WO2021088098A1 - Fine processing method and device for preparing micro/nano powder - Google Patents

Fine processing method and device for preparing micro/nano powder Download PDF

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WO2021088098A1
WO2021088098A1 PCT/CN2019/117250 CN2019117250W WO2021088098A1 WO 2021088098 A1 WO2021088098 A1 WO 2021088098A1 CN 2019117250 W CN2019117250 W CN 2019117250W WO 2021088098 A1 WO2021088098 A1 WO 2021088098A1
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micro
nano
particles
powder
rotor
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PCT/CN2019/117250
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French (fr)
Chinese (zh)
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雷宇雄
盖国胜
华炜迪
盖东海
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南京清大迈特新材料有限公司
马鞍山迈特峰新材料科技有限公司
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Publication of WO2021088098A1 publication Critical patent/WO2021088098A1/en

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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
    • 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
    • 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
    • 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
    • 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

Definitions

  • the invention relates to the field of powder deep processing, in particular to a method and device for fine processing of micro-nano powder.
  • powder materials have always been in an important position. Among them, powder smelting has continuously put forward higher requirements for powder materials. With the maturity of 3D printing technology and market applications in recent years, powder materials have also been brought to the public. At the same time, it also further promotes the development of powder materials; the new energy field is aimed at the demand for high-performance lithium batteries, especially involving the manufacture of lithium battery anode materials, which has also accelerated the development of powder materials.
  • powder materials are used as product raw materials, and the composition, purity, shape, particle distribution and other characteristics of their particles are closely related to the production and processing links and affect product quality.
  • Chinese patent application CN1827301A discloses a powder processing method and device, which realizes the shape trimming of powder particles to form a regular spherical shape, a small aspect ratio, and a large loose packing and tap density.
  • materials are required to have more excellent performance and purity.
  • people have proposed a composite particle for powder material particles.
  • traditional processing for composite powder material processing
  • chemical processing mechanical stirring or high-temperature pressing are used.
  • the powder particles produced by the above methods have the problems of low material purity and poor structural performance.
  • the present invention provides a fine processing method and device for micro-nano powder to solve the problem of existing composite powder processing.
  • a fine processing method of micro-nano powder is to add nano-scale sub-particles and micro-scale mother particles into a shaping device, and use a mechanical impact grinding method to process the nano-scale sub-particles and the micro-scale mother particles to obtain
  • the processing time of the micro-nano powder ranges from 0.5 min to 60 min
  • the particle size of the nano-scale sub-particles ranges from 0.1 nm to 10 ⁇ m
  • the particle size range of the micron-scale mother particles is 0.5 ⁇ m-1000 ⁇ m
  • the proportion of each component (weight ratio): the nano-scale daughter particles/the micron-scale mother particles are between 0.1% and 50%;
  • the processing process is:
  • Particle shaping The nano-sized sub-particles and micron-sized mother particles enter the shaping device through the feed inlet, and are impacted by high-speed blades and high-speed airflow, and irregular particles are shaped into spherical or quasi-spherical particles through high-speed physical impact;
  • Particle coating The nano-sized child particles impact the surface of the micron-level mother particle under the condition of high-speed movement, and are combined with the surface of the micron-level mother particle by adhesion, embedding or riveting.
  • the particle shaping process covers the surface of the micron-level mother particles.
  • water cooling is used to indirectly cool the material.
  • the high-speed gas flow is an inert gas flow.
  • the inert gas is selected from one of helium, nitrogen or argon.
  • nano-scale daughter particles and micron-scale mother particles are one or more of non-metallic mineral powder, metal powder, or organic polymer powder.
  • the average particle size of the micron-level mother particle powder is ⁇ 100 ⁇ m.
