CN112176319A - Powder coating device and powder coating method - Google Patents
Powder coating device and powder coating method Download PDFInfo
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- CN112176319A CN112176319A CN202010906350.XA CN202010906350A CN112176319A CN 112176319 A CN112176319 A CN 112176319A CN 202010906350 A CN202010906350 A CN 202010906350A CN 112176319 A CN112176319 A CN 112176319A
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- 239000000843 powder Substances 0.000 title claims abstract description 186
- 238000000576 coating method Methods 0.000 title claims abstract description 93
- 239000011248 coating agent Substances 0.000 title claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 221
- 239000002243 precursor Substances 0.000 claims abstract description 197
- 238000001179 sorption measurement Methods 0.000 claims abstract description 34
- 239000011247 coating layer Substances 0.000 claims abstract description 24
- 238000011049 filling Methods 0.000 claims description 61
- 230000007246 mechanism Effects 0.000 claims description 30
- 238000010926 purge Methods 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 23
- 238000005086 pumping Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229920006395 saturated elastomer Polymers 0.000 claims description 7
- 238000005243 fluidization Methods 0.000 abstract description 15
- 238000000605 extraction Methods 0.000 abstract description 9
- 239000002699 waste material Substances 0.000 abstract description 9
- 230000002035 prolonged effect Effects 0.000 abstract description 8
- 230000014759 maintenance of location Effects 0.000 abstract description 7
- 239000007789 gas Substances 0.000 description 123
- 239000002245 particle Substances 0.000 description 32
- 230000008569 process Effects 0.000 description 15
- 239000010410 layer Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000007888 film coating Substances 0.000 description 5
- 238000009501 film coating Methods 0.000 description 5
- 238000000231 atomic layer deposition Methods 0.000 description 4
- 238000005253 cladding Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000006557 surface reaction Methods 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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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
-
- 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
-
- 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
- C23C16/52—Controlling or regulating the coating process
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Glanulating (AREA)
Abstract
The invention relates to a powder coating device and a powder coating method. Thus, a higher pressure will be maintained within the reaction chamber. Therefore, the precursor can be prevented from being pumped away before adsorption or reaction occurs, the retention time of the precursor in the reaction cavity is prolonged, and the surface of the powder is ensured to have sufficient adsorption reaction. Meanwhile, because the pressure in the reaction cavity is higher, the pressure difference between the air suction side and the air inlet side is smaller, and the height of a splashing area during powder fluidization can be effectively controlled. Therefore, the adsorption and the removal of the precursor can be prevented from being influenced due to the fact that a large amount of powder is adsorbed on the gas extraction side. Therefore, the powder coating device and the powder coating method can reduce the waste of the precursor and improve the growth efficiency of the coating layer.
Description
Technical Field
The invention relates to the technical field of coating, in particular to a powder coating device and a powder coating method.
Background
The surface functionalization of powder particles is an important component of a material surface engineering technology, and especially has important significance for improving the original performance of the particles. The surface functionalization of the powder particles can be realized by coating the surface of the powder particles with a layer, namely coating.
The ald technology has been widely used in the powder particle coating process because of its excellent uniformity, conformality and size controllability. In the current stage of the coating process, the adopted equipment is the fluidized bed ALD (Atomic layer deposition) equipment. Fluidized bed ALD equipment requires continuous pumping of the reaction chamber and charging of the fluidizing gas. In this way, the powder particles in the reaction chamber will be fluidized and dispersed.
However, during the continuous pumping process of the fluidized bed ALD apparatus, the precursor is pumped away before the reaction, which wastes the precursor and results in low growth efficiency of the coating layer.
Disclosure of Invention
In view of the above, it is desirable to provide a powder coating apparatus and a powder coating method that can effectively improve the growth efficiency of the coating layer.
A powder coating apparatus comprising:
the coating cavity is formed and provided with a reaction cavity body, and the reaction cavity body is provided with an air inlet port and an air outlet port;
the gas path system is communicated with the gas inlet port and is used for filling gas into the reaction cavity; and
and the air exhaust mechanism is communicated with the coating cavity and exhausts the reaction cavity through the air outlet port, and the air exhaust speed of the air exhaust mechanism for exhausting the reaction cavity is adjustable.
In one embodiment, the coating device further comprises an exhaust gas treatment mechanism arranged between the air exhaust mechanism and the coating cavity.
In one embodiment, the air pumping mechanism comprises a vacuum pump and a butterfly valve arranged between the vacuum pump and the coating cavity.
In one embodiment, the pumping mechanism comprises a vacuum pump, and an exhaust bypass which is connected with the vacuum pump in parallel and can be opened or closed, wherein the exhaust rate of the exhaust bypass is smaller than the pumping rate of the vacuum pump.
