CN204058588U - A kind of device for micro-nano granules finishing - Google Patents
A kind of device for micro-nano granules finishing Download PDFInfo
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- CN204058588U CN204058588U CN201420297884.7U CN201420297884U CN204058588U CN 204058588 U CN204058588 U CN 204058588U CN 201420297884 U CN201420297884 U CN 201420297884U CN 204058588 U CN204058588 U CN 204058588U
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Abstract
The utility model discloses a kind of device for micro-nano granules finishing, comprising: reaction chamber, its inner cavity formed is used for the reaction compartment as presoma and micro-nano granules; Multiple presoma feeding mechanism, it to pass to mutually from described reaction chamber respectively by pipeline and provides different presomas; Carrier gas delivery system, the carrier gas that presoma is exported by this carrier gas delivery system is transported in reaction chamber; And powder granule stowage unit, for carrying micro-nano granules to be finished; Alternately presoma is carried respectively to reaction chamber by multiple presoma feeding mechanism, and enter in the powder granule stowage unit of rotation to carry out ald reaction with micro-nano granules surface contact, thus form coated film on the surface of micro-nano granules, realize finishing.The invention also discloses the method utilizing said apparatus to carry out the finishing of micro-nano granules.The utility model can obtain the coating layer of particle surface high uniformity, and improves the integral coating rate of powder granule and the utilization ratio of presoma.
Description
Technical field
The utility model belongs to powder granule surface coating technology field, is specifically related to a kind of device for micro-nano granules finishing.
Background technology
Compare block materials, powder granule material has large specific surface sum high surface, there is the small-size effect not available for conventional solid material, surface effects and quantum tunneling effect, cause the change of structure and energy state, the physics-chem characteristics such as the light of many uniquenesses, heat, electricity, magnetic, mechanics, catalysis can have been produced.
Between the specific surface area that it is huge, by suitable finishing, can expand further and improve its premium properties.The main method of micro-nano granules finishing is as required at the coated thin film of particle surface, forms nucleocapsid structure.Such structure can make nano particle have better stability, weathering resistance and excellent physics-chem characteristic.Meanwhile, finishing also contributes to the understanding to micro-nano-scale material.
At present, micro-nano powder coating technology can be divided into solid phase method, liquid phase method and vapor phase process according to the state of reaction system.Solid phase method is mainly activated particle surface by mechanical effect, high-temperature calcination or high energy ion beam, makes it to adsorb other materials and reaches the coated of surface.But the bonding force of the nucleocapsid structure realized due to mechanically mixing is strong, high energy beam excitation is lower easily forms the coated of thickness and uneven components, and requires that powder granule has the problems such as single dispersiveness, and the method overall application is comparatively limited.Liquid phase method comprises heterogeneous flocculence, sol-gel method, polymer encapsulation, the precipitator method etc., there is the advantage that equipment is simple, cost is low, it is the method that micro-nano granules surface coating technology is most widely used, but there is the shortcomings such as reaction process more complicated, coated thickness and composition not easily accurately control, and film forming purity and compactness are high not.
Vapor phase process mainly comprises physical vaporous deposition and chemical Vapor deposition process.The former realizes particles coat by the effect of Van der Waals force, core-shell structure copolymer bonding force is not strong, chemical Vapor deposition process is then utilize gaseous substance generate solid deposited thing in nano grain surface reaction and reach the coated of nano particle, existing comparatively perfect deposition is theoretical, and can carry out coated on the surface of any shape, the purity of rete is high.As a kind of special chemical vapour deposition technique, technique for atomic layer deposition accurately can control material composition and pattern on nano-scale dimension, by be deposited material with the form of monatomic film in layer be plated in body surface, there is high deposition uniformity, by controlling the number of times of reaction alternate cycles, realize the nano level controllable growth of film thickness.Technique for atomic layer deposition is utilized to carry out the densification of nanoscale on micro-nano granules surface coated, can accurate coated thickness and component, and there is good conformality.
Current existing powder granule finishing equipment or method mainly adopt the mode of fluidisation, but, because technique for atomic layer deposition is rooted in traditional flat film growing technology, existing apparatus and method need further raising for the suitability of micro-nano granules surface deposition, major embodiment has marked difference compared with planar substrates depositing operation, and in deposition process powder granule due to reunion difficulties in dispersion, the advantage which results in ald high uniformity can not give full play in particle surface is coated, coating efficiency is lower, presoma utilizes may be abundant not.
Utility model content
Main purpose of the present utility model is to provide a kind of device for micro-nano granules finishing, the advantage of technique for atomic layer deposition can be made full use of, the coating layer of particle surface high uniformity can be obtained, and improve the integral coating rate of powder granule and the utilization ratio of presoma.
