CN103008672B - Pulse small hole many vibrating arms gunite efficiently prepares method and the device of homogeneous spherical micro-particle - Google Patents
Pulse small hole many vibrating arms gunite efficiently prepares method and the device of homogeneous spherical micro-particle Download PDFInfo
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- CN103008672B CN103008672B CN201210540923.7A CN201210540923A CN103008672B CN 103008672 B CN103008672 B CN 103008672B CN 201210540923 A CN201210540923 A CN 201210540923A CN 103008672 B CN103008672 B CN 103008672B
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000011859 microparticle Substances 0.000 title claims abstract description 12
- 239000011378 shotcrete Substances 0.000 title claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 25
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- 239000013528 metallic particle Substances 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 16
- 238000006073 displacement reaction Methods 0.000 claims abstract description 12
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- 239000007769 metal material Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 5
- 239000011148 porous material Substances 0.000 claims description 11
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000009792 diffusion process Methods 0.000 claims description 5
- 230000007423 decrease Effects 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 239000012798 spherical particle Substances 0.000 claims 1
- 238000010257 thawing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000012809 cooling fluid Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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Abstract
Pulse small hole many vibrating arms gunite efficiently prepares method and the device of homogeneous spherical micro-particle, belongs to technical field prepared by spherical micro-particle.It is characterized in that under the condition passing into inert gas Ar generation back pressure, use heater that the metal material in molten bath multiple in crucible is heated to molten condition, then it produces the micro-displacement of a longitudinal direction to input certain pulse enable signal to piezoelectric ceramics, and act on molten metal by driving rod, thus make a certain amount of fine liquid form drop from the ejection of each molten bath small hole at bottom part, and by the sized data of camera system in conjunction with computer software real-time analysis drop, and then adjustment optimized parameter, drop forms homogeneous spherical metallic particles without solidifying in descent.Effect of the present invention and benefit are can homogeneous spheroidal particle that simultaneously efficient preparation size is different, and the hot resume of particle are consistent, and sphericity is good, and size is controlled, greatly enhances productivity, and saves production cost.
Description
Technical field
The invention belongs to technical field prepared by spherical micro-particle, particularly a kind of method and device utilizing pulse small hole many vibrating arms gunite efficiently to prepare homogeneous spherical micro-particle.
Background technology
The size of uniform-spherical micro-size particles, between nanometer to millimeter, is a kind of special spherical powder particle.No matter hold the upper limit of nanoprocessing under this particulate, above hold the lower limit of machining, be in size linking and performance requirement, or be shaped and micro Process manufacture field clean, has the importance and functions that it can not be substituted.By solidifying without container landing or solidify by methods such as cooling fluid quenchings the particulate that drop can obtain required out of roundness and particle diameter, and can special occasions be applied to, as spherical solar cells (silicon particle), BGA Electronic Packaging (Pb-free solder ball particle, copper-Xi nucleocapsid structure particle), spherical shaped semiconductor integrated circuit (silicon, germanium particle), chemical catalysis field (activated carbon particles, nickel-base alloy particle), raw body Material Field (ASTMF75 particle, β-TCP particle), pen ball of ball pen (ZrO
2ceramic microsphere), high temperature nuclear reactor element (UO
2ceramic particle) etc., these particulates not only require that out of roundness is high, uniform particle sizes, size tunable, also require that the hot resume of preparation process are consistent further, and then microstructure is consistent, thus meets the harsh requirement such as modern manufacturing industry precise treatment, microminiaturization and reproducibility;
The method of producing spherical metallic particles at present both at home and abroad has atomization, chopping or punching remelting process, the homogeneous drop method of forming etc.The decentralization that atomization prepares tin ball is wider, must by repeatedly sieving and detecting the particle that just can obtain meeting instructions for use; Chopping or punching remelting process more difficult for the material that plastic working is bad, obtained tin ball must be carried out ungrease treatment in addition; The homogeneous drop method of forming in process of production metal jet is easily subject to the impact of environment, causes the metallic particles produced to there is certain domain size distribution, and cannot adjust in real time and control in process of production.