According to the powder coating device, when the first precursor and the second precursor are filled into the reaction cavity, the air exhaust rate of the air exhaust mechanism can be adjusted, so that the air inlet rate of the reaction cavity is greater than the air outlet rate. Thus, a higher pressure will be maintained within the reaction chamber. Therefore, the precursor can be prevented from being pumped away before adsorption or reaction occurs, the retention time of the precursor in the reaction cavity is prolonged, and the surface of the powder is ensured to have sufficient adsorption reaction. Meanwhile, because the pressure in the reaction cavity is higher, the pressure difference between the air suction side and the air inlet side is smaller, and the height of a splashing area during powder fluidization can be effectively controlled. Therefore, the adsorption and the removal of the precursor can be prevented from being influenced due to the fact that a large amount of powder is adsorbed on the gas extraction side. Therefore, the powder coating device can reduce the waste of the precursor and improve the growth efficiency of the coating layer.
A powder coating method comprising the steps of:
s1: pretreating the powder in the reaction cavity;
s2: filling fluidizing gas into the reaction cavity to fluidize and disperse the powder;
s3: filling a first precursor into the reaction cavity, and enabling the first precursor to be adsorbed on the surface of the powder, wherein the gas inlet rate of the reaction cavity is greater than the gas outlet rate;
s4: filling the reaction cavity with fluidizing gas again to fluidize and disperse the powder;
s5: and filling a second precursor into the reaction cavity so that the second precursor reacts with the first precursor adsorbed on the surface of the powder to generate a coating layer, wherein the air inlet rate of the reaction cavity is greater than the air outlet rate.
In one embodiment, the step S1 includes the steps of:
s101: filling powder to be coated into a reaction cavity;
s102: vacuumizing the reaction cavity;
s103: and heating the reaction cavity and presetting the temperature in the reaction cavity.
In one embodiment, the step S3 includes the steps of:
s301: filling a sufficient amount of the first precursor into the reaction cavity so as to enable the first precursor and the surface of the powder to be adsorbed in a saturated mode, and enabling the gas inlet rate of the reaction cavity to be larger than the gas outlet rate;
s302: filling purge gas into the reaction cavity to discharge redundant first precursors, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate;
the step S5 includes the steps of:
s501: filling a sufficient amount of the second precursor into the reaction cavity, so that the second precursor and the first precursor adsorbed on the powder surface are fully reacted, and the gas inlet rate of the reaction cavity is greater than the gas outlet rate;
s502: and filling purge gas into the reaction cavity to discharge the redundant second precursor, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate.
In one embodiment, the step S3 includes the steps of:
s301': filling the first precursor into the reaction cavity, and enabling the surfaces of the first precursor and the powder to be subjected to unsaturated adsorption, wherein the gas inlet rate of the reaction cavity is greater than the gas outlet rate;
s302': filling purge gas into the reaction cavity to discharge redundant first precursors, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate;
s303': repeating the steps S301 'and S302' until the first precursor and the powder are adsorbed on the surface in a saturated manner;
the step S5 includes the steps of:
s501': filling the second precursor into the reaction cavity, and enabling the second precursor to react with the first precursor adsorbed on the powder surface, wherein the gas inlet rate of the reaction cavity is greater than the gas outlet rate;
s502': filling purge gas into the reaction cavity to discharge the redundant second precursor, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate;
s503': repeating the steps S501 'and S502' until the second precursor sufficiently reacts with the first precursor adsorbed on the powder surface.
In one embodiment, the method further comprises the steps of: repeating the above steps S2 to S5 until the coating layer reaches a predetermined thickness.
According to the powder coating method, when the first precursor and the second precursor are filled into the reaction cavity, the air inlet rate of the reaction cavity is greater than the air outlet rate. Thus, a higher pressure will be maintained within the reaction chamber. Therefore, the precursor can be prevented from being pumped away before adsorption or reaction occurs, the retention time of the precursor in the reaction cavity is prolonged, and the surface of the powder is ensured to have sufficient adsorption reaction. Meanwhile, because the pressure in the reaction cavity is higher, the pressure difference between the air suction side and the air inlet side is smaller, and the height of a splashing area during powder fluidization can be effectively controlled. Therefore, the adsorption and the removal of the precursor can be prevented from being influenced due to the fact that a large amount of powder is adsorbed on the gas extraction side. Therefore, the powder coating method can reduce the waste of the precursor and improve the growth efficiency of the coating layer.
A powder coating method comprising the steps of:
s10: pretreating the powder in the reaction cavity;
s20: synchronously filling fluidizing gas and a first precursor into the reaction cavity so as to enable the first precursor to be adsorbed on the surface of the fluidized powder;
s30: and synchronously filling the fluidizing gas and a second precursor into the reaction cavity so as to enable the second precursor to react with the first precursor adsorbed on the surface of the powder to generate a coating layer.