In order to solve the problems of the technologies described above, a kind of device for micro-nano granules finishing of the utility model, the multiple presoma carried by utilizing carrier gas carries out ald, coated film is formed on the surface of micro-nano granules, realize finishing, it is characterized in that, this device comprises:
Reaction chamber, its inner cavity formed is used for the reaction compartment as presoma and micro-nano granules;
Multiple presoma feeding mechanism, it communicates with described reaction chamber respectively by pipeline, for respectively to providing different presomas in reaction cavity;
Carrier gas delivery system, it is arranged on the pipeline of described presoma feeding mechanism, and this pipeline is provided with mass flow controller, and the carrier gas that described presoma is exported by this carrier gas delivery system is transported in reaction chamber; And
Powder granule stowage unit, it to be contained in described reaction chamber and can axial-rotation wherein, for carrying micro-nano granules to be finished, this powder granule stowage unit one end is connected with the rotary drive mechanism be positioned at outside reaction chamber, and the other end is connected with the vacuum system outside reaction chamber;
Alternately presoma is carried respectively to described reaction chamber by described multiple presoma feeding mechanism, and enter in the powder granule stowage unit of described rotation and carry out ald reaction to contact with micro-nano granules, thus form coated film on the surface of micro-nano granules, realize finishing.
As improvement of the present utility model, described powder granule stowage unit is that two-layer cylinder set forms, inside and outside two-layer barrel is the powder of stainless steel sintering filter screen in micron order aperture, cylindrical shell both ends of the surface are provided with cover plate, and be interconnected to be clamped by double-layer circular columnar filter screen by stud, ensure that powder granule can not spill from particle stowage unit, the cover plate at cylindrical shell two ends is connected with vacuum system and rotary drive mechanism respectively by device for sealing magnetic fluid.
As improvement of the present utility model, described presoma feeding mechanism comprises the presoma steel cylinder storing precursor source, the presoma be arranged on pipeline that presoma steel cylinder is connected with reaction chamber responds valve fast, the manual needle valve between valve and steel cylinder is responded fast at presoma, alternately opening by the quick response valve on each presoma feeding mechanism, realize different presoma and alternately enter reaction chamber, the manually adjustment of needle-valve, realizes the control of the presoma pulsating pressure size of input.
As improvement of the present utility model, also there is heating and temperature controlling system, comprise the ring heater, heating unit in presoma supply system and the temperature sensor that are arranged on inside cavity, wherein, ring heater and heating unit are respectively used to as reaction chamber and the heating of presoma feeding mechanism, and described temperature sensor is for measuring the temperature of reaction chamber.
As improvement of the present utility model, described vacuum system comprises vacuum, throttling valve and device for sealing magnetic fluid, wherein said vacuum pump is used for vacuumizing reaction chamber, ensure the clean of reaction environment and cleaning reaction by product and unnecessary presoma, described device for sealing magnetic fluid is connected with powder granule stowage unit, be provided for air-flow in reaction chamber to be drawn out of by this powder granule stowage unit, described throttling valve is arranged on device for sealing magnetic fluid downstream, for controlling the air-flow velocity by powder granule layer in powder granule stowage unit.
As improvement of the present utility model, described rotary drive mechanism comprises motor, shaft coupling, device for sealing magnetic fluid, wherein device for sealing magnetic fluid is connected with reaction chamber, motor to the rotating shaft of device for sealing magnetic fluid, thus drives the powder granule stowage unit that is connected with this rotating shaft to rotate by coupled shaft coupling transmission.
In the utility model, presoma supply system ligation cavity systems, powder granule stowage unit is placed in reaction cavity inside, and powder granule stowage unit one end connects vacuum system, and the other end connects rotary motion power system.The connecting pipeline of presoma supply system and reaction cavity system is connected with carrier gas delivery system, heating system comprises the heating unit be arranged in inside cavity and presoma supply system.
Presoma supply system comprises two or more parallel branch, there is provided different presoma as reactant gases respectively, its major parts comprises single-ended or both-end presoma steel cylinder, presoma responds valve fast, responds the manual needle valve between valve and steel cylinder fast at presoma.It is normal closed gate that presoma responds valve fast, and the minimum opening time can reach 5ms.In the utility model, reaction cavity is made up of three parts of left, center, right by oxygen free copper gasket seal, and three parts are connected by bolt and nut.Exocoel left part, in operation for taking apart, takes out the powder granule stowage unit of outer chamber.In the middle part of exocoel, there are two flange-interfaces upper and lower both sides, are respectively used to connect the temperature sensor of pressure warning unit in vacuum system and temp measuring system, for the pressure and temperature of test chamber inside.In the middle part of exocoel, the left and right sides is connected from different presoma supply systems.About cavity, the inner side of two parts is provided with well heater.Reaction cavity can preferably cylinder design, is conducive to being uniformly distributed of internal temperature homogeneity and air-flow.
