CN116060626A - Device and method for preparing nano alloy particles - Google Patents

Device and method for preparing nano alloy particles Download PDF

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Publication number
CN116060626A
CN116060626A CN202211567737.2A CN202211567737A CN116060626A CN 116060626 A CN116060626 A CN 116060626A CN 202211567737 A CN202211567737 A CN 202211567737A CN 116060626 A CN116060626 A CN 116060626A
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laser
target
alloy particles
preparation
nano
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贾强
胡虎安
郭福
王乙舒
马立民
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Beijing University of Technology
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Beijing University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/12Making metallic powder or suspensions thereof using physical processes starting from gaseous material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention relates to the technical field of nano alloy material preparation, and provides a device and a method for preparing nano alloy particles. The laser generating unit is used for emitting at least two laser beams. The preparation unit comprises a preparation device, a preparation cavity is formed in the preparation device, at least two placement platforms for placing heterogeneous target materials are arranged in the preparation cavity, and the preparation device is further provided with an incident window for passing through laser and a collection port for collecting nano alloy particles. The laser generating unit can drive the laser to move along the diameter direction of the target. The full cross compounding of plasmas is realized, and the uniformity of nano alloy particles is improved.

Description

Device and method for preparing nano alloy particles
Technical Field
The invention relates to the technical field of nano alloy material preparation, in particular to a device and a method for preparing nano alloy particles.
Background
Along with the development of technology, simple substance nano particles can not meet the demands of people in practical application, and nano alloy particles have unique properties of nano particles and alloys, and have excellent characteristics in aspects of electricity, magnetism, catalysis, corrosion resistance, hardness, melting point and the like.
The existing nano alloy particles mainly comprise physical preparation and chemical preparation, and in the preparation method of the nano alloy particles in the related technology, the mixing degree of different plasmas is insufficient when the alloy particles are formed, so that the nano alloy particles are unevenly distributed.
Disclosure of Invention
The invention provides a preparation device of nano alloy particles, which is used for solving the technical problem of uneven distribution of the nano alloy particles prepared in the prior art, realizing full cross-compounding of plasmas and improving the uniformity of the nano alloy particles.
The invention also provides a preparation method of the nano alloy particles.
The technical scheme of the invention provides a preparation device of nano alloy particles, which comprises the following components:
the laser generating unit is used for emitting at least two laser beams;
the preparation unit comprises a preparation device, wherein a preparation cavity is formed in the preparation device, at least two placement platforms for placing heterogeneous targets are arranged in the preparation cavity, and the preparation device is further provided with an incident window for passing through laser and a collection port for collecting nano alloy particles;
the laser generating unit can drive the laser to move along the diameter direction of the target.
According to the preparation device of the nano alloy particles provided by the invention, the laser emission unit comprises:
a laser emitter for generating laser light;
the reflectors are arranged at intervals and are used for reflecting laser so as to enable the laser to propagate along a preset light path;
the light splitting mechanisms are sequentially arranged at intervals along the direction of the preset light path and are used for splitting one laser beam into two laser beams;
the vibrating mirror is arranged at the tail end of the preset light path and is used for focusing laser so that the focal points of the laser processed by the vibrating mirror are located on the same focal plane, and the vibrating mirror is matched with the light splitting mechanism;
the laser power instrument is arranged on one of the light paths after the beam splitting of the beam splitting mechanism and is used for detecting the laser power of the corresponding light path.
According to the preparation device of the nano alloy particles provided by the invention, the light splitting mechanism comprises:
the half-wave plate and the beam splitting plate are sequentially arranged at intervals along the direction of the preset light path, the half-wave plate is used for rotating laser, and the beam splitting plate is used for reflecting and transmitting the laser so that one beam of laser is split into two beams of laser through the beam splitting plate;
The beam splitter plate is used for adjusting the intensity ratio of the two split laser beams based on the deflection angle of the half-wave plate.
According to the preparation device of the nano alloy particles provided by the invention, the preparation unit further comprises:
the telescopic mechanism is telescopically arranged in the preparation cavity;
the rotating mechanism is arranged in the preparation cavity, one end of the rotating mechanism is connected with the placing platform and used for driving the placing platform to rotate, and the other end of the rotating mechanism is connected with the telescopic mechanism and used for driving the placing platform to lift.
According to the preparation device of the nano alloy particles, each vibrating mirror can enable laser emitted from the vibrating mirror to reciprocate along the diameter direction of the corresponding target;
the speed of the laser driven by the vibrating mirror is positively correlated with the rotation angular speed of the target, and the speed of the laser driven by the vibrating mirror is positively correlated with the difference between the radius of the target and the laser moving distance.
The device for preparing the nano alloy particles provided by the invention further comprises a central control unit, wherein the central control unit is respectively and electrically connected with each vibrating mirror and used for driving each vibrating mirror to synchronously act, the central control unit is also electrically connected with the rotary driving piece and the laser power instrument and used for receiving laser power signals fed back by the laser power so as to drive the rotary driving piece to act, and the central control unit is also electrically connected with the telescopic mechanism and the rotary mechanism and used for driving the target to rotate and adjust the height.
