CN101925402A - Stirring device, device with said stirring device for producing nanometer powder and its method - Google Patents
Stirring device, device with said stirring device for producing nanometer powder and its method Download PDFInfo
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- CN101925402A CN101925402A CN2008801254116A CN200880125411A CN101925402A CN 101925402 A CN101925402 A CN 101925402A CN 2008801254116 A CN2008801254116 A CN 2008801254116A CN 200880125411 A CN200880125411 A CN 200880125411A CN 101925402 A CN101925402 A CN 101925402A
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/11—Stirrers characterised by the configuration of the stirrers
- B01F27/15—Stirrers with tubes for guiding the material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/11—Stirrers characterised by the configuration of the stirrers
- B01F27/17—Stirrers with additional elements mounted on the stirrer, for purposes other than mixing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
Abstract
A stirring device, a device with said stirring device for producing nanometer powder and its method are provided. The device for producing nanometer powder includes a stirring tank (530) for containing supporters (520) of nanometer material, a vertical transportation part (531) located in the stirring tank (530) for transporting said supporters (520) from lower portion to upper portion of the stirring tank (530) by helical rotation, a support plate (534) located in the stirring tank (530) and at upper portion of the vertical transportation part (531) for supporting supporters (520) from said vertical transportation part (531), said support plate (534) is cone-shaped or frustum of a cone in shape of which central section is higher and circumference section is lower, and a depositing device including a depositing source located in the stirring tank (530) and above the support plate (534) for depositing nanometer powder on the supporters in manner of physics disposition. The device for producing nanometer powder can mix the supporters or supporter chips uniformly and reduce the friction between supporters or supporter chips.
Description
Chinese patent application No. 200810004352. 9 full content, is now herein incorporated by the priority for the Chinese patent application No. 200810004352. 9 that agitating device, the nanometer powder manufacture device with agitating device and manufacture method were submitted this application claims on January 22nd, 2008 by reference.
Technical field
The present invention relates to field of nanometer technology, concretely, it is related to a kind of agitating device, nanometer powder manufacture device and manufacture method with agitating device.Background technology
Nanometer technology is in the important technical fields such as the ICT of new and high technology (IT), Life Sci-Tech (BT), Environmental Technology (ET) are referred to as, as most basic basis, and there is strong influence power to Technical Development Area.Nanometer（Nano) refer to equivalent to 10-9The unit of rice, so-called nanometer technology refers to isolation atom and molecular configuration or control and the technology for operating compositing factor.The characteristics of nanometer technology, is in terms of high-tech intensity, high involving property of economy, the maximization of energy efficiency, environment compatibility.
The industrial field of nanometer can be categorized as nanometer engineering（Nano Processes), nanostructured（Nano Structures), nanometer work(Hui (Nano Functions), nano-component standing grain port system（Nano Components ＆ Systems), nanometer basis (Nano Infrastructures) and nano material (Nano Materials) etc..Nanometer technology can be applied to a nanometer raw material（Nano Materials), nano-component（Nano Devices), nano biological (Nano Bio), the field such as medical treatment, environment, the energy, nanosystems, safety, application is extremely wide.The most basic nano material in field of nanometer technology, can be divided into nano-particle by shape（Nano Particles), nano wire (Nano Wire), nanotube (Nano Tube), nanometer wall (Nano Wall), Nano capsule（Nano Capsule), nanometer rods（Nano Rod) etc..
Nanometer powder refers to the size and shape for not lying in particle, ultra-fine grain of the average grain diameter in below lOOnm.The manufacture method of nanometer powder can be divided into vapor phase method, liquid phase method and solid phase method.Having using the representative manufacture method of vapor phase method in gas evaporation/condensing method and gas phase synthesis method, liquid phase method has the side such as the precipitation method and spray drying process
There is mechanization comminuting method etc. in method, solid phase method.The microminiaturization that the nanometer powder manufactured is constructed by material（100 below nm) and thing followed surface area increase, special electricity, magnetic, machinery and the catalyst property that can not be observed in original material can be shown.It therefore, it can be applied among the functional material of new generation of magnetic parts, sensor, filter, catalyst etc..
The manufacture method of nano-particle has a variety of methods in the prior art, can be generally divided into physical method and chemical method.Because what chemical method was utilized is chemical reaction, it is necessary to using oxidant（) and reducing agent oxidizer（redUCtant).Therefore the nano-particle produced by chemical reaction can have residual ion in many courses of reaction, so easily there is the cohesion between particle.In order to prevent interparticle cohesion, it will usually use surfactant（) and dispersant Surfactant（The additive such as Dispersant), so the ratio that the purity of nano-particle becomes is relatively low.When manufacturing application product, reaction easily also is produced with additive, after nano-particle manufacturing process terminates, virose derivative can be produced.In addition, the method for nano-particle is manufactured using chemical mode, in mixed inert metal or the metal salt of mutually different property, it is difficult to the nano-particle of quantification be produced, so having limitation in the material selection of nano-particle.Due to there are problems, the method for manufacturing nano-particle using chemical mode can reduce the original function of nano-particle, it is necessary to the extra charge handled derivatives such as oxidant, reducing agent, residual acids.