Summary of the invention
The object of this invention is to provide the device that a kind of pulse small hole many vibrating arms gunite efficiently prepares homogeneous spherical micro-particle, this device increases molten bath quantity on the basis of existing pulse small hole gunite, by installing the potsherd with different pore size, make under the driving of same piezoelectric ceramics, the homogeneous spherical metallic particles that production in enormous quantities particle diameter different simultaneously; Pulse small hole many vibrating arms gunite of the present invention efficiently prepares the method for homogeneous spherical micro-particle, under the condition passing into inert gas Ar gas, heater heating crucible is utilized to become molten condition to its interior metal, certain pulse signal is applied to piezoelectric ceramics, it is made to drive driving rod to produce a longitudinal micro-displacement, this displacement acts on the metal bath of crucible bottom, and make fine droplet from the injection of crucible bottom aperture, drop is frozen into homogeneous spherical metallic particles without container in decline process; Solve that existing technology of preparing particle diameter heterogeneity, production efficiency are low, the uncontrollable deficiency of particle diameter.
Technical solution of the present invention is the device that a kind of pulse small hole many vibrating arms gunite efficiently prepares homogeneous spherical micro-particle, and this device is arranged in vacuum cavity 3, and vacuum cavity 3 comprises vacuum chamber 17, vavuum pump at different levels and external control system; Vacuum chamber 17 top is fixed with ejection electrodes assembly, and bottom is made up of collection unit 11, and be that particle is formed and observation section between the two, three is fixed together by support; Described injection portion mainly contains drive system, crucible 15 and heater 4 and forms; Drive system mainly comprises piezoelectric ceramics 1 and driving rod 14; There is the molten bath 5 that 4-10 size is identical crucible 15 inside, puts band aperture 8 potsherd 7 being equipped with and being connected with vacuum chamber 17 bottom molten bath 5; It is outside that piezoelectric ceramics 1 is positioned at vacuum cavity 3, is connected, is positioned at above potsherd 7 bottom driving rod 14 with driving rod 14; The external stability having heaters 4 of crucible 15, the top of crucible 15 is connected to breather pipe 2, and object is for crucible 15 provides differential pressure; Vacuum cavity 3 sidewall has observation window 18, and is provided with ccd video camera 19, and ccd video camera 19 is connected with computer; Collection unit 11 is made up of accumulator tank 22 and supporter 23, collection unit 11 just to potsherd 7 aperture 8, for the spherical metallic particles 10 that collection cut size is different;
Described device crucible 15 is made up of the molten bath 5 that 4-10 size is identical, and bottom molten bath 5, install the potsherd 7 of different pore size, its pore diameter range is between 0.020-1.500mm;
This device crucible 15 is built-in with the thermocouple 9 be connected with temperature regulating device, and the heater 4 of crucible is connected with temperature regulating device;
The vibration frequency of this device piezoelectric ceramics 1 is between 1Hz-2kHz.
A kind of pulse small hole many vibrating arms gunite efficiently prepares the method for homogeneous spherical micro-particle, its technical scheme is fixed on bottom crucible 15 by the potsherd 7 with different pore size, adjust the diameter of driving rod 14 in each crucible 15 simultaneously, under the condition passing into inert gas Ar gas, heater 4 heating crucible 5 is utilized to become molten condition to its interior metal, certain pulse signal is applied to piezoelectric ceramics 1, it is made to drive driving rod 14 to produce a longitudinal micro-displacement, this displacement acts on the molten metal 16 bottom crucible 15, fine droplet is penetrated from crucible 15 small hole at bottom part 8, drop is frozen into homogeneous spherical metallic particles 10 without container in decline process, piezoelectric ceramics 1 each micropore place that often moves once can form a drop, its step is as follows:
(1) feed, the potsherd 7 with different pore size is fixed on bottom crucible 15, in crucible 15, add the metal material of needs preparation, and seal;
(2) wash vacuum cavity 3, utilize mechanical pump 12 and diffusion pump 13 pairs of crucibles and vacuum chamber 17 to vacuumize, and be filled with inert protective gas Ar, repeatedly carry out several times, finally make pressure in vacuum cavity 3 reach an atmospheric pressure;
(3) heating crucible 15, utilize heater 4 to melt metal material in crucible 15, the temperature in thermocouple 9 Real-Time Monitoring molten bath 5, metal material melts rear insulation 15-20 minute completely;
(4) apply differential pressure, in crucible 15, pass into inert gas by enterprising tracheae 2, utilize differential pressure control system to make to reach stable differential pressure 0-50kPa between crucible 15 and vacuum chamber 17;
(5) vibration is applied, the pulse drive signal editted is applied to piezoelectric ceramics 1, it is made to produce micro-displacement, the molten metal 16 bottom crucible 15 is passed to by driving rod 14, thus fine droplet is penetrated from aperture 8, the drop of injection forms spherical metallic particles 10 because gravity and capillary effect are solidified without container in dropping process;
(6) particle collection, after having sprayed, collects the homogeneous spherical metallic particles 10 that particle diameter is different in different collection units 11.
