CN105951058B - A kind of nano particle space isolation atomic layer deposition apparatus and method based on fluid bed - Google Patents
A kind of nano particle space isolation atomic layer deposition apparatus and method based on fluid bed Download PDFInfo
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- CN105951058B CN105951058B CN201610361332.1A CN201610361332A CN105951058B CN 105951058 B CN105951058 B CN 105951058B CN 201610361332 A CN201610361332 A CN 201610361332A CN 105951058 B CN105951058 B CN 105951058B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C23C16/442—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 using fluidised bed process
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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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Abstract
The invention discloses a kind of, and atomic layer deposition apparatus and method is isolated in the nano particle space based on fluid bed, nano particle to be covered is put into the middle section of powder reaction chamber by it, make intermittent circular motion under the drive of power source in the middle section of powder reaction chamber, pass through the first cleaning area, adsorption zone, the second cleaning area, reaction zone successively, one layer of cladding film is formed in nano grain surface, shuttling movement is to obtain ideal film thickness.The present invention can realize the quick cladding of nano particle under normal pressure, have many advantages, such as that clad ratio is high, being evenly coated property is good, coating efficiency is high.
Description
Technical field
The invention belongs to powder technique for atomic layer deposition fields, more particularly, to a kind of nanometer based on fluid bed
Grain space isolation atomic layer deposition apparatus and method.
Background technology
With the fine of substance, powder granule can show a series of microeffects, macroscopically show it is a series of
Excellent physics and chemical property, but powder granule exists and easily reunites simultaneously, is easily aoxidized, property is unstable etc. a series of lacks
Point.By coating protective layer on powder granule surface, disadvantages mentioned above can be effectively overcome, the powder granule with protective film can be with
Composite material as new function admirable.
The method for coating of powder granule mainly has solid phase method, liquid phase method and vapor phase method, technique for atomic layer deposition conduct at present
A kind of special chemical vapor deposition method has excellent uniformity and controllability compared with other deposition techniques.Pass through powder
Certainly the limitation Chemisorption in body surface face can coat one layer of highly uniform nano-level thin-membrane in particle surface, pass through control
Cycle-index processed accurately controls the thickness of clad.
Traditional Atomic layer deposition method can directly be used in substrate surface, can obtain good covered effect, but
It is, for the nano particle with excessive specific surface area and excessively high specific surface energy, using conventional atomic layer deposition side
Method is coated, and serious agglomeration can be caused, and affects the clad ratio of powder deposition most critical and being evenly coated property, and
Traditional technique for atomic layer deposition based on fluid bed needs to carry out under higher vacuum environment, while cleaning process is longer,
Directly affect the efficiency of nanoparticle deposition.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of nano particles based on fluid bed
Atomic layer deposition apparatus and method is isolated in space, wherein using the principle of space isolation, each process of atomic layer deposition is empty
Between keep apart, realize the Quick uniform cladding of nano particle under normal pressure, have that clad ratio is high, being evenly coated property is good, coating efficiency
The advantages that high.
To achieve the above object, according to one aspect of the present invention, it is proposed that a kind of nano particle based on fluid bed is empty
Between atomic layer deposition apparatus is isolated, which is characterized in that the equipment includes apparatus for atomic layer deposition, two groups of nitrogen feedways,
One forerunner's body feeding and second forerunner's body feeding, wherein：
The apparatus for atomic layer deposition includes multigroup circumferential sedimentation unit, and every group of sedimentation unit includes four
Powder reaction chamber, the powder reaction chamber are divided into the part of upper, middle and lower three, and the middle section of wherein powder reaction chamber is relatively independent,
And its upper and lower ends is sealed by strainer, and all powder reaction chambers in the apparatus for atomic layer deposition are distributed in the same circumference
On, and the middle section of all powder reaction chambers on the same circumference can make intermittent circular motion simultaneously；
The nitrogen feedway is for supplying nitrogen, in one of which nitrogen feedway and first group of sedimentation unit
The lower part of first powder reaction chamber is connected, the third powder in another group of nitrogen feedway and first group of sedimentation unit
The lower part of reaction chamber is connected, and the first forerunner body feeding is for supplying the first presoma, with first group of deposition list
The lower part of second powder reaction chamber in member is connected, and the second forerunner body feeding is used to supply the second presoma,
It is connected with the lower part of the 4th powder reaction chamber in first group of sedimentation unit.
