CN111218669B - Rotary drum type reactor for pulse chemical vapor deposition coating and application thereof - Google Patents
Rotary drum type reactor for pulse chemical vapor deposition coating and application thereof Download PDFInfo
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- CN111218669B CN111218669B CN202010024442.5A CN202010024442A CN111218669B CN 111218669 B CN111218669 B CN 111218669B CN 202010024442 A CN202010024442 A CN 202010024442A CN 111218669 B CN111218669 B CN 111218669B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4417—Methods specially adapted for coating powder
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Abstract
The invention discloses a rotary drum type reactor for pulse chemical vapor deposition coating and application thereof. The reactor comprises a precursor supply part, a reaction part and a tail gas treatment part; the precursor supply part comprises a first gas supply part and a second gas supply part, and the first gas supply part comprises a source bottle with a heating device; the second air supply part is communicated with air and is sucked in by the reaction part under negative pressure; the reaction part comprises a reaction rotary drum and a driving device for driving the reaction rotary drum, and the reaction rotary drum is transversely placed on the driving device; the tail gas treatment part is used for vacuumizing the reaction rotary drum and absorbing tail gas after reaction. The reactor of the invention is mainly used for anatase type TiO2The reactor adopting the structure can improve the gas-solid contact condition, solve the problem of slow reaction caused by difficult gas diffusion, accelerate the reaction rate of gas phase coating, simplify the operation condition and avoid the influences of uneven thickness, raw material loss, dust pollution and the like in the process of raw material tiling.
Description
Technical Field
The invention belongs to the technical field of reactors, and particularly relates to a rotary drum type reactor for pulse chemical vapor deposition coating and application thereof.
Background
TiO2As white pigment in the fields of coating, plastics and paper, but TiO2The photocatalytic performance of the paint can promote the oxidative decomposition of organic matters, so that the paint has the phenomena of fading, rough surface, pulverization and the like. In TiO2The inert film layer deposited on the surface of the particles can inhibit the photocatalytic performance of the particles and maintain the excellent pigment performance of the particles.
In TiO2The field of coating comprises a liquid phase synthesis method and a gas phase synthesis method,the liquid phase synthesis method is currently applied industrially. However, the liquid phase synthesis method is difficult to accurately control the membrane layer, the membrane layer is porous and can be applied after separation and drying, the flow is long, and the energy consumption is high. To solve these problems, the gas phase synthesis method can be used for TiO2And (5) performing coating operation. Among the vapor phase synthesis methods, Chemical Vapor Deposition (CVD) is the most common method, which is performed by introducing several reactive precursors into a reactor simultaneously to react with particles. CVD deposited coatings are prone to particulate, porous film layers and are coated with whole particle aggregates rather than individual particles. Atomic Layer Deposition (ALD) is a process in which a vapor phase reaction precursor is contacted with particles one after another, and the ALD process is self-limiting, so that the thickness of a film can be precisely controlled to grow to an atomic scale, but the thickness of the film grown at a single time is very thin (GPC < 0.04nm), and a sufficiently thick film layer can be formed by performing a plurality of ALD cycles. And the pulse chemical vapor deposition (P-CVD) adopts partial removal after a first precursor is introduced for reaction, and then another precursor is introduced. Thus, P-CVD is an ALD process with a small amount of CVD that can achieve both precise control of film thickness and large single-pass film growth thickness (GPC).
Existing coating of TiO by P-CVD2The reaction device of (2) is in the form of a fixed bed, gas molecules flow through the gaps of the particle bed to contact and react with the particle surface, and the molecular flow is a diffusion process and requires a long reaction time. To facilitate gas diffusion, it is desirable to incorporate TiO before the reaction2The artificial dispersion is carried out to form a thinner particle bed layer, the treatment capacity of a reaction device is greatly limited, and the dispersion process has the problems of difficult and uneven operation, dust pollution and the like.