In the utility model, powder granule stowage unit adopts double-layer circular columnar structure, inside and outside both sides are the powder of stainless steel sintering filter screen in micron order aperture, the stainless steel end face one at two ends is connected with the device for sealing magnetic fluid in the vacuum system of cavity side, and another is connected with the device for sealing magnetic fluid of cavity opposite side rotary motion transmission system.Double-layer circular columnar filter screen is clamped by stud by both ends of the surface, and ensure that powder granule can not spill from particle stowage unit, they and device for sealing magnetic fluid are installed by screw thread.
When utilizing the device of micro-nano granules finishing of the present utility model to carry out the method for micro-nano granules finishing, it carries out ald by the multiple presoma utilizing carrier gas to carry, form coated film on the surface of micro-nano granules, realize finishing.The method comprises:
Under certain ald (ALD) temperature of reaction, described vacuum system is utilized to vacuumize reaction chamber;
Powder granule stowage unit rotates under the drive of rotary motion transmission system, drives powder granule rotary motion wherein;
Multiple presoma alternately enters reaction chamber under carrier gas drives, and on powder granule surface, chemisorption occurs through after described powder granule stowage unit outer screen;
Under the effect of the vacuum pump of vacuum system, utilize carrier gas to clean unnecessary presoma and byproduct of reaction, thus obtain the micro-nano granules of required carrying out finishing.
Wherein, the absorption detailed process of each presoma is: after precursor pulse passes into reaction cavity, the vacuum pump of vacuum system stops bleeding, keep the pressure environment in reaction cavity, the micro-nano granules be rotated with powder granule stowage unit after rising to certain altitude due to the effect freely falling body of gravity, powder granule fall process in disperse mutually, its separately surface uniform adsorb this presoma
Wherein, the dwell time is relevant to the size of the specific surface area of powder granule, is preferably 10 ~ 120s, which increases the duration of contact on presoma and powder granule surface, facilitate fully carrying out of absorption.
Wherein, the presoma burst length is relevant to the size of the specific surface area of powder granule, and surface-area is larger, and the burst length is longer, is generally 10 ~ 180s/m
2, ensure that the absorption of all surface is abundant.
Wherein, the rotating speed of powder granule stowage unit is preferably 30 ~ 160rpm, which increases the duration of contact on presoma and powder granule surface, facilitates fully carrying out of absorption.
Wherein, the absorption detailed process of each presoma is: with higher rotational speed powder granule stowage unit, powder granule carries out circumferential motion due to very large centrifugal force thereupon together, presoma is input in reaction cavity together along with the carrier gas compared with large discharge, be directed radially through powder granule layer from the outer screen of powder granule stowage unit and be adsorbed on particle surface, adjust the air-flow velocity by powder granule layer, the pressure warning unit be connected with venting port upstream with reaction cavity is respectively utilized to detect the pressure difference of powder granule layer both sides, when this pressure difference reaches stable, it balances each other to the centrifugal force suffered by the pressure gradient power of powder granule generation and powder, thus realize the dispersion of powder granule, promote the homogeneity of presoma absorption.
Wherein, the rotating speed of powder granule stowage unit is preferably 160 ~ 900rpm.
Wherein, 30 ~ 500cm/s is preferably by the air-flow velocity of powder granule layer.
Wherein, the temperature of reaction cavity system is within the scope of room temperature to 550 DEG C.
The surface modification method of micro-nano granules of the present utility model adopts pressurize deposition method to carry out powder granule finishing in actual carrying out.Specifically, after precursor pulse passes into reaction cavity, close the vacuum pump of vacuum system, stopping is bled, keep the pressure environment in reaction cavity, the micro-nano granules be rotated with powder granule stowage unit after rising to certain altitude due to the effect freely falling body of gravity, powder granule disperses mutually in the process fallen, it is surface uniform absorption presoma separately, pressure maintaining period terminates final vacuum pump and byproduct of reaction and unnecessary presoma is taken away, then carries out the absorption of the second presoma in the same way;
The surface modification method of the micro-nano granules in the utility model adopts balance dispersed deposition method to carry out powder granule finishing in actual carrying out, specifically, with higher rotational speed powder granule stowage unit, powder granule carries out circumferential motion due to very large centrifugal force thereupon together, presoma is input in reaction cavity together along with the carrier gas compared with large discharge, be directed radially through powder granule layer from the outer screen of powder granule stowage unit and be adsorbed on particle surface, adjust the air-flow velocity by powder granule layer, the pressure warning unit be connected with venting port upstream with reaction cavity is respectively utilized to detect the pressure difference of powder granule layer both sides, when this pressure difference reaches stable, it balances each other to the centrifugal force suffered by the pressure gradient power of powder granule generation and powder, thus realize the dispersion of powder granule, promote the homogeneity of presoma absorption.The rotating speed that the method is larger also contributes to the size reducing the coacervate that powder granule is formed, and with further augmenting response surface-area, improves the utilization ratio of presoma.
