CN1194834C - Equipment with separation and collection structure for continuously preparing nano material - Google Patents
Equipment with separation and collection structure for continuously preparing nano material Download PDFInfo
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- CN1194834C CN1194834C CNB02100692XA CN02100692A CN1194834C CN 1194834 C CN1194834 C CN 1194834C CN B02100692X A CNB02100692X A CN B02100692XA CN 02100692 A CN02100692 A CN 02100692A CN 1194834 C CN1194834 C CN 1194834C
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Abstract
The present invention relates to a nanometer material continuous preparing device with a separating collecting structure, which has a function of composite modulation and belongs to the technical field of the preparation of nanometer materials. The device is composed of more than six mutually communicated pot-shaped vacuum working chambers, a reflux pipeline 7, an air inlet pipeline 8 and a vacuum pump 9, wherein the vacuum working chambers are respectively an electric arc evaporating working chamber 1, a refrigerating working chamber 2, an axial flow fan working chamber 3 and separating working chambers with more than three stages, wherein a magnetic separating device and a high voltage electrostatic corona separating device are arranged in the separating working chamber at each stage. The device can continuously and efficiently produce nanometer materials with multiple varieties and granularity, such as nanometer powder and nanometer articles.
Description
Technical field
The present invention relates to a kind of arc evaporation vapor condensation method nano material continuous preparation device, belong to the nano material preparation technical field with separation and collection structure and complex modulated function.
Background technology
Electric arc steam condensation method is to be evaporated material (metal, alloy, compound) with the high arc temperature heating in the inert gas (argon nitrogen etc.) in low pressure, make it flash to steam and cool off again, make steam become the typical preparation method that the mist attitude becomes the solid nano particle again by gaseous state.Developed by the evaporative condenser process in the pure inert gas by Ryozi UyeAC in 1963 and obtain clean nanoparticle, accumulate on the cooling stick surface, scrape, collect the acquisition nanoparticle with the polytetrafluoroethylene (PTFE) scraper.Since the nineties in 20th century, the method and apparatus for preparing nano powder with electric arc steam condensation method has been declared many patents, as ZL94100768.5, and ZL94218595.1, ZL94218594.3, ZL98114069, ZL94117416, ZL00233180 etc.Some implements these patents and succeeds, but along with developing rapidly of world's nanometer technology, technology of preparing to nano material also proposes more and more higher requirement, require mass as output, kind requires variation, the granularity requirements multipolarity, and require to reduce cost, and above-mentioned patent all can't satisfy these requirements.
Summary of the invention
The nano material continuous preparation device that the purpose of this invention is to provide a kind of arc evaporation vapor condensation with separation and collection structure and complex modulated function.This device can the continuous high-efficient rate the nano material of the multistage granularity of the many kinds of production.
The object of the present invention is achieved like this:
Described device is by the jar shape vacuum workshop that is interconnected more than 6, reflux line, admission line and vavuum pump composition.Described 6 were respectively arc evaporation operating room, refrigeration operating room, axial flow blower operating room, 3 grades of (individual) above sorting work chambers with last vacuum workshop.Described 3 grades of (individual) above sorting work chambers are first order sorting work chamber, sorting work chamber, the second level, third level sorting work chamber, according to the nano particle size requirement, also can set up fourth stage sorting work chamber, level V sorting work chamber etc., be generally 3～5 grades (individual).
Described arc evaporation operating room is a kind of improvement to existing arc evaporation operating room, on the tank skin of arc evaporation operating room, be equipped with feed arrangement, be lifted on the middle arc discharge negative electrode of vacuum chamber and be placed in the water-cooled crucible that bottom splendid attire moving up and down is evaporated material; The bottom of described arc evaporation operating room has the pipeline that is connected with vavuum pump, and its top has vapor outlet port, and the fire door of sealing is equipped with in its front.
Be equipped with in the described refrigeration operating room and be lifted on the middle liquid nitrogen container of vacuum chamber, be contained in the cold scattering piece on the liquid nitrogen container tank skin, the dish valve is installed on the top exit of refrigeration operating room.The bottom of described arc evaporation operating room and refrigeration operating room is by being connected by the pipeline that has the dish valve.
The axial flow blower of adjustable rotating speed is housed in the described axial flow blower operating room, respectively there are a gas outlet and air inlet in both sides, axial flow blower operating room, gas outlet, axial flow blower operating room is connected with the air inlet of refrigeration operating room, and axial flow blower operating room air inlet is connected by the gas outlet of reflux line with afterbody sorting work chamber.
One end of described admission line is connected with the vapor outlet port of arc evaporation operating room, its other end is connected with the air inlet of first order sorting work chamber, wherein have many uniform apertures on the tube wall of a segment pipe at admission line, the outside cover is with vacuum-packed sleeve pipe, and the top exit of refrigeration operating room is connected with this sleeve pipe by the dish valve.
Described vavuum pump is connected with the arc evaporation operating room by pipeline, has the atmosphere charge valve on the pipeline, vacuum table, inert gas charge valve and reacting gas charge valve.
The guide shell group all is equipped with on the top of described sorting works at different levels chamber, and described guide shell group is made up of 7～9 guide shells of going up up/down perforations, and each guide shell is evenly distributed or weld together side by side.Each guide shell group is lifted on the sorting work locular wall by the insulation sleeve insulation; Magnetic force sorting unit and/or high-pressure electrostatic corona sorting unit are housed in every grade of sorting operating room (promptly magnetic force sorting unit or high-pressure electrostatic corona sorting unit can be installed in that every grade of sorting is indoor separately, perhaps the collocation of magnetic force sorting unit and high-pressure electrostatic corona sorting unit is installed and used, and magnetic force sorting unit and high-pressure electrostatic corona sorting unit also can be installed simultaneously).The top of every grade of sorting operating room all has air inlet and gas outlet, the air inlet of first order sorting work chamber is connected by the vapor outlet port of admission line with the arc evaporation operating room, the gas outlet of first order sorting work chamber is connected by pipeline with the air inlet of sorting work chamber, the second level, the gas outlet of sorting work chamber, the second level is connected by pipeline with the air inlet of next stage sorting work chamber, the gas outlet of next stage sorting work chamber is connected by pipeline with the air inlet of its next stage sorting work chamber again, be connected step by step in this way, and the gas outlet of afterbody sorting work chamber is connected with reflux line.The bottom of every grade of sorting operating room is a hopper, and the lower end of hopper is equipped with the dish valve, and the bottom of dish valve connects a blanking barrel, the lower end of each blanking barrel and a drawing mechanism sealed attachment.
