CN107502873B - A kind of powder cladding apparatus for atomic layer deposition - Google Patents
A kind of powder cladding apparatus for atomic layer deposition Download PDFInfo
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- CN107502873B CN107502873B CN201710945497.8A CN201710945497A CN107502873B CN 107502873 B CN107502873 B CN 107502873B CN 201710945497 A CN201710945497 A CN 201710945497A CN 107502873 B CN107502873 B CN 107502873B
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- powder
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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
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of powder to coat apparatus for atomic layer deposition, it includes powder container and reaction cavity, one end of reaction cavity is provided with into Yuan Kou, there is the air inlet pipe for inputting reaction gas or carrier gas into sealed set in source mouthful, the other end of reaction cavity offers chamber door, powder container is set on the inside of chamber door, rotation can be achieved under the driving of power device, air inlet is offered on powder container, air inlet pipe enters the inner cavity of powder container by air inlet, reaction cavity is internally provided with ultrasonic vibration bar, after powder container enters reaction cavity by guiding device, the lateral wall of powder container is contacted with ultrasonic vibration bar.The present invention combines spinning solution and ultrasonic vibration method, can use the contact probability that rotation increases powder and reaction gas, also can use the energy releasing powder that vibration generates and reunites, disperses powder, fine and close film is finally evenly coated on powder surface.
Description
Technical field
The present invention relates to a kind of apparatus for atomic layer deposition more particularly to a kind of powder bags based on ultrasonic vibration divergent function
Cover apparatus for atomic layer deposition.
Background technique
The powder particle of micro-or nano size possesses since opposite common material specific surface area is bigger different from one
As in macro-scale particle physicochemical characteristics, so being widely used in the fields such as fuel, coating, electronics, catalyst.But
Nanometer powder is since there is also some defects for inherent characteristic itself: due to its high surface energy, nanometer powder easily occurs to reunite existing
As making its distinctive physicochemical characteristics be difficult to completely be played；Simultaneously because it, with big surface-active, causes to have
Although the more general energetic material of nano material containing energy possesses bigger enthalpy of combustion a bit, the sky for being also easier to and storing in atmosphere
Gas and steam etc. react, and so that it is lost the internal active constituent contained leads to the storage life mistake of these nanometer powders containing energy
It is low.Accordingly, it is considered to protective film be coated on powder surface, to overcome drawbacks described above.
Technique for atomic layer deposition is a kind of advanced nano thin-film preparation means, is widely used in each field, especially exists
The modified aspect in the surface of micro-nano powder, can directly be used in substrate surface, can obtain good covered effect.But
It is, for specific surface area in contrast very big nanometer powder, to be coated, be difficult at it using conventional atom deposition method
Surface uniform coated, and there are particle agglomeration phenomenon problem very serious, directly reduce powder surface clad ratio and
Uniformity limits the further utilization of nanometer powder industrially.
Summary of the invention
The purpose of the present invention is to provide a kind of powder to coat apparatus for atomic layer deposition, overcomes nanometer powder in reaction cavity
In be easy reunite the shortcomings that so that powder clad is evenly coated, thickness is controllable, conformality is good.
To achieve this purpose, the present invention adopts the following technical scheme:
A kind of powder cladding apparatus for atomic layer deposition comprising one end of powder container and reaction cavity, reaction cavity is set
It is equipped with into Yuan Kou, has the air inlet pipe for being passed through reaction gas or carrier gas, the other end of reaction cavity into sealed set in source mouthful
Chamber door is offered, powder container is set on the inside of chamber door, and rotation can be achieved under the driving of power device, open up on powder container
There is air inlet, air inlet pipe enters the inner cavity of powder container by air inlet, and reaction cavity is internally provided with ultrasonic vibration bar, powder
After last container enters reaction cavity by guiding device, the lateral wall of powder container is contacted with ultrasonic vibration bar.By spinning solution
It is combined with ultrasonic vibration method, can use the contact probability that rotation increases powder and reaction gas, also can use vibration
The energy of generation releases powder and reunites, and disperses powder, forms uniform clad on powder surface.
Wherein, power device includes driving motor and device for sealing magnetic fluid, and the outside protrusion of chamber door is provided with the first method
Orchid adapter tube, device for sealing magnetic fluid and first flange adapter tube are tightly connected, and container support frame is installed on the inside of chamber door, and powder holds
The both ends of device pass through support of bearing lid respectively and are fixed on container support frame, and one end of powder container is provided with transmission shaft, separately
Air inlet is offered on one end forms through-hole axis, the output shaft of driving motor, the drive shaft of device for sealing magnetic fluid and transmission shaft
It is connected respectively by shaft coupling between any two.Powder ceaselessly rolling up and down in a reservoir is controlled by power device, and is reacted
Gas comes into full contact with and reacts, and reaches good deposition effect.