According to the preparation device of the nano alloy particles, the placement platform is arranged at an included angle with the horizontal plane, so that the included angle between the plane of the target and the horizontal plane is 10-60 degrees;
the laser emitted from the vibrating mirror and the plane of the target material form an included angle, and the included angle between the laser emitted from the vibrating mirror and the plane of the target material ranges from 10 degrees to 60 degrees;
the placement platforms are arranged at intervals, so that the distance range of each target in the horizontal direction is 0-100 mm, and the distance range of each target in the height direction is 0-100 mm.
According to the preparation device of the nano alloy particles, the top surface of the preparation device is provided with the collection port corresponding to the placement platform, the collection port is connected with the collector through the collection channel, the collector is arranged in a tapered shape from top to bottom, the lower end of the collector is connected with the collection bottle, and the upper end of the collector is provided with the air outlet channel.
According to the preparation device of the nano alloy particles, provided by the invention, the preparation cavity is internally provided with the air supply device, the air outlet of the air supply device faces the target material and is used for mixing plasmas generated by different targets and enabling the plasmas to move along the collecting port, wherein the air supply device is suitable for blowing inert gas, and the gas flow rate of the air supply device is 0.1L/min to 5.0L/min;
The collecting channel is communicated with an air inlet channel, and the air inlet channel is suitable for blowing inert gas in the direction of the collector.
According to the preparation device of the nano alloy particles, the preparation device is further connected with a vacuum device and a vacuum gauge, the vacuum device is used for vacuumizing the preparation cavity, and the vacuum gauge is used for detecting the vacuum degree of the preparation cavity.
The technical scheme of the invention also provides a preparation method of the nano alloy particles, which comprises the following steps:
respectively placing at least two targets on a placing platform of a preparation device, and adjusting the relative positions of the targets and the vibrating mirror;
the preparation cavity is regulated to a vacuum environment or an atmosphere environment, at least two beams of laser are emitted by the laser generating unit, and the deflection angle of the half wave plate is regulated based on the proportion requirement of the alloy in the nano alloy particles so as to regulate the laser power of each beam of laser;
at least two laser beams are respectively transmitted into the preparation cavity from the incident window and respectively irradiated to at least two targets;
driving a vibrating mirror to act by utilizing a central control unit so as to enable laser to reciprocate along the diameter direction of the target, driving the target to rotate by utilizing a rotating mechanism so as to generate at least two plasmas, and enabling the at least two plasmas to be crossed and compounded to form nano alloy particles;
The speed of the laser driven by the vibrating mirror is positively correlated with the rotation angular speed of the target, and the speed of the laser driven by the vibrating mirror is positively correlated with the difference between the radius of the target and the laser moving distance.
According to the nano alloy particle preparation device provided by the embodiment of the invention, at least two laser beams generated by the laser generation unit are respectively transmitted into the preparation cavity from the incident window, and the at least two laser beams are respectively irradiated to the heterogeneous target material placed on the placement platform so as to generate at least two plasmas. The laser generation unit drives the laser to move along the diameter direction of the target, the placement platform drives the target to rotate along the circle center of the target, the intersection of the plane of the target and the focal plane of the laser coincides with the diameter of the target, uniform consumption of the target is ensured based on control of a laser moving path, and meanwhile, the situation that the laser can not be subjected to cross recombination between different plasmas in the moving path is avoided, so that the plasmas can be fully subjected to cross recombination, and uniformity of formed nano alloy particles is ensured.
According to the preparation method of the nano alloy particles, at least two beams of laser generated by the laser generation unit are respectively transmitted into the preparation cavity from the incident window, and the at least two beams of laser are respectively irradiated to the heterogeneous target placed on the placement platform so as to generate at least two plasmas. The laser generation unit drives the laser to move along the diameter direction of the target, the placement platform drives the target to rotate along the circle center of the target, the intersection of the plane of the target and the focal plane of the laser coincides with the diameter of the target, uniform consumption of the target is ensured based on control of a laser moving path, and meanwhile, the situation that the laser can not be subjected to cross recombination between different plasmas in the moving path is avoided, so that the plasmas can be fully subjected to cross recombination, and uniformity of formed nano alloy particles is ensured.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural view of a preparation unit in a preparation apparatus of nano alloy particles provided by the present invention;
FIG. 2 is a schematic structural view of a laser generating unit in the apparatus for preparing nano alloy particles according to the present invention;
FIG. 3 is a schematic view of a path of a laser moving on a target in the apparatus for preparing nano alloy particles according to the present invention;
FIG. 4 is a schematic view of a path of a gas supply device blowing plasma movement in a nano alloy particle preparation device provided by the invention;
FIG. 5 is a schematic view of the structure of a collector in the apparatus for preparing nano-alloy particles according to the present invention;
FIG. 6 is a schematic flow chart of a method of preparing nano-alloy particles according to the present invention;
FIG. 7 is a scanning electron microscope image of Ag-Pd nano-alloy particles;
FIG. 8 is a scanning electron microscope image of Ag-Cu nano-alloy particles.
Reference numerals:
10. a laser generating unit; 110. a laser emitter; 120. a reflecting mirror; 130. vibrating mirror; 140. a laser power meter; 150. a half-wave plate; 160. splitting the beam slice; 170. a rotary driving member; 180. a beam expander; 20. a preparation device; 210. preparing a cavity; 220. an entrance window; 230. a collection port; 240. an observation window; 30. a rotation mechanism; 410. a collector; 420. a collection bottle; 430. an air outlet channel; 440. an air inlet channel; 50. an air supply device; 60. a vacuum device; 70. a vacuum gauge; 80. and (3) a target material.