Described magnetic force sorting unit is tapered collision to be housed respectively in guide shell group bottom collect metal plate, leaves the gap between the outer rim that metal plate is collected in tapered collision and the tank skin of sorting work chamber, place, and each taper is collided and all is equipped with electromagnet N respectively below metal plate; Outer electronic vibrator is installed on each hopper outer wall.
Described high-pressure electrostatic corona sorting unit is corona wire of hanging on the axis of each guide shell of described guide shell group, the cathode and the high-voltage conducting wires that have 4～16kv high direct voltage are in parallel, described high-voltage conducting wires enters sorting works at different levels chamber from the High-Voltage Insulation enclosed electrode at each top, sorting work chamber, links with the corona wire at the central axis place of each guide shell in each guide shell group that dangles.The ceramic weight that makes its maintenance plumbness prevent short circuit in the hanging of the bottom of corona wire, an electronic vibrator 43 is installed in the outside of a certain water conservancy diversion barrel in each guide shell group, and the variable resistance R of a vacuum seal insulating joint and ground connection is arranged in the bottom of every grade of sorting operating room.
Described vavuum pump vacuumizes and is charging into noble gas after the termination of pumping in each vacuum chamber, axial flow blower in the axial flow blower operating room flows the inert gas that charges into by reflux line continuously and stably, the arc evaporation operating room will need substances processed to evaporate, becoming high-temperature gas mixture flows to into admission line, after meeting with the cooling blast that enters admission line by the refrigeration operating room, the steam that is evaporated material is by the mist formation attitude of condensing rapidly, and then be frozen into nano particle, enter the refinement step by step of sorting works at different levels chamber then, obtain meeting the nanometer powder of granularity requirements.
Description of drawings
Below in conjunction with accompanying drawing the present invention is described in detail:
Fig. 1 is the general structure schematic diagram that the present invention has the nano material continuous preparation device of three grades of sorting operating rooms;
Fig. 2 is that the particle collision of this device adheres to the grading principle schematic diagram;
Fig. 3 is the high-pressure electrostatic separation chamber structure and the principle schematic of this device;
Fig. 4 is the corona field movement of particles schematic diagram of this device;
Fig. 5 is the A-A cutaway view of Fig. 4;
Fig. 6 is the outer water-cooled arc electrodes structural representation of this device;
Fig. 7 is the internal water cooling arc electrodes structural representation of this device;
Fig. 8 is the crucible of this a device position view in parallel;
Fig. 9 is the crucible bush structure schematic diagram of this device;
Figure 10 is the continuous feed apparatus structure schematic diagram of this device;
Figure 11 is the drawing mechanism structural representation of this device;
Figure 12 is the B-B cutaway view of Figure 11.
Among the figure: 1-arc evaporation operating room, 2-refrigeration operating room, 3-axial flow blower operating room, 4-first order sorting work chamber, sorting work chamber, the 5-second level, 6-third level sorting work chamber, the 7-reflux line, the 8-admission line, the 9-vavuum pump, the 10-feed arrangement, the 11-aperture, the 12-sleeve pipe, 13-is evaporated material, 14-arc discharge negative electrode, 15-water-cooled crucible, 16,17,21-dish valve, the 18-cold scattering piece, 19-liquid nitrogen container, 20-axial flow blower, the 22-drawing mechanism, 23-refrigeration operating room air inlet, 24-axial flow blower operating room air inlet, 25-arc evaporation operating room vapor outlet port, 26-refrigeration operating room top exit, 27-first order sorting work chamber guide shell group, metal plate, sorting work chamber, 29-second level guide shell group are collected in the tapered collision in 28-first order sorting work chamber, metal plate is collected in the tapered collision in sorting work chamber, the 30-second level, 31-third level sorting work chamber guide shell group, metal plate, 33 are collected in the tapered collision in 32-third level sorting work chamber, 48, the 49-high-voltage conducting wires, 34-High-Voltage Insulation enclosed electrode, 37-pottery weight, 41-corona wire, 42-guide shell, electronic vibrator in the 43-, 44-vacuum seal insulating joint, 45-insulation sleeve, 46-high direct voltage cathode, the outer water collar of 50-, the outer water collar water inlet of 51-, the outer water collar delivery port of 52-, 53-internal water cooling arc electrodes water inlet, 54-internal water cooling arc electrodes delivery port, the 55-pipeline, 56-vent valve, 57-vacuum table, 58-inert gas charge valve, 59-reacting gas charge valve, 60-arc evaporation operating room sealing door, 62-water-cooled crucible lining, 63-is sealed into bin gate, 64-is evaporated material, 65-T shape feeding slide plate, the wounded in the battle key of 66-close the envelope turning cylinder, the 67-vent valve, 69-inserts metal plate valve, 70-feed arrangement barrel, 71-vavuum pump, the 72-vacuum table, 73-noble gas charge valve, 74-cylindrical box, 75-gloves hole, the 77-observation window, the outer electronic vibrator of 79-, 80-discharging chamber door, 81-hopper, the 82-blanking barrel, 83-gloves port lid, the flat metal plate of 85-pedestal, 86-dish valve, 87-noble gas charge valve, 89-vent valve, 90-vacuum table, the 91-container that connects material; The 92-cylinder, 93-vavuum pump, 101-separation chamber 4 air inlets, 102-separation chamber 5 air inlets, 103-separation chamber 6 air inlets, 104-separation chamber 4 gas outlets, 105-separation chamber 5 gas outlets, 106-separation chamber 6 gas outlets.
