CN112589089A - Device and method for preparing spherical powder based on laser-coaxial powder feeding coupling high throughput - Google Patents
Device and method for preparing spherical powder based on laser-coaxial powder feeding coupling high throughput Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0888—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid casting construction of the melt process, apparatus, intermediate reservoir, e.g. tundish, devices for temperature control
Abstract
The invention discloses a device and a method for preparing spherical powder based on laser-coaxial powder feeding coupling high-throughput. The device includes: the multi-channel powder feeder is used for simultaneously filling a plurality of raw material powders with different component types; the laser generator is used for emitting laser to heat and melt the powder provided by the multi-channel powder feeder; the collecting tower is positioned below the laser generator and used for cooling the melted powder and forming spherical powder; and the powder collector is positioned below the collecting tower and used for collecting the spherical powder. The invention can realize the high-flux preparation of alloy powder, ceramic powder, metal-based composite powder containing ceramic reinforcing phase, metal-based composite powder containing carbon nano tube reinforcing and other powder materials with uniform components.
Description
Technical Field
The invention relates to the field of powder material preparation, in particular to a device for preparing spherical powder in a high-flux manner based on laser-coaxial powder feeding coupling and a preparation method thereof.
Background
In recent years, with the development of national economy and science and technology, the demand for new materials is more urgent. Research and development and application of novel structural materials and functional materials are directly related to national defense safety, technological progress, the living standard of people and national competitiveness. The current commonly used trial-and-error method depends on a large amount of experiments and experiences of researchers, the research and development period is long, the cost is high, and the research and development efficiency of new materials is severely restricted. For example, with the continuous improvement of thrust-weight ratio of an aircraft engine, the temperature of gas inside the engine is continuously improved, and the research and development of novel high-temperature alloy blades with higher temperature bearing capacity are urgently needed, and according to the traditional research and development mode, the research and development of novel high-temperature alloy from a laboratory to the service of an installation need at least 20 years. In recent years, materials scientists have sought new ways to develop and develop new materials more quickly, economically and efficiently. In order to accelerate the research and development of new materials, the united states announced a "material genome project" in 2011, aiming at establishing a quantitative relationship between material components/processes-organizational structures-performance by developing a new material innovation platform integrating high-throughput computing, high-throughput experiments, characterization and database technologies, so as to realize the conversion of a material research and development mode from an "empirical mode" to a theoretical "predictive mode" and attempt to shorten the research and development cycle of new materials by half. Meanwhile, an ' accelerated metallurgy ' plan is also proposed in Europe, and then China also starts a ' material genetic engineering ' plan of China edition, namely a key technology and a supporting platform of the material genetic engineering ' key special item.
As an important aspect of material genetic engineering, the high-throughput preparation technology is an important link for linking high-throughput experimental design and a database and is also a precondition for realizing high-throughput characterization. The high-throughput preparation techniques developed at present include a diffusion multiplex method, a codeposition method, a physical mask method, a jet printing synthesis method, a microfluidic synthesis method and the like, but most of the techniques are suitable for preparing bulk and thin film material samples, and the high-throughput preparation techniques for designing powders such as alloy powder, compound powder and the like are rarely reported.
Disclosure of Invention
In view of the above problems, the present invention provides an apparatus for high-throughput preparation of spherical powder based on laser-coaxial powder feeding coupling and a preparation method thereof, which are used for solving at least one of the above problems.
In order to achieve the aim, the invention provides a device for preparing spherical powder in a high-flux manner based on laser-coaxial powder feeding coupling. The device includes:
the multi-channel powder feeder is used for simultaneously filling a plurality of raw material powders with different component types;
the laser generator is used for emitting laser to heat and melt the powder provided by the multi-channel powder feeder;
a collecting tower located below the laser generator for cooling the melted powder and forming a spherical powder;
and the powder collector is positioned below the collecting tower and used for collecting the spherical powder.
In this embodiment, the apparatus further comprises:
and the gas spraying plate is used for adjusting the particle size of the spherical powder through a pressure gas flow medium.
In this embodiment, the apparatus further comprises:
the laser balling head is located above the gas spraying plate and used for melting the powder by using laser generated by a laser generator.
In this embodiment, the laser spheroidizing head and the gas spray disk are located in the material collecting tower, and the material collecting tower has an inert atmosphere.
In this embodiment, the multi-channel powder feeder includes a powder mixer for mixing the raw material powders of different component kinds in the multi-channel powder feeder.
In the present embodiment, the raw material powder is transported by gas.