Detailed Description
Embodiments of the present invention are described in further detail below with reference to the accompanying drawings and examples. The following examples are illustrative of the invention but are not intended to limit the scope of the invention.
In the description of the embodiments of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the embodiments of the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the embodiments of the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In describing embodiments of the present invention, it should be noted that, unless explicitly stated and limited otherwise, the terms "coupled," "coupled," and "connected" should be construed broadly, and may be either a fixed connection, a removable connection, or an integral connection, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium. The specific meaning of the above terms in embodiments of the present invention will be understood in detail by those of ordinary skill in the art.
In embodiments of the invention, unless expressly specified and limited otherwise, a first feature "up" or "down" on a second feature may be that the first and second features are in direct contact, or that the first and second features are in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the embodiments of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
Embodiments of the present invention are described below in conjunction with fig. 1-8.
As shown in fig. 1 to 5, the present embodiment provides a device for preparing nano alloy particles, which includes a laser generating unit 10 and a preparing unit. The laser generating unit 10 is configured to emit at least two laser beams. The preparation unit comprises a preparation device 20, wherein a preparation cavity 210 is formed in the preparation device 20, at least two placement platforms for placing heterogeneous targets 80 are arranged in the preparation cavity 210, and the preparation device 20 is further provided with an incident window 220 for passing laser and a collection port 230 for collecting nano alloy particles. Wherein, the target 80 is set to be round, the intersection of the plane of the target 80 and the focal plane of the laser coincides with the diameter of the target 80, the placement platform can drive the target 80 to rotate along the center of the circle, and the laser generating unit 10 can drive the laser to move along the diameter direction of the target 80.
In this embodiment, at least two laser beams generated by the laser generating unit 10 are respectively transmitted from the incident window 220 into the preparation chamber 210, and the at least two laser beams are respectively irradiated to the heterogeneous target 80 placed on the placement platform to generate at least two plasmas. The laser generating unit 10 drives the laser to move along the diameter direction of the target 80, the placement platform drives the target 80 to rotate along the circle center of the target 80, the intersection of the plane of the target 80 and the focal plane of the laser coincides with the diameter of the target 80, uniform consumption of the target 80 is ensured based on control of a laser moving path, and meanwhile, the situation that the laser can not cross-compound different plasmas in the moving path is avoided, so that the different plasmas can fully cross-compound, and uniformity of formed nano alloy particles is ensured.
Along with the irradiation of the laser to the palladium target 80, bright plasmas are generated at the intersection line of the laser focal plane and the surface of the target 80, and the plasmas formed on the surface of the target 80 continuously act with the laser to perform isothermal emission along the direction perpendicular to the target 80. Different plasmas generated between different targets 80 can be fully cross-combined after being emitted, so that the uniformity of the alloy is ensured.
Based on that the generated plasma will be emitted in a direction perpendicular to the target 80, the collection port 230 is disposed opposite to the target 80, so that the nano alloy particles formed after the generated unused plasma is sufficiently cross-compounded can be discharged along the collection port 230, thereby facilitating collection. Or a substrate may be provided at the collection port 230 and the formed nano-alloy particles can be directly deposited on the surface of the substrate. Wherein, the material of the substrate can be steel, heat-resistant steel, ceramic, glass and the like. Based on the unique advantages of the apparatus and method for preparing the nano-alloy particles, the diameter of the substrate can be selected to be relatively large, specifically, the diameter of the substrate can be in the range of 0-200mm (millimeters).
In this embodiment, the diameter of the target 80 may be 10mm-100mm, and the target 80 may be a metal material such as Au, ag, cu, fe, al, ti, pd, pt, sr, sn, sb, in, ni or a semiconductor material such as Si, se, ge, ga, te.
Wherein, in order to facilitate the observation of the condition inside the preparation chamber 210, an observation window 240 is further provided on the preparation device 20.
According to the nano alloy particle preparation device provided by the invention, the laser emission unit comprises a laser emitter 110, a plurality of reflectors 120, at least two light splitting mechanisms, at least two vibrating mirrors 130 and a laser power meter 140. The laser transmitter 110 is used to generate laser light. The plurality of reflectors 120 are spaced apart from each other to reflect the laser light so that the laser light propagates along a predetermined optical path. The at least two light splitting mechanisms are sequentially arranged at intervals along the direction of a preset light path, and the light splitting mechanisms are used for splitting one laser beam into two laser beams; at least two galvanometer 130 are arranged at the tail end of the preset light path, the galvanometer 130 is used for transmitting and focusing laser so that the focuses of the laser processed by the galvanometer 130 are positioned on the same focal plane, and the galvanometer 130 is matched with the light splitting mechanism; the laser power meter 140 is disposed on one of the light paths after the beam splitting by one of the beam splitting mechanisms, and is used for detecting the laser power located on the corresponding light path.
The reflecting mirror 120 is used for changing the propagation direction of the laser, as shown in fig. 2, a reflecting mirror 120 is disposed at the position opposite to the emitting port of the laser emitter 110, and reflecting mirrors 120 are sequentially disposed on the optical path reflected by the reflecting mirror 120 at intervals, so as to guide the laser, so that the laser propagates along the preset optical path, and the laser energy is transmitted from the incident window 220 to the preparation cavity 210 for irradiation after being processed by the galvanometer 130.