The specific embodiment
In Fig. 1, the present invention is made up of 6 the pot type vacuum workshop that are interconnected, reflux line 7, admission line 8 and vavuum pumps 9.Described 6 vacuum workshop are respectively arc evaporation operating room 1, refrigeration operating room 2, axial flow blower operating room 3, first order sorting work chamber 4, sorting work chamber, the second level 5, third level sorting work chamber 6.
Described arc evaporation operating room 1 is a kind of improvement to existing arc evaporation operating room, on arc evaporation operating room 1 tank skin, be equipped with feed arrangement 10, be lifted on the middle arc discharge negative electrode 14 of vacuum chamber and be placed in the water-cooled crucible 15 that bottom splendid attire moving up and down is evaporated material 13; The bottom of described arc evaporation operating room 1 has the pipeline 55 that is connected with vavuum pump 9, and its top has vapor outlet port 25, and the fire door 60 of sealing is equipped with in its front.
Have in the described refrigeration operating room 2 to be lifted on the middle liquid nitrogen container 19 of vacuum chamber, be contained in the cold scattering piece 18 on liquid nitrogen container 19 tank skins, on refrigeration operating room 2 top exits 26, dish valve 17 is installed.
The bottom of described arc evaporation operating room 1 and refrigeration operating room 2 is connected by pipeline, is equipped with dish valve 16 on the pipeline.
Described separation chamber 4,5,6 is same structure, on the top of each sorting work chamber guide shell group 27,29 and 31 is housed respectively.Described guide shell group 27,29 and 31 is made up of the guide shell 42 of 2,2 and 4 up/down perforations respectively, and above-mentioned guide shell welds together side by side, and each guide shell group is lifted on the sorting locular wall by insulation sleeve 45 insulation; Top one side of described separation chamber 4,5,6 has air inlet 101,102 and 103, and its opposite side has gas outlet 104,105 and 106.The air inlet 101 of first order sorting work chamber 4 is connected with admission line 8, the air inlet 102 of the gas outlet 104 of first order sorting work chamber 4 and sorting work chamber, the second level 5 is connected by pipeline, the air inlet 103 of the gas outlet 105 of sorting work chamber, the second level 5 and third level sorting work chamber 6 is connected by pipeline, and the gas outlet 106 of third level sorting work chamber 6 is connected with reflux line 7.Set up the above sorting work of fourth stage chamber as need, the gas outlet of third level sorting work chamber 6 is connected by pipeline with the air inlet of fourth stage sorting work chamber at this moment, the gas outlet of fourth stage sorting work chamber is connected by pipeline with the air inlet of next stage sorting work chamber, and the gas outlet of afterbody sorting work chamber is connected with reflux line 7.The bottom of described separation chamber 4,5,6 is a hopper 81, and the lower end of hopper 81 is equipped with dish valve 21, and the bottom of dish valve 21 connects a blanking barrel 82, the lower end of each blanking barrel 82 and a drawing mechanism 22 sealed attachment.Magnetic force sorting unit and high-pressure electrostatic corona sorting unit all are installed in each separation chamber 4,5,6 simultaneously.
As shown in Figure 2, described magnetic force sorting unit is in guide shell group 27,29 and 31 bottoms tapered collision collection metal plate 28,30 and 32 to be housed respectively, leave the gap between the outer rim that metal plate is collected in tapered collision and the tank skin of sorting work chamber, place, each taper is collided and is equipped with electromagnet N respectively below metal plate
1, N
2, N
3Outer electronic vibrator 79 is installed on each hopper 81 outer wall.
Shown in Fig. 1,3, described high-pressure electrostatic corona sorting unit is corona wire 41 of hanging on the axis of each guide shell 42 of described guide shell group 27,29 and 31, cathode 46 and three high-voltage conducting wires 33,48,49 of having 4～16kv high direct voltage are in parallel, high-voltage conducting wires 33,48,49 enters sorting works at different levels chamber 4,5,6 from the High-Voltage Insulation enclosed electrode 34 at each top, sorting work chamber, links with the corona wire 41 at the central axis place of each guide shell 42 in each guide shell group that dangles.The ceramic weight 37 that makes its maintenance plumbness prevent short circuit in the hanging of the bottom of corona wire 41, an electronic vibrator 43 is installed in the outside of a water conservancy diversion barrel in each guide shell group 27,29,31, and the variable resistance R of a vacuum seal insulating joint 44 and ground connection is arranged in the bottom of every grade of sorting operating room.
As shown in Figure 3, be that example is introduced its structure with the three grades of sorting operating rooms 4,5,6 that have high-pressure electrostatic corona sorting unit below: the guide shell group 27 of described first order sorting work chamber 4 has two guide shells 42, high-voltage conducting wires 33 enters first order sorting work chamber 4 from High-Voltage Insulation enclosed electrode 34, with two to dangle at diameter be D
0The corona wire 41 at central axis place of guide shell 42 be in parallel.Ceramic weight 37 in the difference hanging in the bottom of two corona wires 41.Electronic vibrator 43 in the outside of the barrel of a guide shell 42 is installed one.The length of the guide shell 42 of described sorting work chamber 4 is L
1The guide shell group 29 of sorting work chamber, the described second level 5 also has two guide shells 42, and a corona wire 41 is all being hung at each guide shell center from above, its guide shell length L
2=2L
1The guide shell group 31 of described third level electrostatic separation operating room 6 is provided with four guide shells 42 of lifting side by side, and each guide shell center is all being hung a corona wire 41, the length L of its guide shell from above
3=L
2Except that the length of guide shell with quantity is different, other structure of sorting work chamber 5,6 is identical with first order electrostatic separation operating room 4 structures.