The invention also provides a method for preparing spherical powder based on laser-coaxial powder feeding coupling high flux, which comprises the following steps:
transmitting the proportioned raw material powder to a laser spot through a multi-channel powder feeder;
melting the proportioned raw material powder by laser and forming powder liquid drops;
the powder drops fall and are cooled in the material collecting tower to form spherical powder;
the spherical powder is collected by a powder collector.
In the present embodiment, the raw material powder is melted under an inert atmosphere, and the powder droplets are cooled under an inert atmosphere and form spherical powder.
In the present embodiment, the method further includes the steps of:
and screening the prepared spherical powder to obtain finished powder with different particle size grades.
Compared with the prior art, the invention has the positive improvement effects that:
firstly, the design of multiple masterbatches fully embodies the concept of high-throughput preparation, can be well combined with high-throughput design calculation, and realizes the high-throughput preparation of novel powder materials with any proportion;
the invention can realize the spheroidization and homogenization of single powder and can also realize the preparation of composite powder materials with various components and contents.
Thirdly, the high-speed airflow in the conical annular airflow nozzle can realize the rapid cooling and crushing of the molten liquid drops, and the prepared powder material has smaller particle size and uniform diameter than the original powder.
And fourthly, the design of the processing cavity with controllable atmosphere pressure and temperature can ensure that the invention uses the preparation of high-activity metal materials, thereby greatly expanding the application range of the invention and further embodying the high-flux property of the invention.
The invention can realize the high-throughput preparation of alloy powder, ceramic powder, metal-based composite powder containing ceramic reinforcing phase, metal-based composite powder containing carbon nano tube reinforcing and other powder materials with uniform components.
Specific embodiments of the present invention are disclosed in detail with reference to the following description and drawings, indicating the manner in which the principles of the invention may be employed. It should be understood that the embodiments of the invention are not so limited in scope. The embodiments of the invention include many variations, modifications and equivalents within the spirit and scope of the appended claims.
Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments, in combination with or instead of the features of the other embodiments.
It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps or components.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a schematic structural diagram of an apparatus for high-flux preparation of spherical powder based on laser-coaxial powder feeding coupling according to the present invention;
FIG. 2a is a microscopic view of the flaky Fe-based amorphous powder before spheroidizing;
FIG. 2b is a microscopic view of the spheroidized flaky Fe-based amorphous powder;
FIG. 2c is an XRD spectrum before and after spheroidization of the flaky iron-based amorphous powder;
FIG. 3 is a schematic flow chart of a preparation method for preparing spherical powder based on laser-coaxial powder feeding coupling high flux.
Detailed Description
While the invention will be described in detail with reference to the drawings and specific embodiments, it is to be understood that these embodiments are merely illustrative of and not restrictive on the broad invention, and that various equivalent modifications may occur to those skilled in the art upon reading this disclosure and fall within the scope of the appended claims.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Fig. 1 is a schematic structural diagram of an apparatus for high-flux preparation of spherical powder based on laser-coaxial powder feeding coupling according to an embodiment of the present invention. The apparatus may include: the device comprises a multi-channel powder feeder 1, a laser generator 2, a laser spheroidizing head 3, a laser head 4, a material collecting tower 5, a powder collector 6 and a gas spray disk 7. Wherein, multichannel powder feeder 1 can fill the raw materials powder of multiple different composition types simultaneously, and then realizes matching different alloy composition according to the demand. Preferably, the multi-channel powder feeder 1 can be integrated with a powder mixer (not shown), so that the uniform mixing function of multiple powders can be realized. The raw material powder is transported by gas. The laser generator 2 mainly forms an energy supply and control system with the laser spheroidizing head 3 and the laser head 4, so that the functions of rapid powder melting and alloying are realized. The collecting tower 5 and the powder collector 6 form a material collecting and atmosphere protecting system, so that the spheroidized powder can be prevented from being oxidized and quickly collected and cleaned, and efficient operation is realized. Optionally, the inside of the aggregate tower 5 is provided with inert atmosphere gas. The spray disk 7 is mainly used for laser melting powder microstructure and particle size regulation and control functions, when powder which is melted by laser and alloyed flies through a spray disk area, high-pressure airflow medium is applied, the powder can be rapidly cooled to obtain an amorphous structure, the powder can be secondarily crushed by adjusting airflow pressure, and the particle size distribution range of the alloy powder is improved.
The construction and use of the device will be described in detail below with reference to several embodiments.