In one embodiment, after step S10 and before step S20, the method further includes the steps of: and filling a non-return airflow into the reaction cavity.
In one embodiment, after step S20, the method further includes the steps of: stopping filling the fluidizing gas, and filling a purge gas into the reaction cavity to discharge the redundant first precursor;
after step S30, the method further includes the steps of: stopping filling the fluidizing gas, and filling a purge gas into the reaction chamber to discharge the excess second precursor.
In one embodiment, the method further comprises the following steps: repeating the above steps S20 to S30 until the coating layer reaches a predetermined thickness.
The powder coating method can coat the powder which is not easy to form a continuous fluidization state. While the first precursor is charged into the reaction chamber, a fluidizing gas is charged. Thus, the powder can be mixed with the first precursor and adsorbed in a short time once fluidized, and the uniformity of adsorption can be maintained even if the powder cannot maintain a continuous fluidized state. Similarly, the fluidizing gas is filled into the reaction cavity to fluidize the powder while the second precursor is filled, so that the second precursor can be fully reacted with the first precursor adsorbed on the surface of the powder in a short time. Therefore, the powder coating method can improve the uniformity of coating.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a powder coating apparatus according to a preferred embodiment of the present invention;
FIG. 2 is a diagram showing the relationship between the amount of air input and the height of the splashing region under different pressures in the reaction chamber of the powder coating apparatus shown in FIG. 1;
FIG. 3 is a schematic flow chart of a powder coating method according to a preferred embodiment of the present invention;
FIG. 4 is a schematic flow chart of step S1 in the powder coating method shown in FIG. 3;
FIG. 5 is a schematic view illustrating a process of step S3 in the powder coating method according to an embodiment;
FIG. 6 is a schematic view illustrating a process of step S5 in the powder coating method according to an embodiment;
FIG. 7 is a schematic view showing a flow of step S3 in the powder coating method according to another embodiment;
FIG. 8 is a schematic view showing the flow of step S5 in the powder coating method according to another embodiment;
FIG. 9 is a schematic flow chart of a powder coating method according to a preferred embodiment of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like as used herein are for illustrative purposes only and do not denote a unique embodiment.
Referring to fig. 1, a powder coating apparatus 10 according to a preferred embodiment of the present invention includes a coating chamber 100, a gas path system 200, a heating system 300, and an air pumping mechanism 400.
A reaction cavity is formed in the coating cavity 100 for allowing the powder to be coated, such as micro-nano particles, to react and obtain a coating layer coated on the surface of the powder particles. The coating chamber 100 may have a single-layer chamber structure or a double-layer chamber structure.
Further, the reaction chamber has an inlet port (not shown) and an outlet port (not shown). The powder to be coated can be accommodated in one end of the reaction cavity close to the air inlet port. The gas inlet port and the gas outlet port are generally provided with filter screens, and the filter screens can allow precursors and purge gas to pass through and can block powder particles to be coated. In addition, the air inlet port and the air outlet port can be provided with air receiving flanges.
The gas path system 200 is communicated with the gas inlet port and is used for filling gas into the reaction cavity. The gas circuit system 200 generally includes a process gas circuit and a fluidization gas circuit for filling the precursor, the purge gas, and the fluidization gas, respectively, into the reaction chamber. Gas circuit system 200 may be arranged as is known in the art. For example, the process gas circuit in the gas circuit system 200 includes a process gas pipeline, a source bottle connected to the process gas pipeline, a gas mass flow controller, and the like. The fluidizing gas path comprises a pulse valve, a gas mass flow controller and a fluidizing gas pipeline. The source bottle is used for containing a liquid or solid precursor source, and the gas mass flow controller is used for introducing a precursor with a specified flow into the reaction cavity. The pneumatic valve (not marked) on the source bottle is opened, the nitrogen purge gas can be carried with the precursor to enter the reaction cavity, and the pneumatic valve on the source bottle is closed, so that the function of only introducing the nitrogen (i.e. the purge gas) can be realized. If a plurality of precursors are needed to be provided for the reaction cavity, a plurality of process gas pipelines can be arranged according to the actual needs of the process production. In addition, a pulse valve can be arranged on the process gas pipeline and used for controlling various precursors to alternately enter the reaction cavity.
The heating system 300 is used for heating the film coating chamber 100 and the gas path system 200. The heating system 300 may be an electrical heating assembly, generally comprising two parts. Wherein, one part can be an electric heating sheet structure coated outside the film coating cavity 100, and the heat can be conducted into the reaction cavity by electrifying and heating; the other part is a soft-packaged heating belt which can be wrapped on the pipeline of the gas circuit system 200 and the source bottle. The heating system is primarily used to maintain the reaction chamber at a suitable temperature, typically 40 ℃ to 350 ℃.