Wherein, guiding device includes the linear guide being equipped with and sliding block, and the chamber door side of reaction cavity is provided with installation
Pedestal, linear guide are axially set in mounting seat along reaction cavity, and sliding block can be along linear guide relative to anti-
Answer cavity mobile, driving motor and chamber door passes through electric machine support respectively and chamber door bracket is fixed on sliding block.Guiding device is used to
The linear motion of driving motor, chamber door etc. is guided, realizes chamber door folding.
Wherein, sliding block is driven by lead screw motor or cylinder.
Wherein, reaction cavity corresponds to ultrasonic vibration bar and is provided with second flange adapter tube, second flange adapter tube and external ultrasound
Vibration device is tightly connected, and ultrasonic vibration bar enters from second flange adapter tube, with powder container dynamic Contact.Made by vibration
Nanometer powder de-agglomerated realizes the uniform cladding of nanometer powder.
Wherein, ultrasonic vibration vibration of bar frequency is 10~60kHz, and oscillation power is greater than 1kW.
Wherein, the Intranet of powder container being axially inside provided with for increasing powder and container-contacting surface product.For
Better dispersing nano powder and conduction ultrasonic vibration wave.
Wherein, third flange connecting pipe is also provided on reaction cavity, third flange connecting pipe and external vacuum generating device are close
Envelope connection.Vacuum environment is created, reaction condition is met.
Wherein, venthole is also provided on powder container, the aperture of venthole is provided with the strainer for preventing powder from leaking out.In order to
It prevents powder from leaking out from the venthole of powder container, and reaction product and carrier gas is not hindered to flow out.
It is an advantage of the current invention that compared with prior art, the powder cladding apparatus for atomic layer deposition will rotate and
Vibration is introduced into traditional sedimentary system, and container static before is changed to rotatable tubular powder container, the powder
Container is placed in vacuum chamber, is ceaselessly rotated, while reaction gas being passed through in powder container, is passed through under driving motor drive
The centrifugal force that control rotation generates is less than the gravity of powder, such powder can ceaselessly rolling up and down in a reservoir, and it is anti-
It answers gas to come into full contact with reaction, reaches good deposition effect, in addition, introducing external vibrator, pass through ultrasonic vibration bar and powder
Last container contact, makes nanometer powder de-agglomerated by vibration, solves the problems, such as that nanometer powder is easy to reunite, to realize
The uniform cladding of nanometer powder has the advantages that reaction gas utilization rate is high, reaction is abundant, covered effect is good, at low cost.
Detailed description of the invention
Fig. 1 is the general structure schematic diagram for the powder cladding apparatus for atomic layer deposition that the specific embodiment of the invention provides；
Fig. 2 is the powder container transmission shaft end for the powder cladding apparatus for atomic layer deposition that the specific embodiment of the invention provides
Schematic diagram；
Fig. 3 is the powder container through-hole shaft end for the powder cladding apparatus for atomic layer deposition that the specific embodiment of the invention provides
Schematic diagram；
Fig. 4 is the internal junction of the powder container for the powder cladding apparatus for atomic layer deposition that the specific embodiment of the invention provides
Composition.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
It please refers to shown in Fig. 1 to 4, the present embodiment provides a kind of powder to coat apparatus for atomic layer deposition, including powder container 1
With reaction cavity 2, one end of reaction cavity 2 is provided with into source mouthful 3, has into sealed set in source mouthful 3 for inputting reaction gas
Or the air inlet pipe 4 of carrier gas, the other end of reaction cavity 2 offer chamber door 5, the outside protrusion of chamber door 5 is provided with first flange and connects
Pipe 18 is tightly connected device for sealing magnetic fluid 6 at first flange adapter tube 18, and device for sealing magnetic fluid 6 is controlled by driving motor 7 to be revolved
Turn, the inside of chamber door 5 is installed with container support frame 8, and the both ends of powder container 1 are individually fixed in container branch by support of bearing lid
On support 8, and one end of powder container 1 is provided with transmission shaft 9, and air inlet is offered on the other end and forms through-hole axis 10, driving
The output shaft of motor 7, the drive shaft of device for sealing magnetic fluid 6 and transmission shaft 9 are connected by shaft coupling 11 respectively between any two, are controlled
Powder processed ceaselessly rolling up and down in a reservoir, comes into full contact with reaction gas and reacts, realize good deposition effect.Wherein,
Driving motor 7 can use stepper motor, since it does not have accumulated error, be applied in opened loop control, fixed by changing
The energized state of sub- winding controls revolving speed and the direction of rotor, and the change speed of energized state is faster, and revolving speed is higher, changes it
Power-up sequence can change direction of rotation, keep the energized state of stepper motor is constant it can be made to be parked in some position.