The method of nano-particle is manufactured with physical method can be divided into downdraft mode（Top Down) method and on to formula (Bottom Up) method.Downdraft mode method is, for example, that block is mechanically crushed to produce nano-particle；On for example refer to external energy in the material to formula method, manufacture nano-particle with evaporation/condensing method.Downdraft mode physics mode manufacture nano-particle typical example be mechanical high-energy source comminuting method (High Energy Mi lling), on to formula typical example be the condensing method of gas evaporation（Inert Gas Condensation, IGC).On to formula nano-particle manufacture method in addition to gas phase is condensing, also thermal evaporation（Thermal Evaporation), electron beam evaporation (E-beam Evaporation), Zhi Liu Splash penetrate (DC Sputtering, DCS), radio-frequency sputtering（RF Sputtering, RFS), ion beam sputtering（Ion Beam Sputtering, IBS), molecular beam epitaxy（Molecular Beam Epitaxy, MBE), flame atomizing device process（FAP, Flame Aerosol Process), chemical vapor deposition standing grain only (Chemical Vapor Deposition, CVD), chemical gaseous phase synthesis (Chemical Vapor Synthesis, CVS), arc discharge method（Arc Discharge
) and laser ablation Process（Laser Ablation) etc. a variety of methods.Generally existing following problem in the method for existing physics mode manufacture nanometer powder：Particle size is uneven, particle size is difficult to control, manufacturing process's inefficiency and is also easy to produce pollution and produces in enormous quantities and limited to.In the method for existing physics mode manufacture nano-particle, most representational method can be divided into mechanical crushing method, electric blasting method, condensing method of inert gas (Inert Gas Condensation, IGC) etc..
Although mechanical crushing method is suitable for use in production in enormous quantities, but is difficult that the size of nano-particle is controlled in below lOOnm, also has the problem of pollution occurs in crushing process.
The method for making nano-particle using electric blasting legal system is, in vacuo using pulse power (pulse power) on battery (capacitor) plain conductor, high voltage that abrupt release has been charged, high current evaporating/condensing manufacture nano-particle.What is utilized due to the method is moment explosion, so in the presence of being difficult to control to Nanoparticle Size and need to collect after nano-particle just usable shortcoming again.Although having tried to manufacture nano-particle with Same Way in solution, such method also needs to use after separation solution and nanometer powder, so it is difficult to carry out unification to process, and obtaining pure nano-particle.
Although the condensing method of inert gas can produce the nanometer powder of higher degree, can be used for the material of manufacture has limitation.The condensing method of inert gas need by nano-particle it is condensing cooling rod after, it is necessary to collect condensing nano-particle again.Final products such as are applied to, it is necessary to be handled by additional process, so being not suitable for producing in enormous quantities.The nanometer powder produced by the condensing method of inert gas, due to can rapidly aoxidize in an atmosphere, so after being reclaimed in vacuum tank, or product is applied at once, or inject a small amount of oxygen in vacuum tank, the surface of slow oxidation nanometer powder is easy to fetch and deliver nanometer powder in atmosphere.Such method is most of when manufacturing nanometer powder, and the support being used directly in application product is not used.The nanometer powder manufactured using support[1— 11], easily fetch and deliver, during using the constituent material of final products as support, manufacturing process can be simplified.But the nanometer powder manufacture device pointed out in existing patent or paper, it is low all to there is deposition efficiency, Nanoparticle Size wider distribution, and support stirring is uneven, is carried in the overload on support, the low problem of durability of equipment.Especially when manufacturing production in enormous quantities with nano-particle manufacture device, the successive sedimentation of non-efficiency is there is（Deposition), support stirring it is uneven,
The durability of equipment is low, stirring structure thing excess load, the problems such as support is crushed because of caused by the load between support.
The situation of successive sedimentation is that particle can form core and core can grow up, core grow to it is overlapping with adjacent core generation if, the particle of nanosized can rapidly grow into film.Nanometer powder uniform in size, stable is manufactured using support, it is important that noncontinuity is deposited, that is, control time and non-deposited time of the depositing nano-materials on support.The excessive growth of nano-particle is prevented by suitable control sedimentation time, in the non-deposited time, nano-particle is tended towards stability, even when exposed to deposition region, nano-particle also will not continue to growth, and other core is formed on support.In addition, to manufacture pure and evenly sized nano-particle, it is necessary to carry out uniform stirring to support.
Now, a variety of sedimentary origins are used among industrial field（For example utilize resistance heating, induced heat, plasma jet（Plasma Jet), electron beam, the sedimentary origin of laser beam and using ion beam sputtering, DC (Direct Current) sputtering, RF (Radio Frequency) sputtering, electron cyclotron resonace（ECR, Electron Cyclotron Resonance) etc. sedimentary origin）It is applied in nano-particle manufacture device, the multiple materials such as metal, ceramics, oxide, organic matter is manufactured into nano-particle.
Most of nano-particle manufacture device of first original physics mode is all the case made with research purpose, and it, which is designed, is only suitable for a small amount of production, and the production in enormous quantities that such device is not appropriate for industrialization is used.The example that the first technology of nano-particle is manufactured with support agitating mode is shown in Fig. 1-Fig. 4.