In order to accurately control the temperature in the reaction chamber, a temperature measuring terminal 140 is further disposed on the coating chamber 100. The temperature measuring terminal 140 is used for monitoring the temperature in the reaction chamber and displaying the temperature through a display screen arranged outside the film coating chamber 100.
The air exhaust mechanism 400 is communicated with the film coating cavity 100 and exhausts the reaction cavity through the air outlet port. The pumping mechanism 400 is used to evacuate the reaction chamber, thereby ensuring the isolation of the reaction region from air. The pumping mechanism 400 may be a vacuum pump, an exhaust valve, or the like.
Specifically, in the present embodiment, the powder coating device 10 further includes an exhaust gas treatment mechanism 500 disposed between the air exhaust mechanism 400 and the coating chamber 100. When the air pumping mechanism 400 pumps air, the tail gas of the reaction chamber is pumped into the tail gas treatment mechanism 500, and then a certain amount of air is charged to react with the tail gas to generate harmless particles.
The flow of the powder coating device 10 for performing the coating process is as follows:
filling powder to be coated into a reaction cavity; the pumping mechanism 400 is started to pump the reaction chamber to vacuum, thereby maintaining effective isolation of the reaction chamber from the air environment; starting the heating system 300 to heat so as to enable the reaction cavity to reach the appropriate temperature required by the reaction; starting the gas path system 200, introducing fluidizing gas into the reaction cavity to fluidize and fully disperse the powder particles; then introducing a first precursor into the reaction cavity, and enabling the first precursor to be adsorbed on the surfaces of the powder particles; introducing purge gas to remove redundant first precursors in the reaction cavity; introducing a second precursor into the reaction cavity, and reacting the second precursor with the first precursor adsorbed on the surfaces of the powder particles to form a coating layer; and introducing purge gas to remove the redundant second precursor in the reaction cavity.
The above steps can be repeated, if necessary, until the thickness of the obtained clad layer is sufficient.
Further, the air pumping speed of the air pumping mechanism 400 for pumping air to the reaction chamber is adjustable. When the first precursor and the second precursor are filled into the reaction chamber, the air intake rate in the reaction chamber can be made greater than the air exhaust rate by reducing the air exhaust rate of the air exhaust mechanism 400. In this way, a higher pressure will be maintained in the reaction chamber.
After the pressure in the reaction cavity rises, on one hand, the precursor can be prevented from being sucked away before adsorption or reaction, and the retention time of the precursor in the reaction cavity is prolonged, so that the surface of the powder is ensured to have sufficient adsorption reaction, and the waste is reduced. On the other hand, the pressure difference between the suction side (outlet port) and the inlet side (inlet port) can be reduced, and the height of the splashing zone when the powder is fluidized can be effectively controlled. Therefore, the phenomenon that the adsorption and removal of the precursor are influenced due to the fact that a large amount of powder is adsorbed on the air exhaust side can be prevented, and the growth efficiency of the coating layer is improved.
As shown in fig. 2, the higher the pressure in the reaction chamber, the lower the height of the powder splash zone is, with the same inlet gas flow rate.
When the purge gas is introduced and used to remove the excess precursor, the pumping rate of the pumping mechanism 400 can be increased. Therefore, the redundant precursors can be rapidly removed, and the coating efficiency is improved.
There are many ways to achieve adjustments to the pumping rate of the pumping mechanism 400. Such as:
referring to fig. 1 again, in the present embodiment, the air-extracting mechanism 400 includes a vacuum pump 410 and a butterfly valve 420 disposed between the vacuum pump 410 and the coating chamber 100. Since the power of the vacuum pump 410 is constant after it is started. Therefore, by controlling the opening degree of the butterfly valve 420, the air exhaust rate of the whole air exhaust mechanism 400 can be adjusted.
Another example is as follows:
in another embodiment, the pumping mechanism 400 comprises a vacuum pump, and an exhaust bypass (not shown) connected in parallel with the vacuum pump and capable of being opened or closed, wherein the exhaust rate of the exhaust bypass is smaller than the pumping rate of the vacuum pump.
The exhaust bypass can be a conduit with a small pipe diameter, and the conduit can be connected in parallel with the vacuum pump through an angle valve and communicated with the coating cavity 100. And when the precursor is injected into the reaction cavity, the vacuum pump is closed and the exhaust bypass is opened, so that only the tail gas is discharged through the guide pipe. However, the small diameter of the conduit will make the air intake rate in the reaction chamber larger than the air exhaust rate, thereby maintaining a higher pressure in the reaction chamber.