  • the rotational speed of the high-speed blade is between 1000 rpm and 10000 rpm.
  • the present invention also relates to the above-mentioned micro-nano powder fine processing shaping device, which includes: a stator, a rotor, a sealing cover, a sealing ring, a rotor blade, a fixed blade, an inner liner, a cooling water inlet, a cooling water outlet, and a feed inlet , Discharge port, protective gas inlet, protective gas outlet, rotating shaft.
  • the stator is a cylindrical shell, a through hole is opened at the center of the end face to install the rotating shaft, and the inner liner is nested inside;
  • the stator housing is provided with through holes to install the cooling water inlet and the cooling water outlet;
  • the stator and the inner liner are provided with 4 sets of corresponding through holes, and the inlet, the outlet, the protective gas inlet and the protective gas outlet are installed;
  • the rotor is a disc-shaped structure
  • the sealing ring is a disc-shaped structure, which is installed between the sealing cover and the embedded liner, and is provided with a special-shaped hole corresponding to the fixed blade with the embedded liner;
  • a through hole is provided at the center of the end face of the inner liner to install the rotating shaft;
  • the center of one side of the rotor is connected to the rotating shaft, and the other side is uniformly provided with 8 rotor blades along the rotation circumferential direction;
  • the rotor and the rotor blades are both located in the cavity of the inner liner.
  • the installation radius of the rotor blade is larger than the installation radius of the fixed blade, and rotation does not interfere in working conditions.
  • the inner surface of the inner liner is a ceramic lining of sprayed aluminum oxide or titanium nitride, and the rotor, the rotor blade and the fixed blade are all aluminum oxide, zirconium oxide or titanium nitride.
  • a ceramic material is
  • an interlayer is provided between the stator and the inner liner to store cooling water, and the interlayer is in communication with the cooling water inlet and the cooling water outlet.
  • the invention also relates to the micro-nano powder produced by the above-mentioned micro-nano powder fine processing method.
  • particle shaping adds the function of coating at the same time, and the final shape of the shaped particles is controlled by adjusting the speed and shaping time.
  • the impeller speed is between 1000rpm and 10000rpm. It has obvious polishing, shaping and coating effects for metal powders, especially small metal powders (average particle size of micron-level mother particles ⁇ 100 ⁇ m), which can increase the size of the ball. The characteristics of body fluidity and bulk density.
  • the internal surface of the shaping device is a ceramic structure.
  • the inner wall of the machine can be made of ceramic linings such as sprayed alumina and titanium nitride, and the rotor can be made of ceramic materials such as all alumina, zirconia or titanium nitride.
  • This kind of internal structure is wear-resistant, high-temperature resistant, corrosion-resistant, and has no pollution to the powder.
  • the interlayer of the shaping device is filled with cooling water, and the interior is filled with inert gas, so that the device can process flammable and explosive powders, increasing safety, and preventing oxidation reactions between materials and gases in the air, and improving the purity of powder materials.
  • Figure 1 is a schematic diagram of the particle shaping machine of the present invention
  • Figure 2 is a side view of the impeller rotor
  • Figure 3 is a side view of the sealing cover
  • Figure 4 is an electron microscope photo of aluminum powder coated with zirconium hydride before and after treatment (Figure 4-a is zirconium hydride powder, Figure 4-b is aluminum powder, Figure 4-c is aluminum powder coated zirconium hydride composite powder);
  • Figure 5 is the electron microscope photos before and after the copper powder coating aluminum treatment (Figure 5-d is the mixed powder before treatment, and Figure 5-e is the composite powder after treatment).
  • Nano-scale sub-particles and micro-scale mother particles are one or more of non-metallic mineral powder, metal powder, and organic polymer powder; the processing time of micro-nano powders ranges from 0.5 min to 60 min, and nano-scale sub-particles
  • the particle size range is 0.1nm-10 ⁇ m
  • the particle size range of micron-level mother particles is 0.5 ⁇ m-1000 ⁇ m
  • the proportion of each component (weight ratio): nano-level daughter particles/micron-level mother particles are between 0.1%-50%;
  • the average particle size of the selected micron-level mother particle powder is less than or equal to 100 ⁇ m.
  • the processing method is to add nano-scale sub-particles and micro-scale mother particles to the shaping device, and use mechanical impact grinding to process the powder particles to obtain micro-nano powder.