Further, the presoma burst length is relevant to the size of the total surface area of powder granule, and surface-area is larger, and the burst length is longer, is generally 10 ~ 180s/m
2, ensure that the absorption of all surface is abundant.
Further, in pressurize deposition method, the dwell time is relevant to the size of the specific surface area of powder granule, specific surface area is larger, and the dwell time is longer, is generally 10 ~ 120s, which increase the duration of contact on presoma and powder granule surface, facilitate fully carrying out of absorption.
Further, in pressurize deposition method, the rotating speed of powder granule stowage unit is unsuitable too fast, and powder granule can be fallen after rotating to certain altitude, and generally choosing rotating speed is 30 ~ 160rpm.
Further, in balance dispersed deposition method, the rotating speed of powder granule stowage unit is very fast, and make powder granule all the time and carry out circumferential motion along with stowage unit and can not fall, generally choosing rotating speed is 160 ~ 900rpm.
Further, in balance dispersed deposition method, carry the flow of the carrier gas of presoma by control and utilize the adjustment of the throttling valve of venting port upstream by the air-flow velocity of powder granule layer to reach finally stable pressure difference, rotating speed used is higher, and the required flow rate realizing balance is larger.General employing flow velocity is 30 ~ 500cm/s.
Further, the temperature of reaction cavity system is room temperature to 550 DEG C.
In general, the above technical scheme conceived by the utility model compared with prior art, owing to adopting technique for atomic layer deposition, the dispersiveness that micro-nano powder particle is excellent in deposition process can be ensured, reduce the size of powder reuniting body, thus increase participate in reaction surface-area, realize particle surface to presoma even, fully adsorb.Particularly, following beneficial effect can be obtained:
(1) in the device of this micro-nano granules finishing, utilize the pressurize deposition method under centrifugation, the Long contact time on presoma and powder granule surface can be realized under the state of dispersion powder particle, presoma absorption is full and uniform, ensure that the homogeneity of surface deposition film, improve the utilization ratio of presoma simultaneously.
(2) in the device of this micro-nano granules finishing, utilize the balance dispersed deposition method under centrifugation, the size of the coacervate that micro-nano granules is formed can be reduced to a certain extent, ensure dispersiveness simultaneously, increase the specific surface area participating in reaction, increase the area of institute's modification of surfaces, facilitate the full and uniform absorption of presoma, improve the homogeneity of deposit film and batch processed amount can be increased.
(3) in the device of this micro-nano granules finishing, presoma and carrier gas stream are directed radially through powder granule layer by the outer screen of powder granule stowage unit, and be drawn out of from interior side screen, this air-flow balances with centrifugal force simultaneously at high speed, avoid powder granule in the design that air-flow flows vertically and be easy to be deposited in the defect of side screen surface of bleeding, the improvement effect of centrifugation for particle surface deposition uniformity and adequacy can be given full play to.
Accompanying drawing explanation
Fig. 1 is a kind of total system schematic diagram for micro-nano granules surface modification apparatus of the utility model embodiment;
Fig. 2 is the powder granule stowage unit outside drawing of the utility model embodiment;
Fig. 3 is the axial sectional view of powder granule stowage unit;
Fig. 4 is powder granule stowage unit radial cross-section;
Fig. 5 is powder granule stowage unit schematic three dimensional views.
Embodiment
In order to make the purpose of this utility model, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the utility model is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the utility model, and be not used in restriction the utility model.In addition, if below in described each embodiment of the utility model involved technical characteristic do not form conflict each other and just can mutually combine.
As shown in Figure 1, a kind of surface modification apparatus of micro-nano granules, comprises vacuum system, reaction cavity, powder granule stowage unit, presoma supply, heating and temperature control system, carrier gas delivery system, rotary motion transmission system, Controlling System.Presoma supply system ligation cavity, powder granule stowage unit is placed in reaction cavity inside, and powder granule stowage unit one end connects vacuum system, and the other end connects rotary motion transmission system.
Be connected by carrier gas delivery system with reaction cavity in presoma supply system, carrier gas transfer line be provided with mass flow controller 5.
Presoma supply system comprises the presoma branch road of two or more parallel connection, different precursor source is provided respectively, its major parts comprises presoma and responds valve 6 and presoma steel cylinder 8 fast, responds the manual needle valve 7 between valve and steel cylinder fast at presoma.Presoma responds valve 6 fast for normal closed gate, and the minimum opening time can reach 5ms.Each fast response valve alternately open, the presoma in the steel cylinder of its branch road separately alternately enters reaction cavity internal system.
