detail with reference to the accompanying drawings.
As shown in FIGS. 1 to 5, the improved doping reaction apparatus provided by the present invention mainly comprises three parts, namely an upper cover 2, a gas generating crucible 7 and a doping reaction crucible 6. Wherein, the upper cover 2 is matched with the doping reaction crucible 6 and is used for sealing the doping reaction crucible 6, and the gas generating crucible 7 is an independent crucible and can be placed in the doping reaction crucible 6.
The upper cover 2 is tightly fixed with the doping reaction crucible 6 through a fastening structure to form a reaction chamber, a sealing structure is arranged between the upper cover 2 and the doping reaction crucible 6, the upper cover 2 is further provided with a through vacuumizing channel 3 for exhausting gas in the reaction chamber, and a control valve is arranged above the vacuumizing channel 3 for opening or closing the vacuumizing channel 3. The fastening structure can be a bolt fixing structure, namely, a plurality of corresponding threaded holes 1 are formed in the edge parts of the upper cover 2 and the doping reaction crucible 6, the upper cover 2 and the doping reaction crucible 6 are tightly fixed through bolts, and other buckling and locking structures and the like can be adopted. The sealing structure is as follows: corresponding surrounding grooves 4 are formed in the edge portions of the upper cover 2 and the doping reaction crucible 6, protruding sealing rubber strips are embedded in the surrounding grooves 4 of the upper cover 2 or the doping reaction crucible 6, and when the upper cover 2 and the doping reaction crucible 6 are closed, the sealing rubber strips fill surrounding channels formed by the surrounding grooves 4 of the upper cover 2 and the doping reaction crucible 6 so as to isolate air.
The gas generation crucible 7 comprises a gas generation chamber 9 for containing reactants required during gas preparation, the gas generation crucible 7 is placed in the doping reaction crucible 6 during doping reaction, a certain distance exists between the gas generation crucible 7 and the upper cover 2 to ensure gas circulation in the reaction chamber, and after the doping reaction is finished, the upper cover 2 is opened to take the gas generation crucible 7 out of the doping reaction crucible 6.
The inner diameter of the lower half part of the doping reaction crucible 6 is smaller than that of the upper half part thereof, and the maximum outer diameter of the gas generation crucible 7 is larger than that of the lower half part of the doping reaction crucible 6, namely, the gas generation crucible 7 can be placed in the doping reaction crucible 6 and is not contacted with the bottom of the doping reaction crucible 6, so that a doping reaction chamber 8 is formed between the gas generation crucible 7 and the bottom of the doping reaction crucible 6 and is used for containing reactants required by the doping reaction.
In order to ensure the full progress of the doping reaction, a stirring structure is also arranged in the device. A stirring link 12 penetrating the upper cover 2 is arranged at the center of the upper cover 2, the stirring link 12 is connected with a clockwork mechanism 10 through a gear 11 fixed at the upper end of the stirring link 12, the clockwork mechanism 10 drives the stirring link 12 to rotate through the gear 11, the clockwork mechanism 10 is fixed on the upper surface of the upper cover 2, and the clockwork mechanism 10 is clockwork through a clockwork hole 15. When the upper cover 2 and the doping reaction crucible 6 are closed, the lower end of the stirring connecting rod 12 is inserted into a bearing 5 fixed at the bottom of the doping reaction crucible 6, the inner ring structure of the bearing 5 is matched with the shape of the lower end of the stirring connecting rod 12, the inner ring of the bearing 5 rotates along with the rotation of the connecting rod, a plurality of stirring blades 14 are further arranged at the bottom of the doping reaction crucible 6, the stirring blades 14 are fixedly connected with the inner ring of the bearing 5, and the stirring blades 14 are driven to rotate by the rotation of the inner ring of the bearing 5 so as to stir reactants.
In order to ensure the air tightness of the reaction chamber, the stirring connecting rod 12 penetrates through the upper cover 2 after passing through an air-tight bearing 16, the air-tight bearing 16 is positioned on the upper surface of the upper cover 2, the contact surface (air-tight surface 18) of the air-tight bearing 16 and the upper cover 2 has the same finish and is coated with lubricating oil to form an air isolating layer, and the air-tight surface 18 is made of extremely smooth material, and the finish is more than 12 grades (Ra < 0.05). The middle part of the gas generating crucible 7 is a through connecting rod channel, the outer wall of the connecting rod channel and the inner wall of the gas generating crucible 7 form a gas generating chamber 9, and a certain gap is formed between the stirring connecting rod 12 and the connecting rod channel when the stirring connecting rod passes through the connecting rod channel so as to ensure the gas circulation in the reaction chamber.
The device is simple to use, takes the preparation of the sulfur-doped graphite-phase carbon nitride as an example, and has the following use flow:
(1) medicine charge
Firstly, graphite-phase carbon nitride is put into a doping reaction crucible 6, thiourea is put into a gas generation crucible 7, and then the gas generation crucible 7 is put into the doping reaction crucible 6 and is kept stable.
