CN205741206U - Apparatus for atomic layer deposition at powder surface uniform coated - Google Patents
Apparatus for atomic layer deposition at powder surface uniform coated Download PDFInfo
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- CN205741206U CN205741206U CN201620711350.3U CN201620711350U CN205741206U CN 205741206 U CN205741206 U CN 205741206U CN 201620711350 U CN201620711350 U CN 201620711350U CN 205741206 U CN205741206 U CN 205741206U
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Abstract
The utility model discloses a kind of apparatus for atomic layer deposition at powder surface uniform coated, source device, reaction chamber, heater, air inlet pipeline and exhaust pipe is entered including motor, rotating porous, rotating porous enters source device for be made up of hollow axle and blade, hollow axle two ends are seal, sidewall is provided with pore, blade spiral is fixed on hollow axle, and blade is provided with the micropore connected with hollow axle；Rotating porous enters source device and is erected in reaction chamber, and upper end is connected with motor shaft, and air inlet pipeline connects with hollow axle, and exhaust pipe connects with reaction chamber；On heater coating reaction cavity outer wall.Can effectively solve because of there is rigid contact and powder agglomeration in powder and can not be in the problem of its surface uniform coated, a large amount of micro-nano pore by being distributed on rotary fluid blade injects reacting gas and purge gas to whole powder inner homogeneous simultaneously, it is effectively shortened the response time, improves plated film efficiency.
Description
Technical field
This utility model relates to technique for atomic layer deposition field, a kind of atomic layer at powder surface uniform coated
Precipitation equipment.
Background technology
The dusty material of micro-or nano size, because showing the physical and chemical performance of many excellences and at such as battery electrode material
The fields such as material, catalyst are widely used, if last layer nano-level thin-membrane uniformly can be plated on its surface, it will bring more actively
Effect.Presently mainly utilize solid phase method, liquid phase method and vapor phase method at micro-nano powder surface coating, but these methods all without
Method solves the problems such as uniform coated, thickness accurately control simultaneously.
Technique for atomic layer deposition be one utilize reacting gas material surface replace saturated from absorption concurrent biochemical instead
The vapor phase chemical vapor deposition technology of target substance should be generated.Up to the present, Atomic layer deposition method is uniquely can be greatly
Specific surface area material surface uniform coated and accurately control the technology of thickness, but mostly these application are that material surface is completely exposed
Aerial situation.
For dusty material, even the Atomic layer deposition method of routine also is difficult at its surface uniform coated, former
Because mainly there being 2 points: first, dusty material there will be contact with each other, the phenomenon such as reunion, the Atomic layer deposition method of existing improvement
Use and utilize air blast to blow afloat powder so that it is fluidisation, but the shortcoming of which is: under air blast effect, reaction gas
The stability that body reacts in powder surface adsorption ability and surface all will be greatly affected, and can show asking of membrane thickness unevenness
Topic.Second, conventional Atomic layer deposition method all enters source (i.e. input reacting gas and purge gas), then profit outside powder
By modes such as free diffusing, pressurize diffusion, powder fluidising diffusions, reacting gas and purge gas are delivered to inside powder, but outward
Source mode is entered in portion can increase the biggest time cost, the valency that this time cost brings more than powder surface atom layer deposition plating
Value promotes, and, when amount of powder increases, the source mode of entering of above-mentioned routine the most all cannot be completely by reacting gas and purgative gas
Body is delivered to each region of powder, so yield is the least.
Utility model content
This utility model, for the deficiencies in the prior art, proposes a kind of ald at powder surface uniform coated and fills
Put, efficient uniform, easy and simple to handle.
In order to realize above-mentioned utility model purpose, this utility model provides techniques below scheme: a kind of equal on powder surface
The apparatus for atomic layer deposition of even plated film, enters source device, reaction chamber, heater, air inlet pipeline and exhaust tube including motor, rotating porous
Road, rotating porous enters source device and is made up of hollow axle and blade, and hollow axle two ends are seal, and sidewall is provided with pore, blade spiral shell
Being rotated with and be scheduled on hollow axle, blade is provided with the micropore connected with hollow axle；Rotating porous enters source device and is erected in reaction chamber, on
End is connected with motor shaft, and air inlet pipeline connects with hollow axle, and exhaust pipe connects with reaction chamber；Heater coating reaction cavity outer wall
On.