Reaction cavity is made up of left, center, right three part, is sealed by oxygen free copper pad 2.Cavity left part, in operation for taking apart, takes out the powder granule stowage unit 3 of outer chamber.In the middle part of exocoel, there are two flange-interfaces upper and lower both sides, are respectively used to connect the temperature sensor 4 of pressure warning unit 14 in vacuum system and temp measuring system, for the pressure and temperature of test chamber inside.In the middle part of exocoel, the left and right sides is connected from different presoma supply systems.About cavity, the inner side of two parts is provided with ring heater 16.Reaction cavity left part is connected with the device for sealing magnetic fluid 18 of rotary motion transmission system, and reaction cavity right part is connected with the device for sealing magnetic fluid 9 of vacuum system.
Heating with temperature controlling system comprise be arranged on inside cavity ring heater 16 and presoma supply system on heating unit 15 and temperature sensor 14.Heating unit 15 in ring heater 16 and presoma supply system is respectively the pipeline heating that reaction cavity 1 and presoma steel cylinder 8, presoma respond valve 6 and presoma branch road fast.The temperature of reaction cavity 1 inside measured by temperature sensor 14.
As shown in Fig. 2,3,4,5, powder granule stowage unit adopts double-layer circular columnar structure, inside and outside both sides are the powder of stainless steel sintering filter screen 24,26 in micron order aperture, aperture is preferably 5 ~ 10 microns, double-layer circular columnar filter screen is clamped by stud 22 and nut 23 by the stainless steel end face 21,25 at two ends, ensure that powder granule can not spill from particle stowage unit, take out by the connection of removing these two end faces and stud the powder granule completing finishing.End face 25 is connected with the device for sealing magnetic fluid 9 in vacuum system, and end face 21 is connected with the device for sealing magnetic fluid 18 of rotary motion transmission system.
Vacuum system comprises vacuum pump 12, magnetic valve 11, throttling valve 10 and device for sealing magnetic fluid 9.Device for sealing magnetic fluid 9 ensures that the air-flow in reaction cavity 1 is drawn out of by powder granule stowage unit 3 completely, instead of is directly taken away by vacuum pump 12.Throttling valve 10 is directly connected with device for sealing magnetic fluid 9 downstream, for controlling the air-flow velocity by powder granule layer in powder granule stowage unit 3.After magnetic valve 11 is connected on throttling valve, determine whether to bleed to reaction cavity 1, vacuum pump 12 is responsible for the pressure of reaction cavity 1 to be extracted into vacuum tightness needed for ALD reaction, ensures the clean of reaction environment and cleaning reaction by product and unnecessary presoma.
Rotary motion transmission system comprises motor 20, shaft coupling 19, device for sealing magnetic fluid 18 and bearing 17.Motor 20 provides motivating force, and coupled shaft coupling 19 is for transmission to the rotating shaft of device for sealing magnetic fluid 18, and inner and reaction cavity 1 left part of device for sealing magnetic fluid 18 is provided with bearing 17 and carrys out the motion of supporting revolving shaft and stressed.Device for sealing magnetic fluid 18 is connected with reaction cavity 1, ensures the resistance to air loss of reaction cavity simultaneously.
Controlling System controls the control of the open and close of vacuum system, time of presoma pulse and reaction cleaning and cycle index, temperature, powder granule stowage unit 9 and 18 rotating speed.Controlling System also comprises two pressure warning units, and pressure warning unit 14 is connected with reaction cavity 1, and pressure warning unit 13 is connected to the upstream of throttling valve 10 in vacuum system.
The utility model embodiment utilize said apparatus to the method for the finishing of micro-nano granules, its detailed process is as follows:
Wherein, atom layer deposition process can adopt pressurize depositing operation or balance dispersed deposition technique.
Below, the embodiment adopting pressurize depositing operation is first introduced:
Step S10: pretreatment stage.Powder granule is put into powder granule stowage unit, drive powder to rotate with certain rotating speed, selection of speed is at 30 ~ 60rpm.Open the magnetic valve before vacuum pump completely and throttling valve vacuumizes (vacuum level requirements pressure is less than or equal to 1Pa) reaction cavity.Reaction cavity is heated simultaneously, temperature according to selected, reaction controlling be room temperature ~ 550 DEG C.Keep this process at least 1 hour.Arranging line temperature is 100 DEG C, and it is 120 DEG C that presoma responds valve temperature fast.Subsequent technique can be carried out when the displays temperature of reaction cavity reaches established temperature and fluctuation range is no more than 1 DEG C.