The nano-particle manufacture device of support manufacture nanometer powder or chip is previously utilizing, it is most of all by the way of the stirring of horizontal agitating shaft.Wherein being divided into has using single agitating shaft and using multiple agitating shafts situation.Shown in Fig. 1, Fig. 2 is the example of the agitating device of trunnion axis agitating mode.These devices can be drawn close due to the rotation of tank diameter 130,230, supporting body material to a direction, thus can not uniform stirring supporting body material.Agitating device shown in Fig. 1 is the construction of the body of tank diameter 130 rotation, takes the stirring structure of the trunnion axis rotation mode of drum type, and sedimentary origin 111 is located inside rotary barrel.In Fig. 1 by the way of drum is rotated to direction 131, support 120 can not be stirred completely in whipping process, rotation drum and supporting body material are mutually slided, some powder be possible to stirring less than.The landing phenomenon being especially in the presence of between the support of cohesiveness and tank diameter can be even more serious.In order to solve these problems, it is necessary to rotation drum construct into
Row is improved, and is that sedimentary origin is located inside rotation drum in addition with a problem, if so in the case of using tiny or low density supporting body material, the contaminated possibility of sedimentary origin is high.Fig. 2 shows the stirring structure of trunnion axis rotation mode in agitating device, and tank diameter 230 is fixed, and sedimentary origin 211 is located at outside tank diameter.Fig. 2 is also the same with the device in Fig. 1, because the phenomenon that the secundly of support 220 is toppled over occurs in rotation, and causes the generation of the supporting body material excess accumulation phenomenon in specific area, therefore the uniform stirring of supporting body material difficult to realize.In addition, when stirring supporting body material, rotary wings（Or agitator）231 are exposed to top, and so far nano-particle is deposited on rotary wings, and nano-particle can reduce the deposition efficiency of nano-particle, so that the process as non-efficiency if unnecessary place deposition like this.Production in enormous quantities device is manufactured with single-rotation axis construction, there is certain limitation, in order to expand capacity, multiple single trunnion axis can be used in Fig. 2 with series connection to constitute.In the case of the rotary shaft for setting multiple axles like this, each rotary shaft can be rotated to certain orientation, and supporting body material can be moved to same direction, be allowed to realize can not uniform stirring effect.In order to prevent this phenomenon, to need the direction of rotation of rotary shaft being converted into Random-Rotation.The Random-Rotation of agitating shaft can cause the friction between supporting body material, by the instantaneous rotation of rotation direction of principal axis switch and cause the irregular movement of supporting body material, support stirring it is uneven, supporting body material come off, the problems such as the decline of equipment.In the mode that nano-particle is manufactured using supporting body material, the persistent movement and uniform stirring of supporting body material are important.The direction of rotation rapidly changed can cause stirring structure thing to reinforce supporting body material, cause the serious crushing of support particle or supporting body material Bei Shun Jian Wind to outside phenomenon.In addition, the shortcoming of these devices, which is random stirring, will occur heat, so heat labile supporting body material can not be used.The crushing of supporting body material can form fine particle, so as to produce dust.Support is flowed into Vacuum exhaust tube after going out from Jiao Ban Cao Wind, and supporting body material can pollute vavuum pump, shortens maintenance/maintenance prompt, produces extra maintenance/upkeep cost, and reduce the production efficiency of product.In addition, the direction of rotation switching rapidly changed, can apply powerful external force to rotation portion, reduce the durability of equipment.It is difficult to produce a certain size nano-particle if stable and uniform stirring can not be carried out to supporting body material from the point of view of the controllings such as the size, content, distribution of nano-particle layer.As a whole, the possibility not of uniform size of most of nano-particle of formation can be higher.
Fig. 3, shown in 4 be the agitating device for having broken away from feathering axis construction to manufacture nano-particle example.
Device shown in Fig. 3 is considered as the agitating mode similar with Fig. 1 devices, and difference is that the rotary shaft of tank diameter 330 has certain angle from level, and sedimentary origin 311 is moved to external position inside tank diameter.Device as Figure 3 is it is difficult to ensure that deposition region, so there is problem on the efficiency of deposition and the equipment making of Large Copacity.It is suggested identical to the problem of point in Fig. 1 devices, it may occur that the phenomenon that supporting body material slides from wall, when particularly having the micro powder of cohesiveness between stirring support, it is difficult to realize the uniform stirring of micro powder.Therefore, such device is difficult to solve the problems, such as the uniform stirring of support powder and ensure deposition region, therefore the efficiency of reduction nanometer manufacturing process, there is limitation while producing in enormous quantities in manufacture on device.Fig. 4 is the example for the agitating device that agitating shaft is constructed using vertical stirring.Such device is in the material of agitating solution phase, it is very effective method, but when stirring the powder of a certain size solid forms or chip etc material, in order to two positions above and below mixing supporting body material, it is necessary to improve the rotary speed of agitator or change its construction.And if improving agitator speed, be not only unable to reach above and below two materials mixing efficiency, opposite rotary wings periphery material will be possible to be crushed by external force.So, such construct is considered as the reducing mechanism being more suitable for for the agitating device than supporting body material.The content of the invention
In view of the respective defect of existing nano-particle manufacture device presence, an object of the present invention is to provide a kind of agitating device, so that support or support chip hybrid are uniform, and reduces the friction between support or support chip.
Another object of the present invention is to provide a kind of nanometer powder manufacture device, to produce nanometer powder of uniform size.
Correspondingly, the present invention also provides a kind of nanometer powder manufacture method, to produce nanometer powder of uniform size.
To achieve these goals, the embodiment of the present invention provides a kind of agitating device, and the agitating device includes：Tank diameter, the support for accommodating nano material；
Vertical transport part, in tank diameter, the top for the support to be delivered to tank diameter by screw type rotary from the lower vertical of tank diameter；And
Support plate, in tank diameter and vertical transport part top, for supporting the vertical transport
The support that part conveying comes, the support plate is the low taper in middle high, periphery or taper type.