Example 1: high flux powder alloying
Referring to fig. 3, the method for preparing spherical powder based on laser-coaxial powder feeding coupling high throughput of the present invention comprises the following steps:
1) raw material preparation (step S101) is performed by putting powders of raw material A, B, C and the like having different compositions into a multi-channel powder feeder 1 isolated from each other. As shown in fig. 1, the ratio of different powders can be controlled by controlling the flow of the multi-channel powder feeder 1 through a computer system, and a powder mixer is arranged below the multi-channel powder feeder 1 to ensure that the different powders are uniformly mixed and then are conveyed to a laser spot through a carrier gas;
2) powder alloying (step S102), adjusting the power of a laser generator to match different raw material characteristics and laser spot diameters according to different characteristics of raw material powder, such as melting point, wave absorption and the like, starting the laser generator 2, conveying the raw material powder to a laser spot convergence part of the laser generator 2 through a powder feeder, and rapidly melting and alloying the mixed powder under the action of instantaneous laser high energy;
3) and (S103) controlling the microstructure and the particle size of the alloy powder, and automatically shrinking the powder drops alloyed in the step 2 into a spherical shape in the aggregation tower 5 and the powder collector 6 due to the surface tension effect in the falling and flying process so as to obtain the alloyed spherical powder. In particular, in order to obtain amorphous powder or powder with a fine particle size, rapid cooling and secondary crushing can be performed by the gas spray disk 7 disposed below the laser spheroidizing head 3, thereby obtaining amorphous spherical powder or alloy powder material with a finer particle size;
4) and (S104) collecting the powder, cooling the alloyed powder in an aggregate tower 5 in inert atmosphere, finally converging the alloyed powder in a powder collector 6 at the bottom end, taking out the alloyed powder after complete cooling, and screening the prepared alloyed powder to obtain finished powder with different grain size grades.
Example 2 spheronization of flaky iron-based amorphous powder
1) Loading the flaky FeSiCuNb powder into a multi-channel powder feeder 1, wherein the microscopic morphology of the flaky FeSiCuNb powder is irregular flaky morphology as shown in figure 2a, accurately controlling the powder feeding speed V-20 g/min by a computer system, and conveying the powder to the lower part of an annular nozzle by carrier gas for laser spot convergence;
2) according to the characteristics of the raw material powder, the power of the laser generator 2 is adjusted to match the characteristics of the raw material and the diameter of the laser spot, the laser generator 2 is started, the raw material powder is conveyed to the laser spot convergence position through the multi-channel powder feeder 1, and the mixed powder is rapidly melted under the action of instantaneous laser high energy. In the embodiment, the laser power is 2000W, the rotating speed of the multichannel powder feeder 1 is 50 r/min, and the powder feeding flow is 10L/min.
3) The molten powder liquid drop in the step 2 automatically shrinks into a sphere due to the action of surface tension in the falling and flying process, in order to obtain amorphous powder or powder with small particle size, a gas spray disk 7 arranged below the laser spheroidizing head 3 is used for rapid cooling and secondary crushing, so that amorphous spherical powder or alloy powder material with smaller particle size is obtained, the obtained spherical powder has the microscopic morphology as shown in figure 2c, the powder after laser melting is seen to form a regular sphere, and XRD diffraction results show that the alloy powder is amorphous.
4) Collecting powder, cooling the sphericized powder in an aggregate tower 5 in inert atmosphere, finally converging the powder to a powder collector 6 at the bottom end, taking out the powder after complete cooling, and screening the prepared alloy powder to obtain finished powder with different grain size grades.
Compared with the prior art, the invention has the positive improvement effects that:
firstly, the design of multiple masterbatches fully embodies the concept of high-throughput preparation, can be well combined with high-throughput design calculation, and realizes the high-throughput preparation of novel powder materials with any proportion;
the invention can realize the spheroidization and homogenization of single powder and can also realize the preparation of composite powder materials with various components and contents.
Thirdly, the high-speed airflow in the conical annular airflow nozzle can realize the rapid cooling and crushing of the molten liquid drops, and the prepared powder material has smaller particle size and uniform diameter than the original powder.
And fourthly, the design of the processing cavity with controllable atmosphere pressure and temperature can ensure that the invention uses the preparation of high-activity metal materials, thereby greatly expanding the application range of the invention and further embodying the high-flux property of the invention.
The invention can realize the high-throughput preparation of alloy powder, ceramic powder, metal-based composite powder containing ceramic reinforcing phase, metal-based composite powder containing carbon nano tube reinforcing and other powder materials with uniform components.