The number of galvanometers 130 is the same as the number of beam splitting mechanisms, and two beam splitting mechanisms and two galvanometers 130 are used as an example of the laser emission unit in fig. 2, where one beam splitting mechanism splits one beam of laser generated by the laser reflector into two beams of laser. One of the two split laser beams passes through the beam expander 180 and the reflecting mirror 120 and irradiates one of the galvanometer 130, so that the laser beam is focused by the galvanometer 130 and then transmitted from the incident window 220 to the preparation cavity 210 to irradiate the target 80. The other beam splitting mechanism is arranged on the optical path of the other beam of the two beams of laser beams, the other beam splitting mechanism splits the beam of laser beams into two beams of laser beams, one beam of laser beam passes through the beam expander 180 and the reflecting mirror 120 and irradiates the other vibrating mirror 130, so that the laser beam is focused by the vibrating mirror 130 and then transmitted from the incident window 220 to the preparation cavity 210 to irradiate the target 80, and the other beam of laser beam irradiates the laser power meter 140, so that the laser power of the changed beam of laser beam is detected. The beam expander 180 can expand the diameter of the laser beam and reduce the divergence angle of the laser beam, so that the laser beam can be better focused when being incident on the galvanometer 130.
Based on the detection of the laser power of one of the laser beams by the laser power meter 140, the laser power of the laser beam can be directly obtained, and the laser power of the other laser beam split by the same beam splitting mechanism and the laser powers of the two laser beams corresponding to the last beam splitting mechanism can be obtained through calculation. Therefore, the laser power of each laser beam can be detected and calculated in real time, and the laser power of each laser beam can be conveniently regulated in real time.
After the laser transmitter 110 emits a beam of high-energy laser light, the plurality of mirrors 120, the at least two beam splitting mechanisms, and the at least two galvanometers 130 become at least two beams of pulsed laser light with controlled energy and trajectory to irradiate the target 80.
Specifically, the beam splitting mechanism includes a half-wave plate 150 and a beam splitting plate 160, where the half-wave plate 150 and the beam splitting plate 160 are sequentially arranged at intervals along a direction of a preset optical path, the half-wave plate 150 is used for rotating laser, and the beam splitting plate 160 is used for reflecting and transmitting the laser, so that one laser beam is split into two laser beams by the beam splitting plate 160. Each half-wave plate 150 is connected to a rotary driving member 170, and is used for adjusting the deflection angle of the half-wave plate 150, and the beam splitter 160 adjusts the intensity ratio of the two split laser beams based on the deflection angle of the half-wave plate 150.
The deflection angle of half wave plate 150 can determine the ratio of the intensities of the laser light in the two directions after splitting by beam splitter 160. The power ratio of the two split laser beams is adjusted based on the adjustment of the intensity ratio of the two split laser beams. For example, at a certain deflection angle, after one laser beam is split into two laser beams by the half-wave plate 150 and the beam splitter 160, the ratio of the power of the two laser beams is 1:1. At this time, when the laser power meter 140 detects that the power of one laser beam is 20W (watts), the power of the other laser beam split by the same set of half-wave plate 150 and beam splitter 160 is also 20W. The sum of the two laser powers can be calculated to be 40W before beam splitting. In this way, the laser power of each laser beam can be calculated, and the laser power of each laser beam can be adjusted by rotating the deflection angle of the half-wave plate 150, so as to change the proportion of different components in the alloy.
The beam splitter 160 is used to reflect and transmit laser light, so that one laser light can be transmitted through the beam splitter 160 or reflected by the beam splitter 160, thereby forming two laser light beams.
The rotary driving member 170 employs a rotary motor that can quantitatively control the deflection angle of the half-wave plate 150.
Based on the setting mode of the laser emission unit, the beam splitting of laser and the real-time controllable and energy real-time adjustable of the laser output track can be realized.
The preparation unit further comprises a telescopic mechanism and a rotation mechanism 30. The telescopic mechanism is telescopically arranged in the preparation cavity 210. The rotary mechanism 30 is arranged in the preparation cavity 210, one end of the rotary mechanism 30 is connected with the placement platform and used for driving the placement platform to rotate, and the other end of the rotary mechanism 30 is connected with the telescopic mechanism and used for driving the placement platform to lift by the telescopic mechanism.
The telescopic mechanism can be an electric telescopic rod, and the electric telescopic rod is obliquely arranged and stretches out and draws back along the length direction of the electric telescopic rod, so that the horizontal distance and the vertical distance between different placing platforms are adjusted. The fixed height of the target 80 is adjusted by the telescopic mechanism, so that the distance from the target 80 to the collecting opening 230 can be changed, and the particle size of the prepared nano alloy particles is controlled based on the adjustment of the distance from the target 80 to the collecting opening 230.
The rotating mechanism 30 is used for driving the placement platform to rotate, so that the target 80 rotates.
Each galvanometer 130 can reciprocate the laser beam emitted from the galvanometer 130 along the diameter direction of the corresponding target 80. The speed at which the galvanometer 130 drives the laser to move is positively correlated with the rotational angular velocity of the target 80, and the speed at which the galvanometer 130 drives the laser to move is also positively correlated with the difference between the radius of the target 80 and the distance of the laser to move.