To achieve these goals, the embodiment of the present invention also provides a kind of nanometer powder manufacture device, and the device includes：
Tank diameter, the support for accommodating nano material；
Vertical transport part, in tank diameter, the top for the support to be delivered to tank diameter by screw type rotary from the lower vertical of tank diameter；
Support plate, in tank diameter and vertical transport part top, for the support for supporting vertical transport part conveying, the support plate is the low taper in middle high, periphery or taper type；And precipitation equipment, precipitation equipment include sedimentary origin, the sedimentary origin be located at tank diameter in and support plate top, for using physical deposition mode to support deposit nanometer powder.
To achieve these goals, the embodiment of the present invention also provides a kind of nanometer powder manufacture method, and this method includes：
Load step, for support to be loaded into tank diameter and deposition source material installation is carried out, the tank diameter and sedimentary origin are arranged in the vacuum tank in atmospheric condition；
Vacuum step, the vacuum tank is exhausted using vavuum pump, so that the vacuum tank reaches predetermined vacuum；
Stirring and deposition step, the support is stirred using the agitating mode of screw type vertical transport support, and nanometer powder is deposited to the support in deposition region by physical deposition mode while stirring；
Vacuum in nanometer powder obtaining step, breaking vacuum groove, the nanometer powder being attached on support is obtained from the tank diameter.The nanometer powder being attached on support can pass through following process or be applied directly in application product.
The nano-particle manufacturing equipment of the embodiment of the present invention employs the support agitating device of screw type vertical transport mode, realize the minimum of mechanization load, convey support with certain speed and direction, so as to realize to support progress uniform stirring, improve deposition efficiency, so that while producing a certain size nano-particle, the minimum of mechanical load and the load of equipment is realized, the nano-particle manufacture device of equipment durability is enhanced.
Brief description of the drawings
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the application, does not constitute limitation of the invention.In the accompanying drawings：
Fig. 1 is in the prior art using one of schematic diagram of agitating device of trunnion axis rotation mode；
Fig. 2 is the two of the schematic diagram of agitating device in the prior art using trunnion axis rotation mode；
Fig. 3 is the schematic diagram of agitating device in the prior art using sloping shaft rotation mode；
Fig. 4 is the schematic diagram of agitating device in the prior art using vertical rotary mode；
Fig. 5 be the embodiment of the present invention in using vertical transport mode nanometer powder manufacture device structural representation；
Fig. 6 is the schematic diagram of middle and upper part of embodiment of the present invention support support plate and broadcast seeder；
Fig. 7 is the simple examples of the structure of nanometer powder manufacture device in the embodiment of the present invention；
Fig. 8 is Nano silver grain transmission electron microscope (TEM) example images produced using existing nanometer powder manufacture device；
The TEM image example for the Nano silver grain that Fig. 9 is prepared according to the nanometer powder manufacture device of the present invention；Figure 10 a and Figure 10 b are the size distribution schematic diagram for the Nano silver grain prepared according to the nanometer powder manufacture device of the present invention.Embodiment
To make the object, technical solutions and advantages of the present invention clearer, the specific embodiment of the present invention is described in detail below in conjunction with the accompanying drawings.Here, the schematic description and description of the present invention is used to explain the present invention, but it is not as a limitation of the invention.
Embodiment one
The embodiment of the present invention provides a kind of support agitating device manufactured for nanometer powder and nanometer powder manufacture device.Fig. 5 is uses the structural representation of the nanometer powder manufacture device of vertical transport mode in the embodiment of the present invention, Fig. 7 is more specifically exemplary plot.Fig. 5 and Fig. 7 is refer to, the nanometer powder manufacture device of the present embodiment includes：
Support agitating device, the agitating device includes：Tank diameter, vertical transport part, support plate 534,
And one or more top rotary wings (or broadcast seeder) 532；
Precipitation equipment, the precipitation equipment includes sedimentary origin, and the sedimentary origin is located at the top of the support plate of agitating device, for depositing nanometer powder to support using physical deposition mode；
Vacuum tank, accommodates and vacuum state is kept in the sedimentary origin and agitating device, the vacuum tank, so that the sedimentary origin and agitating device are in vacuum；And
Vavuum pump, the described vacuum tank of connection, for carrying out vacuum pumping to the vacuum tank, to keep the vacuum in the vacuum tank.In the embodiment of the present invention, in vacuum tank vacuum can control as needed 5 X 10-1Support to 1 X 10-6Support, but it is not limited to this.In order to remove support contained humidity, gas or volatile materials, heater 536 can be set outside the tank diameter, to be heated to the support in tank diameter.And in vacuum tank using there is volatility support in the case of, cooling device 536 can be set outside the tank diameter, to be cooled down to the support in tank diameter.Also heating and cooling device can be provided with simultaneously, to decide whether to open the heating or cooling device as needed.
In above-mentioned agitating device：
The vertical transport part is located in tank diameter 530, the top for the support 520 to be delivered to tank diameter from the lower vertical of tank diameter；In the present embodiment, the vertical transport part includes again：Rotary shaft and the spiral rotating wing being fixed in the rotary shaft.For convenience, also can the vertical transport part be called spiral shape main rotating shaft 531 or spiral shape bolt.