5 side of chamber door of reaction cavity 2 is provided with mounting seat 12, sets in mounting seat 12 along the axial direction of reaction cavity 2
It is equipped with linear guide 13, sliding block 14 that can be mobile relative to reaction cavity 2, driving motor are correspondingly arranged in linear guide 13
7 and chamber door 5 be fixed on sliding block 14 by electric machine support 15 and chamber door bracket 16 respectively, sliding block 14 passes through lead screw motor or gas
Cylinder driving or manually etc., for guiding the linear motion of driving motor 7, chamber door 5 etc., realizes the folding of chamber door 5.
The corresponding ultrasonic vibration bar 17 of reaction cavity 2 is provided with second flange adapter tube 19, and second flange adapter tube 19 and outside are super
Acoustic vibration device is tightly connected, after powder container 1 enters reaction cavity 2 along linear guide 13, ultrasonic vibration bar 17 from second
Enter in flange connecting pipe 19, with 1 dynamic Contact of powder container, nanometer powder de-agglomerated is made by vibration, realizes nanometer powder
Uniformly cladding, the vibration frequency of ultrasonic vibration bar 17 are 10~60kHz, and oscillation power is greater than 1kW.By spinning solution and ultrasound
Method for oscillating combines, and can use the contact probability that rotation increases powder and reaction gas, also can use what vibration generated
Energy overcomes agglomerating force, disperses powder, and nanometer powder surface forms uniform clad.
It should be noted that vibration is added on powder container 1 by ultrasonic vibration bar 17, powder container 1 again transmits vibration
To powder, in this way, the energy of vibration can be such that powder preferably disperses, and since the needs of powder container 1 vibrate, and shake
It is dynamic transmission parts to be had an impact, it is likely that cause the service life of component not grown, influence of this influence to motor is especially
Obviously, therefore, quincunx elastic shaft coupling is selected in the connection of the transmission shaft 9 of the drive shaft of device for sealing magnetic fluid 6 and powder container 1
Device, the shaft coupling have the performance of vibration damping, buffering, and plough groove type folder is selected in the connection of device for sealing magnetic fluid 6 and step motor shaft
Hold type shaft coupling.
Third flange connecting pipe 20 is also provided on reaction cavity 2, third flange connecting pipe 20 and external vacuum generating device are close
Envelope connection, creates vacuum environment, meets reaction condition.
Particularly, in order to make vibration more fully pass to powder from powder container 1, need to increase powder container 1 and powder
The contact area at end, is axially inside welded with three apertures between the Intranet 21 of 500um~2mm in powder container 1, in this way,
Vibration can pass to powder by Intranet 21.
Venthole is also provided on powder container 1, powder is leaked out from 1 venthole of powder container in order to prevent, and is not hindered anti-
Product and carrier gas is answered to flow out, the aperture of venthole, which is provided with, prevents the aperture of powder leakage between the strainer of 10~50um, specifically
, end net fixed plate is respectively set in venthole two sides, strainer is sandwiched among two end net fixed plates, is held and is used between net fixed plate
Bolt is fixed.
Furthermore, it is necessary to which supplement, the geomery of reaction cavity 2 should meet the lower powder container 1 and container that can be accommodated
The shape and size of support frame 8, while also wanting as small as possible, to reduce sucking rate and utilize presoma in practical work process
Rate is as high as possible, therefore uses cylinder horizontal type structure, and optimal, chamber door 5 is also selected to circle, and thickness is about 10mm.With rectangle
Door is compared, and round door is easier to manufacture, and seal groove also more holds processing.Since this 2 diameter of reaction cavity is smaller, directly in cavity or chamber
Installation clamp system is more complex on door 5, therefore determines the preload before being vacuumized using individual clamp.And due to the present apparatus
Operating temperature be below 300 DEG C, thermic load is smaller, therefore is cooled down by the way of welding water pipe to sealing station.