Specifically, the relation function among the speed of laser movement, the rotational angular speed of the target 80, the radius of the target 80, and the laser movement distance is as follows:
V=A·ω·(r-x)+V 1
wherein V is 1 The initial speed of the laser is determined according to different preparation requirements;
a is a constant and depends on different preparation requirements;
ω is the angular velocity of target 80;
r is the radius of the target 80;
x is the moving distance of the laser.
Based on the functional relation, the nano alloy particles can be fully crossed and compounded among different plasmas in the preparation process, and the uniformity of the formed nano alloy particles is ensured. Meanwhile, by matching with the arrangement mode that the intersection of the plane of the target 80 and the focal plane of the laser coincides with the diameter of the target 80, the speed of the laser at different positions in the diameter direction of the target 80 can be different, so that the consumption of the inner side and the outer side of the target 80 in the rotation process is uniform, and the phenomena of more consumption of the inner side and less consumption of the outer side of the target 80 are avoided.
The galvanometer 130 acts to emit light from the galvanometer 130The laser beam emitted from one of the galvanometers 130 reciprocates along the diameter direction of one of the targets 80, as shown in fig. 3, from the C of one of the targets 80 1 The point moves to C along the diameter 2 Point where the laser light emitted from the other galvanometer 130 is directed from the other target 80 1 The point moves to D along the diameter 2 And (5) a dot.
In this embodiment, the apparatus for preparing nano alloy particles further includes a central control unit, where the central control unit is electrically connected to each vibrating mirror 130, and is used to drive each vibrating mirror 130 to act synchronously, the central control unit is further electrically connected to the rotation driving member 170 and the laser power meter 140, and the central control unit is used to receive a laser power signal fed back by the laser power to drive the rotation driving member 170 to act, and the central control unit is further electrically connected to the telescopic mechanism and the rotation mechanism 30, and is used to drive the target 80 to rotate and adjust the height.
The central control unit can ensure the synchronous action of the vibrating mirrors 130, so that each vibrating mirror 130 can synchronously trigger and synchronously work, laser energy emitted by each vibrating mirror 130 synchronously strikes the target 80, plasma is synchronously generated to carry out cross mixing, and the uniformity of the cross mixing is ensured.
The central control unit also receives a laser power signal fed back by the laser power meter 140, and calculates the laser power of another beam of laser beam split by the same beam splitting mechanism and the laser powers of two beams of laser beams corresponding to the beam splitting mechanism at the upper stage based on the laser power signal. Therefore, the laser power of each laser beam can be detected and calculated in real time, and the rotation driving member 170 can be controlled in real time to drive the half-wave plate 150 to rotate, so that the deflection angle of the half-wave plate 150 is changed to adjust the laser power of each laser beam.
The central control unit controls the telescopic mechanism and the rotating mechanism 30 to act so as to adjust the height position of the target 80 before the preparation process starts, and to continuously rotate the target 80 in the preparation process and to control the angular speed of rotation of the target 80.
The placement platform is disposed at an angle to the horizontal plane, so that the angle between the plane of the target 80 and the horizontal plane is in the range of 10 ° to 60 °. The laser beam emitted from the galvanometer 130 forms an included angle with the plane of the target 80, and the included angle between the laser beam emitted from the galvanometer 130 and the plane of the target 80 ranges from 10 ° to 60 °. The placement platforms are arranged at intervals so that the pitch range of each target 80 in the horizontal direction is 0 to 100mm, and the pitch range of each target 80 in the height direction is 0 to 100mm. The alloy proportion of the nano alloy particles can be adjusted based on the arrangement of the distance and the included angle, and the plasma can be fully and uniformly mixed.
As shown in fig. 1 and 5, the top surface of the preparing device 20 is formed with a collecting port 230 corresponding to the placing platform, the collecting port 230 is connected with a collector 410 through a collecting channel, the collector 410 is provided with a tapered shape from top to bottom, the lower end of the collector 410 is connected with a collecting bottle 420, and the upper end of the collector 410 is configured with an air outlet channel 430.
The formed nano-alloy particles are settled and collected in a collection bottle 420 from a collection port 230 and a collector 410. Specifically, during the collection process, the gas flow moves the nano-alloy particles, and the mixture of gas and nano-alloy particles rotates around the inner wall of the collector 410 because the collector 410 is tapered from top to bottom. Based on the heavier nano-alloy particles, the nano-alloy particles will continuously sink and fall into the lower collection bottle 420 during collection, while the lighter gas will gradually float up and be discharged from the upper air outlet channel 430.
The preparation chamber 210 is further provided with an air supply device 50, an air outlet of the air supply device 50 faces the target 80, and the air supply device 50 is used for mixing plasmas generated by different targets 80 and enabling the plasmas to move along the collection port 230, wherein the air supply device 50 is suitable for blowing inert gas, and the gas flow rate of the air supply device 50 is 0.1L/min to 5.0L/min (liter/min). The collection channel communicates with an air inlet channel 440, the air inlet channel 440 being adapted to blow inert gas in the direction of the collector 410.
The gas supply device 50 can charge gas into the preparation chamber 210, and can blow inert gas to the plasmas along a certain angle so that the plasmas of different types are uniformly mixed under the driving of the gas flow. The mixed nano-alloy particles are discharged from the collection port 230 and the collection channel into the collector 410 for collection. The inert gas may be selected from helium, argon, nitrogen, carbon dioxide, and the like.