The support plate 534 is located at the top of vertical transport part, and for the support for supporting the vertical transport part conveying, in order to contribute to slip of the support on support plate, the support plate is preferably set to centre（Close to rotary shaft）High, periphery（Away from rotary shaft）Low taper or taper type.Optionally, an isolating cylinder can be set in the periphery of the spiral shape main rotating shaft 531, the top of cylinder can set with support plate and be integrated or be fixed together, there is a fixed gap between the bottom of cylinder and the bottom of tank diameter, so that support is moved to main rotating shaft by the space, and by the rotation of the spiral rotating wing, support is again moved into the top of tank diameter.Certainly, the length of the isolating cylinder can also set shorter, such as only surround the top of spiral shape main rotating shaft, and expose following part.The support plate can pass through a variety of existing modes with isolating cylinder（Such as pass through support）It is fixed in tank diameter, herein without being described in detail.
One or more than one top rotary wings (or broadcast seeder) 532 are located on the support plate, for stirring the support on the support plate.
Support on support plate is moved to support plate edge and dropped to when falling in the tank diameter.
Because the rotation of main rotating shaft 531 is to rotate in certain direction, not only minimize the applied force to supporting body material, also the phenomenon of support powder crushing is minimized, supporting body material is moved to by top with the rotation of screw type bolt 531, be moved to top supporting body material moved with the inclined plane of support support plate 534 during simultaneously by deposition region.Being installed to the deposition materials of sedimentary origin can use as noble metal or oxide, organic matter, alloy, common metals such as gold, silver, platinum, ruthenium, rhodium, palladium, osmium, iridium（Such as aluminium A1), caesium (Se), silicon（Si), germanium（) etc. Ge material as sedimentary origin deposition materials.In the case where deposition materials are conductive, the methods such as DC sputterings, ion beam sputtering can be used, in the case where deposition materials do not have electric conductivity, can be using methods such as RF sputterings, ion beam sputterings, but this is not limited to, can also be using mid frequency sputtering, microwave deposition, the sputtering of double magnetic, heat deposition, electron beam deposition, laser deposition, electron cyclotron resonace or ion plating etc..In deposition region, due to top agitator（Broadcast seeder, spreader) 532 rotation drive, supporting body material is moved with the inclined plane of support plate 534, so as to realize uniform stirring.Being moved to the support of support plate marginal position can drop in support tank diameter, make to deposit to the nano-particle on support and acquired the stabilized non-deposited time.In order to control the time that nano-particle is deposited on support, a some holes 612 is bored on support plate (as shown in Figure 6）, support is hurtled down from support plate, support open-assembly time controlled with this, so as to control the time that deposition materials are deposited on support.The quantity in hole and the size in aperture can be carried out change.Support open-assembly time is controlled substantially to refer in deposition region, the regulation non-deposited time contrasts the ratio of sedimentation time, so as to realize the control to support nano surface particle size.In the present invention, in order that support is swimmingly moved to bottom, when being designed to tank diameter 530, the bottom construction narrower than top is designed to（It is i.e. upper coarse and lower fine）.In order to which the support of uniform stirring bottom there is also mounted at least one layer of bottom rotary wings 533, (each layer can be different from the angle of main rotating shaft, and two or more rotary wings can be set in each layer）.The top rotary wings, bottom rotary wings are securable on spiral shape main rotating shaft 531（But it is not limited to this）.Be moved to the supporting body material of tank diameter 530, with bottom rotary wings 533 continuously stirring slowly be moved to tank diameter bottom, shifting
The support of main rotating shaft 531 is moved by the rotation of bolt, the top of tank diameter is again moved into.This class process is done repeatedly, and the nano-particle supplied by sedimentary origin can be attached on the support surface of powder or chip form.The mixer structure of the present invention is, by the support conveying of screw type mode is constituted with main rotating shaft, top stirring with auxiliary agitator, the stirring of lower support body with auxiliary agitator etc., to employ the HELICAL ROTATING axle 531 of vertical transfer mode to reduce the external force for applying support to greatest extent.In addition, the mixer of the present embodiment is in structure, in order to improve deposition efficiency in deposition region, the support mixing part 532 for being also fabricated to top is not exposed to the structure of sedimentary origin, i.e. top rotary wings and is embedded in the support on the support plate.The nano-particle manufacture device with as above mixer structure of the embodiment of the present invention is on agitating mode compared with existing support agitating mode, with the uniform stirring that can ensure that supporting body material, the deposition efficiency in deposition region is improved, and reduction to the full extent has prevented the strong point of support crushing etc. in whipping process since being applied to the external force of support.The nano-particle manufacture device of the embodiment of the present invention, reduces the pollution of vavuum pump and the load of agitating shaft to the full extent, and reduces the maintenance cost of equipment, enhances the durability of equipment.Nano-particle manufacture device according to the present invention is in the control of nano-particle, the surface area of support volume vs deposition region is easily operated when designing equipment, the ratio regulation of sedimentation time contrast non-deposited time is can easily be accommodated, the size of nano-particle is generally speaking can easily be accommodated.By the nanometer powder manufacture device of the present invention can be within the scope of lnm-500nm come the nanometer powder mean size produced, the nanometer powder content being deposited on above support can be within the scope of lppm-10, OOOppm.