Magnetic force sorting unit or high-pressure electrostatic corona sorting unit can be installed separately in each separation chamber, and perhaps the collocation of magnetic force sorting unit and high-pressure electrostatic corona sorting unit is installed and used, and magnetic force sorting unit and high-pressure electrostatic corona sorting unit also can be installed simultaneously.It is high more that sharpness of separation requires, then the progression i that is provided with of sorting work chamber just require many more, general i=3～5.The critical condition that each guide shell 42 in every grade of sorting operating room possesses the sorting effect is v
Ri〉=(D
0/ 2L
i) v
Yi, wherein: v
RiWith v
YiBe respectively the radial motion speed and the axial velocity of suspended particulate on the vertical section of i level sorting operating room guide shell 42; D
0Diameter for guide shell 42 is generally 200～300mm; L
iBe the length of i level sorting operating room guide shell 42, general L
2=2L
1=L
3=L
4=L
5At v
RiAnd D
0Having become will satisfy under the prerequisite of definite value above-mentioned critical condition has only the length that increases this grade guide shell and reduces the flow velocity v of aerosol in guide shell
YiValue; Suppose U
0For entering the aerocolloidal flow velocity in this grade sorting operating room, n
iBe the radical of every group of guide shell in parallel, then v
Yi=U
0/ n
i, obviously reduce v step by step
YiMust increase n
iValue, thus make the overstriking of this grade separation chamber, general n
1=2～7, n
2=2n
1, n
3=2n
2, n
4=1.5n
3, n
5=1.5n
4
The axial flow blower 20 of adjustable rotating speed is housed in the described axial flow blower operating room 3, respectively there are a gas outlet and air inlet in 3 both sides, axial flow blower operating room, gas outlet, axial flow blower operating room is connected with the air inlet 23 of refrigeration operating room 2, and axial flow blower operating room air inlet 24 is connected by the gas outlet 106 of reflux line 7 with third level sorting work chamber 6.
One end of described admission line 8 is connected with the vapor outlet port 25 of arc evaporation operating room 1, its other end is connected with the air inlet 101 of first order sorting work chamber 4, have many uniform apertures 11 on the tube wall of the AB section of admission line 8, the outside cover is with vacuum-packed sleeve pipe 12, and the top exit 26 of refrigeration operating room 2 is connected with sleeve pipe 12 by dish valve 17.
Described vavuum pump 9 is connected with arc evaporation operating room 1 by pipeline 55, has vent valve 56, vacuum table 57, inert gas charge valve 58 and reacting gas charge valve 59 on the pipeline 55.
As shown in figure 10, described feed arrangement (10) tilts to be installed on arc evaporation operating room 1 tank skin slanted angle α
1Be the central axis of feed arrangement (10) and the angle of horizontal plane, this slanted angle α
1Be 25～45 degree, its best angle is 30 degree, by being sealed into bin gate 63, barrel 70, be responsible for being communicated with feed arrangement and the slotting metal plate valve 69 that evaporates the operating room, T shape feeding slide plate 65, the closing of wounded in the battle key that is inserted on the barrel 70 sealed turning cylinder 66, be installed in the vent valve 67 on barrel 70 outer walls, vacuum table 72, noble gas charge valve 73 and vavuum pump 71 constitute.The part of described turning cylinder 66 wounded in the battle keys is positioned within the barrel 70, and this two ends are that bearing stretches out barrel 70 outsides to close sealing of hole, can manually shake; The middle bottom of described T shape feeding slide plate 65 is connected with spline turning cylinder 66, and can rotate with it, lays the material 64 that will evaporate on the T shape feeding slide plate 65.Its course of work is: charging for the first time can utilize the sealing door 60 of arc evaporation operating room 1 to carry out, when whole system brings into operation, the material 13 that is evaporated in the crucible 15 soon evaporates when needing continuous feed, shut this moment and insert metal plate valve 69, put into atmosphere by vent valve 67, open feeding gate 63, material 64 is contained on the feeding slide plate 65, shut feeding gate 63, vacuumize with vavuum pump 71, charge into inert gas by noble gas charge valve 73, its dividing potential drop is controlled by vacuum table 72, and it is equated with pressure in the arc evaporation operating room 1.Open then and insert metal plate valve 69, rotate spline turning cylinder 66 and make feeding slide plate 65 rotate α angle, α＞α
1, make material 64 rise to 68 places, position, slide and fall into the water-cooled crucible 15 of arc evaporation operating room 1 along the feeding slide plate.Then feeding slide plate 65 is gone back to original position, shut and insert metal plate valve 69, finish a charging, the still production run continuously of whole system this moment.Charging next time repeats above-mentioned action again.
As shown in Figure 1, be installed in the arc discharge negative electrode 14 in the middle of the arc evaporation operating room 1 and be placed in the water-cooled crucible 15 that bottom splendid attire moving up and down is evaporated material 13.Arc discharge negative electrode 14 is positioned at directly over the water-cooled crucible 15.In Fig. 6, the arc discharge negative electrode of being made by tungsten or tantalum 14 is arranged in the outer cold water jacket 50 that red copper is made, and both closely cooperate, and have water inlet 51 and delivery port 52 on the outer water collar 50, and its underpart is the actual measurement thermoisopleth in arc district.In Fig. 7, described arc discharge negative electrode 14 is an internal water cooling arc electrodes, and the arc discharge negative electrode 14 by the tungsten or the tantalum of cavity are made has water inlet 53 and delivery port 54 in it.In Fig. 9, a circular cone lining 62 of being made by conduction refractory is installed in the inside of water-cooled crucible 15 of the present invention, to play the effect of heat-insulation and heat-preservation economize on electricity, is convenient to simultaneously change, and improves the life-span of metal crucible.According to production requirement, more than one arc discharge negative electrode 14 and water-cooled crucible 15 can be installed in arc evaporation operating room 1, so that melting simultaneously and the multiple material that is evaporated of evaporation, each arc discharge negative electrode 14 respectively has independent power supply, electric current can be adjusted separately.Fig. 8 is four crucibles arranged side by side 15 and hangs arc discharge negative electrode 14 schematic diagrames above crucible from above.The course of work of described arc discharge negative electrode 14 and crucible 15 is common direct-current arc welding principle.