As shown in fig. 4, the air supply device 50 may include an air supply hose and an air supply head, one end of the air supply hose is connected to the air outlet mechanism, and the other end is connected to the air supply head, and an air outlet of the air supply head faces the target 80. The air supply hose can be convenient for adjust the position and the orientation of the air supply head to adjust the position and the angle of the air supply head according to different requirements. As shown in FIG. 4, the triangular region is approximately an indication of the location of the plasma, and the arrangement of the gas delivery device 50 allows one of the targets 80 to deliver plasma from A 1 Is blown to A at the position of (2) 2 At a position where plasma emitted from another target 80 is emitted from B 1 Blow to B at the position of (2) 2 Is realized to disturb the plasma, ensuring sufficient mixing between the plasmas.
The gas flow rate of the gas supply device 50 is 0.1L/min to 5.0L/min, and the gas flow rate is submitted based on different preparation requirements. Based on the adjustment of the gas flow, the nano alloy particles with different particle sizes can be prepared.
In the present embodiment, the particle size of the nano alloy particles is adjusted by the cooperative combination of the adjustment of the gas flow rate of the gas supply device 50 and the telescopic adjustment of the distance from the target 80 to the collection port 230 by the telescopic mechanism.
Since the collector 410 is provided in a tapered shape from top to bottom, the mixture of gas and nano-alloy particles rotates around the inner wall of the collector 410 by blowing inert gas into the collection channel and the collector 410 through the air inlet channel 440. Based on the heavier nano-alloy particles, the nano-alloy particles will continuously sink and fall into the lower collection bottle 420 during collection, while the inert gas is lighter and will be discharged from the upper air outlet channel 430.
Based on the arrangement of the air supply device 50, the nano alloy particles may be prepared in an atmosphere environment in which the air pressure may be 1Pa to 10000 Pa.
The vacuum device 60 and the vacuum gauge 70 are also connected to the preparation apparatus 20, the vacuum device 60 is used for vacuumizing the preparation cavity 210, and the vacuum gauge 70 is used for detecting the vacuum degree of the preparation cavity 210.
Based on the arrangement of the vacuum device 60 and the vacuum gauge 70, nano alloy particles can be prepared in a vacuum environment in which the air pressure can be 1×10 -1 Pa-1×10 -5 Pa. It is now appropriate to provide a substrate at the collection port 230 for deposition of the resulting nano-alloy particles.
When nano alloy particles are prepared in a vacuum environment, the nano alloy particles can be collected by the collector 410 and the collecting bottle 420, and the air outlet channel 430 at the upper end of the collector 410 and the air inlet channel 440 on the collecting channel are required to be closed.
The protection is carried out by adopting inert gas in the atmosphere environment, so that the nano alloy particles can not be oxidized in the atmosphere environment or in the vacuum environment, and the product quality of the nano alloy particles is ensured.
Based on the above arrangement of the apparatus for preparing nano alloy particles in the present embodiment, the particle size of the prepared nano alloy particles can be adjusted by controlling the size of the passing air and the distance of the target 80 from the collection port 230; the alloy ratio of the nano-alloy particles can be adjusted by controlling the deflection angle of the half-wave plate 150, the total laser power and the relative positions of different targets 80. The prepared nano alloy particles have controllable particle size, adjustable components, uniform particle size, high alloying degree, large-area preparation and multi-component alloy preparation. The corresponding preparation method is simple to operate, economical, environment-friendly and high in efficiency.
The method for preparing the nano alloy particles provided by the invention is described below, and the method for preparing the nano alloy particles described below and the method for preparing the nano alloy particles described above can be correspondingly referred to each other.
As shown in fig. 6, the preparation method of the nano alloy particle provided in this embodiment specifically includes the following steps:
S100, respectively placing at least two targets 80 on a placing platform of the preparation device 20, and adjusting the relative positions of the targets 80 and the vibrating mirror 130.
And S200, adjusting the preparation cavity 210 to a vacuum environment or an atmosphere environment, utilizing the laser generating unit 10 to emit at least two laser beams, and adjusting the deflection angle of the half wave plate 150 based on the proportion requirement of the alloy in the nano alloy particles so as to adjust the laser power of each laser beam.
S300, at least two laser beams are respectively transmitted from the incident window 220 to the preparation cavity 210 and respectively irradiated to at least two targets 80.
S400, driving the vibrating mirror 130 to act by utilizing the central control unit so as to enable laser to reciprocate along the diameter direction of the target 80, driving the target 80 to rotate by utilizing the rotating mechanism 30 so as to generate at least two plasmas, and enabling the at least two plasmas to be crossed and compounded to form nano alloy particles.
The speed at which the galvanometer 130 drives the laser to move is positively correlated with the rotational angular velocity of the target 80, and the speed at which the galvanometer 130 drives the laser to move is also positively correlated with the difference between the radius of the target 80 and the distance of the laser to move.
In this embodiment, at least two laser beams generated by the laser generating unit 10 are respectively transmitted from the incident window 220 into the preparation chamber 210, and the at least two laser beams are respectively irradiated to the heterogeneous target 80 placed on the placement platform to generate at least two plasmas. The laser generating unit 10 drives the laser to move along the diameter direction of the target 80, the placement platform drives the target 80 to rotate along the circle center of the target 80, the intersection of the plane of the target 80 and the focal plane of the laser coincides with the diameter of the target 80, uniform consumption of the target 80 is ensured based on control of a laser moving path, and meanwhile, the situation that the laser can not cross-compound different plasmas in the moving path is avoided, so that the different plasmas can fully cross-compound, and uniformity of formed nano alloy particles is ensured.