Step S20: presoma stage pulse.Close the magnetic valve before vacuum pump to stop bleeding.Turn on the presoma work output that manual needle valve corresponding to presoma steel cylinder reaches certain.Open presoma and respond valve fast, the opening time is chosen as 60 ~ 180s/m
2, the saturation steam carrying precursor source with the mass flow controller of carrier gas delivery system input carrier gas 20 ~ 200sccm when it is opened passes into reaction cavity.After unlatching presoma responds valve closes fast, stop carrier gas delivery system input carrier gas.Give the rotary powder motion of powder granule stowage unit and inside thereof in this stage by rotary motion transmission system, selection of speed is 30 ~ 160rpm.In this process, precursor A starts to be adsorbed on powder granule surface.
Step S30: pressurize absorption phase.Maintain the rotating speed in previous step and pressure 10 ~ 120s, micro-nano granules is due to the effect freely falling body of gravity after rising to certain altitude, and powder granule disperses mutually in the process fallen, and precursor A is fully adsorbed on powder granule surface.
Step S40: wash phase.Carrier gas input system is to reaction cavity input carrier gas 100 ~ 1000sccm, and the magnetic valve simultaneously opened before vacuum pump starts to bleed, cleaning reaction by product and unnecessary precursor A, and this process maintains 60 ~ 180s.
Step S50: the stage pulse carrying out precursor B according to the method for step S20.
Step S60: the pressurize absorption carrying out precursor B according to the method for step S30.
Step S70: the wash phase carrying out precursor B according to the method for step S40.
Step S80: circulation step S20 ~ S70 as stated above, cycle index depends on the film thickness of required deposition.The film of desired thickness can be formed after deposition terminates at particle surface, complete the finishing to micro-nano granules.
Adopt the embodiment of balance dispersed deposition technique as follows:
Step S10 ': pretreatment stage.Identical with the step S10 in deposition method one.
Step S20 ': presoma stage pulse.Selection of speed is 180 ~ 900rpm.Keep the unlatching of the magnetic valve before vacuum pump.The carrier gas flux of adjustment carrier gas process system and throttle valve control pass through the air-flow velocity of powder granule layer, the pressure warning unit be connected with venting port upstream with reaction cavity is respectively utilized to detect the pressure difference of powder granule layer both sides, flow velocity when reaching stable with pressure difference carries out the dispersed surface deposition to powder granule, and general employing flow velocity is 30 ~ 500cm/s.For presoma from the output steel cylinder, method, as step S20, is opened presoma and is responded valve times 10 ~ 100s/m fast
2, the saturation steam that precursor source is carried in carrier gas passes into reaction cavity.Presoma is directed radially through powder granule layer along with carrier gas from the outer screen of powder granule stowage unit and is adsorbed on particle surface.
Step S30 ': wash phase.All identical with the condition of previous step except stopping the conveying of presoma.Cleaning reaction by product and unnecessary precursor A, this process maintains 60 ~ 180s.
Step S40 ': the stage pulse carrying out precursor B according to the method for step S20.
Step S50 ': the wash phase carrying out precursor B according to the method for step S30.
Step S60 ': circulation step S20 ' ~ S50 ' as stated above, cycle index depends on the film thickness of required deposition.The film of desired thickness can be formed after deposition terminates at particle surface, complete the finishing to micro-nano granules.
In order to illustrate further structure, the principle of apparatus and method of the present utility model, below in conjunction with the surface modification process of concrete micro-nano granules, it is described further.
Embodiment one
Be the AlH of 50 μm to particle diameter
3the Al that particle surface coated one deck 10nm is thick
2o
3film, to reduce its impact sensitivity, improves security.Choose trimethyl aluminium (TMA) and water (H
2o) be presoma, its
main anti- equation is answered to be:
(A)AlOH
*+Al(CH
3)
3→AlOAl(CH
3)
2 *+CH
4
(B)AlCH
3 *+H
2O→AlOH
*+CH
4
Adopt above-mentioned micro-nano granules surface modification apparatus and corresponding pressurize deposition processing recipe:
By 0.1g AlH
3particle is put into powder granule stowage unit and is arranged on reaction cavity, connects with device for sealing magnetic fluid.Sealed reaction cavity afterwards.
Open vacuum pump, opens solenoid valve is connected with vacuum pump to make reaction cavity with throttling valve, is evacuated to by reaction cavity pressure and is less than or equal to 1pa.Reacting by heating cavity makes its internal temperature be stabilized in 120 DEG C, and heating presoma steel cylinder, presoma bypass line and presoma respond valve fast all to 80 DEG C.Give powder granule stowage unit rotating speed 60rpm, maintain this state 1 hour.