In Figure 11 and 12, described drawing mechanism 22 is a cylindrical box 74, on the barrel surface of cylindrical box 74, have two gloves holes 75, be equipped with gloves port lid 83 on the gloves hole 75, be arranged in 75 tops, two gloves holes and have observation window 77, be positioned at drawing mechanism 22 1 sides and have discharging chamber door 80, in casing 74, have one to be used to lay the flat metal plate 85 of pedestal of container 91 of connecting material; One down cylinder 92 is arranged in the bottom of casing 74, have a dishful of valve 86 that it is divided into two sections in the middle of the cylinder 92, its hypomere is equipped with vacuum table 90, vent valve 89, noble gas charge valve 87 respectively, and the bottom of cylinder 92 is connected with vavuum pump 93.Casing 74 tops are separation chamber's blanking barrel 82, the lower end of blanking barrel 82 put in casing 74 and with its sealed attachment together.Its course of work is: when apparatus of the present invention ordinary production, described dish valve 21 is in open mode, and the inner space of drawing mechanism 22 is full of inert gas.Make powder fall into the container 91 that connects material by vibrator 79 rappings via blanking barrel 82, can manual weighing and pack by gloves hole 75, and observe by observation window 77.When reaching some, the sealed packing of powder carries out discharging, shut dish valve 21 this moment, open dish valve 86 and vent valve 89 is put into atmosphere, open discharging chamber door 80, take out the packing powder, shut discharging chamber door 80 and gloves port lid 83 then, start vavuum pump 93 and begin to vacuumize, charge into inert gas, charge into the inert gas of regulation dividing potential drop by vacuum table 90 controls by noble gas charge valve 87, open dish valve 21 at last drawing mechanism 22 is communicated with the sorting work chamber, and can continue blanking.Above-mentioned entire work process all is to carry out under not stopping production situation.
The course of work of the nano material continuous preparation device of described band separation and collection structure is as follows:
Evaporated material 13 is placed in the water-cooled crucible 15 of arc evaporation operating room 1, open dish valves all in the described continuous preparation device and push-pull valve valve, close gloves port lid 83 and all hermatic doors, vacuumize opening vavuum pump 9 after the whole vacuum chamber UNICOM, reach termination of pumping after the vacuum of technological requirement.By the vacuum table 57 on the vacuum-pump line 55, control inert gas charge valve 58 charges into noble gas in vacuum chamber then.Start axial flow blower 20 and make the inert gas flows that charges into.After air-flow enters refrigeration operating room 2 from a point of axial flow blower operating room 3, air-flow is divided into two-way: the air communication of c direction is crossed dish valve 16 and is entered arc evaporation operating room 1, and heating and sneak into the high-temperature vapour that is evaporated material 13 through the high arc temperature district forms the high-temperature gas mixture stream c that makes progress
1, enter admission line 8; The air-flow of b direction all through obtain behind liquid nitrogen container 19 and the cold scattering piece 18 cooling after, cooling blast b
1Process dish valve 17, sleeve pipe 12 and some apertures 11 enter the AB section in the described admission line 8, with high-temperature gas mixture stream c
1Meet.At this moment, evenly be blended in high-temperature gas mixture stream c
1In the steam that is evaporated material 13 by the mist formation attitude of condensing rapidly, and then be frozen into nano particle.This process is vapor condensation.Compare with the condensation of any cold-trap surface heat transfer, its characteristics are exactly that heat energy transmits the form of direct collision between the cryogenic gas molecule with the high-temperature gas molecule comprehensively fast, realize comprehensive chilling deep cooling.Make the rapid refinement of the nanoparticle that is obtained, the scope of size distribution is narrow.Can regulate and control high-temperature gas mixture stream c by adjusting dish valve 16 and 17 open angles
1With cooling blast b
1Flow proportional, and then reach the degree of modulation nano particle refinement.Realize modulation function of the present invention.Aerosol (Aerosol) is solid phase or the suspended substance of liquid-phase particle in gas.Obviously, be exactly aerosol by the later air-flow e in AB district.Below with the first order sorting work chamber 4 among Fig. 1, sorting work chamber, the second level 5, third level sorting work chamber 6, zoom into Fig. 2.So that grading principle is described." ⊙ " represents thick sized particles among the figure, " zero " expression medium size particle, and " ● " represents thin sized particles.When aerosol e through admission line 8 when the air inlet 101 of first order sorting work chamber 4 becomes that aerosol f flows into first order sorting work chamber 4 and flow downward along guide shell groups 27, arrive the turning of the streamline of arrow demonstration, the attraction in gravity, air-flow motive force, centrifugal force and magnetic field that coarse granule ⊙ is suffered is all bigger, thus coarse granule ⊙ with regard to the track that at first broken away from streamline, collide on the rough surface of taper collision metal plate 28 and adhered to sorting.Medium grain zero and fine grained ● just do not adhered to form aerosol f
1Air inlet 102 through the gas outlet 104 of first order sorting work chamber 4 and sorting work chamber, the second level 5 enters sorting work chamber, the second level 5, along guide shell group 29 flow down to taper collision metal plate 30 and wraparound upwards, be suspended in aerosol f this moment
1In medium grain zero will be collided the sorting that the surface adheres to of metal plate 30 by taper; Remaining aerosol f
2In the fine grained that also suspending ●.Enter third level sorting work chamber 6 through the gas outlet 105 of sorting work chamber, the second level 5 and the air inlet 103 of third level sorting work chamber 6, along guide shell group 31 flow down to taper collision metal plate 32 and wraparound upwards, be suspended in aerosol f this moment
2In fine grained ● will be collided the sorting that the surface adheres to of metal plate 32 by taper.If remain in aerosol f
3In also have thinner particle to need separation and collection, the progression that then can suitably increase sorting promptly increases the sorting work chamber.For magnetic or weak magnetic-particle, the present invention has installed electromagnet N respectively below taper collision metal plate 28,30,32
1, N
2, N
3, electromagnet is very effective for sorting.Because the magnetic field intensity of electromagnet and the number of turn structure of electromagnet and wherein electric current be directly proportional, and identical magnetic field intensity is just big, just little to the granule attraction to the bulky grain attraction.Just can choose the particle of respective diameters scope like this with the method for the number of turn structural class of adjusting electric current I and electromagnet.When electric current I being adjusted to when making electromagnetic force be enough to adsorb the thinnest particle, collection efficiency can be near 100%, when each taper collision metal plate 28,30,32 powder layers that adhered to reach certain thickness, the power supply of turning off electromagnet makes I=0, with corresponding vibrator 79 rappings, powder can be fallen into corresponding drawing mechanism 22.