When the purge gas is filled into the reaction cavity, the vacuum pump can be opened, so that the air extraction efficiency is improved, and the cleaning efficiency of the precursor is improved. The vacuum pump is opened, and the exhaust bypass can be closed, so that the conduit with a thin pipe diameter is prevented from being blocked after long-time work. Compared with a butterfly valve, the exhaust bypass is arranged to achieve the mode that the air exhaust speed is adjustable, and the cost is lower.
Obviously, in other embodiments, an electric control device may be provided to adjust the power of the vacuum pump, so as to achieve the purpose of adjusting the pumping rate.
In the powder coating device 10, when the first precursor and the second precursor are filled into the reaction chamber, the air exhaust rate of the air exhaust mechanism 400 can be adjusted so that the air inlet rate of the reaction chamber is greater than the air outlet rate. Thus, a higher pressure will be maintained within the reaction chamber. Therefore, the precursor can be prevented from being pumped away before adsorption or reaction occurs, the retention time of the precursor in the reaction cavity is prolonged, and the surface of the powder is ensured to have sufficient adsorption reaction. Meanwhile, because the pressure in the reaction cavity is higher, the pressure difference between the air suction side and the air inlet side is smaller, and the height of a splashing area during powder fluidization can be effectively controlled. Therefore, the adsorption and the removal of the precursor can be prevented from being influenced due to the fact that a large amount of powder is adsorbed on the gas extraction side. Therefore, the powder coating device 10 can reduce the waste of the precursor and improve the growth efficiency of the coating layer.
Referring to fig. 3, the present invention further provides a powder coating method. The powder coating method includes steps S1 to S5:
s1: and pretreating the powder in the reaction cavity.
The powder coating method can be performed by the powder coating device 10 shown in fig. 1, and the reaction chamber is the inside of the cavity structure formed by the coating chamber 100. The pretreatment is to carry out pretreatment on the powder particles so that the powder particles reach the basic condition of coating before coating.
Referring to fig. 4, in the present embodiment, the step S1 includes the steps of: s101: and filling the powder to be coated into the reaction cavity. S102: and vacuumizing the reaction cavity. S103: and heating the reaction cavity and presetting the temperature in the reaction cavity.
In particular, the reaction chamber can be maintained effectively isolated from the air environment by evacuation. Typically, the pressure within the reaction chamber is maintained between 10mbar and 20mba after evacuation. The reaction cavity is heated, so that the powder inside the reaction cavity can reach the preset temperature. The predetermined temperature is an optimum temperature for the adsorption reaction to occur on the surface of the powder particles, and is generally 40 to 350 ℃.
S2: a fluidizing gas is charged into the reaction chamber to fluidize and disperse the powder.
The fluidizing gas is not adsorbed and reacts with the powder surface and may be an inert gas. The total gas inflow of the fluidizing gas and the area of the flow cross section of the reaction chamber together determine the gas flow velocity, which ultimately determines the fluidization state of the powder particles. In principle, the faster the gas velocity, the better the powder fluidization, all other things remaining unchanged. The total amount of inflow of fluidizing gas introduced in the present embodiment is about 50sccm to 100sccm in consideration of the fluidizing effect and the control of the height of the powder scattering region.
In order to obtain a better dispersion effect, vibration, rotation or stirring can be started while the fluidizing gas is introduced, so that the powder particles can be subjected to auxiliary dispersion by mechanical action.
S3: and filling a first precursor into the reaction cavity, and enabling the first precursor to be adsorbed on the surface of the powder, wherein the air inlet rate of the reaction cavity is greater than the air outlet rate.
The first precursor can be adsorbed to the surface of the powder particles, and since the powder has been fluidized in step S2, the dispersion between the particles is high, and the uniformity of the adsorption of the first precursor is better. Also, since the gas inlet rate is greater than the gas outlet rate, a higher pressure will be maintained in the reaction chamber.
After the pressure in the reaction cavity rises, on one hand, the first precursor can be prevented from being sucked before time or being pumped away after reaction, and the staying time of the first precursor in the reaction cavity is prolonged, so that the surface of the powder is ensured to be fully adsorbed, and the waste is reduced. On the other hand, the pressure difference between the suction side and the gas inlet side can be reduced, and the height of the splashing zone during powder fluidization can be effectively controlled. Thus, it is possible to prevent the adsorption of the first precursor from being affected by the adsorption of a large amount of powder on the gas-extraction side.
As shown in fig. 2, the higher the pressure in the reaction chamber, the lower the height of the powder splash zone is, with the same inlet gas flow rate.