As it is further preferred that the nitrogen feedway passes through first, in pipeline and first group of sedimentation unit
The lower part of three powder reaction chambers is connected, and ball valve and gas flow control valve are provided on the pipeline.
As it is further preferred that the first forerunner body feeding and second forerunner's body feeding structure phase
Together, include nitrogen feed unit and forerunner's object supply unit, the nitrogen feed unit and forerunner's object supply unit pass through pipe
Road is connected with the lower part of powder reaction chamber, and forerunner's object supply unit is by solenoid valve control.
As it is further preferred that the strainer is 3000 mesh filter screens.
As it is further preferred that the upper part of the powder reaction chamber is connected by filter with aspiration pump.
It is another aspect of this invention to provide that providing a kind of nano particle space isolation atomic layer deposition based on fluid bed
Method, which is characterized in that include the following steps：
(1) it is packed into nano particle in the middle section of first powder reaction chamber, it is logical opens first group of nitrogen feedway
Enter nitrogen, air remaining in first powder reaction chamber is discharged, and clean to nano particle；
(2) so that the middle section of first powder reaction chamber is circled, cause it to move to second powder reaction chamber
Upper and bottom section between, then open first forerunner's body feeding, make the first presoma under the action of nitrogen lead to
Enter the middle section of first powder reaction chamber, and is adsorbed on the surface of nano particle；
(3) make the middle section of first powder reaction chamber continue to circle, it is anti-to cause it to move to third powder
It between the upper and bottom section for answering chamber, opens second group of nitrogen feedway and is passed through nitrogen, clean and remaining first is discharged
Presoma；
(4) so that the middle section of first powder reaction chamber is circled again, it is anti-to cause it to move to the 4th powder
Between the upper and bottom section for answering chamber, second forerunner's body feeding is then opened, makes the second presoma in the effect of nitrogen
Under be passed through the middle section of first powder reaction chamber, and the shape that reacts with the first presoma for being adsorbed on nano grain surface
At film layer, an atomic layer deposition reaction is thus completed.
As it is further preferred that the flow of the nitrogen is 10sccm-5000sccm.
As it is further preferred that the flow of the nitrogen is 500sccm.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, mainly have below
Technological merit：
1. the powder reaction chamber of the present invention is designed to three-stage structure, and the middle section of powder reaction chamber is relatively independent,
And intermittent circular motion can be made, different cleanings and conversion zone are passed sequentially through, completes and repeats entire atomic layer deposition
Process, shuttling movement obtain ideal film thickness so that cleaning and reaction process have obtained space isolation, effectively shorten entire atom
The time of layer reaction process and equipment cleaning time, improve the coating efficiency of powder.
2. the single powder reaction chamber of the present invention uses the principle of fluid bed, gas logical from the lower part of powder reaction chamber
Enter, after completing the cleaning of particle and the cladding of presoma using the middle part of powder reaction chamber, finally by powder reaction chamber
Side reaction product and remaining presoma is discharged in top, has many advantages, such as simple in structure, easy to operate.
3. the step that the powder reaction cavity of the present invention will clean, be passed through the first presoma, clean again, be passed through the second presoma
Rapid space keeps apart, while by unit as repetition, keeping the structure of equipment compacter, can disposably coat more
Nano particle, being evenly coated property is good, and clad ratio is high.
4. the flow for the fluidized gas (nitrogen) that the present invention is passed through by control below powder reaction chamber, powder is lasting
Under the comprehensive function of lift and particle its own gravity that gas provides, the shuttling movement in reaction chamber, to utilize fluidized bed principle
Overcome the agglomeration between powder.
It carries out under normal pressure 5. the atomic layer deposition of the present invention is reacted, and fluidizes throughput, nano particle increment etc.