Effect of the present invention and benefit are preparation method and the device of provided homogeneous spherical metallic particles, process controllability is strong, crucible temperature can be controlled, the pressure differential of crucible and vacuum cavity, utilize image detecting system can carry out the adjustment of technological parameter, reduce the error of molten drop and the setting drop size produced, obtain the spherical metallic particles of uniform-dimension, enhance productivity; By method and apparatus of the present invention, homogeneous, the hot resume of size simultaneously efficiently can preparing the different-grain diameter met the demands are consistent, the spherical metallic particles of sphericity height size tunable; There is the features such as production efficiency is high, structure is simple, cost is low; Suitability for industrialized is produced.
Accompanying drawing explanation
Accompanying drawing 1 is the device schematic diagram that pulse small hole many vibrating arms gunite efficiently prepares homogeneous spherical micro-particle.
Accompanying drawing 2 is the A-A sectional views in accompanying drawing 1.
In figure: 1 piezoelectric ceramics, breather pipe on 2,3 vacuum cavities, 4 heaters, 5 molten baths, 6 times breather pipes, 7 potsherds, 8 apertures, 9 thermocouples, 10 spherical metallic particles, 11 collection units, 12 mechanical pumps, 13 diffusion pumps, 14 driving rods, 15 crucibles, 16 molten metal, 17 vacuum chambers, 18 observation windows, 19CCD video camera, 20 metallics tentatively condensed, 21 collection unit side doors, 22 accumulator tanks, 23 supporters.
Detailed description of the invention
The specific embodiment of the present invention is described in detail below in conjunction with technical scheme and accompanying drawing.
The technical solution used in the present invention is fixed on bottom crucible 15 by the potsherd 7 with different pore size, adjust the diameter of driving rod 14 in each crucible 15 simultaneously, under the condition passing into inert gas Ar gas, heater 4 heating crucible 15 is utilized to become molten condition to its interior metal, certain pulse signal is applied to piezoelectric ceramics 1, it is made to drive driving rod 14 to produce a longitudinal micro-displacement, this displacement acts on the molten metal 16 bottom crucible 15, thus fine droplet is penetrated from crucible 15 small hole at bottom part 8, drop is frozen into homogeneous spherical metallic particles 10 without container in decline process.
Embodiment:
Batch preparation Sn-0.3Ag-0.7CuBGA encapsulates the detailed description of the invention of ball:
(1) Sn-0.3Ag-0.7Cu wire scissors is cut into isometric metal bar, after carrying out ultrasonic vibration, puts into crucible 15, select the pore size of potsherd 7 according to demand; The amount of putting into of Sn-0.3Ag-0.7Cu metal bar reaches 3/4 of molten bath 5, as shown in Figure 1;
(2) with mechanical pump 12, injection portion crucible 15, vacuum chamber 17 are extracted into below low vacuum 5Pa, injection portion crucible 15, vacuum chamber 17 are extracted into high vacuum 0.001Pa by recycling diffusion pump 13; In utilization, breather pipe 2 and lower breather pipe 6 pass into inert gas Ar gas, make the pressure in injection portion crucible 15, vacuum chamber 17 reach 0.1MPa;
(3) power arranging heater 4 is 400W, heating-up temperature is 260 DEG C, close switch heating crucible 15, melts the metal material in crucible, is incubated 20 minutes after temperature reaches 260 DEG C;
(4) utilize differential pressure control system, in crucible 15, pass into inert gas argon gas by gas siphunculus 2, make to produce certain differential pressure with vacuum chamber 17; External pulse drive singal is applied to piezoelectric ceramics 1, under its incentive action, piezoelectric ceramics 1 produces downward micro-displacement, passes to the metal bath bottom molten bath 5 by driving rod 14, thus minute metallic melt is sprayed by the aperture 8 on potsherd 7 bottom crucible 15; The molten drop of injection forms spherical metallic particles 10 owing to solidifying without container in dropping process under gravity and capillary effect, finally falls into collection unit 11;
(5) Liquid particle image captured by ccd video camera 19 regulates vibration frequency, thus produces the symmetrical liquid drop of setting size;
(6) after due-in assembly bundle, close external pulse signal, heater 4 successively, treat that temperature is down to room temperature, open collection unit side door 21 and take out spherical metallic particles 10 in collection unit 11; Finally, turn off breather pipe 2 and lower breather pipe 7, molten bath 5 and vacuum chamber 17 are extracted into below low vacuum 5Pa, to make equipment be in vacuum state when inactive with mechanical pump 12 and diffusion pump 13.