After the first precursor is adsorbed on the particle surface, if the unadsorbed first precursor remains in the reaction chamber, the method further includes: and filling a purge gas into the reaction chamber to remove the excess first precursor. The purge gas may be nitrogen. When the redundant first precursor is removed, compared with the process of filling the first precursor, the air extraction speed can be increased to realize rapid air extraction, so that the film coating efficiency is improved.
S4: the reaction chamber is again charged with fluidizing gas to fluidize and disperse the powder.
The powder particles settle while the first precursor is being charged and excess first precursor is being purged. Therefore, in order to smoothly react the second precursor to be subsequently reacted with the first precursor adsorbed on the surface of the powder particles, the powder particles need to be fluidized again. The specific process of step S4 is substantially the same as step S2, and therefore, the detailed description thereof is omitted here.
S5: and filling a second precursor into the reaction cavity so that the second precursor reacts with the first precursor adsorbed on the surface of the powder to generate a coating layer, wherein the air inlet rate of the reaction cavity is greater than the air outlet rate.
The specific process of charging the second precursor is the same as that of charging the first precursor, except that the type of the charged precursor is different. Likewise, higher pressures will be maintained in the reaction chamber at this point.
When the precursors (the first precursor and the second precursor) are filled into the reaction cavity, the gas inlet rate of the reaction cavity is greater than the gas outlet rate. Thus, a higher pressure will be maintained within the reaction chamber. Therefore, the precursor can be prevented from being pumped away before adsorption or reaction occurs, the retention time of the precursor in the reaction cavity is prolonged, the surface of the powder is ensured to generate sufficient adsorption reaction, and the growth efficiency of the coating layer is improved.
Every time an adsorption reaction occurs, a deposition layer with a thickness corresponding to the atomic diameter can be formed on the surface of the powder particles. Therefore, in this embodiment, the powder coating method further includes the steps of: repeating the above steps S2 to S5 until the coating layer reaches a predetermined thickness. After a number of repetitions, the thickness of the resulting cladding layer is equal to the sum of the thicknesses of the deposited layers, so that a thicker cladding layer can be obtained.
Referring to fig. 5 and fig. 6, in the present embodiment, the step S3 includes the steps of:
s301: and filling a sufficient amount of the first precursor into the reaction cavity so as to enable the first precursor and the surface of the powder to be saturated and adsorbed, and enabling the air inlet rate of the reaction cavity to be greater than the air outlet rate. S302: and filling purge gas into the reaction cavity to discharge the redundant first precursor, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate.
According to the specific surface area and the treatment capacity of the powder to be plated, enough first precursor is filled, so that the first precursor can be adsorbed on the surfaces of all the powder particles by filling once.
Further, step S5 includes the steps of: s501: and filling sufficient second precursor into the reaction cavity so as to enable the second precursor to fully react with the first precursor adsorbed on the surface of the powder, and enabling the air inlet rate of the reaction cavity to be greater than the air outlet rate. S502: and filling purge gas into the reaction cavity to discharge the redundant second precursor, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate.
Similarly, the second precursor is filled in a sufficient amount at a time, and can react with the first precursor adsorbed on the surfaces of all the powder particles to obtain the coating layer. Therefore, the coating efficiency can be obviously improved.
Referring to fig. 7 and 8, in another embodiment, step S3 includes the steps of: s301': and filling a first precursor into the reaction cavity, and enabling the surfaces of the first precursor and the powder to be in unsaturated adsorption, wherein the air inlet rate of the reaction cavity is greater than the air outlet rate. S302': and filling purge gas into the reaction cavity to discharge the redundant first precursor, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate. S303': repeating the steps S301 'and S302' until the surface of the first precursor and the powder is saturated and adsorbed.
Since only a small amount of the first precursor is charged into the reaction chamber at a time, it is not sufficient to adsorb all the powder particles to saturation. Therefore, it is necessary to repeat the process several times to saturate the surface of the first precursor and the powder. Because the total amount of the first precursor required for realizing saturated adsorption is not changed, the first precursor charged each time can be obviously reduced, and the time for charging each time can be obviously shortened.
Further, step S5 includes the steps of: s501': and filling a second precursor into the reaction cavity, and enabling the second precursor to partially react with the first precursor adsorbed on the surface of the powder, wherein the gas inlet rate of the reaction cavity is greater than the gas outlet rate. S502': and filling purge gas into the reaction cavity to discharge the redundant second precursor, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate. S503': repeating the steps S501 'and S502' until the second precursor is sufficiently reacted with the first precursor adsorbed on the powder surface.
Since only a small amount of the second precursor is charged into the reaction chamber at a time, it is not enough to react with the first precursor adsorbed by all the powder particles. Therefore, it is necessary to repeat the process several times to fill the reaction chamber with enough second precursor to fully react with the first precursor. Likewise, the time per charge of the second precursor can be significantly reduced.