Parameter is simply easily adjusted, and is facilitated and is carried out process ration experiment, obtains best fluidisation throughput and particles supply amount, is ensureing particle
On the basis of covered effect, maximum cladding rate is realized.
Description of the drawings
Fig. 1 is that the structure of the nano particle space isolation atomic layer deposition apparatus based on fluid bed of the embodiment of the present invention is shown
It is intended to；
Fig. 2 is the structural schematic diagram of the apparatus for atomic layer deposition of the embodiment of the present invention；
Fig. 3 is the apparatus for atomic layer deposition intermediate member structural schematic diagram of the embodiment of the present invention；
Fig. 4 is the structural schematic diagram of the powder reaction chamber of the embodiment of the present invention；
Fig. 5 is the motion control sequence diagram of the apparatus for atomic layer deposition of the embodiment of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
The basic principle of the present invention is put into powder in the powder reaction chamber of special apparatus for atomic layer deposition, and powder is anti-
It answers chamber to make intermittent circular motion under the drive of power source, passes sequentially through cleaning and conversion zone, realize entire atomic layer
Deposition process, wherein presoma and carrier gas are alternately passed through inside powder reaction chamber successively by bottom, and presoma is passing through powder
Nano grain surface will be adsorbed on when reaction chamber, the different presomas to be passed through with after occur chemical reaction and form one layer of atom
The film of thickness.
As shown in Figure 1, atomic layer deposition is isolated in a kind of nano particle space based on fluid bed provided in an embodiment of the present invention
Product equipment, the equipment include mainly 9, two groups of nitrogen feedways 1 of apparatus for atomic layer deposition, first forerunner's body feeding, 2 and
Second forerunner's body feeding 3, wherein apparatus for atomic layer deposition 9 provides required place for atomic layer deposition reaction, and nitrogen supplies
It is used to be passed through nitrogen into apparatus for atomic layer deposition 9 to device 1, to be cleaned to pipeline and nano particle, the first presoma
For feedway 2 for being passed through the first presoma into apparatus for atomic layer deposition 9, which is uniformly adsorbed on atomic layer
The surface of nano particle in precipitation equipment 9, second forerunner's body feeding 3 is for being passed through the into apparatus for atomic layer deposition 9
Two presomas, first forerunner's precursor reactant of second presoma and the nano grain surface absorption in apparatus for atomic layer deposition 9, with
It is deposited in nano grain surface and obtains film.By the mutual cooperation of above-mentioned each device, nano grain surface atomic layer is realized
The quick cladding of film has many advantages, such as that coating efficiency is high, uniformity is good.
Each device is described and described in detail below in conjunction with attached drawing.
As shown in Figure 1, two groups of nitrogen feedways 1 are for supplying nitrogen, it is real to be cleaned to pipeline and nano particle
The air-flow fluidisation of existing nano-powder particle, the magnitude range of air-flow is specially 10sccm-5slm.One of which nitrogen feedway
1 is connected by pipeline with the lower part of first powder reaction chamber in first group of sedimentation unit, another group of nitrogen feedway 1
It is connected with the lower part of the third powder reaction chamber in first group of sedimentation unit by pipeline, for remaining presoma is discharged
And byproduct of reaction, pollution cavity is prevented, particle surface film coated is influenced.Ball valve 4, gas flow control are provided on pipeline
Valve 6, the ball valve 4 are used to control the open and close of nitrogen feedway, and gas flow control valve 6 is used to control the supply of nitrogen
Flow.
First forerunner's body feeding 2 is used to supply second powder in the first presoma, with first group of sedimentation unit
The lower part of precursor reactant chamber is connected, and the second forerunner body feeding 3 is for supplying the second presoma, with first group of deposition
The lower part of the 4th powder reaction chamber in unit is connected.The first forerunner body feeding 2 and the supply of the second presoma
The structure of device 3 is identical, includes nitrogen feed unit and forerunner's object supply unit, and the nitrogen feed unit and presoma supply
It is connected with the lower part of powder reaction chamber by pipeline to unit, equally, the gas of control gas flow is provided on the pipeline
Flow control valve 6, wherein nitrogen feed unit is controlled by ball valve 4, and forerunner's object supply unit is controlled by solenoid valve 5.