Shut electromagnetic valve, opens the manual needle valve after presoma steel cylinder, opens presoma and respond valve fast, with the carrier gas (N of 100sccm
2) carry presoma TMA steam and enter reaction cavity, close presoma after TMA pulse 60s and respond valve fast, stop passing into carrier gas, enter the packing stage of 30s.The powder granule freely falling body after reaching a certain height rotated, completes absorption with presoma TMA uniform contact in dropping process.Open magnetic valve to bleed, simultaneously to pass into the carrier gas of 100sccm, clean up byproduct of reaction with for presoma TMA.Presoma H
2the pulse of O, pressurize and wash phase are similar.
Carry out the circulation 100 times of two kinds of presoma pulses, pressurize and wash phase, can at AlH after deposition terminates
3particle surface forms the Al that thickness is about 14nm
2o
3film.
Embodiment two
Be the SiO of 200nm to particle diameter
2the Al that particle surface coated one deck 5nm is thick
2o
3film is to study SiO
2the surface tissue of particle.Choose trimethyl aluminium (TMA) and water (H
2 17o) be presoma.
Adopt above-mentioned micro-nano granules surface modification apparatus and corresponding balance dispersed deposition processing method:
By SiO
2particle is put into powder granule stowage unit and is arranged on reaction cavity, connects with device for sealing magnetic fluid.Sealed reaction cavity afterwards.
Open vacuum pump, opens solenoid valve is connected with vacuum pump to make reaction cavity with throttling valve, is evacuated to by reaction cavity pressure and is less than or equal to 1pa.Reacting by heating cavity makes its internal temperature be stabilized in 200 DEG C, and heating presoma steel cylinder, presoma bypass line and presoma respond valve fast all to 120 DEG C.Give powder granule stowage unit rotating speed 60rpm, maintain this state 2 hours.
Selection of speed is 300rpm.Keep the unlatching of the magnetic valve before vacuum pump.Adjustment carrier gas (N
2) flow and throttle valve control be 100cm/s by the air-flow velocity of powder granule layer, reaches the steady state of powder granule layer pressure at both sides difference.Turn on the manual needle valve after presoma TMA steel cylinder, open presoma and respond valve 60s fast, the saturation steam that presoma TMA is carried in carrier gas passes into reaction cavity.Presoma TMA is directed radially through powder granule layer along with carrier gas from the outer screen of powder granule stowage unit and is adsorbed on particle surface.After the quick response valve closes of presoma TMA, other conditions are constant, clean particle surface, extraction by product and unnecessary presoma TMA.Presoma H
2 17the pulse of O, pressurize and wash phase are similar.
Carry out the circulation 50 times of two kinds of presoma pulses, pressurize and wash phase, can at SiO after deposition terminates
2particle surface forms the Al that thickness is about 5nm
2o
3film.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present utility model; not in order to limit the utility model; all do within spirit of the present utility model and principle any amendment, equivalent to replace and improvement etc., all should be included within protection domain of the present utility model.
Claims (6)
1., for a device for micro-nano granules finishing, the multiple presoma carried by utilizing carrier gas carries out ald, thus forms coated film on the surface of micro-nano granules, realizes finishing, it is characterized in that, this device comprises:
Reaction chamber, its inner cavity formed is used for the reaction compartment as presoma and micro-nano granules;
Multiple presoma feeding mechanism, it communicates with described reaction chamber respectively by pipeline, for respectively to providing different presomas in reaction cavity;
Carrier gas delivery system, it is arranged on the pipeline of described presoma feeding mechanism, and this pipeline is provided with mass flow controller, and the carrier gas that described presoma is exported by this carrier gas delivery system is transported in reaction chamber; And
Powder granule stowage unit, it to be arranged in described reaction chamber and can axial-rotation wherein, for carrying micro-nano granules to be finished, this powder granule stowage unit one end is connected with the rotary drive mechanism be positioned at outside reaction chamber, and the other end is connected with the vacuum system outside reaction chamber;
Alternately presoma is carried respectively to described reaction chamber by described multiple presoma feeding mechanism, and enter in the powder granule stowage unit of described rotation to carry out ald reaction with micro-nano granules surface contact, thus form coated film on the surface of micro-nano granules, realize finishing.
2. a kind of device for micro-nano granules finishing according to claim 1, it is characterized in that, described powder granule stowage unit is that two-layer cylinder set forms, inside and outside two-layer barrel is the powder of stainless steel sintering filter screen in micron order aperture, cylindrical shell both ends of the surface are provided with cover plate, and be interconnected to be clamped by double-layer circular columnar filter screen by stud, ensure that powder granule can not spill from particle stowage unit, the cover plate at cylindrical shell two ends is connected with vacuum system and rotary drive mechanism respectively by device for sealing magnetic fluid.
