CN110935394B - Micro-nano powder fine processing method and device - Google Patents
Micro-nano powder fine processing method and device Download PDFInfo
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- CN110935394B CN110935394B CN201911070126.5A CN201911070126A CN110935394B CN 110935394 B CN110935394 B CN 110935394B CN 201911070126 A CN201911070126 A CN 201911070126A CN 110935394 B CN110935394 B CN 110935394B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/003—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic followed by coating of the granules
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/10—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in stationary drums or troughs, provided with kneading or mixing appliances
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/0012—Devices for disintegrating materials by collision of these materials against a breaking surface or breaking body and/or by friction between the material particles (also for grain)
- B02C19/005—Devices for disintegrating materials by collision of these materials against a breaking surface or breaking body and/or by friction between the material particles (also for grain) the materials to be pulverised being disintegrated by collision of, or friction between, the material 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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Abstract
The invention discloses a micro-nano powder fine processing method and a device, which are used for producing composite micro-nano powder particles; the method is characterized in that nanoscale powder particles are coated on micron-sized powder particles in a mechanical impact grinding mode, the powder particles are shaped into spherical and spheroidal particles, the performance of powder materials is improved, the inner surface of a processing device is improved, powder pollution is reduced, and the processing quality is improved.
Description
Technical Field
The invention relates to the field of deep processing of powder, in particular to a micro-nano powder fine processing method and a micro-nano powder fine processing device.
Background
In the field of existing materials, powder materials are always in an important position, wherein powder smelting continuously puts higher requirements on the powder materials, and brings the powder materials into the field of vision of the public along with the maturity and market application of 3D printing technology in recent years, and further promotes the development of the powder materials; the new energy field aims at the requirements of high-performance lithium batteries, particularly relates to the manufacture of a lithium battery cathode material, and also accelerates the development of powder materials. In actual work, powder materials are used as raw materials of products, the characteristics of components, purity, appearance, particle distribution and the like of particles of the powder materials are closely related to production and processing links, and the product quality is influenced, and a powder processing method and a powder processing device are disclosed in the publication No. CN1827301A, so that the appearance of powder particles is trimmed to form a regular spherical appearance, the length-diameter ratio is small, and the loose packing and tap density are high. However, in actual production, with the continuous improvement of product requirements, materials with more excellent performance and purity are required, so people propose a composite particle for powder material particles, in the traditional processing, a chemical processing, mechanical stirring or high-temperature pressing method is generally adopted for composite powder material processing, and the powder particles manufactured by the method have the problems of low material purity and poor structural performance.
In summary, there is a need for a powder processing method and apparatus that can not only produce high-performance powder materials, but also ensure the purity of the materials during the production of composite powder materials.
Disclosure of Invention
In view of the above, the invention provides a micro-nano powder fine processing method and device, which can solve the problem of processing the existing composite powder.
For this purpose, the present invention is implemented by the following technical means.
A micro-nano powder fine processing method is characterized by comprising the following steps: the method comprises the steps of adding nanoscale child particles and micron-sized mother particles into a shaping device, and processing the powder particles by using a mechanical impact grinding method to obtain required composite powder particles, wherein the processing time range of the micro-nano powder is 0.5-60 min, the particle size range of the nanoscale child particles is 0.1-10 mu m, the particle size range of the micron-sized mother particles is 0.5-1000 mu m, and the weight ratio of each component is as follows: the nano-scale sub-particles/micro-scale mother particles are between 0.1% and 50%;
the processing process comprises the following steps:
1. particle reshaping: the nanometer-level sub-particles and the micron-level mother particles enter a shaping device through a feeding hole, and irregular particles are shaped into spherical and quasi-spherical particles through high-speed physical impact through high-speed blades and high-speed airflow impact;
2. coating the particles: and the nanoscale child particles impact the surface of the micron-sized mother particles under the condition of high-speed motion, are combined with the surface of the micron-sized mother particles in an attaching, embedding or rivet welding mode, and are coated on the surface of the micron-sized mother particles through the particle shaping process.
In the processing process, the material is cooled indirectly by adopting a water cooling mode.
Further, the particle shaping and particle coating processes are performed simultaneously under the same conditions.