In conclusion in the present embodiment powder cladding apparatus for atomic layer deposition will rotate and vibration be introduced into it is traditional
In sedimentary system, container static before is changed to rotatable tubular powder container, which is placed in vacuum chamber,
It is ceaselessly rotated under driving motor drive, while reaction gas being passed through in powder container, the centrifugal force that control rotation generates
Less than the gravity of powder, such powder can ceaselessly roll up and down in a reservoir, come into full contact with and react with reaction gas, real
Now good deposition effect is contacted by ultrasonic vibration bar with powder container in addition, introducing external vibrator, is made by vibration
Nanometer powder de-agglomerated solves the problems, such as that nanometer powder is easy to reunite, realizes the uniform cladding of nanometer powder, has anti-
Answer the advantage that gas effciency is high, reaction is abundant, covered effect is good, at low cost.
The above embodiments only describe the basic principles and characteristics of the invention, and the invention is not restricted by the above cases,
Without departing from the spirit and scope, the invention also has various changes and changes, and these changes and changes are both fallen within
In scope of the claimed invention.The scope of the present invention is defined by the appended claims and its equivalents.
Claims (8)
1. a kind of powder coats apparatus for atomic layer deposition, including powder container and reaction cavity, which is characterized in that the reaction chamber
One end of body is provided with into Yuan Kou, described to have the air inlet pipe for being passed through reaction gas or carrier gas, institute into sealed set in source mouthful
The other end for stating reaction cavity offers chamber door, and the powder container is set on the inside of chamber door and in the driving backspin of power device
Turning, air inlet is offered on the powder container, the air inlet pipe enters the inner cavity of the powder container by the air inlet,
The reaction cavity is internally provided with ultrasonic vibration bar, and the powder container enters the reaction cavity by guiding device
Afterwards, the lateral wall of the powder container is contacted with the ultrasonic vibration bar, and the axially inside setting of the powder container is useful
In the Intranet for increasing powder and container-contacting surface product.
2. powder according to claim 1 coats apparatus for atomic layer deposition, it is characterised in that: the power device includes driving
Dynamic motor and device for sealing magnetic fluid, the outside protrusion of the chamber door are provided with first flange adapter tube, the magnet fluid sealing dress
It sets to take over the first flange and be tightly connected, be installed with container support frame on the inside of the chamber door, the two of the powder container
End is fixed on the container support frame by support of bearing lid respectively, and one end of the powder container is provided with transmission shaft,
The air inlet is offered on the other end forms through-hole axis, the output shaft of the driving motor, the device for sealing magnetic fluid
Drive shaft is connected by shaft coupling respectively between any two with the transmission shaft.
3. powder according to claim 2 coats apparatus for atomic layer deposition, it is characterised in that: the guiding device includes matching
The linear guide and sliding block, the chamber door side of the reaction cavity for closing setting are provided with mounting seat, and the linear guide is along institute
Being axially set in the mounting seat for reaction cavity is stated, the sliding block can be along the linear guide relative to described anti-
Answer cavity mobile, the driving motor and chamber door passes through electric machine support respectively and chamber door bracket is fixed on the sliding block.
4. powder according to claim 3 coats apparatus for atomic layer deposition, it is characterised in that: the sliding block passes through screw rod electricity
Machine or cylinder driving.
5. powder according to claim 1 coats apparatus for atomic layer deposition, it is characterised in that: the reaction cavity corresponds to institute
It states ultrasonic vibration bar and is provided with second flange adapter tube, the second flange adapter tube is tightly connected with external ultrasound vibration device, institute
It states ultrasonic vibration bar to enter from second flange adapter tube, with the powder container dynamic Contact.
6. powder according to claim 5 coats apparatus for atomic layer deposition, it is characterised in that: the vibration of the ultrasonic vibration bar
Dynamic frequency is 10~60kHz, and oscillation power is greater than 1kW.
7. powder according to claim 1 coats apparatus for atomic layer deposition, it is characterised in that: also opened on the reaction cavity
Equipped with third flange connecting pipe, the third flange connecting pipe and external vacuum generating device are tightly connected.
8. powder according to claim 1 coats apparatus for atomic layer deposition, it is characterised in that: also opened on the powder container
There is venthole, the aperture of the venthole is provided with the strainer for preventing powder from leaking out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710945497.8A CN107502873B (en) | 2017-09-30 | 2017-09-30 | A kind of powder cladding apparatus for atomic layer deposition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710945497.8A CN107502873B (en) | 2017-09-30 | 2017-09-30 | A kind of powder cladding apparatus for atomic layer deposition |
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| CN107502873A CN107502873A (en) | 2017-12-22 |
| CN107502873B true CN107502873B (en) | 2019-02-15 |
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