As in Figure 2-4, apparatus for atomic layer deposition 9 includes multigroup circumferential sedimentation unit, every group of sedimentation unit
Include four powder reaction chambers, each powder reaction chamber is divided into part 10, middle section 8 and lower three parts 7, wherein powder
The middle section 8 of precursor reactant chamber is relatively independent, and the upper/lower terminal of the middle section 8 of powder reaction chamber is sealed by strainer, specifically
The strainer for selecting 3000 mesh pollutes cavity to prevent powder from leaking.For the middle section for ensureing powder reaction chamber and each powder
The binding face of effective assembly of the upper and lower part of reaction chamber, middle section and upper and lower part has higher processing cooperation essence
Degree can realize half isolation of conversion zone and external environment, while being conducive to flow by the way that relatively independent middle section is arranged
Change gas (nitrogen) and presoma being passed through and being discharged, by the flow velocity of adjusting fluidized gas, different-grain diameter and the particle of quality can be made
It is fully dispersed.
Wherein, all powder reaction chambers in apparatus for atomic layer deposition 9 are distributed on the same circumference, and positioned at same
The middle section of all powder reaction chambers on a circumference can make intermittent circular motion, the upper part of powder reaction chamber simultaneously
10 are connected by filter 11 with aspiration pump 12.The characteristics of single powder reaction chamber uses conventional fluidization, gas is reacted from powder
The lower part of chamber is passed through, and after completing the cleaning of particle and the cladding of presoma using the middle part of powder reaction chamber, passes through powder
The air extractor discharge side reaction product on precursor reactant chamber top and remaining presoma.Specifically, on the same circumference
The middle section of all powder reaction chambers is mounted on a retainer, which can be under the drive of power source such as motor
Make intermittent circular motion, be achieved in the circular motion of powder reaction chamber middle section, so that the same powder reaction chamber
Middle section first pass through cleaning area (lower part of first powder reaction chamber in same group of sedimentation unit) and make in reaction chamber
Between nano particle in part cleaned, using adsorption zone (second powder reaction chamber in same group of sedimentation unit
Lower part) so that the first presoma is adsorbed on the surface of the nano particle cleaned, then using (same group of next cleaning area
The lower part of third powder reaction chamber in sedimentation unit) so that the nano particle for being adsorbed with the first presoma is cleaned, most
Make the second presoma and nanometer by reaction zone (lower part of the 4th powder reaction chamber in same group of sedimentation unit) afterwards
First forerunner's precursor reactant on grain surface, obtains required atom film layer.
Further, it is very suitable for equipped with a heating unit because reaction cavity is that circumference is symmetrical in powder reaction chamber
It is heated in radiant type, therefore, the design of heating unit is to be based on heat radiation principle, and high power heating lamp is placed in the middle part of cavity and is made
For heat source, while using tinfoil and asbestos to coat entire reaction cavity as heat-barrier material can to realize that temperature range is 200 DEG C -400
DEG C heating, ensure that reaction in the temperature window, meets the temperature requirement of experiment.
The atomic layer deposition of nano particle is carried out below with the nano particle space isolation atomic layer deposition apparatus of the present invention
Product, specifically comprises the following steps：
(1) nano particle, such as SiO are packed into the middle section of first powder reaction chamber2Particle opens control first
The ball valve of group nitrogen feedway 1 is passed through nitrogen and is discharged air remaining in first powder reaction chamber, and to nano particle into
Row cleaning；
(2) after the remaining air of discharge, so that the middle section of first powder reaction chamber is circled, make its fortune
It moves between the upper and bottom section of second powder reaction chamber, then opens the electricity of first forerunner's body feeding 2 of control
Magnet valve and ball valve, the first presoma are passed through the middle section of first powder reaction chamber under the action of nitrogen, and are adsorbed on and receive
The surface of rice grain；First presoma closes solenoid valve and ball valve after powder surface completes absorption；
(3) make the middle section of first powder reaction chamber continue to circle, it is anti-to cause it to move to third powder
Between the upper and bottom section for answering chamber, the ball valve of second group of nitrogen feedway 1 of control is opened, nitrogen is passed through and cleans and be discharged
The first remaining presoma after having cleaned the first remaining presoma, closes ball valve；
(4) so that the middle section of first powder reaction chamber is circled again, it is anti-to cause it to move to the 4th powder
Between the upper and bottom section for answering chamber, the solenoid valve and ball valve of second forerunner's body feeding 3 of control are then opened, before second
Drive body and be passed through the middle section of first powder reaction chamber under the action of nitrogen, and be adsorbed on the first of nano grain surface
Presoma reacts, and film layer is formed in nano grain surface, completes an atomic deposition reaction, the second presoma is in powder
After reaction is completed on surface, solenoid valve and ball valve are closed.