Further, the high velocity gas stream is an inert gas stream. Further, the inert gas may be selected from helium, nitrogen, or argon.
Further, the nanoscale sub-particles and the micron-sized mother particles are one or more of non-metal mineral powder, metal powder or organic polymer powder; furthermore, for the metal powder, the average grain diameter of the micron-sized mother particle powder is less than or equal to 100 mu m.
Further, the high-speed blade rotating speed is between 1000rpm and 10000 rpm.
The shaping device for fine processing of the micro-nano powder comprises: the device comprises a stator, a rotor, a sealing cover, a sealing ring, rotor blades, fixed blades, an embedded inner container, a cooling water inlet, a cooling water outlet, a feeding hole, a discharging hole, a protective gas inlet, a protective gas outlet and a rotating shaft;
the stator is a cylindrical shell, a through hole is formed in the center of the end face of the stator and used for installing the rotating shaft, and the embedded inner container is embedded inside the stator;
the stator shell is provided with a through hole for installing the cooling water inlet and the cooling water outlet;
the stator and the embedded liner are provided with 4 groups of corresponding through holes, and the feed inlet, the discharge outlet, the protective gas inlet and the protective gas outlet are arranged;
the rotor is of a disc-shaped structure;
8 fixed blades are uniformly distributed on the sealing cover along the circumferential direction;
the device is characterized in that the sealing ring is of a disc-shaped structure, is arranged between the sealing cover and the embedded liner, and is provided with a special-shaped hole corresponding to the fixed blade together with the embedded liner; a through hole is formed in the center of the side end face of the embedded liner and used for mounting the rotating shaft; the center of one side of the rotor is connected with the rotating shaft, and the other side of the rotor is uniformly provided with 8 rotor blades along the rotating circumferential direction; the fixed blade, the rotor and the rotor blade are all positioned in the cavity of the embedded inner container.
Further, the installation radius of the rotor blade is larger than that of the fixed blade, and the rotor blade does not interfere with the fixed blade in rotation under the working condition.
Further, the inner surface of the embedded liner is a ceramic lining of sprayed aluminum oxide or titanium nitride, and the rotor, the rotor blades and the fixed blades are made of one of ceramic materials of full aluminum oxide, zirconium oxide or titanium nitride.
Furthermore, an interlayer is arranged between the stator and the embedded inner container and can store cooling water, and the interlayer is communicated with the cooling water inlet and the cooling water outlet.
The invention has the following advantages:
1. the method is not limited by the feasibility of thermodynamic and chemical reactions between two or more particles, the function of coating is added during the particle shaping, and the final shape result of the shaped particles is controlled by adjusting the rotating speed and the shaping time. The impeller rotating speed is between 1000rpm and 10000rpm, the polishing, shaping and coating effects on metal powder, especially small-particle metal powder (the average particle size of micron-sized mother particles is less than or equal to 100 mu m) are obvious, and the characteristics of increasing the ball granularity, the powder flowability and the apparent density can be realized.
2. The inner surface of the shaping device is of a ceramic structure. The inner wall of the machine body can be selected to be sprayed with ceramic linings such as alumina, titanium nitride and the like, and the rotor can be made of ceramic materials such as full alumina, zirconia or titanium nitride and the like. The inner structure is wear-resistant, high temperature resistant and corrosion resistant, and has no pollution to powder.
3. The shaping device interlayer is filled with cooling water, and inert gas is filled in the shaping device interlayer, so that the device can process inflammable and explosive powder, the safety is improved, the material and gas in the air are prevented from generating oxidation reaction, and the purity of the powder material is improved.
Drawings
In the figure:
1-a stator; 2-a rotor; 3-sealing the cover; 4-sealing ring; 5-rotor blades; 6-fixed blades; 7-embedding an inner container; 8-cooling water inlet; 9-cooling water outlet; 10-a feed inlet; 11-a discharge hole; 12-a shielding gas inlet; 13-a shielding gas outlet; 14-rotating shaft.