It can be seen that the time for each charging of the first precursor and the second precursor can be significantly reduced compared to the conventional art. Therefore, it is possible to prevent a large amount of waste and powder agglomeration caused by the introduction of the precursor for a long time.
According to the powder coating method, when the first precursor and the second precursor are filled into the reaction cavity, the air inlet rate of the reaction cavity is greater than the air outlet rate. Thus, a higher pressure will be maintained within the reaction chamber. Therefore, the precursor can be prevented from being pumped away before adsorption or reaction occurs, the retention time of the precursor in the reaction cavity is prolonged, and the surface of the powder is ensured to have sufficient adsorption reaction. Meanwhile, because the pressure in the reaction cavity is higher, the pressure difference between the air suction side and the air inlet side is smaller, and the height of a splashing area during powder fluidization can be effectively controlled. Therefore, the adsorption and the removal of the precursor can be prevented from being influenced due to the fact that a large amount of powder is adsorbed on the gas extraction side. Therefore, the powder coating method can reduce the waste of the precursor and improve the growth efficiency of the coating layer.
Referring to fig. 9, the present invention further provides a powder coating method. The powder coating method includes steps S10 to S50:
s10: and pretreating the powder in the reaction cavity.
The purpose and specific flow of step S10 are substantially the same as those of step S1 shown in fig. 5, and therefore, the description thereof is omitted here. It should be noted that the non-coating method in this embodiment generally applies coating to powder particles with large specific gravity and large particle size and not easy to fluidize.
S20: and synchronously filling the fluidizing gas and the first precursor into the reaction cavity so as to adsorb the first precursor and the surface of the fluidized powder.
The first precursor is typically pulsed so that the fluidizing gas is also pulsed into the reaction chamber. For particles that are not easily fluidized, it is difficult to form a continuous fluidized state. Therefore, the fluidizing gas is charged while the first precursor is charged into the reaction chamber. In this way, the fluidization of the powder can be synchronized with the charging of the first precursor. Once the powder is fluidized, it can be mixed with the first precursor in a short time to effect adsorption, and the uniformity of adsorption can be maintained even if the powder cannot maintain a continuous fluidized state.
Specifically, in this embodiment, after step S20, the powder coating method further includes the steps of: the charging of the fluidizing gas is stopped and a purge gas is charged into the reaction chamber to expel excess first precursor.
S30: and synchronously filling the fluidizing gas and the second precursor into the reaction cavity so that the second precursor reacts with the first precursor adsorbed on the surface of the powder to generate the coating layer.
Similarly, a fluidizing gas is introduced into the reaction chamber simultaneously with the introduction of the second precursor. In this way, the fluidization of the powder can be synchronized with the charging of the second precursor. Once the powder is fluidized, it can be mixed with the second precursor in a short time and the first precursor and the second precursor adsorbed on the surface of the powder are hardened, and even if the powder cannot maintain a continuous fluidized state, the reaction can be maintained sufficiently.
After step S30, the powder coating method further includes the steps of: the charging of the fluidizing gas is stopped and a purge gas is charged into the reaction chamber to discharge excess second precursor.
In the present embodiment, after step S10 and before step S20, the method further includes the steps of: and a non-return air flow is filled into the reaction cavity. The non-return air flow can be fluidizing air with small flow or blowing air, and the non-return air flow can not cause powder fluidization but can prevent the material in the reaction cavity from flowing back to the air inlet side.
Every time an adsorption reaction occurs, a deposition layer with a thickness corresponding to the atomic diameter can be formed on the surface of the powder particles. Therefore, in this embodiment, the powder coating method further includes the steps of: repeating the above steps S20 to S30 until the coating layer reaches a predetermined thickness. After a number of repetitions, the thickness of the resulting cladding layer is equal to the sum of the thicknesses of the deposited layers, so that a thicker cladding layer can be obtained.
The powder coating method can coat the powder which is not easy to form a continuous fluidization state. While the first precursor is charged into the reaction chamber, a fluidizing gas is charged. Thus, the powder can be mixed with the first precursor and adsorbed in a short time once fluidized, and the uniformity of adsorption can be maintained even if the powder cannot maintain a continuous fluidized state. Similarly, the fluidizing gas is filled into the reaction cavity to fluidize the powder while the second precursor is filled, so that the second precursor can be fully reacted with the first precursor adsorbed on the surface of the powder in a short time. Therefore, the powder coating method can improve the uniformity of coating.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (13)
1. A powder coating device, comprising:
the coating cavity is formed and provided with a reaction cavity body, and the reaction cavity body is provided with an air inlet port and an air outlet port;
the gas path system is communicated with the gas inlet port and is used for filling gas into the reaction cavity; and
and the air exhaust mechanism is communicated with the coating cavity and exhausts the reaction cavity through the air outlet port, and the air exhaust speed of the air exhaust mechanism for exhausting the reaction cavity is adjustable.