Disclosure of Invention
Aiming at the problems, the invention provides a rotary drum type reactor for pulse chemical vapor deposition coating, which is beneficial to amplification and industrial application, can improve the gas-solid contact condition, solve the problem of slow reaction caused by difficult gas diffusion, accelerate the reaction rate of vapor coating, simplify the operation condition and avoid the influences of uneven thickness, raw material loss, dust pollution and the like in the process of raw material tiling.
In order to achieve the purpose, the invention adopts the technical scheme that: the rotary drum type reactor for the pulse chemical vapor deposition coating is provided, and comprises a precursor supply part, a reaction part and an exhaust gas treatment part; the precursor supply includes supplying SiCl4The first gas supply part comprises a source bottle, the outer wall of the source bottle is provided with a heating device, and the second gas supply part is a pipeline with openings at two ends; the reaction part comprises a reaction rotary drum and a driving device for driving the reaction rotary drum to rotate, and the reaction rotary drum is transversely placed on the driving device; a reaction cavity is arranged in the reaction rotary drum, a plurality of stirring bodies are placed in the reaction cavity, a four-way joint communicated with the reaction cavity is arranged at one end of the reaction rotary drum, and a pressure detection device for detecting the pressure of the reaction cavity is arranged at the other end of the reaction rotary drum; the tail gas treatment part is used for vacuumizing the reaction drum and absorbing tail gas after reaction; the source bottle, the second gas supply part and the tail gas treatment part are hermetically connected with the four-way joint through pipelines provided with valves.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the source bottle is equipped with a temperature controller, and the heating device is electrically connected with the temperature controller
Further, the heating device is an electric heating ring which is wound on the source bottle.
Further, the driving device comprises a base, a driving motor is arranged in the base, a driving roll shaft and a driven roll shaft which are parallel to each other are arranged at the top of the base, and the driving roll shaft is connected with a belt of the driving motor; the reaction drums are arranged on the driving roll shaft and the driven roll shaft.
Further, the reaction drum comprises a cylinder body and an end cover; the two ends of the cylinder body are provided with threaded mounting openings, the bottom of each threaded mounting opening is padded with a sealing ring, and the end cover is screwed in the threaded mounting openings; the four-way joint is arranged on the end cover at one end of the cylinder body through an air inlet pipe, and the pressure detection device is arranged on the end cover at the other end of the cylinder body.
Furthermore, the tail end of the air inlet pipe extends into the cylinder body.
Further, the stirring body was a cube made of polypropylene, and the specification thereof was 30mm × 30mm × 30 mm.
Further, the tail gas treatment part comprises an absorption bottle and a vacuum pump; the vacuum pump is connected with the absorption bottle, and the absorption bottle is connected with the four-way joint; the absorption bottle is filled with strong alkali solution.
The rotary drum type reactor of the invention is mainly used for TiO2Pulse chemical vapor deposition coating of, in particular, anatase TiO2The coating is formed by pulse vapor deposition. Anatase type TiO2The vapor deposition coating comprises the following steps:
s1: drying the anatase type TiO2Putting the reaction product into a reaction rotary drum, and assembling a rotary drum type reactor;
s2: heating SiCl in the source bottle by a heating device4Heating to form gas; meanwhile, the pressure in the reaction drum is pumped to-0.085 to-0.1 MPa by a tail gas treatment part;
s3: gasified SiCl4Charging SiCl into the evacuated reaction drum4With TiO2The mass ratio of (A) to (B) is 1: 10; then the reaction rotary drum rotates for 120min at the rotating speed of 16 r/min;
s4: pumping the pressure of the reaction drum after the S3 reaction to-0.04 MPa by using an exhaust gas treatment part;
s5: filling air into the reaction drum vacuumized by the S4 through the air supply part; then the reaction rotary drum rotates for 30min at the rotating speed of 16 r/min;
s6: the excess SiCl in the reaction drum is pumped out by a tail gas treatment part4And byproducts to obtain the coated SiO2TiO of film layer2Producing a product;
s7: repeating S2-S6 to obtain SiO with different thicknesses2TiO of film layer2And (5) producing the product.