Experiment shows that it is difficult more that particle segments the choosing collection more.Magnetic force sorting function provided by the present invention only limits to magnetic and weak magnetic-particle.For a large amount of nonmagnetic substances, the present invention also provides a kind of sorting work chamber 4,5,6 that has high-pressure electrostatic corona sorting unit.As shown in Figure 3, become aerosol f with flow velocity U through admission line 8 from the air inlet 101 of first order sorting work chamber 4 as aerosol e
0When entering first order sorting work chamber 4, will be respectively with flow velocity U
0/ 2 enter the corona discharge region in the middle of two guide shells 42, and coarse granule ⊙ will be pushed to the inwall of guide shell 42 by the Coulomb force of corona field, and are adhered to sorting; Medium grain zero and fine grained ● just do not adhered to form aerosol f
1Through the air inlet 102 of the gas outlet 104 of first order sorting work chamber 4 and sorting work chamber, the second level 5 with flow velocity U
0Enter sorting work chamber, the second level 5, will be respectively with flow velocity U
0/ 2 enter the corona discharge region in the middle of two guide shells 42, and medium grain zero will be pushed to the inwall of guide shell 42 by the Coulomb force of corona field, and are adhered to sorting; Remaining aerosol f
2In the fine grained that also suspending ●, through the air inlet 103 of the gas outlet 105 of sorting work chamber, the second level 5 and third level sorting work chamber 6 with flow velocity U
0Enter third level sorting work chamber 6, will be respectively with flow velocity U
0/ 4 enter the corona discharge region in the middle of four guide shells 42, fine grained ● will be pushed to the inwall of guide shell 42 by the Coulomb force of corona field, and adhered to sorting.If remain in aerosol f
3In also have thinner particle to need separation and collection, the progression that then can suitably increase sorting promptly increases the sorting work chamber.Each guide shell 42 inner surface all is a collection surface.When adhering to certain thickness powder, the electronic vibrator of installing with the guide shell 42 barrels outside 43 carries out rapping, powder can be fallen into corresponding drawing mechanism 22.
Describe the grain sorting process in three electrostatic separation operating rooms below in detail:
Fig. 4 is with a guide shell 42 in the first order electrostatic separation operating room 4 among Fig. 3 and hangs the enlarged drawing of a corona wire 41 on center line from above.4a is illustrated in the distribution curve of electric field strength E in the corona field (kv/cm) along radius r (cm) among the figure; 4b represents the axially-movable speed v of suspended particulate on the vertical section of guide shell 42
yWith radial velocity v
rThe vector composite diagram.The negative electrical charge that coarse granule ⊙ obtains in the negative corona discharge district is many, and it just is subjected to, and radially coulomb repulsion power is just big in the electric field, the radial velocity v that is obtained
R1Just big, arrive the below endpoint location d of guide shell 42
3The time, relational expression v
R1=(D
0/ 2L
1) v
ySet up, work as v
R1〉=(D
0/ 2L
1) v
y, pairing all particle position d
2, d
1Coarse granule ⊙ all can adhere to the inner surface of guide shell 42.And than its thinner particle d
4To flow through from guide shell 42, in next stage separation chamber.The next stage sorting is still undertaken by said process.
As shown in Figure 3, the variable resistance R of a vacuum seal insulating joint 44 and ground connection is arranged in the bottom of every grade of electrostatic separation operating room, its effect is exactly to make all instant earthings of the negative electrical charge of guide shell acquisition.Make guide shell still keep certain negative potential, make the particle that sticks to inner surface also keep certain negative potential, still be subjected to the repulsive interaction of certain Coulomb force, it is unlikely knock-on takes place and suspends once more and accumulate in reliably on the inner surface that guide shell is a surge drum, so that the rapping blanking.
High-pressure electrostatic corona sorting unit proposed by the invention has following characteristics: 1, the nano particle to any material can carry out high-accuracy high-efficiency rate separation and collection; 2, the voltage of high-voltage electrostatic power is high more, helps improving sharpness of separation and collection efficiency more.High-pressure electrostatic voltage industrialization higher limit is 14KVA at present.
Below complex function of the present invention is illustrated:
Continuous preparation device proposed by the invention can not only prepare the nanometer powder of many kinds, and nanometer goods that can the many kinds of compound preparation: nanotube, receive and be silk, nanometer film and nanometer piece.It is compound to carry out physics, and can carry out chemically composited.