The preparation method of the nano alloy particles provided in the embodiment has a vacuum environment mode and an atmosphere environment mode. A vacuum environment may be created by vacuum apparatus 60 in conjunction with vacuum gauge 70 for preparation chamber 210 in a vacuum environment mode, where it is appropriate to place a substrate at collection port 230 for deposition of the nano-alloy particles. In the atmosphere mode, the gas supply device 50 may be used to supply inert gas, where the gas supply device 50 may supply gas to the preparation chamber 210, and may supply inert gas to the plasma at a certain angle, so that different kinds of plasmas are uniformly mixed under the driving of the gas flow. The mixed nano-alloy particles are discharged from the collection port 230 and the collection channel into the collector 410 for collection.
Taking two targets 80 as examples, one target 80 is silver (Ag), the other target 80 is palladium (Pb), the two targets 80 are round targets 80 with the diameter of 50mm and the thickness of 3mm, and the metal purity is 99.99%. Correspondingly, two placement platforms are disposed in the preparation chamber 210 of the preparation apparatus 20, and two observation windows 240 are disposed in the preparation apparatus 20.
Silver target 80 and palladium target 80 are respectively placed on two placing platforms, the relative positions of silver target 80 and palladium target 80 are adjusted through telescopic mechanisms, the positions and angles of two vibrating mirrors 130 are adjusted through vibrating mirrors 130, the deflection angles of two half-wave plates 150 are adjusted through rotary driving pieces 170, and therefore the power of two laser beams is adjusted.
The preparation was performed under an atmosphere of argon gas, and argon gas was introduced into the air supply device 50 at a pressure of approximately 500Pa, the laser power of the laser emitter 110 was set to 70W, and the two laser beams were irradiated to the silver target 80 and the palladium target 80 for 10 minutes, respectively.
Along with the continuous irradiation of the silver target 80 and the palladium target 80 by the two laser beams, bright plasmas are generated at the intersection line of the laser focal plane and the surface of the target 80, and the plasmas formed on the surface of the target 80 continuously act with the laser beams to perform isothermal emission along the direction perpendicular to the target 80. Because the rapid quenching in a molten or vapor state is far from equilibrium, the solid solubility of the Ag-Pd system is extended, supersaturated alloy is obtained, and the Ag-Pd elements in the nano alloy particles are distributed uniformly.
Fig. 7 is a scanning electron microscope image of ag—pd nano alloy particles, from which it can be seen that Ag and Pd form nano alloy with good uniformity.
Taking two targets 80 as examples, one target 80 is silver, the other target 80 is copper (Cu), the two targets 80 are round targets 80 with the diameter of 50mm and the thickness of 3mm, and the metal purity is 99.99%. Correspondingly, two placement platforms are disposed in the preparation chamber 210 of the preparation apparatus 20, and two observation windows 240 are disposed in the preparation apparatus 20.
Silver target 80 and copper target 80 are respectively placed on two placing platforms, the relative positions of silver target 80 and copper target 80 are adjusted through telescopic mechanisms, the positions and angles of two vibrating mirrors 130 are adjusted through vibrating mirrors 130, the deflection angles of two half-wave plates 150 are adjusted through rotary driving pieces 170, and therefore the power of two laser beams is adjusted.
The preparation was performed under an atmosphere of argon gas, and argon gas was introduced into the air supply device 50 at a pressure of approximately 500Pa, the laser power of the laser emitter 110 was set to 70W, and the two laser beams formed were irradiated to the silver target 80 and the copper target 80 for 10min, respectively.
Along with the continuous irradiation of the silver target 80 and the copper target 80 by the two laser beams, bright plasmas are generated at the intersection line of the laser focal plane and the surface of the target 80, and the plasmas formed on the surface of the target 80 continuously act with the laser beams to perform isothermal emission along the direction perpendicular to the target 80. Because the rapid quenching in a molten or vapor state is far from equilibrium, the solid solubility of the Ag-Cu system is extended, supersaturated alloy is obtained, and the distribution of Ag-Cu elements in the nano alloy particles is relatively uniform.
Fig. 8 is a scanning electron microscope image of Ag-Cu nano alloy particles, from which it can be seen that Ag and Cu form nano alloys and have good uniformity.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (11)

1. A device for preparing nano-alloy particles, comprising:
the laser generating unit is used for emitting at least two laser beams;
the preparation unit comprises a preparation device, wherein a preparation cavity is formed in the preparation device, at least two placement platforms for placing heterogeneous targets are arranged in the preparation cavity, and the preparation device is further provided with an incident window for passing through laser and a collection port for collecting nano alloy particles;
the laser generating unit can drive the laser to move along the diameter direction of the target.
2. The apparatus for preparing nano-alloy particles according to claim 1, wherein the laser emitting unit comprises:
a laser emitter for generating laser light;
the reflectors are arranged at intervals and are used for reflecting laser so as to enable the laser to propagate along a preset light path;
the light splitting mechanisms are sequentially arranged at intervals along the direction of the preset light path and are used for splitting one laser beam into two laser beams;
the vibrating mirrors are arranged at the tail ends of the preset light paths and are used for focusing laser so that the focuses of the laser processed by the vibrating mirrors are located on the same focal plane, and the vibrating mirrors are matched with the light splitting mechanism;
the laser power instrument is arranged on one of the light paths after the beam splitting of the beam splitting mechanism and is used for detecting the laser power of the corresponding light path.