The invention has the beneficial effects that:
1. compared with the existing research, the reactor and the process of the invention can realize the pulse chemical vapor deposition of the coated TiO2The scale application of the method. The reaction device provided by the invention can improve gas conductivity and greatly reduce gas diffusion time by providing disturbance to the particle bed layer through the rotation of the cylinder; a plurality of stirring bodies and TiO are adopted in the reaction process2Rotate togetherStrengthen TiO2The disturbance of the particle bed layer and the falling of the cubic stirring body after the cubic stirring body rises to a certain height due to the action of inertia and centrifugal force2The aggregate is broken, and TiO can be effectively avoided2The particles adhere to the walls of the cylinder.
2. The reaction device of the invention is used for the anatase type TiO2Directly feeding materials during pulse chemical vapor deposition coating without dispersing and spreading TiO2The particle is more convenient to operate, and the raw material loss and dust pollution are avoided. And after the reaction gas is filled, the reaction rotary drum rotates, solid particles in the reaction rotary drum are continuously exposed and contacted with the reaction gas, and the retention time of precursor molecules in the particle bed is obviously prolonged.
3. The invention avoids the problem of strong corrosion of the precursor and the reaction by-product by reasonably designing the structure of the reactor and selecting the material of the reaction chamber, and is easy to process and manufacture.
Drawings
FIG. 1 is a view showing the connection of the components of the rotary drum type reactor of the present invention;
FIG. 2 is a schematic view of a drive device;
FIG. 3 is a cross-sectional view of a reaction drum;
FIG. 4 shows uncoated anatase TiO2A TEM representation of (A);
FIG. 5 is a coated TiO2/SiO2TEM representation of the product;
FIG. 6 shows uncoated anatase TiO2With coated TiO2/SiO2Comparing the photocatalytic activity of the product;
a, a precursor supply part; B. a reaction section; C. an exhaust gas treatment unit; 1. a temperature controller; 2. a source bottle; 3. a heating device; 4. a four-way joint; 5. a stirring body; 6. a reaction drum; 61. a barrel; 62. a seal ring; 63. an end cap; 64. an air inlet pipe; 7. a pressure detection device; 8. a drive device; 81. a base; 82. a drive motor; 83. a drive roll shaft; 9. an absorption bottle; 10. a vacuum pump.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
In an embodiment of the present invention, as shown in fig. 1 to 3, a drum reactor for a pulse chemical vapor deposition coating is provided, the drum reactor of the present invention includes a precursor supply part a, a reaction part B, and an exhaust gas treatment part C. As shown in FIG. 1, the precursor supply A includes supplying SiCl4And a second gas supply part for supplying water vapor; wherein, the second air supply part is a pipeline with two open ends, which is used for charging air with moisture into the reaction rotary drum 6; the first gas supply part comprises a source bottle 2, the source bottle 2 is made of stainless steel, and is internally provided with a precursor such as SiCl4The top of the cavity is provided with a flange cover with a pressure gauge, which is detachably connected, and the flange cover seals the source bottle 2 through bolts and gaskets; the heating device 3 is arranged outside the source bottle 2, and the heating device 3 is used for heating the source bottle 2 to enable the precursor inside the source bottle to be heated into gas, so that heating parts which have a heating function and can be installed on the surface of the source bottle 2 are all alternatives of the heating device 3, such as a steam heating sleeve, an electric heating wire and the like. In order to monitor the amount of the precursor in the source bottle 2, the source bottle 2 can be placed on an industrial counting scale, and the whole system becomes lighter after the precursor becomes gas and escapes, so that the purpose of monitoring the adding quality of the precursor is achieved. In a preferred embodiment of the present invention, in order to heat the source bottle 2 uniformly and control the heating temperature precisely, the heating device 3 is preferably an electric heating coil, and the source bottle 2 is equipped with a thermostat 1, the thermostat 1 is electrically connected with the heating device 3, and the model of the thermostat 1 can be XMTD2001, TCH702, DWPAT702, etc.; the temperature required to be heated is set through the temperature controller 1, and the source bottle 2 can be heated to the set temperature by the electric heating ring.