Claims (2)
1. pulse small hole many vibrating arms gunite efficiently prepares a homogeneous spherical micro-particle device, it is characterized in that:
A () this device is arranged in vacuum cavity (3), vacuum cavity (3) comprises vacuum chamber (17), vavuum pump at different levels and external control system; Vacuum chamber (17) top is fixed with injection parts, and bottom is made up of collection unit (11), and be that particle is formed and observation section between the two, three is fixed together by support; Described injection portion mainly contains drive system, crucible (15) and heater (4) composition; Drive system mainly comprises piezoelectric ceramics (1) and driving rod (14); There is the molten bath (5) that 4-10 size is identical crucible (15) inside, and band aperture (8) potsherd (7) being equipped with and being connected with vacuum chamber (17) is put in molten bath (5) bottom; It is outside that piezoelectric ceramics (1) is positioned at vacuum cavity (3), is connected with driving rod (14), and driving rod (14) bottom is positioned at potsherd (7) top; The external stability having heaters (4) of crucible (15), the top of crucible (15) is connected to breather pipe (2), and object is for crucible (15) provides differential pressure; Vacuum cavity (3) sidewall has observation window (18), and is provided with ccd video camera (19), and ccd video camera (19) is connected with computer; Collection unit (11) is made up of accumulator tank (22) and supporter (23), collection unit (11) just to potsherd (7) aperture (8), for the spherical metallic particles (10) that collection cut size is different;
B () described device crucible (15) is made up of the molten bath (5) that 4-10 size is identical, install the potsherd (7) of different pore size in molten bath (5) bottom, its pore diameter range is between 0.020-1.500mm;
C () this device crucible (15) is built-in with the thermocouple (9) be connected with temperature regulating device, the heater (4) of crucible is connected with temperature regulating device;
D the vibration frequency of () this device piezoelectric ceramics (1) is between 1Hz-20kHz.
2. pulse small hole many vibrating arms gunite efficiently prepares a homogeneous spherical particle submethod, it is characterized in that:
Potsherd (7) with different pore size is fixed on crucible (15) bottom, adjust the diameter of driving rod (14) in each crucible (15) simultaneously, under the condition passing into inert gas Ar gas, heater (4) heating crucible (15) is utilized to become molten condition to its interior metal, pulse signal is applied to piezoelectric ceramics (1), it is made to drive driving rod (14) to produce a longitudinal micro-displacement, this displacement acts on the molten metal (16) of crucible (15) bottom, fine droplet is penetrated from crucible (15) small hole at bottom part (8), drop is frozen into homogeneous spherical metallic particles (10) without container in decline process, piezoelectric ceramics each micropore place that often moves once can form a drop, its step is as follows:
(1) feed, the potsherd (7) with different pore size is fixed on crucible (15) bottom, in crucible (15), adds the metal material of needs preparation, and seal;
(2) vacuum cavity (3) is washed, mechanical pump (12) and diffusion pump (13) is utilized to vacuumize crucible and vacuum chamber (17), and be filled with inert protective gas Ar, repeatedly carry out, finally make vacuum cavity (3) interior pressure reach an atmospheric pressure;
(3) heating crucible (15), utilize the metal material in heater (4) thawing crucible (15), temperature in thermocouple (9) Real-Time Monitoring molten bath (5), metal material melts rear insulation 15-20 minute completely;
(4) apply differential pressure, in crucible (15), pass into inert gas by enterprising tracheae (2), utilize differential pressure control system to make to reach stable differential pressure 0-50kPa between crucible (15) and vacuum chamber (17);
(5) vibration is applied, the pulse drive signal editted is applied to piezoelectric ceramics (1), it is made to produce micro-displacement, the molten metal (16) of crucible (15) bottom is passed to by driving rod (14), thus fine droplet is penetrated from aperture (8), the drop of injection forms spherical metallic particles (10) because gravity and capillary effect are solidified without container in dropping process;
(6) particle collection, after having sprayed, collects the homogeneous spherical metallic particles (10) that particle diameter is different in different collection units (11).
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