  • the processing process is:
  • Nano-sized sub-particles and micron-sized mother particles enter the shaping device through the feed inlet, and are impacted by high-speed blades and high-speed airflow to shape irregular particles into spherical or quasi-spherical particles through high-speed physical impact;
  • the high-speed gas flow introduced into the device is an inert gas flow, and it is preferably designed such that the inert gas can be one of helium, nitrogen or argon;
  • the speed of high-speed blades is between 1000rpm-10000rpm;
  • Particle coating When the nano-scale child particles are moving at high speed, they impact the surface of the micron-level mother particles, and are combined with the surface of the micron-level mother particles by adhesion, embedding or riveting, and then they are coated on the micron after the particle shaping process. Grade mother particle surface.
  • the shaping device includes: stator 1, rotor 2, sealing cover 3, sealing ring 4, rotor blades 5, fixed blades 6, embedded liner 7, cooling water inlet 8, cooling water outlet 9, and feed Port 10, discharge port 11, protective gas inlet 12, protective gas outlet 13, and rotating shaft 14.
  • the stator 1 is a cylindrical shell with a through hole at the center of the end face to install the shaft 14;
  • the rotor 2 is a disc-shaped structure, and the center is connected to the shaft 14;
  • the rotor 2, the rotor blades 5 and the fixed blades 6 are all It is in the built-in liner 7;
  • the stator 1 shell is provided with through-holes to install the cooling water inlet 8 and the cooling water outlet 9;
  • the stator 1 and the embedded liner 7 form an interlayer to store the cooling water, and are opened with the built-in liner 7
  • There are 4 sets of corresponding through holes, and the inlet 10, the outlet 11, the protective gas inlet 12, and the protective gas outlet 13 are installed.
  • 8 rotor blades 5 are evenly distributed along the rotation circumferential direction on one side of the rotor 2, and the center of the other side is connected with the rotating shaft 14.
  • the sealing cover 3 evenly distributes 8 fixed blades 6 along the circumferential direction.
  • the sealing ring 4 and the inner liner 7 are provided with special-shaped holes corresponding to the fixed blades 6; the installation radius of the rotor blades 5 is larger than that of the fixed blades 6. Radius, rotation does not interfere under working conditions;
  • the internal surface of the shaping device is a ceramic structure, preferably designed such that the inner surface of the inner liner 7 is sprayed with a ceramic lining of alumina or titanium nitride, and the rotor 2, the rotor blade 5 and the fixed blade 6 are all alumina, oxidized One of the ceramic materials of zirconium or titanium nitride.
  • Preparation stage According to the requirements of the powder material product, select the powder with the appropriate average particle size of the child and mother particles respectively, calculate the composition ratio, and mechanically stir and mix the prepared powder; the device is filled with inert gas, connected to the external cooling water cycle, and Power-on start device.
  • Zirconium hydride is a nuclear reaction moderator.
  • the above methods and devices are used to coat the surface of aluminum powder particles with zirconium hydride particles.
  • the processing conditions are as follows:
  • the (mass ratio) ratio of zirconium hydride particles to aluminum powder particles 5%;
  • Average particle size of zirconium hydride particles 58nm;
  • Average particle size of aluminum powder particles 43 ⁇ m;
  • the protective gas composition is: nitrogen;
  • the speed of the high-speed blade is: 5500rpm;
  • the zirconium hydride particle powder in Figure 4-a and the aluminum powder in Figure 4-b are processed, and the zirconium hydride particles are coated on the surface of the aluminum powder particles to form a hemp-like coating in Figure 4-c. Effectively improve the performance of aluminum.
  • the above method and device are used to coat a layer of aluminum on the outside of the copper powder particles.
  • the processing conditions are as follows:
  • the ratio of aluminum powder particles to copper powder particles (mass ratio): 30%;
  • Average particle size of aluminum powder particles 1 ⁇ m
  • Average particle size of copper powder particles 22 ⁇ m
  • the protective gas composition is: nitrogen;
  • the speed of the high-speed blade is: 6800rpm;
  • the mixed particles of aluminum powder and copper powder in Figure 5-d are processed to form composite particles with a core-shell structure in Figure 5-e that are wrapped with aluminum, which can reduce the external corrosiveness of copper powder and reduce copper oxidation.
  • the purpose of speed can reduce the external corrosiveness of copper powder and reduce copper oxidation.