Chemically composited being achieved in that opened reacting gas charge valve 59 shown in Figure 1, in inert gas, charge into quantitative reacting gas (as oxygen, nitrogen etc.), mix mutually with the high-temperature vapour that is evaporated material and chemical reaction takes place, the aerosol that can become this compound after the condensation carries out separation and collection.
Compound being achieved in that of the physics of CNT is changed to graphite bars with arc discharge negative electrode 14, and the graphite block of packing in water-cooled crucible 15 promptly generates CNT after beating arc by technological requirement, carries out separation and collection.
In the compound inert atmosphere that is achieved in that in drawing mechanism 22 of nano wire, rod, film, utilize the nano particle that is suspended in the inert gas aerosol to be raw material, can synthesize multiple nano wire, rod, film with template technology.
In the compound inert gas atmosphere that is achieved in that in drawing mechanism 22 of nanometer piece, the artificial sealing gloves that utilize are operated.The nanometer powder of having collected or the nanometer powder dismounting of packing in advance weighed pack among the mould of packing in advance, then with tin paper bag with the die package that assembles.Close dish valve 21, open dish valve 86, put into atmosphere, open chamber door 80, take out the mould bag of encapsulation with vent valve 89.Send in the vacuum heating-press sintering stove, exhaust vacuum, charge into noble gas, open the encapsulation bag with manually-operated and take out the mould of assembling, the sintering station of packing into, vacuum heating-press sintering becomes piece.
The present invention has following advantage:
The nano powder that 1, can prepare many kinds as by changing crucible lining 62, carries out purified rinse water to the full device inner surface, just can change the kind that is evaporated material;
2, can prepare other nanometer powder of many particle size fractions;
3, because the present invention has charging and drawing mechanism, but therefore continuous feed and discharging, thus enhance productivity;
4, has the compound and compound function of physics of aerosol chemistry.
Claims (7)
1, a kind of nano material continuous preparation device with separation and collection structure is characterized in that described device is made up of the jar shape vacuum workshop, reflux line (7), admission line (8) and the vavuum pump (9) that are interconnected more than 6; Described 6 were respectively arc evaporation operating room (1), refrigeration operating room (2), axial flow blower operating room (3), sorting work chamber more than 3 grades with last vacuum workshop; On the tank skin of described arc evaporation operating room (1), be equipped with feed arrangement (10), be lifted on the middle arc discharge negative electrode (14) in arc evaporation operating room and be placed in the water-cooled crucible (15) that bottom splendid attire moving up and down is evaporated material (13), the bottom of described arc evaporation operating room (1) has the pipeline (55) that is connected with vavuum pump (9), its top has vapor outlet port (25), and the fire door (60) of sealing is equipped with in its front; Be equipped with in the described refrigeration operating room (2) and be lifted on the middle liquid nitrogen container (19) of vacuum chamber, be contained in the cold scattering piece (18) on liquid nitrogen container (19) tank skin, dish valve (17) is installed on refrigeration operating room (2) top exit (26); The bottom of described arc evaporation operating room (1) and refrigeration operating room (2) is connected by the pipeline that has dish valve (16); The axial flow blower (20) of adjustable rotating speed is housed in the described axial flow blower operating room (3), respectively there are a gas outlet and air inlet (24) in both sides, axial flow blower operating room (3), the gas outlet of axial flow blower operating room (3) is connected with the air inlet (23) of refrigeration operating room (2), and axial flow blower operating room air inlet (24) is connected by the gas outlet of reflux line (7) with afterbody sorting work chamber; One end of described admission line (8) is connected with the vapor outlet port (25) of arc evaporation operating room (1), its other end is connected with the air inlet of first order sorting work chamber, have many uniform apertures (11) on the tube wall of the centre one section (AB) of admission line (8), the outside cover is with vacuum-packed sleeve pipe (12), and the top exit (26) of described refrigeration operating room (2) is connected with sleeve pipe (12) by dish valve (17); Described vavuum pump (9) is connected with arc evaporation operating room (1) by pipeline (55), has vent valve (56), vacuum table (57), inert gas charge valve (58) and reacting gas charge valve (59) on the pipeline (55); The guide shell group all is equipped with on the top of described sorting works at different levels chamber, each guide shell group is lifted on the sorting locular wall by insulation sleeve (45) insulation, described guide shell group is made up of the guide shell (42) of 7～9 up/down perforations, each guide shell is evenly distributed or weld together side by side, magnetic force sorting unit and/or high-pressure electrostatic corona sorting unit are housed in every grade of sorting operating room, the top of every grade of sorting operating room all has air inlet and gas outlet, the air inlet of first order sorting work chamber is connected with the vapor outlet port (25) of arc evaporation operating room by admission line (8), the gas outlet of first order sorting work chamber is connected by pipeline with the air inlet of sorting work chamber, the second level, the gas outlet of sorting work chamber, the second level is connected by pipeline with the air inlet of next stage sorting work chamber, the gas outlet of next stage sorting work chamber is connected by pipeline with the air inlet of its next stage sorting work chamber again, be connected step by step, and the gas outlet of afterbody sorting work chamber is connected with reflux line (7), the bottom of every grade of sorting operating room is a hopper (81), the lower end of hopper (81) is equipped with dish valve (21), the bottom of dish valve (21) connects a blanking barrel (82), lower end of each blanking barrel (82) and a drawing mechanism (22) sealed attachment; Described magnetic force sorting unit is tapered collision to be housed respectively in each guide shell group bottom collect metal plate, leave the gap between the outer rim of described tapered collision collection metal plate and the tank skin of sorting work chamber, place, be equipped with electromagnet (N) respectively below each taper collision metal plate, outer electronic vibrator (79) is installed on each hopper (81) outer wall; A corona wire of hanging (41) on the axis that described high-pressure electrostatic corona sorting unit is each guide shell (42) in described guide shell group, the cathode (46) that has 4～16kv high direct voltage links with high-voltage conducting wires, high-voltage conducting wires enters sorting works at different levels chamber from the High-Voltage Insulation enclosed electrode (34) at each top, sorting work chamber, link with the corona wire (41) at the central axis place of each guide shell (42) in each guide shell group that dangles, the ceramic weight (37) that makes its maintenance plumbness prevent short circuit in the bottom hanging of corona wire (41), an electronic vibrator (43) is installed in the outside of a certain water conservancy diversion barrel in each guide shell group, and the variable resistance (R) of a vacuum seal insulating joint (44) and ground connection is arranged in the bottom of every grade of sorting operating room.