Further, blade is several, arranges for multi-layer helical.
Further, blade is one-piece auger shape, makes the powder in described reaction chamber exchange the most up and down.
Further, being provided with drainage screen in reaction chamber, exhaust pipe connects with drainage screen upper cavity.
Further, exhaust pipe is provided with powder catcher.
Further, blade material is porous metals, porous ceramics or porous membrane.
Compared with prior art, this utility model has the advantage that to use and is passed through reaction gas inside the powder of stirring,
And be carried out in time after reaction, circulation is carried out, and may be implemented in powder surface uniform coated, and navigability is good.Can efficient solution
Certainly can not be in the problem of its surface uniform coated because powder exists rigid contact and powder agglomeration, simultaneously by being distributed in rotation
A large amount of micro-nano pore on turn of tidal stream blade injects reacting gas and purge gas to whole powder inner homogeneous, effectively shortens
In the response time, improve plated film efficiency.
Accompanying drawing explanation
Fig. 1 is this utility model structural representation at the apparatus for atomic layer deposition of powder surface uniform coated；
Fig. 2 is the schematic appearance that rotating porous enters source device；
The most each reference is: 1 motor, 2 magnetic fluid seal, 3 reaction chambers, 5 rotating porous enter source device, 6 powder mistakes
Filter screen, 7 powder catchers, 8 shutoff valves, 9 vacuometers, 10 vacuum pumps, 11ALD three-way solenoid valve, 12 the first reaction mass
Source bottle, 13 the second reactant material sources, 14 pressure transducers, 15 mass flow controllers, 16 air inlet pipelines, 17 shutoff valves,
19 heaters.
Detailed description of the invention
Being described in detail this utility model below in conjunction with the accompanying drawings, the description of this part is only exemplary and explanatory,
Protection domain of the present utility model should there be is not any restriction effect.
As illustrated in fig. 1 and 2, a kind of apparatus for atomic layer deposition at powder surface uniform coated, including motor 1, rotate many
Kong Jinyuan device 5, reaction chamber 3, heater 19, air inlet pipeline 16 and exhaust pipe, wherein:
Described rotating porous enters source device 5 and is made up of rotary shaft and blade, and rotary shaft is the hollow-core construction that two ends seal, and rotates
The substantial amounts of micro-nano pore of axle surface configuration, these pores connect with the inner space of rotary shaft, and the connection of rotary shaft top is described
Air inlet pipeline 16；Blade screw is fixing on the rotary shaft, and inside is hollow, and connects with the inner space of rotary shaft, blade table
The substantial amounts of micro-nano pore of EDS maps, these pores connect with blade interior space and then connect with interior of rotating shaft space,
Whole and described air inlet pipeline 16 connects.
Described rotating porous enters source device 5 and is erected at described reaction chamber 3 inside, and magnetic fluid seal 2 is passed through with described in upper end
Motor 1 is connected, and described motor 1 drives described rotating porous to enter source device 5 to set speed rotation.
Described reaction chamber 3 is internal, and equipped with powder, powder sample is wrapped in described rotating porous and enters source device 5 external surface peripheral,
Especially wrap up the micro-nano pore on rotary shaft and blade；Described rotating porous enters source device 5 when rotated by described reaction chamber 3
In powder even fluidizing.
Described air inlet pipeline 16 is for entering to input reacting gas and cleaning in source device 5 hollow rotary shaft to described rotating porous
Gas, reacting gas and purge gas enter in source device 5 rotary shaft and on blade micro-nano pore by described rotating porous
It is uniformly injected into inside powder；Utilize described rotating porous to enter source device 5 and reacting gas and purge gas entered source mouth quantity from list
The individual number that increases to is in terms of trillion, and these enter source mouth by powder coated and along with blade 4 moves in a specific way, even fluidizing powder
While to make again different powder particle identical with the statistical probability entered source mouth and contact.
Air inlet pipeline 16 is provided with pressure transducer 14, mass flow controller 15 and shutoff valve 17.
Described reaction chamber 3 is bled by described exhaust pipe, for taking reacting gas, byproduct of reaction and the cleaning of excess away
Gas, it is possible to make described reaction chamber 3 inside reach target vacuum.