(2) Preparation before reaction
The upper cover 2 is covered on the doping reaction crucible 6, and the stirring connecting rod 12 is inserted into the connecting rod inserting hole 13 of the bearing 5 after passing through the connecting rod channel of the gas generating crucible 7;
aligning the threaded hole 1 of the upper cover 2 with the threaded hole 1 of the doping reaction crucible 6, inserting a bolt and screwing;
the control valve of the vacuum-pumping channel 3 is opened, the device of the invention is connected to a vacuum-pumping machine, the control valve is closed after the air in the device is exhausted, and the control valve can also be closed after the inert gas is introduced.
(3) Starting the reaction
The reaction is initiated by winding the spring mechanism 10 through the spring hole 15 and placing the apparatus of the invention in a muffle furnace for heating.
(4) Post-processing
After the reaction is finished, taking out the device from the muffle furnace, cooling to room temperature, connecting the vacuumizing channel 3 with a waste gas collector or a waste gas processor, and opening a control valve to pump out waste gas in the device;
and opening the upper cover 2, taking out the gas reaction crucible, recovering and treating residual substances in the gas reaction crucible, and taking out a reaction product at the bottom of the doping reaction crucible 6 to obtain a doping reaction product.
It should be noted that the terms "upper", "lower", "left", "right", "front", "back", etc. used in the present invention are for clarity of description only, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the terms is not limited by the technical contents of the essential changes.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.
Claims (6)
1. An improved doping reaction device is characterized by comprising an upper cover, a gas generation crucible and a doping reaction crucible;
the upper cover is tightly fixed with the doping reaction crucible through a fastening structure to form a reaction chamber, a sealing structure is arranged between the upper cover and the doping reaction crucible, the upper cover is also provided with a through vacuumizing channel for exhausting gas in the reaction chamber, and a control valve is arranged above the vacuumizing channel for opening or closing the vacuumizing channel;
the gas generation crucible comprises a gas generation chamber, a gas generation reaction chamber and an upper cover, wherein the gas generation chamber is used for containing reactants required during gas preparation, the gas generation crucible is placed in the doping reaction crucible during doping reaction, a certain distance is reserved between the gas generation crucible and the upper cover to ensure gas circulation in the reaction chamber, and after the doping reaction is finished, the upper cover is opened to take the gas generation crucible out of the doping reaction crucible;
the inner diameter of the lower half part of the doping reaction crucible is smaller than that of the upper half part of the doping reaction crucible, the maximum outer diameter of the gas generation crucible is larger than that of the lower half part of the doping reaction crucible, a doping reaction chamber is formed between the gas generation crucible and the bottom of the doping reaction crucible, and the doping reaction chamber is used for containing reactants required by doping reaction.
2. An improved doping reaction device as set forth in claim 1, wherein said fastening structure is: the edge parts of the upper cover and the doping reaction crucible are separately provided with a plurality of corresponding threaded holes, and the upper cover and the doping reaction crucible are tightly fixed through bolts.
3. An improved doping reaction device as set forth in claim 1 or 2, wherein said sealing structure is: corresponding surrounding grooves are formed in the edge portions of the upper cover and the doping reaction crucible, protruding sealing rubber strips are embedded in the surrounding grooves of the upper cover or the doping reaction crucible, and when the upper cover and the doping reaction crucible are closed, the sealing rubber strips fill surrounding channels formed by the surrounding grooves of the upper cover and the doping reaction crucible.
4. An improved doping reaction device as set forth in claim 1, wherein the upper cover is centrally provided with a stirring link penetrating the upper cover, the stirring link being connected to a clockwork mechanism through a gear fixed to an upper end thereof, the clockwork mechanism being rotated by the stirring link through the gear, the clockwork mechanism being fixed to an upper surface of the upper cover and being clockwork by the clockwork hole;
when the upper cover and the doping reaction crucible are closed, the lower end of the stirring connecting rod is inserted into a bearing fixed at the bottom of the doping reaction crucible, the inner ring structure of the bearing is matched with the shape of the lower end of the stirring connecting rod, the inner ring of the bearing also rotates along with the connecting rod when the connecting rod rotates, a plurality of stirring blades are further arranged at the bottom of the doping reaction crucible, the stirring blades are fixedly connected with the inner ring of the bearing, and the inner ring of the bearing rotates to drive the stirring blades to rotate so as to stir reactants.
5. An improved doping reaction device as set forth in claim 4, wherein said stirring rod penetrates through the upper cover through an airtight bearing, the airtight bearing is located on the upper surface of the upper cover, the contact surface of the airtight bearing and the upper cover has the same smoothness and is coated with lubricating oil to form an air insulation layer.
6. An improved doping reaction device as set forth in claim 4, wherein the gas generating crucible has a through connecting rod passage at the middle, the outer wall of the connecting rod passage and the inner wall of the gas generating crucible form a gas generating chamber, and the stirring connecting rod passes through the connecting rod passage with a certain gap from the connecting rod passage to ensure gas circulation in the reaction chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210020221.XA CN114405404A (en) | 2022-01-10 | 2022-01-10 | Improved doping reaction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210020221.XA CN114405404A (en) | 2022-01-10 | 2022-01-10 | Improved doping reaction device |
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| Publication Number | Publication Date |
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| CN114405404A true CN114405404A (en) | 2022-04-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210020221.XA Pending CN114405404A (en) | 2022-01-10 | 2022-01-10 | Improved doping reaction device |
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Application publication date: 20220429 |