FIG. 1 is a schematic view of a pellet shaper of the present invention;
FIG. 2 is a side view of the impeller rotor;
FIG. 3 is a side view of the seal cap;
FIG. 4 is an electron micrograph before and after zirconium hydride-coated aluminum powder treatment (FIG. 4-a shows zirconium hydride powder, FIG. 4-b shows aluminum powder, and FIG. 4-c shows zirconium hydride-coated aluminum composite powder);
FIG. 5 is an electron micrograph of the copper powder coated with aluminum before and after the treatment (FIG. 5-d shows the mixed powder before the treatment, and FIG. 5-e shows the composite powder after the treatment).
Detailed Description
The invention will be further explained with reference to the drawings.
The nanometer-level sub-particles and the micron-level mother particles are one or more of non-metallic mineral powder, metal powder and organic polymer powder; the micro-nano powder processing time range is 0.5min-60min, the particle size range of the nano-grade sub-particles is 0.1nm-10 mu m, the particle size range of the micro-grade mother particles is 0.5 mu m-1000 mu m, and the proportion (weight ratio) of each component is as follows: 0.1% -50% of the nanometer-level child particles/micron-level mother particles;
preferably, when the processed powder is metal powder, the average grain diameter of the selected micron-sized mother particle powder is less than or equal to 100 mu m.
The processing method comprises the following steps of adding nanoscale child particles and micron-sized mother particles into a shaping device, and treating powder particles by using a mechanical impact grinding method to obtain the required composite particles, wherein the processing process comprises the following steps:
1. particle reshaping: the nanoscale child particles and the micron-sized mother particles enter a shaping device through a feeding hole, and irregular particles are shaped into spherical and quasi-spherical particles through high-speed physical impact through high-speed blades and high-speed airflow impact;
the high-speed gas flow introduced into the device is inert gas flow, and preferably, the inert gas can be one of helium, nitrogen or argon;
the rotating speed of the high-speed blade is between 1000rpm and 10000 rpm;
2. coating the particles: the nanometer-level child particles impact the surface of the micron-level mother particles under the condition of high-speed motion, are combined with the surface of the micron-level mother particles in an attaching, embedding or rivet welding mode, and are coated on the surface of the micron-level mother particles through a particle shaping process.
The two parts of the processing process are simultaneously carried out under the same condition; in the processing process, the material is cooled indirectly by adopting a water cooling mode.
The structure of the shaping device is described in detail:
as shown in fig. 1, the shaping device includes: stator 1, rotor 2, sealed lid 3, sealing washer 4, rotor blade 5, fixed blade 6, embedded inner bag 7, cooling water import 8, cooling water export 9, feed inlet 10, discharge gate 11, protective gas entry 12, protective gas export 13, pivot 14.
As shown in fig. 1, the stator 1 is a cylindrical shell, and a through hole is formed in the center of the end face to install a rotating shaft 14; the rotor 2 is a disc-shaped structure, and the center of the rotor is connected with a rotating shaft 14; the rotor 2, the rotor blades 5 and the fixed blades 6 are all arranged in the embedded liner 7; the shell of the stator 1 is provided with a through hole for installing a cooling water inlet 8 and a cooling water outlet 9; an interlayer is formed between the stator 1 and the embedded inner container 7 and can store cooling water, 4 groups of corresponding through holes are formed in the embedded inner container 7, and a feed inlet 10, a discharge outlet 11, a protective gas inlet 12 and a protective gas outlet 13 are installed.
As shown in fig. 2, 8 rotor blades 5 are uniformly distributed on one side of the rotor 2 along the rotating circumferential direction, and the center of the other side is connected with a rotating shaft 14; as shown in fig. 3, 8 fixed blades 6 are uniformly distributed on the sealing cover 3 along the circumferential direction, and the sealing ring 4 and the embedded liner 7 are provided with special-shaped holes corresponding to the fixed blades 6; the installation radius of the rotor blade 5 is larger than that of the fixed blade 6, and the rotation is not interfered under the working condition;
the inner surface of the shaping device is of a ceramic structure, preferably, the inner surface of the embedded liner 7 is a ceramic lining sprayed with alumina or titanium nitride, and the rotor 2, the rotor blades 5 and the fixed blades 6 are made of one of full alumina, zirconia or titanium nitride.
The specific processing flow is as follows:
1. a preparation phase. Respectively selecting powder with proper average particle size of the primary particles and the secondary particles according to the requirements of powder material products, calculating the composition ratio of the components, and mechanically stirring and mixing the prepared powder; the device is introduced with inert gas, is connected with external cooling water circulation and is electrified to start the device.