Described reaction chamber 3 is arranged around heater 19, for heating powder sample so that reacting gas is in the temperature set
Lower generation ald reacts, thus at powder surface filming.
Exhaust pipe configures shutoff valve 8, closes this valve and described reaction chamber 3 inside can be made to be in overvoltage condition,
It is of value to reacting gas and purge gas leaks into inside powder.
Described rotating porous enters connection more blades in the rotary shaft of source device 5, and the parameter of blade is disposed to ensure not
The statistical probability contacted with the powder in region pore micro-nano with on blade is identical so that powder fluidising evenly, and instead
Gas and purge gas is answered to be uniformly injected into inside powder.Easy to understand, blade quantity and surface texture are optimized and revised, can enter
One step improves coating effects.
The most micro-nano rank of air inlet on blade, it is to avoid resulting in blockage in powder access aperture, the material of blade can
To be porous metals, porous ceramics or other porous membrane.
The rotary shaft outer wall that blade enters source device 5 around described rotating porous helically combines arrangement, the advantage of this structure
It is that the powder allowing the powder bottom described reaction chamber 3 constantly be sent in top, i.e. reaction chamber exchanges the most up and down.
Blade quantity is multi-disc, all can independently change for every, i.e. micro-nano pore on blade can be replaced.
Higher than the position of the powder upper surface loaded in described reaction chamber 3, described powder filter net 6 is set, it is to avoid powder
Kick up during the later and decadent stage of a school of thought entrance exhaust pipe.
Powder catcher 7 is set between described exhaust pipe and described reaction chamber 3, it is to avoid powder is drawn into vacuum pump.
Compared with existing powder coatings technique for atomic layer deposition, this utility model device has done powder fluidising mode and has entered
The improvement of source mode, it is possible to obtain following beneficial effect:
This utility model energy fluidizing powder, blows powder without air blast in fluid mapper process, and the speed of rotary fluid can
Particle diameter according to powder, the amount of powder adjust.
When powder sample amount increases, equal proportion can be only needed to increase the diameter dimension of described reaction chamber, described rotating porous
Enter radius of turn and the quantity of described rotary fluid blade of source device so that this utility model both may be used on a small quantity
The surface atom layer depositing homogeneous plated film of (such as 1-10g) powder is it can also be used to the surface of a large amount of (such as 100g-100kg) powder is former
Sublayer depositing homogeneous plated film.
This utility model also powder filter net and powder catcher in described reaction chamber upper design, make powder enter and take out
The probability of air pipe drops to the least value, it is ensured that exhaust pipe safety and the service life of prolongation vacuum pump.
Rotating porous of the present utility model enters source device, even fluidizing powder and the sample introduction serving as reacting gas and purge gas
Device.Because rotating porous enter source device all the time rotate and and powder contact, so utilize its replace conventional atomic layer deposition skill
Reacting gas single in art and purge gas air inlet, in conjunction with Rotating with Uniform fluidisation design, will will react with the highest efficiency
Gas and purge gas are transported to the inside of powder, improve ald in the film thickness monitoring ability of powder surface coating and plating
Membrane efficiency.Another aspect, is injected into the reacting gas within powder and purge gas is constantly brought to upper surface, can improve
The efficiency of cleaning step.3rd aspect, when the described rotating porous of follow-up cleaning enters source device, is placed in cleaning solution,
Rotated by driven by motor, simultaneously enter the interior of rotating shaft of source device to described Stirring and be passed through the gas of elevated pressures, because
Gas can only enter the micro-nano pore on the device of source by rotating porous and discharge, and can realize Rapid Cleaning, improve described rotating porous
Enter the service efficiency of source device, reduce use cost.4th aspect, it is multi-disc that rotating porous enters the blade on the device of source, every phase
The most independent and replaceable, can be individually replaced after a certain blade breaks down.