The above process only describes the primary first-order equation process of a powder reaction chamber middle part, in practical operation, often
It is respectively arranged with nano particle in the middle section of a powder reaction chamber, the nano particle in previous powder reaction chamber middle section
After cleaning is completed in the first cleaning area, when entering adsorption zone through circular motion, in next powder reaction chamber middle section
Nano particle is then cleaned into the first cleaning area, and the nano particle in previous powder reaction chamber middle section is adsorbing
After area completes the absorption of the first presoma, when into the second cleaning area, the nanometer in next powder reaction chamber middle section
Particle is then adsorbed into adsorption zone, and so on.During actual deposition, it can be recycled according to required deposition thickness
Repeatedly, to complete Multiple depositions reaction, to deposit required film thickness.
Specifically, the flow that all source nitrogens are passed through nitrogen is 10sccm-5000sccm, preferably 500sccm, in the speed
Under rate, it can realize that high efficiency serialization coats under the premise of ensureing covered effect.Further, the first presoma can be selected
H can be selected in TMA, the second presoma2O。
As shown in figure 5, due to the order of reaction process, reaction the beginning and end stage according to sequence shown in Fig. 5
Be passed through nitrogen or presoma, ordinate indicates whether to open solenoid valve and is passed through gas or presoma in figure, wherein N2 indicate nitrogen,
A indicates that the first presoma, B indicate the second presoma, the unit of abscissa indicate between powder reaction chamber rotate twice used in
Time, the time that the specific time is needed by the absorption of presoma and reaction time and cleaning are determined.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (8)
1. atomic layer deposition apparatus is isolated in a kind of nano particle space based on fluid bed, which is characterized in that the equipment is using empty
Between separation principle each process space of atomic layer deposition is kept apart, realize normal pressure under nano particle Quick uniform cladding,
It includes apparatus for atomic layer deposition (9), two groups of nitrogen feedways (1), first forerunner's body feeding (2) and the second presoma
Feedway (3), wherein：
The apparatus for atomic layer deposition (9) includes multigroup circumferential sedimentation unit, and every group of sedimentation unit includes four
Powder reaction chamber, each powder reaction chamber are divided into the part (10,8,7) of upper, middle and lower three, wherein in same sedimentation unit
As the first cleaning area, the middle section of first powder reaction chamber is installed with to be deposited the lower part of first powder reaction chamber
Nano particle, the lower part of second powder reaction chamber is as adsorption zone, and the lower part of third powder reaction chamber is as
Two cleaning areas, the lower part of the 4th powder reaction chamber is as reaction zone, and the middle section of each powder reaction chamber is opposite
It is independent, and middle section upper and lower ends are sealed by strainer, all powder reaction chambers distribution in the apparatus for atomic layer deposition (9)
The middle section of all powder reaction chambers on the same circumference, and on the same circumference can be made intermittent simultaneously
Circular motion, so that nano particle to be deposited passes through the first cleaning successively with the middle section of first powder reaction chamber
Area, adsorption zone, the second cleaning area and reaction zone realize the space isolation of cleaning and reaction；
The nitrogen feedway (1) for supplying nitrogen, one of which nitrogen feedway (1) in first group of sedimentation unit
The lower part of first powder reaction chamber be connected, another group of nitrogen feedway (1) and the third in first group of sedimentation unit
The lower part of a powder reaction chamber is connected, and the first forerunner body feeding (2) is for supplying the first presoma, with first
The lower part of second powder reaction chamber in group sedimentation unit is connected, and the second forerunner body feeding (3) is for supplying
Second presoma is connected with the lower part of the 4th powder reaction chamber in first group of sedimentation unit.