2. And (5) a processing stage. When the impeller of the rotor of the device reaches the designed rotating speed, the mixed powder material is pushed into the device through the feed inlet, and the processing is started.
3. And (5) collecting and checking. When the processing time reaches the design time, the power supply of the device is closed, the cooling water circulation is kept until the internal material is cooled to the room temperature, then the device is closed, and the discharge hole is opened to dump the primarily processed powder material; and conveying the powder material to a sorting machine for sorting, and sampling and micro-detecting the sorted product, wherein the product meets the design standard and is completely processed at one time.
Example 1
Zirconium hydride is a nuclear reaction moderator, and when the aluminum material is used in a nuclear reactor component, in order to avoid the influence of the reactor on the component, the zirconium hydride particles are coated on the surfaces of the aluminum powder particles by using the method and the device, and the processing conditions are as follows:
ratio (mass ratio) of zirconium hydride fine particles to aluminum powder particles: 5 percent;
average particle diameter of zirconium hydride fine particles: 58 nm;
average particle diameter of aluminum powder particles: 43 μm;
the protective gas comprises the following components: nitrogen gas;
the rotating speed of the high-speed blade is as follows: 5500 rpm;
processing time: and 8 min.
As shown in FIG. 4, the zirconium hydride particle powder in FIG. 4-a and the aluminum powder in FIG. 4-b are processed, and the zirconium hydride particles are coated on the surfaces of the aluminum powder particles to form a pockmark-like coating in FIG. 4-c, so that the performance of the aluminum material is effectively improved.
Example 2
Copper has excellent conductivity and processability as a raw material and has various applications, but the corrosion and oxidation resistance of copper often limits the application. In order to solve the problems, the method and the device are applied, a layer of aluminum is coated outside copper powder particles, and the processing conditions are as follows:
the ratio (mass ratio) of aluminum powder particles to copper powder particles: 30 percent;
average particle diameter of aluminum powder particles: 1 μm;
average particle diameter of copper powder particles: 22 μm;
the protective gas comprises the following components: nitrogen gas;
the rotating speed of the high-speed blade is as follows: 6800 rpm;
processing time: and (5) 22 min.
As shown in FIG. 5, the aluminum powder and copper powder mixed particles shown in FIG. 5-d are processed to form core-shell structure composite particles coated with aluminum outside as shown in FIG. 5-e, so that the corrosivity of the outside on the copper powder can be reduced, and the purpose of slowing down the oxidation speed of copper is achieved.
Although the present invention has been described in detail with reference to examples, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (2)
1. A micro-nano powder fine processing method is characterized by comprising the following steps: adding nanoscale child particles and micron-sized mother particles into a shaping device, and processing powder particles by using a mechanical impact grinding method to obtain required composite particles, wherein the processing time range of the micro-nano powder is 8min-22min, the particle size range of the nanoscale child particles is 58nm-1 mu m, and the particle size range of the micron-sized mother particles is 22 mu m-43 mu m; the weight ratio of the nanoscale child particles to the micron-sized mother particles is 5-30%;
the nanometer-scale sub-particles are zirconium hydride particles, and the micron-scale mother particles are aluminum powder particles; or the nanometer-scale sub-particles are aluminum powder particles, and the micron-scale mother particles are copper powder particles;
the processing process comprises the following steps:
(1) particle reshaping: the nanometer-level sub-particles and the micron-level mother particles enter a shaping device through a feeding hole, and irregular particles are shaped into spherical and quasi-spherical particles through high-speed physical impact through high-speed blades and high-speed airflow impact;
(2) coating the particles: the nanometer-scale sub-particles impact the surface of the micron-scale mother particles under the condition of high-speed motion, are combined with the surface of the micron-scale mother particles in an attaching, embedding or rivet welding mode, and are coated on the surface of the micron-scale mother particles through the particle shaping process;
in the processing process, the material is cooled indirectly by adopting a water cooling mode; the high-speed gas flow is an inert gas flow;
the particle shaping and the particle coating processes are carried out simultaneously under the same condition;
the nanometer-scale sub-particles and the micron-scale mother particles are metal powder;
the high-speed vane rotating speed is between 5500rpm and 6800 rpm.