The process flow of the nano-particle manufacture device of the embodiment of the present invention is divided into selection nano material and supporting body material, the loading phase of filling nano material and supporting body material, vacuum exhaust stage, nanometer powder manufacture (stirring/deposition）Stage, breaking vacuum stage, the stage for taking out nanometer powder and supporting body material.Nanometer powder is manufactured, the nanometer target material and supporting body material for selecting to be adapted in application field is first had to.As the pre-treatment of nanometer powder manufacturing process, in order to promote the adherence force between support and nano-particle, the physical method or chemical method that can be also commonly used in advance on support surface using prior art are pre-processed.Prepare as process, in loading phase, have selected after nano material and supporting body material, nano material ingot bar is installed on sedimentary origin, supporting body material is encased in tank diameter.In the vacuum exhaust stage, start the 1st vacuum exhaust using roughing pump under atmospheric pressure state, reach after appropriate vacuum, entered using high-vacuum pump
The 2nd vacuum exhaust of row.In vacuum exhaust, in order to effectively remove the air existed between the air being contained on supporting body material or support, it is possible to use mixer is stirred to the supporting body material in tank diameter.Now in order to more effectively remove the air in vacuum tank, the heater (536) as shown in Fig. 5 can be set in the outside of tank diameter.And in vacuum tank using there is volatility support in the case of, can by install cooling device (536) reduce vacuum tank in temperature, so as to reduce the hair degree that support is waved.After completion vacuum exhaust engineering, into the process for nano-particle of being grown up with sedimentary origin on support.In this process, using the agitating mode of screw type vertical transport support, while auxiliary stirring can also be carried out to bottom and top support.The nano material supplied from sedimentary origin grows into the particle of nanosized on supporting body material.Deposition/in the mixing engineering stage, when the particle being deposited on above support is exposed to sedimentary origin, particle can grow up, reach a certain size nano-particle with support stirring from exposed to deposition field to moving inside tank diameter.The nano-particle being moved to inside tank diameter, before being exposed to deposition field with support again untill stablized, a certain size nano-particle can be formed.If being exposed to deposition region before nano-particle is stable, nano-particle can more grow up, it is more likely that grow into very big nano-particle.By the regulation of sedimentation time and non-deposited time, the Nanoparticle Size formed on support can be adjusted., can be by adjusting deposition in stirring/deposition procedures（Deposition Rate), sedimentation time, sedimentation time and the ratio of non-deposited time（The number and size in hole etc. are relevant in gradient, support plate with support plate）, mixing speed, the temperature of evaporation source, the temperature of support, vacuum, whole under deposition region support body surface areas and the ratio of whole support volumes etc. condition to control the size and content of nano-particle.Relative to existing nanometer powder manufacture method, it is main to improve the agitating mode for being support, for other details, such as how to load evaporation source, how to evaporate, how to vacuumize be all that those skilled in the art can complete, therefore the present invention omit detailed description thereof.Complete after nano-particle manufacturing process, the vacuum in breaking vacuum groove is needed as final stage, the support for being attached to nanometer powder is taken out from tank diameter.The another strong point of nanometer powder manufacturing process according to the present invention is, if the material of final application product structure material is carried out use by selection as supporting body material, process can be simplified, and because not adding other additives, so it is close environment, and the intrinsic characteristic of nanometer powder can be played to greatest extent.
What Fig. 8 and Fig. 9 was illustrated is the transmission electron microscope using the nanometer powder manufacture device of existing feathering axis and the Silver nano-powder that there is the nanometer powder manufacture device of vertical transfer rotary shaft to produce of the present invention respectively（TEM) example images.By Fig. 8 and Fig. 9, it is apparent that the nano-particle distribution produced using the nano-particle manufacture device of the present invention is more uniform.
It is respectively the example of the size distribution for the nanometer powder produced using the device of existing nanometer powder manufacture device and manufacture nanometer powder of the invention shown in Figure 10 a and Figure 10 b.The size distribution for the nanometer powder that 10 more than nm are compared in the size distribution of 2-30 nm nanometer powder, Figure 10 b is compared in Figure 10 a.Wherein A represents the Nano silver grain produced using existing agitating mode, and B represents the Nano silver grain produced using the agitating mode of the present invention.Figure 10 a and Figure 10 b are the results after Relative Transformation on the basis of the most particle size of quantity（That is the peak value of two curves is standardized（normalized) ) .As shown in Figure 10 a and Figure 10 b, the nanometer powder produced by existing agitating mode, it may be observed that many big particles produced by uneven stirring.The nanometer powder produced using the agitating mode in the present invention, it may be observed that big number of particles is relatively fewer.Therefore, uniform stirring can be realized using the mixer of vertical transport mode, it is suppressed that the generation of big nano-particle.
Fig. 8 to Figure 10 a, Figure 10 b only illustrate the nanometer powder that the present invention is prepared by taking Silver nano-powder as an example, but the present invention is not limited thereto.Using the nanometer powder manufacture device of the present invention, the nanometer powder of other materials can be equally prepared, such as other metals beyond silver can be equally prepared（Such as gold, platinum, ruthenium, rhodium, palladium, osmium and iridium）, oxide, organic matter, alloy and semiconductor（Such as Se, Si and Ge）Deng the nanometer powder of material.
For the nanometer powder manufactured using existing agitating mode, 10 below nm nano-particle can account for the 89. 9% of all nano-particles, and 10 more than nm nano-particle accounts for the 10. 1% of all nano-particles.And for the nanometer powder manufactured according to the present invention using vertical transport mode, either metal or other materials（Such as oxide, organic matter, alloy, Se, Si and Ge）Nanometer powder, the appropriate experiment condition by adjusting can reach following index：10 below nm nano-particle accounts for the 90% to 96. 1% of all nano-particles, and 10 more than nm nano-particle accounts for the 3. 9% to 10% of all nano-particles.Also, by adjusting above-mentioned sedimentation time, the ratio of sedimentation time and non-deposited time, stirring speed
The conditions such as degree, the nanometer powder of production can be controlled to meet predetermined index, for example, the nanometer powder of production can be controlled, 10 below nm nano-particle is set to account for 91%, 93% or 96% etc., simultaneously/or 10 more than nm nano-particle is accounted for the 5% of all nano-particles, 6 % or 8 % etc., but it is not limited to this.