In use, powder being positioned over reaction chamber 3 internal, after closing reaction chamber 3 hatch door, execution is following operates:
A () opens heater 19 reacting by heating chamber 3；
B () starts motor 1, rotating porous enters source device 5 and starts rotary fluid sample；
C () starts vacuum pump 10, open the shutoff valve 8 on exhaust pipe, and the mass flow on air inlet pipeline 16 controls
Device 15 controls purge gas entrance rotating porous and enters source device 5；
D () closes shutoff valve 8, the ALD three-way solenoid valve 11 on the first reactant material source bottle 12 pipeline is opened, repeatedly
The first reactant material source steam of interval pulse enters air inlet pipeline 16, i.e. reacting gas I, enters along with carrier gas enters rotating porous
In source device 5, reacting gas I enters the micro-nano pore on source device 5 by rotating porous and enters inside powder, saturated on powder surface
From absorption；
E () opens shutoff valve 8, purge gas enters rotating porous and enters source device 5 and then inject inside powder, cleans and removes
The reacting gas I of excess in powder inside and reaction chamber 3；
F () closes shutoff valve 8, the ALD three-way solenoid valve 11 on the second reactant material source bottle 13 pipeline is opened, repeatedly
Interval pulse the second reactant material source steam enters air inlet pipeline 16, i.e. reacting gas II, along with carrier gas enters micropore stirring
In device 5 and then inside injection powder, react generation target substance with adsorbing before at the reacting gas I on powder surface；
G () opens shutoff valve 8, purge gas enters rotating porous and enters source device 5 and then inject inside powder, cleans and removes
Excessive reacting gas II and byproduct of reaction in powder inside and reaction chamber 3；
H () repeats (d)-(g) step repeatedly, finally give the powder surface coating of target thickness；
Test example
Below with at SiO2The upper Al uniformly preparing one layer of 5nm thickness of powder (powder diameter is 10um)2O3As a example by thin film,
The devices and methods therefor of utility model described in practical illustration.
Before reaction starts, first by a certain amount of SiO2Powder puts into reaction chamber, and powder upper surface is less than powder filter net position
Put, load onto powder filter net, close reaction chamber hatch door；Atomic layer deposition method prepares Al2O3Need the two kinds of reaction masses used
Trimethyl aluminium (TMA) and pure water (H2O) it is attached separately in source bottle 12 and in source bottle 13.
A () opens heater 19, begin to warm up reaction chamber 3, and reaction chamber temperature is heated to 100-400 DEG C, preferably
200-300℃；
B () starts motor 1, rotating porous enters source device 5 and starts rotary fluid SiO2Powder sample, described motor 1 is preferably
Rotating speed continuously adjustabe, degree of regulation is up to 0.1 rev/min, and when opening motor first, speed should be slowly increased from minimum speed,
Before ald reaction starts, regulation rotating speed is between 20～600 revs/min；
C () starts vacuum pump 10, open the shutoff valve 8 on exhaust pipe, and air inlet pipeline 16 starts into purgative gas, preferably
Purge gas is N2Or Ar；
D () closes the shutoff valve 8 on exhaust pipe, regulate and control reaction chamber 3 vacuum through vacuometer 9；Open TMA source bottle 12
ALD valve 11 on pipeline, single opening time is 1s, opens altogether 10 times, and every minor tick 5s, TMA vapor source is along with air inlet
Pipeline 16 enters rotating porous and enters in source device 5 and then enter SiO2Inside powder, at SiO2Mono-point of one layer of TMA of powder surface adsorption
Sublayer, after the last pulse of TMA, the time that the shutoff valve 8 on exhaust pipe continues to close is no less than 100s；
E () opens the shutoff valve 8 on exhaust pipe, take the TMA molecule of excess in reaction chamber 3 away, and the time is no less than
30s；
F () closes the shutoff valve 8 on exhaust pipe, open H2ALD valve 11 on bottle 13 pipeline of O source, single is opened
Time is 1s, opens altogether 10 times, every minor tick 5s, H2O vapor source enters in source device 5 along with air inlet pipeline 16 enters rotating porous
And then enter SiO2Inside powder, adsorb at SiO in (d) step2The TMA molecule generation ald reaction on surface, generates
Target substance Al2O3, H2After the last pulse in O source, the time that the shutoff valve 8 on exhaust pipe is closed is no less than 100s；
G () opens the shutoff valve 8 on exhaust pipe, take the H of excess in reaction chamber 3 away2O molecule and byproduct of reaction
CH4Molecule, the time is no less than 30s；
H () repeats (d)-(g) step 50 time, finally give and be uniformly plated in SiO25nm thickness A l on microsphere2O3Thin film.
The above is only preferred implementation of the present utility model, it is noted that for the common skill of the art
For art personnel, on the premise of without departing from this utility model principle, it is also possible to make some improvements and modifications, these improve and
Retouching also should be regarded as protection domain of the present utility model.