Abstract

Provided are a fine processing method and device for preparing a micro/nano powder for use in the production a composite micro/nano powder particle. The method comprises: attaching a nano-powder particle to a micro-powder particle by means of mechanical impact milling; and simultaneously shaping the nano-powder particle and the micro-powder particle into spherical or sphere-like particles. The invention can improve properties of a powdery material. In addition, the invention can reduce impurities in a powder by modifying an inner surface of a processing device, thereby improving processing quality.

Description

一种微纳粉体精细加工方法及装置Method and device for fine processing of micro-nano powder 技术领域Technical field
本发明涉及粉体深加工领域，尤其涉及一种微纳粉体精细加工方法及装置。The invention relates to the field of powder deep processing, in particular to a method and device for fine processing of micro-nano powder.
背景技术Background technique
现有材料领域，粉体物料一直处于重要地位，其中粉末冶炼不断对粉体物料提出更高的要求，并伴随近些年3D打印技术的成熟及市场应用，也将粉体物料带入了大众的视野，同时也进一步推动粉体物料的发展；新能源领域针对高性能锂电池的需求，尤其涉及锂电池负极材料的制造，也加速了粉体物料的发展。实际工作中粉体物料作为产品原材料，其颗粒的成分、纯度、外形、颗粒分布等特征密切关联着生产加工环节，影响着产品质量。In the field of existing materials, powder materials have always been in an important position. Among them, powder smelting has continuously put forward higher requirements for powder materials. With the maturity of 3D printing technology and market applications in recent years, powder materials have also been brought to the public. At the same time, it also further promotes the development of powder materials; the new energy field is aimed at the demand for high-performance lithium batteries, especially involving the manufacture of lithium battery anode materials, which has also accelerated the development of powder materials. In actual work, powder materials are used as product raw materials, and the composition, purity, shape, particle distribution and other characteristics of their particles are closely related to the production and processing links and affect product quality.
中国专利申请CN1827301A中公开了一种粉体加工方法及装置，实现了针对粉体颗粒的外形修整，使其形成规则的球状外形，长径比小且松装与振实密度大。但是实际生产中，随着产品要求不断地提高，需要物料具备更加优异的性能及纯度，为此人们针对粉体物料颗粒提出了一种复合型颗粒，传统加工中，针对复合型粉体物料加工一般采用化学加工、机械搅拌或者高温压制的方法，以上方法制造的粉体颗粒存在材料纯度不高、结构性能不好的问题。Chinese patent application CN1827301A discloses a powder processing method and device, which realizes the shape trimming of powder particles to form a regular spherical shape, a small aspect ratio, and a large loose packing and tap density. However, in actual production, with the continuous improvement of product requirements, materials are required to have more excellent performance and purity. For this reason, people have proposed a composite particle for powder material particles. In traditional processing, for composite powder material processing Generally, chemical processing, mechanical stirring or high-temperature pressing are used. The powder particles produced by the above methods have the problems of low material purity and poor structural performance.
综上，需要一种粉体加工方法及装置，在复合粉体物料生产过程中，既能够生产高性能粉体物料，又能保证物料的纯度。In summary, there is a need for a powder processing method and device that can not only produce high-performance powder materials in the production process of composite powder materials, but also ensure the purity of the materials.
发明内容Summary of the invention
有鉴于此，本发明提供一种微纳粉体精细加工方法及装置，以解决现有复合型粉体加工的问题。In view of this, the present invention provides a fine processing method and device for micro-nano powder to solve the problem of existing composite powder processing.
为此目的，本发明由如下技术方案实施：For this purpose, the present invention is implemented by the following technical solutions:
一种微纳粉体精细加工方法，所述方法是将纳米级子颗粒与微米级母颗粒加入整形装置，利用机械冲击研磨法对所述纳米级子颗粒和所述微米级母颗粒处理，得到所述微纳粉体，所述微纳粉体加工时间范围为0.5min-60min，所述纳米 级子颗粒的粒径范围为0.1nm-10μm，所述微米级母颗粒的粒径范围为0.5μm-1000μm，各成分比例(重量比)：所述纳米级子颗粒/所述微米级母颗粒在0.1％-50％之间；A fine processing method of micro-nano powder, the method is to add nano-scale sub-particles and micro-scale mother particles into a shaping device, and use a mechanical impact grinding method to process the nano-scale sub-particles and the micro-scale mother particles to obtain For the micro-nano powder, the processing time of the micro-nano powder ranges from 0.5 min to 60 min, the particle size of the nano-scale sub-particles ranges from 0.1 nm to 10 μm, and the particle size range of the micron-scale mother particles is 0.5 μm-1000 μm, the proportion of each component (weight ratio): the nano-scale daughter particles/the micron-scale mother particles are between 0.1% and 50%;