As shown in fig. 1, the reaction part B includes a reaction drum 6 and a driving device 8 for driving the reaction drum 6 to rotate, the reaction drum 6 is transversely placed on the driving device, and the reaction drum 6 can rotate around a central axis under the driving of the driving device 8. A reaction cavity is arranged in the reaction rotary drum 6, a plurality of stirring bodies 5 are placed in the reaction cavity, the stirring bodies 5 are made of the same material as the reaction rotary drum 6, and the whole reaction rotary drum is cubic and has the size of about 30mm multiplied by 30 mm; one end of the reaction rotary drum 6 is provided with a four-way joint 4 communicated with the reaction cavity, the other end of the reaction rotary drum is provided with a pressure detection device 7 used for detecting the pressure of the reaction cavity, and the pressure detection device 7 is a digital display type pressure gauge or a pointer type pressure gauge. In order to facilitate the addition of the reactant to the reaction rotor 6, the structure of the reaction rotor 6 is defined in a preferred embodiment of the present invention, as shown in fig. 3, in which the reaction rotor 6 includes a cylinder 61 and an end cap 63, and the cylinder 61 and the end cap 63 are made of polypropylene; two ends of the cylinder body 61 are provided with threaded mounting openings, the bottom of each threaded mounting opening is padded with a sealing ring 62 made of polytetrafluoroethylene, and end covers 63 are screwed in the threaded mounting openings; an air inlet pipe 64 is inserted into an end cover 63 at one end of the cylinder body 61, and the four-way joint 4 is connected to the tail end of the air inlet pipe 64; the pressure detection device 7 is provided on the end cap 63 at the other end of the cylinder 61. In addition, in order to allow the precursor gas to fill the reaction rotor 6 quickly, the gas inlet pipe 64 extends into the interior of the reaction rotor 6.
As shown in fig. 2, the driving device 8 includes a base 81; a driving motor 82 is arranged in the base 81, a driving roller shaft 83 and a driven roller shaft which are parallel to each other are arranged at the top of the base, and the driving roller shaft 83 is in belt connection with the driving motor 82; the reaction bowl 6 is placed on the drive roller shaft 83 and the driven roller shaft. In the reaction process, the driving motor 82 is turned on, the driving roll shaft 83 starts to rotate under the driving of the driving motor 82, friction force exists between the reaction rotary drum 6 and the driving roll shaft 83, the driving roll shaft 83 rotates to drive the reaction rotary drum 6 to rotate, the reaction rotary drum 6 drives the driven roll shaft to rotate, materials in the reaction rotary drum 6 are uniformly mixed in the rotation process and fully contact with precursor gas, and the purpose of vapor deposition coating is achieved.
As shown in fig. 1, the off-gas treatment section C includes an absorption bottle 9 and a vacuum pump 10; the vacuum pump 10 is connected with the absorption bottle 9, the absorption bottle 9 is connected with the four-way joint 4, and strong alkali solution such as potassium hydroxide, sodium hydroxide and the like is filled in the absorption bottle 9. Before the reaction, the vacuum pump 10 can pump out the air in the reaction drum 6 to form a negative pressure environment, so that the precursor can be more uniformly distributed on the substrate, and a granular and porous film layer cannot be generated; after the reaction, the vacuum pump 10 can suck the unreacted precursor and the by-product into the absorption bottle 9, and the strong base solution in the absorption bottle 9 can absorb the qualified precursor by-product, so that the environmental pollution is avoided.
As shown in fig. 1, the source bottle 2 and the second gas supply unit are hermetically connected to the four-way joint 4 through a pipe provided with a valve.