Claims (6)
1. the apparatus for atomic layer deposition at powder surface uniform coated, it is characterised in that: include that motor, rotating porous enter source
Device, reaction chamber, heater, air inlet pipeline and exhaust pipe, rotating porous enters source device for be made up of hollow axle and blade, hollow axle
Two ends are seal, and sidewall is provided with pore, and blade spiral is fixed on hollow axle, and blade is provided with connect with hollow axle micro-
Hole；Rotating porous enters source device and is erected in reaction chamber, and upper end is connected with motor shaft, and air inlet pipeline connects with hollow axle, exhaust tube
Road connects with reaction chamber；On heater coating reaction cavity outer wall.
2. as claimed in claim 1 at the apparatus for atomic layer deposition of powder surface uniform coated, it is characterised in that: blade is some
Individual, arrange for multi-layer helical.
3. as claimed in claim 1 at the apparatus for atomic layer deposition of powder surface uniform coated, it is characterised in that: blade is overall
Helical form, makes the powder in described reaction chamber exchange the most up and down.
4. as claimed in claim 1 at the apparatus for atomic layer deposition of powder surface uniform coated, it is characterised in that: set in reaction chamber
Drainage screen, exhaust pipe is had to connect with drainage screen upper cavity.
5. at the apparatus for atomic layer deposition of powder surface uniform coated as described in claim 1 or 4, it is characterised in that: exhaust tube
Road is provided with powder catcher.
6. as claimed in claim 1 at the apparatus for atomic layer deposition of powder surface uniform coated, it is characterised in that: blade material is
Porous metals, porous ceramics or porous membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620711350.3U CN205741206U (en) | 2016-07-07 | 2016-07-07 | Apparatus for atomic layer deposition at powder surface uniform coated |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620711350.3U CN205741206U (en) | 2016-07-07 | 2016-07-07 | Apparatus for atomic layer deposition at powder surface uniform coated |
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| CN205741206U true CN205741206U (en) | 2016-11-30 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106011791A (en) * | 2016-07-07 | 2016-10-12 | 王禄荣 | Atomic layer deposition device capable of enabling powder surface to be evenly coated and method of device |
| CN112531182A (en) * | 2020-12-05 | 2021-03-19 | 重庆大学 | Portable cylindrical membraneless fuel cell with large reaction volume ratio |
| CN112543820A (en) * | 2018-06-12 | 2021-03-23 | 应用材料公司 | Rotary reactor for uniform particle coating from thin films |
| CN113046728A (en) * | 2021-03-12 | 2021-06-29 | 南开大学 | Atomic layer deposition device and atomic layer deposition method suitable for powder sample |
| CN113564565A (en) * | 2021-07-22 | 2021-10-29 | 江苏微导纳米科技股份有限公司 | Powder coating device and method |
-
2016
- 2016-07-07 CN CN201620711350.3U patent/CN205741206U/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106011791A (en) * | 2016-07-07 | 2016-10-12 | 王禄荣 | Atomic layer deposition device capable of enabling powder surface to be evenly coated and method of device |
| CN112543820A (en) * | 2018-06-12 | 2021-03-23 | 应用材料公司 | Rotary reactor for uniform particle coating from thin films |
| CN112531182A (en) * | 2020-12-05 | 2021-03-19 | 重庆大学 | Portable cylindrical membraneless fuel cell with large reaction volume ratio |
| CN113046728A (en) * | 2021-03-12 | 2021-06-29 | 南开大学 | Atomic layer deposition device and atomic layer deposition method suitable for powder sample |
| CN113564565A (en) * | 2021-07-22 | 2021-10-29 | 江苏微导纳米科技股份有限公司 | Powder coating device and method |
| CN113564565B (en) * | 2021-07-22 | 2023-12-15 | 江苏微导纳米科技股份有限公司 | Powder coating device and method |
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Legal Events
| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190605 Address after: 211800 No. 29 Buyue Road, Qiaolin Street, Pukou District, Nanjing City, Jiangsu Province, 12 305 blocks Patentee after: Nanjing Yuanlei Nanomaterials Co., Ltd. Address before: Room 302, Room 22, Changjiang International Gongyuan, Wuxi New District, Jiangsu Province Patentee before: Wang Lurong |