2. The powder coating device of claim 1, further comprising an exhaust gas treatment mechanism disposed between the pumping mechanism and the coating chamber.
3. The powder coating device of claim 1, wherein the gas-pumping mechanism comprises a vacuum pump and a butterfly valve disposed between the vacuum pump and the coating chamber.
4. The powder coating device according to claim 1, wherein the air suction mechanism comprises a vacuum pump, and an exhaust bypass which is connected in parallel with the vacuum pump and can be opened or closed, and the exhaust rate of the exhaust bypass is smaller than that of the vacuum pump.
5. A powder coating method is characterized by comprising the following steps:
s1: pretreating the powder in the reaction cavity;
s2: filling fluidizing gas into the reaction cavity to fluidize and disperse the powder;
s3: filling a first precursor into the reaction cavity, and enabling the first precursor to be adsorbed on the surface of the powder, wherein the gas inlet rate of the reaction cavity is greater than the gas outlet rate;
s4: filling the reaction cavity with fluidizing gas again to fluidize and disperse the powder;
s5: and filling a second precursor into the reaction cavity so that the second precursor reacts with the first precursor adsorbed on the surface of the powder to generate a coating layer, wherein the air inlet rate of the reaction cavity is greater than the air outlet rate.
6. The powder coating method according to claim 5, wherein the step S1 comprises the steps of:
s101: filling powder to be coated into a reaction cavity;
s102: vacuumizing the reaction cavity;
s103: and heating the reaction cavity and presetting the temperature in the reaction cavity.
7. The powder coating method according to claim 5, wherein the step S3 comprises the steps of:
s301: filling a sufficient amount of the first precursor into the reaction cavity so as to enable the first precursor and the surface of the powder to be adsorbed in a saturated mode, and enabling the gas inlet rate of the reaction cavity to be larger than the gas outlet rate;
s302: filling purge gas into the reaction cavity to discharge redundant first precursors, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate;
the step S5 includes the steps of:
s501: filling a sufficient amount of the second precursor into the reaction cavity, so that the second precursor and the first precursor adsorbed on the powder surface are fully reacted, and the gas inlet rate of the reaction cavity is greater than the gas outlet rate;
s502: and filling purge gas into the reaction cavity to discharge the redundant second precursor, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate.
8. The powder coating method according to claim 5, wherein the step S3 comprises the steps of:
s301': filling the first precursor into the reaction cavity, and enabling the surfaces of the first precursor and the powder to be subjected to unsaturated adsorption, wherein the gas inlet rate of the reaction cavity is greater than the gas outlet rate;
s302': filling purge gas into the reaction cavity to discharge redundant first precursors, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate;
s303': repeating the steps S301 'and S302' until the first precursor and the powder are adsorbed on the surface in a saturated manner;
the step S5 includes the steps of:
s501': filling the second precursor into the reaction cavity, and enabling the second precursor to react with the first precursor adsorbed on the powder surface, wherein the gas inlet rate of the reaction cavity is greater than the gas outlet rate;
s502': filling purge gas into the reaction cavity to discharge the redundant second precursor, wherein the gas inlet rate of the reaction cavity is smaller than the gas outlet rate;
s503': repeating the steps S501 'and S502' until the second precursor sufficiently reacts with the first precursor adsorbed on the powder surface.
9. The powder coating method according to any one of claims 5 to 8, further comprising the steps of: repeating the above steps S2 to S5 until the coating layer reaches a predetermined thickness.
10. A powder coating method is characterized by comprising the following steps:
s10: pretreating the powder in the reaction cavity;
s20: synchronously filling fluidizing gas and a first precursor into the reaction cavity so as to enable the first precursor to be adsorbed on the surface of the fluidized powder;
s30: and synchronously filling the fluidizing gas and a second precursor into the reaction cavity so as to enable the second precursor to react with the first precursor adsorbed on the surface of the powder to generate a coating layer.
11. The powder coating method of claim 10, further comprising, after step S10 and before step S20: and filling a non-return airflow into the reaction cavity.
12. The powder coating method according to claim 10, further comprising, after step S20, the steps of: stopping filling the fluidizing gas, and filling a purge gas into the reaction cavity to discharge the redundant first precursor;
after step S30, the method further includes the steps of: stopping filling the fluidizing gas, and filling a purge gas into the reaction chamber to discharge the excess second precursor.
13. The powder coating method according to any one of claims 10 to 12, further comprising the steps of: repeating the above steps S20 to S30 until the coating layer reaches a predetermined thickness.
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