The reactor of the invention can be used for pulse chemical vapor deposition coating, in particular to anatase TiO2Coating by pulsed chemical vapor deposition. In the anatase type TiO2When the pulse chemical vapor deposition coating is carried out, the method comprises the following steps:
s1: for anatase type TiO2Drying to remove TiO2The outer layer of the surface absorbs water; the drying temperature is 120 ℃, and the drying time is 4 hours;
s2: drying the anatase type TiO2Putting the reaction product into a reaction rotary drum 4, and assembling a rotary drum type reactor;
s3: the precursor SiCl is added4Placing into a source bottle 2, controlling the heating temperature of the heating device 3 to be 100 ℃, and heating for 3h at the temperature to ensure that SiCl is generated4To become gas; meanwhile, the tail gas treatment part D is used for pumping the pressure in the reaction rotary drum 4 to-0.085 to-0.1 MPa;
s4: gasified SiCl4Charging SiCl into the evacuated reaction drum 44With TiO2The mass ratio of (A) to (B) is 1: 10; then the reaction rotary drum 4 rotates for 120min at the rotating speed of 16 r/min;
s5: pumping the pressure of the reaction drum 4 after the S3 reaction to-0.04 MPa by using an exhaust gas treatment part D;
s6: air is filled into the reaction rotary drum 4 after the S4 is vacuumized through the air supply part C; then the reaction rotary drum 4 rotates for 30min at the rotating speed of 16 r/min;
s7: the excess SiCl in the reaction drum 4 was removed by the tail gas treatment section D4And byproducts to obtain the coated SiO2TiO of film layer2Producing a product;
s8: repeating S2-S6 to obtain SiO with different thicknesses2TiO of film layer2And (5) producing the product.
For uncoated anatase TiO2(FIG. 4) and TiO coated by the above method2/SiO2The product (FIG. 5) is used as TEMThe characterization shows that amorphous SiO with the thickness of 2-3 nm can be obtained by one-time coating2And (5) film layer.
To TiO 22Photocatalytic activity was evaluated. Specifically, dispersing the product obtained after primary coating in an organic dye rhodamine B (RhB) aqueous solution, continuously stirring under a dark condition to achieve adsorption and desorption balance, then irradiating the suspension by using a xenon lamp, sampling after a certain time, and taking out the supernatant. The absorbance of the solution was measured by UV-visible spectrophotometer at the absorption maximum wavelength of 551nm, as shown in FIG. 4, indicating that only one coating was required to obtain SiO2The film layer can effectively inhibit TiO2Photocatalytic activity of (1).
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (8)
1. A rotary drum reactor for pulsed chemical vapor deposition coating, characterized by: comprises a precursor supply part (A), a reaction part (B) and an exhaust gas treatment part (C); the precursor supply (A) comprises supplying SiCl4The first gas supply part comprises a source bottle (2), the outer wall of the source bottle (2) is provided with a heating device (3), and the second gas supply part is a pipeline with two open ends; the reaction part (B) comprises a reaction rotating drum (6) and a driving device (8) for driving the reaction rotating drum (6) to rotate, the reaction rotating drum (6) is transversely placed on the driving device (8), the driving device (8) comprises a base (81), a driving motor (82) is arranged in the base (81), a driving roll shaft (83) and a driven roll shaft which are parallel to each other are arranged at the top of the base, and the driving roll shaft (83) is in belt connection with the driving motor (82); the reaction drums (6) are placed on the driving roll shaft (83) and the driven roll shaft; the reaction drum (6) is internally provided with a reaction cavity, a plurality of stirring bodies (5) are placed in the reaction cavity, the stirring bodies (5) are made of materials the same as the reaction drum (6), and are integrally cubicThe size of the stirring drum is 30mm multiplied by 30mm, a plurality of stirring bodies (5) rotate together with particles in the reaction process, the disturbance of a particle bed layer is enhanced, the cubic stirring bodies (5) fall down to smash particle aggregate after rising to a certain height under the action of inertia and centrifugal force, the particles can be effectively prevented from being adhered to the drum wall, one end of the reaction rotary drum (6) is provided with a four-way joint (4) communicated with the reaction cavity, the other end of the reaction rotary drum is provided with a pressure detection device (7) for detecting the pressure of the reaction cavity, and the reaction rotary drum (6) comprises a drum body (61) and an end cover (63); two ends of the cylinder body (61) are provided with threaded mounting openings, the bottom of each threaded mounting opening is padded with a sealing ring (62), and the end cover (63) is screwed in the threaded mounting openings; the four-way joint (4) is arranged on an end cover (63) at one end of the cylinder body (61) through an air inlet pipe (64), and the pressure detection device (7) is arranged on the end cover (63) at the other end of the cylinder body (61); the tail gas treatment part (C) is used for vacuumizing the reaction rotary drum (6) and absorbing tail gas after reaction; the source bottle (2), the second gas supply part and the tail gas treatment part (C) are hermetically connected with the four-way joint (4) through pipelines provided with valves.