Nano-particle manufacture device in the present invention is to employ the physical deposition method of aforementioned list to evaporate nano-particle, in the powder as support (Supporter)（Powder the process of depositing nano particle is formed) or on chip (Chip).The present invention without successional deposition process using controlling the growth of nano-particle, the control size of effective property and the device for producing nanometer powder in enormous quantities of content.
The present invention, by efficient support agitating mode, more enhances the outstanding nanometer powder manufacture device of deposition efficiency and durability using a kind of novel concept compared with existing support agitating mode.The nano-particle manufacture that the present invention is used belong in vacuo formed nano-particle on to formula physics mode nano-particle manufacture method.The nano-particle manufacturing equipment of the present invention employs the support agitating mode of screw type vertical transport mode, realize the minimum of mechanization load, convey support with certain speed and direction, so as to realize to support progress uniform stirring, improve deposition efficiency, so that while producing a certain size nano-particle, the minimum of mechanical load and the load of equipment is realized, the nano-particle manufacture device of equipment durability is enhanced.
The agitating mode of nano-particle manufacture device employs the mode that support powder or chip are conveyed in a vertical manner in the present invention, to minimize the friction between support or between support chip, it is set uniformly to mix, promote the efficiency of manufacture nano-particle and the durability of nano-particle manufacturing equipment, apply to produce in enormous quantities the related invention of equipment.The present invention is the process for also nano material being deposited on Nanoparticle Size using precipitation equipment powder or chip top while in vacuo stirring support powder or chip.
Particular embodiments described above; the purpose of the present invention, technical scheme and beneficial effect are further described; it should be understood that; it the foregoing is only the specific embodiment of the present invention; the protection domain being not intended to limit the present invention; within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc., should be included in the scope of the protection.
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Claims (30)
1. a kind of nanometer powder manufacture device, it is characterised in that the device includes：
Tank diameter, the support for accommodating nano material；
Vertical transport part, in tank diameter, the top for the support to be delivered to tank diameter by screw type rotary from the lower vertical of tank diameter；
Support plate, in tank diameter and vertical transport part top, for supporting the vertical transport to weigh
The support that part conveying comes, the support plate is the low taper in middle high, periphery or taper type；And precipitation equipment, precipitation equipment include sedimentary origin, the sedimentary origin be located at tank diameter in and support plate top, for using physical deposition mode to support deposit nanometer powder.
2. manufacture device according to claim 1, its feature, which is asked, to be, the manufacture device also includes：One or more top rotary wings, on the support plate, for stirring the support on the support plate.
3. manufacture device according to claim 1, it is characterised in that the manufacture device also includes：One or more bottom rotary wings, in the tank diameter, for being stirred to the support in tank diameter.
4. the manufacture device according to Claims 2 or 3, it is characterised in that：The vertical transport part includes：Rotary shaft and the spiral rotating wing being fixed in the rotary shaft.
5. manufacture device according to claim 4, it is characterised in that：The top rotary wings, bottom rotary wings are fixed in the rotary shaft.
6. manufacture device according to claim 1, it is characterised in that：
The top rotary wings are embedded in the support on the support plate.
7. manufacture device according to claim 1, it is characterised in that：
One or more hole is provided with the support plate.
8. manufacture device according to claim 1, it is characterised in that：
The tank diameter is upper coarse and lower fine.
9. manufacture device according to claim 1, it is characterised in that the manufacture device also includes：The heater outside the tank diameter is arranged at, for being heated to the support in tank diameter.
10. manufacture device according to claim 1, it is characterised in that the manufacture device also includes：The cooling device outside the tank diameter is arranged at, for being cooled down to the support in tank diameter.
11. manufacture device according to claim 1, it is characterised in that the manufacture device also includes：Vacuum tank, is arranged at the outside of the sedimentary origin and tank diameter；And
Vavuum pump, for extracting the gas in vacuum tank, to keep inside the vacuum tank as vacuum state.
12. nanometer powder manufacture device according to claim 1, it is characterised in that：
The material of the sedimentary origin includes：At least one of metal, oxide, organic matter, alloy and semiconductor.
13. nanometer powder manufacture device according to claim 12, it is characterised in that：
The metal is gold, silver, platinum, ruthenium, rhodium, palladium, osmium and iridium.
14. nanometer powder manufacture device according to claim 1, it is characterised in that：
The physical deposition mode includes：D.c. sputtering, radio-frequency sputtering, mid frequency sputtering, ion beam sputtering, microwave deposition, the sputtering of double magnetic, heat deposition, electron beam deposition, laser deposition or ion plating.
15.-kind of nanometer powder manufacture method, it is characterised in that this method comprises the following steps：
Load step, for support to be loaded into tank diameter and deposition source material installation is carried out, the tank diameter and sedimentary origin are arranged in the vacuum tank in atmospheric condition；
Vacuum step, the vacuum tank is exhausted using vavuum pump, so that the vacuum tank reaches predetermined vacuum；
Stirring and deposition step, the support is stirred using the agitating mode of screw type vertical transport support, and nanometer powder is deposited to the support in deposition region by physical deposition mode while stirring；
Vacuum in nanometer powder obtaining step, destruction vacuum tank, obtains the nanometer powder being attached on support from the tank diameter.