3. The apparatus for preparing nano-alloy particles according to claim 2, wherein the spectroscopic mechanism comprises:
the half-wave plate and the beam splitting plate are sequentially arranged at intervals along the direction of the preset light path, the half-wave plate is used for rotating laser, and the beam splitting plate is used for reflecting and transmitting the laser so that one beam of laser is split into two beams of laser through the beam splitting plate;
The beam splitter plate is used for adjusting the intensity ratio of the two split laser beams based on the deflection angle of the half-wave plate.
4. The apparatus for producing nano-alloy particles according to claim 3, wherein the production unit further comprises:
the telescopic mechanism is telescopically arranged in the preparation cavity;
the rotating mechanism is arranged in the preparation cavity, one end of the rotating mechanism is connected with the placing platform and used for driving the placing platform to rotate, and the other end of the rotating mechanism is connected with the telescopic mechanism and used for driving the placing platform to lift.
5. The apparatus for producing nano-alloy particles according to claim 4, wherein each of the galvanometer is configured to reciprocate the laser beam emitted from the galvanometer in a diameter direction of the corresponding target;
the speed of the laser driven by the vibrating mirror is positively correlated with the rotation angular speed of the target, and the speed of the laser driven by the vibrating mirror is positively correlated with the difference between the radius of the target and the laser moving distance.
6. The device for preparing nano-alloy particles according to claim 5, further comprising a central control unit, wherein the central control unit is electrically connected with each vibrating mirror respectively and is used for driving each vibrating mirror to synchronously act, the central control unit is further electrically connected with the rotary driving piece and the laser power meter and is used for receiving laser power signals fed back by laser power to drive the rotary driving piece to act, and the central control unit is further electrically connected with the telescopic mechanism and the rotary mechanism and is used for driving the target to rotate and adjust the height.
7. The apparatus for preparing nano-alloy particles according to claim 5, wherein the placement platform is disposed at an angle to a horizontal plane such that the angle between the plane of the target and the horizontal plane is in the range of 10 ° to 60 °;
the laser emitted from the vibrating mirror and the plane of the target material form an included angle, and the included angle between the laser emitted from the vibrating mirror and the plane of the target material ranges from 10 degrees to 60 degrees;
the placement platforms are arranged at intervals, so that the distance range of each target in the horizontal direction is 0-100 mm, and the distance range of each target in the height direction is 0-100 mm.
8. The apparatus for preparing nano-alloy particles according to any one of claims 1 to 7, wherein the collecting port is formed at a top surface of the preparation device, the collecting port is adapted to be connected with a collector through a collecting channel, the collector is provided in a tapered shape from top to bottom, a collecting bottle is connected to a lower end of the collector, and an air outlet channel is configured at an upper end of the collector.
9. The apparatus for preparing nano-alloy particles according to claim 8, wherein an air supply device is further provided in the preparation chamber, an air outlet of the air supply device faces the target for mixing plasma generated by the heterogeneous target and moving the plasma along the collection port, wherein the air supply device is adapted to blow out inert gas, and a gas flow rate of the air supply device is 0.1L/min to 5.0L/min;
the collecting channel is communicated with an air inlet channel, and the air inlet channel is suitable for blowing inert gas in the direction of the collector.
10. The apparatus for preparing nano-alloy particles according to claim 8, wherein the preparation device is further connected with a vacuum device for evacuating the preparation chamber and a vacuum gauge for detecting the degree of vacuum of the preparation chamber.
11. A method for preparing nano alloy particles, which is characterized by comprising the following steps:
respectively placing at least two targets on a placing platform of a preparation device, and adjusting the relative positions of the targets and the vibrating mirror;
the preparation cavity is regulated to a vacuum environment or an atmosphere environment, at least two beams of laser are emitted by a laser generating unit, and the deflection angle of the half wave plate is regulated based on the proportion requirement of the alloy in the nano alloy particles so as to regulate the laser power of each beam of laser;
at least two laser beams are respectively transmitted into the preparation cavity from the incident window and respectively irradiated to at least two targets;
driving a vibrating mirror to act by utilizing a central control unit so as to enable laser to reciprocate along the diameter direction of the target, driving the target to rotate by utilizing a rotating mechanism so as to generate at least two plasmas, and enabling the at least two plasmas to be crossed and compounded to form nano alloy particles;
the speed of the laser driven by the vibrating mirror is positively correlated with the rotation angular speed of the target, and the speed of the laser driven by the vibrating mirror is positively correlated with the difference between the radius of the target and the laser moving distance.
CN202211567737.2A 2022-12-07 2022-12-07 Device and method for preparing nano alloy particles Pending CN116060626A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116921685A (en) * 2023-09-15 2023-10-24 西安赛隆增材技术股份有限公司 Method and device for preparing powder by utilizing microwave plasma

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116921685A (en) * 2023-09-15 2023-10-24 西安赛隆增材技术股份有限公司 Method and device for preparing powder by utilizing microwave plasma
CN116921685B (en) * 2023-09-15 2023-12-08 西安赛隆增材技术股份有限公司 Method and device for preparing powder by utilizing microwave plasma

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