2. The barrel reactor for pulsed chemical vapor deposition coating of claim 1 wherein: the source bottle (2) is equipped with a temperature controller (1), and the heating device (3) is electrically connected with the temperature controller (1).
3. The drum reactor for pulsed chemical vapor deposition coating according to claim 1 or 2, characterized in that: the heating device (3) is an electric heating ring which is wound on the source bottle (2).
4. The barrel reactor for pulsed chemical vapor deposition coating of claim 1 wherein: the tail end of the air inlet pipe (64) extends into the barrel.
5. The barrel reactor for pulsed chemical vapor deposition coating of claim 1 wherein: the stirring body (5) is a cube made of polypropylene, and the specification of the stirring body is 30mm multiplied by 30 mm.
6. The barrel reactor for pulsed chemical vapor deposition coating of claim 1 wherein: the tail gas treatment part (C) comprises an absorption bottle (9) and a vacuum pump (10); the vacuum pump (10) is connected with the absorption bottle (9), and the absorption bottle (9) is connected with the four-way joint (4); the absorption bottle (9) is filled with strong alkali solution.
7. A rotary drum type reactor as claimed in any one of claims 1 to 6 for pulse chemical vapor deposition of coated anatase TiO2The use of (1).
8. Use according to claim 7, characterized in that it comprises the following steps:
s1: drying the anatase type TiO2Putting the reaction product into a reaction rotary drum (6), and assembling a rotary drum type reactor;
s2: SiCl in the source bottle (2) is heated by a heating device (3)4Heating to form gas; simultaneously, the tail gas treatment part (C) is used for pumping the pressure in the reaction rotating cylinder (6) to-0.085 to-0.1 MPa;
s3: gasified SiCl4Charging into the reaction drum (6) after vacuum pumping, and charging SiCl4With TiO2The mass ratio of (A) to (B) is 1: 10; then the reaction rotary drum (6) rotates for 120min at the rotating speed of 16 r/min;
s4: pumping the pressure of the reaction drum (6) after the S3 reaction to-0.04 MPa by an exhaust gas treatment part (C);
s5: filling air into the reaction drum (6) vacuumized by S4 through the air supply part (C); then the reaction rotary drum (6) rotates for 30min at the rotating speed of 16 r/min;
s6: the excess SiCl in the reaction drum (6) is pumped out by a tail gas treatment part (C)4And byproducts to obtain the coated SiO2TiO of film layer2Producing a product;
s7: repeating S2-S6 to obtain SiO with different thicknesses2TiO of film layer2And (5) producing the product.
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| CN102418085A (en) * | 2011-12-14 | 2012-04-18 | 无锡迈纳德微纳技术有限公司 | Micronano-scale powder protective layer wrapping device and method |
| KR20160035824A (en) * | 2014-09-24 | 2016-04-01 | 울산과학기술원 | Apparatus and method for thermal chemical vapor deposition |
| KR20160004136U (en) * | 2015-05-26 | 2016-12-06 | 한양대학교 에리카산학협력단 | Reactor of powder coating apparatus |
| CN105668622A (en) * | 2015-07-30 | 2016-06-15 | 四川大学 | Film coating method for titanium dioxide through vapor atomic deposition |
| CN106011791A (en) * | 2016-07-07 | 2016-10-12 | 王禄荣 | Atomic layer deposition device capable of enabling powder surface to be evenly coated and method of device |
| CN209522919U (en) * | 2018-11-23 | 2019-10-22 | 中化国际(控股)股份有限公司 | Chemical vapor deposition stove and chemical vapor depsotition equipment |
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