16. method according to claim 15, it is characterised in that：
The vacuum step also stirs the branch using the agitating mode of screw type vertical transport support
Hold body.
17. method according to claim 15, it is characterised in that：
The stirring and deposition step also include cooling down the support in the tank diameter.
18. method according to claim 15, it is characterised in that：
Also include pre-processing the support before the loading step.
19. method according to claim 15, it is characterised in that：
The physical deposition mode includes：D.c. sputtering, radio-frequency sputtering, mid frequency sputtering, ion beam sputtering, microwave deposition, the sputtering of double magnetic, heat deposition, electron beam deposition, laser deposition or ion plating.
20. method according to claim 15, it is characterised in that：
The deposition source material includes：Metal, oxide, organic matter, alloy or semiconductor.
21. a kind of agitating device manufactured for nanometer powder, it is characterised in that the device includes：Tank diameter, the support for accommodating nano material；
Vertical transport part, in tank diameter, the top for the support to be delivered to tank diameter by screw type rotary from the lower vertical of tank diameter；And
Support plate, in tank diameter and vertical transport part top, for the support for supporting vertical transport part conveying, the support plate is the low taper in middle high, periphery or taper type.
22. agitating device according to claim 21, it is characterised in that the agitating device also includes：One or more top rotary wings, on the support plate, for stirring the support on the support plate.
23. agitating device according to claim 21, it is characterised in that the agitating device also includes：One or more bottom rotary wings, in the tank diameter, for being stirred to the support in tank diameter.
24. the agitating device according to claim 22 or 23, it is characterised in that：
The vertical transport part includes：Rotary shaft and the spiral rotating wing being fixed in the rotary shaft.
25. agitating device according to claim 24, it is characterised in that：
The top rotary wings, bottom rotary wings are fixed in the rotary shaft.
26. agitating device according to claim 21, it is characterised in that：
The top rotary wings are embedded in the support on the support plate.
27. agitating device according to claim 21, it is characterised in that：
One or more hole is provided with the support plate.
28. agitating device according to claim 21, it is characterised in that：
The tank diameter is upper coarse and lower fine.
29. agitating device according to claim 21, it is characterised in that the agitating device also includes:The heater outside the tank diameter is arranged at, for being heated to the support in tank diameter.
30. agitating device according to claim 21, it is characterised in that the agitating device also includes:The cooling device outside the tank diameter is arranged at, for being cooled down to the support in tank diameter.
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| CN2008801254116A CN101925402A (en) | 2008-01-22 | 2008-04-03 | Stirring device, device with said stirring device for producing nanometer powder and its method |
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| CN200810004352 | 2008-01-22 | ||
| CN200810004352.9 | 2008-01-22 | ||
| CN2008801254116A CN101925402A (en) | 2008-01-22 | 2008-04-03 | Stirring device, device with said stirring device for producing nanometer powder and its method |
| PCT/CN2008/070675 WO2009092207A1 (en) | 2008-01-22 | 2008-04-03 | A stirring device, a device with said stirring device for producing nanometer powder and its method |
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| WO (1) | WO2009092207A1 (en) |
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| CN108237478A (en) * | 2016-12-23 | 2018-07-03 | 浙江金徕镀膜有限公司 | Polishing fluid stirs pumping all-in-one machine and polishing machine |
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| WO2012016382A1 (en) * | 2010-08-05 | 2012-02-09 | 大连科林爱纳米科技有限公司 | Metal nanocatalyst and preparation method thereof |
| AT520505A1 (en) * | 2017-10-03 | 2019-04-15 | Franz Goetschl | mixing device |
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| JPS57127431A (en) * | 1981-01-29 | 1982-08-07 | Nitsukuu Kogyo Kk | Vacuum mixing and defoaming machine |
| CN2098963U (en) * | 1990-12-18 | 1992-03-18 | 肖彪 | Multi-function fountain type mixer |
| CN2354647Y (en) * | 1997-12-15 | 1999-12-22 | 南通罗斯混合设备有限公司 | Vertical mixer |
| CN2403493Y (en) * | 1999-07-12 | 2000-11-01 | 王华业 | Spiral cone stirring homogenizer |
| US7090391B2 (en) * | 2002-09-25 | 2006-08-15 | Reika Kogyo Kabushiki Kaisha | Apparatus and method for mixing by agitation in a multichambered mixing apparatus including a pre-agitation mixing chamber |
| JP3620842B2 (en) * | 2002-12-25 | 2005-02-16 | 孝之 阿部 | Polygonal barrel sputtering apparatus, polygonal barrel sputtering method, coated fine particles formed thereby, and method for producing coated fine particles |
| CN1201887C (en) * | 2003-08-20 | 2005-05-18 | 东华大学 | Nano particle surface physicochemical structure cutting and coating method |
| CN101073771A (en) * | 2007-06-21 | 2007-11-21 | 浙江工业大学 | Method for producing nano-carbon tube load platinum catalyst by laser deposition |
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2008
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Cited By (1)
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| CN108237478A (en) * | 2016-12-23 | 2018-07-03 | 浙江金徕镀膜有限公司 | Polishing fluid stirs pumping all-in-one machine and polishing machine |
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