2. A micro-nano powder produced by the micro-nano powder fine processing method of claim 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911070126.5A CN110935394B (en) | 2019-11-05 | 2019-11-05 | Micro-nano powder fine processing method and device |
| PCT/CN2019/117250 WO2021088098A1 (en) | 2019-11-05 | 2019-11-11 | Fine processing method and device for preparing micro/nano powder |
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| CN201911070126.5A CN110935394B (en) | 2019-11-05 | 2019-11-05 | Micro-nano powder fine processing method and device |
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| CN110935394B true CN110935394B (en) | 2021-07-30 |
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| CN1827301A (en) * | 2006-04-07 | 2006-09-06 | 清华大学 | Particle shaping method and device thereof |
| CN101653826A (en) * | 2009-09-11 | 2010-02-24 | 南京金视显科技有限公司 | Silver powder surface modification processing method |
| CN103785822A (en) * | 2012-10-26 | 2014-05-14 | 深圳市龙岗区华宇新材料研究中心 | Micron-order composite material and preparation method thereof |
| WO2016069604A1 (en) * | 2014-10-27 | 2016-05-06 | Massachusetts, University Of | Micro-and nano-particles with variable surface morphologies and methods of making same |
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| CN1202043C (en) * | 2003-05-29 | 2005-05-18 | 上海交通大学 | Prepn of large grain spherical submicron/nano composite fiber-ceramic powder |
| JP2005162510A (en) * | 2003-12-01 | 2005-06-23 | Sumitomo Chemical Co Ltd | Manufacturing method of metal oxide particulate |
| CN2917941Y (en) * | 2006-04-07 | 2007-07-04 | 清华大学 | Particle shaping apparatus for powder material |
| EP2026961A4 (en) * | 2006-05-22 | 2013-07-24 | Nanomech Llc | Non-metallic nano/micro particles coated with metal, process and applications thereof |
| EP2288440B1 (en) * | 2008-05-10 | 2016-06-22 | Brigham Young University | Porous composite particulate materials, methods of making and using same, and related apparatuses |
| JP5836124B2 (en) * | 2008-10-13 | 2015-12-24 | イノブナノ−マテリアイス アバンサドス，ソシエダッド アノニマＩｎｎｏｖｎａｎｏ−Ｍａｔｅｒｉａｉｓａｖａｎｃａｄｏｓ，Ｓ．Ａ． | Ceramic powder coated with nanoparticle layer and preparation method thereof |
| EP2660268B1 (en) * | 2010-12-28 | 2019-08-07 | Shanghai Genius Advanced Material (Group) Co. Ltd | Nano particle/polyamide composite material, preparation method therefor, and use thereof |
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| CN202962605U (en) * | 2012-11-21 | 2013-06-05 | 芜湖浙鑫新能源有限公司 | Special equipment for reshaping graphite grains |
| WO2014160445A1 (en) * | 2013-03-13 | 2014-10-02 | X-Tend Energy, Llc | Method for the use of slurries in spray pyrolysis for the production of non-hollow, porous particles |
| CN104086176A (en) * | 2013-08-30 | 2014-10-08 | 常州凡登特种材料技术有限公司 | Uniformly-composite spherical ceramic particles and preparation method thereof |
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- 2019-11-11 WO PCT/CN2019/117250 patent/WO2021088098A1/en active Application Filing
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| CN1827301A (en) * | 2006-04-07 | 2006-09-06 | 清华大学 | Particle shaping method and device thereof |
| CN101653826A (en) * | 2009-09-11 | 2010-02-24 | 南京金视显科技有限公司 | Silver powder surface modification processing method |
| CN103785822A (en) * | 2012-10-26 | 2014-05-14 | 深圳市龙岗区华宇新材料研究中心 | Micron-order composite material and preparation method thereof |
| WO2016069604A1 (en) * | 2014-10-27 | 2016-05-06 | Massachusetts, University Of | Micro-and nano-particles with variable surface morphologies and methods of making same |
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| WO2021088098A1 (en) | 2021-05-14 |
| CN110935394A (en) | 2020-03-31 |
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