Any numerical value recited herein includes all values from the lower value to the upper value that are incremented by one unit, provided that there is a separation of at least two units between any lower value and any higher value. For example, if it is stated that the number of a component or a value of a process variable (e.g., temperature, pressure, time, etc.) is from 1 to 90, preferably from 20 to 80, and more preferably from 30 to 70, it is intended that equivalents such as 15 to 85, 22 to 68, 43 to 51, 30 to 32 are also expressly enumerated in this specification. For values less than 1, one unit is suitably considered to be 0.0001, 0.001, 0.01, 0.1. These are only examples of what is intended to be explicitly recited, and all possible combinations of numerical values between the lowest value and the highest value that are explicitly recited in the specification in a similar manner are to be considered.
Unless otherwise indicated, all ranges include the endpoints and all numbers between the endpoints. The use of "about" or "approximately" with a range applies to both endpoints of the range. Thus, "about 20 to 30" is intended to cover "about 20 to about 30", including at least the endpoints specified.
All articles and references disclosed, including patent applications and publications, are hereby incorporated by reference for all purposes. The term "consisting essentially of …" describing a combination shall include the identified element, ingredient, component or step as well as other elements, ingredients, components or steps that do not materially affect the basic novel characteristics of the combination. The use of the terms "comprising" or "including" to describe combinations of elements, components, or steps herein also contemplates embodiments that consist essentially of such elements, components, or steps. By using the term "may" herein, it is intended to indicate that any of the described attributes that "may" include are optional.
A plurality of elements, components, parts or steps can be provided by a single integrated element, component, part or step. Alternatively, a single integrated element, component, part or step may be divided into separate plural elements, components, parts or steps. The disclosure of "a" or "an" to describe an element, ingredient, component or step is not intended to foreclose other elements, ingredients, components or steps.
It is to be understood that the above description is intended to be illustrative, and not restrictive. Many embodiments and many applications other than the examples provided will be apparent to those of skill in the art upon reading the above description. The scope of the present teachings should, therefore, be determined not with reference to the above description, but should instead be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled. The disclosures of all articles and references, including patent applications and publications, are hereby incorporated by reference for all purposes. The omission in the foregoing claims of any aspect of subject matter that is disclosed herein is not intended to forego the subject matter and should not be construed as an admission that the inventors did not consider such subject matter to be part of the disclosed subject matter.
Claims (9)
1. An apparatus for preparing spherical powder based on laser-coaxial powder feeding coupling high flux, which is characterized by comprising:
the multi-channel powder feeder is used for simultaneously filling a plurality of raw material powders with different component types;
the laser generator is used for emitting laser to heat and melt or alloy the powder provided by the multi-channel powder feeder;
a collecting tower located below the laser generator for cooling the melted powder and forming a spherical powder;
and the powder collector is positioned below the collecting tower and used for collecting the spherical powder.
2. The apparatus for preparing spherical powder based on laser-coaxial powder feeding coupling high flux according to claim 1, further comprising:
and the gas spraying plate is used for adjusting the particle size of the spherical powder through a gas flow medium.
3. The apparatus for preparing spherical powder based on laser-coaxial powder feeding coupling high flux according to claim 2, further comprising:
the laser balling head is located above the gas spraying plate and used for melting or alloying the powder by utilizing laser generated by the laser generator.
4. The apparatus for high-flux preparation of spherical powder based on laser-coaxial powder feeding coupling according to claim 3, wherein the laser spheroidizing head and the gas spray disk are located in the collecting tower, and the collecting tower has an inert atmosphere therein.
5. The apparatus for high-throughput spherical powder preparation based on laser-coaxial powder feeding coupling according to claim 1, wherein the multi-channel powder feeder comprises a powder mixer for mixing the raw material powders of different component kinds in the multi-channel powder feeder.
6. The device for preparing the spherical powder based on the laser-coaxial powder feeding coupling high flux according to any one of claims 1 to 5, wherein the raw material powder is transported by gas.
7. A method for preparing spherical powder based on laser-coaxial powder feeding coupling high throughput comprises the following steps:
transmitting the proportioned raw material powder to a laser spot through a multi-channel powder feeder;
melting the proportioned raw material powder by laser and forming powder liquid drops;
the powder drops fall and are cooled in the material collecting tower to form spherical powder;
the spherical powder is collected by a powder collector.
8. The method for preparing spherical powder based on laser-coaxial powder feeding coupling high flux according to claim 7, wherein the raw material powder is melted under an inert atmosphere, and the powder droplets are cooled under the inert atmosphere and form spherical powder.
9. The method for preparing the spherical powder based on the laser-coaxial powder feeding coupling high flux as claimed in claim 8, further comprising the steps of:
and screening the prepared spherical powder to obtain finished powder with different particle size grades.
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