3. a kind of device for micro-nano granules finishing according to claim 1 and 2, it is characterized in that, described presoma feeding mechanism comprises the presoma steel cylinder storing precursor source, the presoma be arranged on pipeline that presoma steel cylinder is connected with reaction chamber responds valve fast, and respond the manual needle valve between valve and steel cylinder fast at described presoma, alternately opening by the quick response valve on each presoma feeding mechanism, realize different presoma and alternately enter reaction chamber, and the adjustment of manually needle-valve, realize the control of the presoma pulsating pressure size of input.
4. a kind of device for micro-nano granules finishing according to claim 1 and 2, it is characterized in that, also there is heating and temperature controlling system, comprise the ring heater (16), heating unit (15) in presoma supply system and the temperature sensor (14) that are arranged on inside cavity, wherein, ring heater (16) and heating unit (15) are respectively used to as reaction chamber and the heating of presoma feeding mechanism, and described temperature sensor (14) is for measuring the temperature of reaction chamber (1).
5. a kind of device for micro-nano granules finishing according to claim 1 and 2, it is characterized in that, described vacuum system comprises vacuum pump (12), throttling valve (10) and device for sealing magnetic fluid (9), wherein said vacuum pump (12) is for vacuumizing reaction chamber, ensure the clean of reaction environment and cleaning reaction by product and unnecessary presoma, described device for sealing magnetic fluid (9) is connected with powder granule stowage unit (3), be provided for air-flows all in reaction chamber to be all drawn out of through after the powder granule layer in this powder granule stowage unit (3), described throttling valve (10) is arranged on device for sealing magnetic fluid (9) downstream, for controlling the air-flow velocity by powder granule layer in powder granule stowage unit (3).
6. a kind of device for micro-nano granules finishing according to claim 1 and 2, it is characterized in that, described rotary drive mechanism comprises motor (20), shaft coupling (19) and device for sealing magnetic fluid (18), wherein device for sealing magnetic fluid (18) is connected with reaction chamber (1), motor (20) to the rotating shaft of device for sealing magnetic fluid (18), thus drives the powder granule stowage unit (3) that is connected with this rotating shaft to rotate by coupled shaft coupling (19) transmission.
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|---|---|---|---|
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| CN106048559A (en) * | 2016-05-30 | 2016-10-26 | 华中科技大学 | Nano-particle atomic layer deposition device and method based on spatial isolation |
| CN107502873A (en) * | 2017-09-30 | 2017-12-22 | 华中科技大学无锡研究院 | A kind of powder coats apparatus for atomic layer deposition |
| WO2019237820A1 (en) * | 2018-06-14 | 2019-12-19 | 华中科技大学 | Atomic layer deposition apparatus for use in batch wrapping of micro-nanoparticles |
| CN112391613A (en) * | 2020-11-11 | 2021-02-23 | 鑫天虹(厦门)科技有限公司 | Atomic layer deposition apparatus for forming thin film on powder |
| WO2021203765A1 (en) * | 2020-04-08 | 2021-10-14 | 厦门韫茂科技有限公司 | Cavity wall structure for gas-phase reaction-based powder surface coating machine |
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2014
- 2014-06-06 CN CN201420297884.7U patent/CN204058588U/en not_active Expired - Lifetime
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| CN106048559A (en) * | 2016-05-30 | 2016-10-26 | 华中科技大学 | Nano-particle atomic layer deposition device and method based on spatial isolation |
| CN106048559B (en) * | 2016-05-30 | 2018-08-31 | 华中科技大学 | A kind of nano particle apparatus for atomic layer deposition and method based on space isolation |
| CN107502873A (en) * | 2017-09-30 | 2017-12-22 | 华中科技大学无锡研究院 | A kind of powder coats apparatus for atomic layer deposition |
| CN107502873B (en) * | 2017-09-30 | 2019-02-15 | 华中科技大学无锡研究院 | A kind of powder cladding apparatus for atomic layer deposition |
| WO2019237820A1 (en) * | 2018-06-14 | 2019-12-19 | 华中科技大学 | Atomic layer deposition apparatus for use in batch wrapping of micro-nanoparticles |
| US11236421B2 (en) | 2018-06-14 | 2022-02-01 | Huazhong University Of Science And Technology | Atomic layer deposition device for massively coating micro-nano particles |
| US11355442B2 (en) * | 2019-05-10 | 2022-06-07 | International Business Machines Corporation | Forming self-aligned multi-metal interconnects |
| US11923311B2 (en) | 2019-05-10 | 2024-03-05 | International Business Machines Corporation | Forming self-aligned multi-metal interconnects |
| WO2021203765A1 (en) * | 2020-04-08 | 2021-10-14 | 厦门韫茂科技有限公司 | Cavity wall structure for gas-phase reaction-based powder surface coating machine |
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