2, the nano material continuous preparation device of band separation and collection structure as claimed in claim 1 is characterized in that described feed arrangement (10) tilts to be installed on arc evaporation operating room 1 tank skin slanted angle (α
1) be the central axis of feed arrangement (10) and the angle of horizontal plane, this slanted angle (α
1) be 25～45 degree, described feed arrangement (10) by be sealed into bin gate (63), barrel (70), be responsible for being communicated with feed arrangement and evaporation operating room slotting metal plate valve (69), T shape feeding slide plate (65), be inserted into closing envelope turning cylinder (66), being installed in vent valve (67), vacuum table (72), noble gas charge valve (73) and vavuum pump (71) formation on barrel (70) outer wall of wounded in the battle key on the barrel (70); Described part of closing the wounded in the battle key of envelope turning cylinder (66) is positioned within the barrel (70), and this two ends are that bearing stretches out barrel (70) outside to close sealing of hole; The middle bottom of described T shape feeding slide plate (65) is connected with spline turning cylinder (66), and can rotate with it, lays the material (64) that will evaporate on the T shape feeding slide plate (65).
3, the nano material continuous preparation device of band separation and collection structure as claimed in claim 1, it is characterized in that described arc discharge negative electrode (14) is positioned at directly over the water-cooled crucible (15), the arc discharge negative electrode of being made by tungsten or tantalum (14) is arranged in the outer water collar (50) that red copper is made, both closely cooperate, and have water inlet (51) and delivery port (52) on the outer water collar (50).
4, the nano material continuous preparation device of band separation and collection structure as claimed in claim 3, it is characterized in that described arc discharge negative electrode (14) is positioned at directly over the water-cooled crucible (15), arc discharge negative electrode (14) is an internal water cooling arc electrodes, tungsten or tantalum by cavity are made, and have water inlet (53) and delivery port (54) in it.
5, the nano material continuous preparation device of band separation and collection structure as claimed in claim 1 is characterized in that a circular cone lining (62) of being made by conduction refractory is installed in the inside of described water-cooled crucible (15).
6, as the nano material continuous preparation device of claim 3 or 4 or 5 described band separation and collection structures, it is characterized in that in arc evaporation operating room (1), installing more than one arc discharge negative electrode (14) and water-cooled crucible (15), each arc discharge negative electrode (14) respectively has independent power supply, and electric current can be adjusted separately.
7, the nano material continuous preparation device of band separation and collection structure as claimed in claim 1, it is characterized in that described drawing mechanism (22) is a cylindrical box (74), on the barrel surface of cylindrical box (74), have two gloves holes (75), be equipped with gloves port lid (83) on the gloves hole (75), be arranged in top, two gloves holes (75) and have observation window (77), be positioned at drawing mechanism (22) one sides and have discharging chamber door (80), in casing (74), have one to be used to lay the flat metal plate of pedestal (85) of container (91) of connecting material; One down cylinder (92) is arranged in the bottom of casing (74), there is a dishful of valve (86) that it is divided into two sections in the middle of the cylinder (92), its hypomere is equipped with vacuum table (90), vent valve (89), noble gas charge valve (87) respectively, the bottom of cylinder (92) is connected with vavuum pump (93), casing (74) top is separation chamber's blanking barrel (82), the lower end of blanking barrel (82) put in casing (74) and with its sealed attachment together.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02100692XA CN1194834C (en) | 2002-02-22 | 2002-02-22 | Equipment with separation and collection structure for continuously preparing nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02100692XA CN1194834C (en) | 2002-02-22 | 2002-02-22 | Equipment with separation and collection structure for continuously preparing nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1381327A CN1381327A (en) | 2002-11-27 |
| CN1194834C true CN1194834C (en) | 2005-03-30 |
Family
ID=4739442
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB02100692XA Expired - Fee Related CN1194834C (en) | 2002-02-22 | 2002-02-22 | Equipment with separation and collection structure for continuously preparing nano material |
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|---|---|
| CN (1) | CN1194834C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304150C (en) * | 2004-02-23 | 2007-03-14 | 大连理工大学 | Equipment and method for producing metal nanometer power by automatic control DC electric arc |
| CN102228890A (en) * | 2011-04-28 | 2011-11-02 | 上海交通大学 | Multistage winnowing-high voltage electrostatic separation method |
| CN103482098A (en) * | 2013-09-26 | 2014-01-01 | 辽宁北宇真空科技有限公司 | Nano-powder quantitative subpackaging device |
| CN104843798B (en) * | 2015-04-14 | 2017-01-18 | 齐齐哈尔医学院 | Device used for preparing ultrasmall superparamagnetic iron oxide (USPIO) nano particles via high-voltage electrostatic helix driven |
| CN105148809A (en) * | 2015-09-29 | 2015-12-16 | 泰州市鑫润天冶金保温材料有限公司 | Nanoscale thermal insulation material production device |
-
2002
- 2002-02-22 CN CNB02100692XA patent/CN1194834C/en not_active Expired - Fee Related
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|---|---|
| CN1381327A (en) | 2002-11-27 |
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