2. atomic layer deposition apparatus is isolated in the nano particle space based on fluid bed as described in claim 1, which is characterized in that
The nitrogen feedway (1) by pipeline and first group of sedimentation unit first, the lower part of third powder reaction chamber
It is connected, ball valve (4) and gas flow control valve (6) is provided on the pipeline.
3. atomic layer deposition apparatus is isolated in the nano particle space based on fluid bed as claimed in claim 2, which is characterized in that
The first forerunner body feeding (2) is identical with the structure of second forerunner's body feeding (3), includes nitrogen feed unit
With forerunner's object supply unit, lower part that the nitrogen feed unit and forerunner's object supply unit pass through pipeline and powder reaction chamber
It is connected, forerunner's object supply unit is controlled by solenoid valve (5).
4. atomic layer deposition apparatus is isolated in the nano particle space based on fluid bed as claimed in claim 3, which is characterized in that
The strainer is 3000 mesh filter screens.
5. atomic layer deposition apparatus is isolated in the nano particle space based on fluid bed as claimed in claim 4, which is characterized in that
The upper part (10) of the powder reaction chamber is connected by filter (11) with aspiration pump (12).
6. Atomic layer deposition method is isolated in a kind of nano particle space based on fluid bed, which is characterized in that it is used such as right
It is required that nano particle space isolation atomic layer deposition apparatus of the 1-5 any one of them based on fluid bed carries out the sky of nano particle
Between atomic layer deposition is isolated, include the following steps：
(1) it is packed into nano particle in the middle section of first powder reaction chamber, opens first group of nitrogen feedway (1) and is passed through
Nitrogen is discharged air remaining in first powder reaction chamber, and is cleaned to nano particle；
(2) so that the middle section of first powder reaction chamber is circled, cause it to move to the upper of second powder reaction chamber
Between part and lower part, first forerunner's body feeding (2) is then opened, the first presoma is made to be passed through under the action of nitrogen
The middle section of first powder reaction chamber, and it is adsorbed on the surface of nano particle；
(3) make the middle section of first powder reaction chamber continue to circle, cause it to move to third powder reaction chamber
Upper and bottom section between, open second group of nitrogen feedway and be passed through nitrogen, clean and the first remaining forerunner is discharged
Body；
(4) so that the middle section of first powder reaction chamber is circled again, cause it to move to the 4th powder reaction chamber
Upper and bottom section between, then open second forerunner's body feeding (3), make the second presoma under the action of nitrogen
It is passed through the middle section of first powder reaction chamber, and reacts to be formed with the first presoma for being adsorbed on nano grain surface
Thus film layer completes an atomic layer deposition reaction.
7. Atomic layer deposition method is isolated in the nano particle space based on fluid bed as claimed in claim 6, which is characterized in that
The flow of the nitrogen is 10sccm-5000sccm.
8. Atomic layer deposition method is isolated in the nano particle space based on fluid bed as claimed in claim 7, which is characterized in that
The flow of the nitrogen is preferably 500sccm.
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| CN101215692B (en) * | 2008-01-04 | 2010-06-02 | 清华大学 | Multiple reaction cavity atom layer deposition device and method |
| CN201962352U (en) * | 2010-11-23 | 2011-09-07 | 英作纳米科技（北京）有限公司 | Rotary space-separating chemical vapor deposition device |
| CN105386011B (en) * | 2015-12-17 | 2017-09-22 | 华中科技大学 | A kind of powder apparatus for atomic layer deposition fluidized based on planet |
| CN105369221B (en) * | 2015-12-17 | 2018-01-30 | 华中科技大学 | The apparatus for atomic layer deposition and its method of a kind of encapsulated nanoparticles |
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