加工过程为：The processing process is:
1.颗粒整形：所述纳米级子颗粒与微米级母颗粒通过进料口进入整形装置，经过高速叶片及高速气流冲击，将不规则的颗粒通过高速物理冲击整形成球形、类球形的颗粒；1. Particle shaping: The nano-sized sub-particles and micron-sized mother particles enter the shaping device through the feed inlet, and are impacted by high-speed blades and high-speed airflow, and irregular particles are shaped into spherical or quasi-spherical particles through high-speed physical impact;
2.颗粒包覆：所述纳米级子颗粒在高速运动的情况下，冲击所述微米级母颗粒表面，并以附着、嵌入或铆焊的方式与所述微米级母颗粒表面结合，经过所述颗粒整形过程包覆于所述微米级母颗粒表面。2. Particle coating: The nano-sized child particles impact the surface of the micron-level mother particle under the condition of high-speed movement, and are combined with the surface of the micron-level mother particle by adhesion, embedding or riveting. The particle shaping process covers the surface of the micron-level mother particles.
加工过程中，采用水冷的方式间接为物料降温。During the processing, water cooling is used to indirectly cool the material.
进一步，所述颗粒整形和颗粒包覆过程为相同条件下，同时发生。Further, the particle shaping and particle coating processes occur simultaneously under the same conditions.
进一步，所述高速气流为惰性气体流。Further, the high-speed gas flow is an inert gas flow.
更进一步，所述惰性气体选自氦气、氮气或氩气其中一种。Furthermore, the inert gas is selected from one of helium, nitrogen or argon.
进一步，所述纳米级子颗粒与微米级母颗粒为非金属矿物粉体、金属粉体或有机高分子粉体中的一种或多种。Further, the nano-scale daughter particles and micron-scale mother particles are one or more of non-metallic mineral powder, metal powder, or organic polymer powder.
更进一步，对于所述金属粉体，微米级母颗粒粉体平均粒径≤100μm。Furthermore, for the metal powder, the average particle size of the micron-level mother particle powder is ≤ 100 μm.
进一步，所述高速叶片转速在1000rpm-10000rpm之间。Further, the rotational speed of the high-speed blade is between 1000 rpm and 10000 rpm.
本发明还涉及上述微纳粉体精细加工的整形装置，其包括：定子、转子、密封盖、密封圈、转子叶片、固定叶片、内嵌内胆、冷却水进口、冷却水出口、进料口、出料口、保护气体入口、保护气体出口、转轴。The present invention also relates to the above-mentioned micro-nano powder fine processing shaping device, which includes: a stator, a rotor, a sealing cover, a sealing ring, a rotor blade, a fixed blade, an inner liner, a cooling water inlet, a cooling water outlet, and a feed inlet , Discharge port, protective gas inlet, protective gas outlet, rotating shaft.
所述定子为圆柱状壳体，端面中心处开设有通孔安装所述转轴，内部嵌套所述内嵌内胆；The stator is a cylindrical shell, a through hole is opened at the center of the end face to install the rotating shaft, and the inner liner is nested inside;
所述定子外壳开设有通孔安装所述冷却水进口及所述冷却水出口；The stator housing is provided with through holes to install the cooling water inlet and the cooling water outlet;
所述定子与所述内嵌内胆开设有4组相对应通孔，安装所述进料口、所述出 料口、所述保护气体入口及所述保护气体出口；The stator and the inner liner are provided with 4 sets of corresponding through holes, and the inlet, the outlet, the protective gas inlet and the protective gas outlet are installed;
所述转子为圆盘状结构；The rotor is a disc-shaped structure;
所述密封盖上沿圆周方向均匀分布8个所述固定叶片；8 fixed blades are evenly distributed along the circumferential direction on the sealing cover;
所述密封圈为圆片状结构，安装于所述密封盖与所述内嵌内胆之间，并与所述内嵌内胆开设有相对应所述固定叶片的异形孔；所述内嵌内胆侧端面中心处开设有通孔安装所述转轴；所述转子一侧中心处连接所述转轴，另一侧沿旋转圆周方向均匀设置有8个所述转子叶片；所述固定叶片、所述转子及所述转子叶片均处于所述内嵌内胆的空腔中。The sealing ring is a disc-shaped structure, which is installed between the sealing cover and the embedded liner, and is provided with a special-shaped hole corresponding to the fixed blade with the embedded liner; A through hole is provided at the center of the end face of the inner liner to install the rotating shaft; the center of one side of the rotor is connected to the rotating shaft, and the other side is uniformly provided with 8 rotor blades along the rotation circumferential direction; The rotor and the rotor blades are both located in the cavity of the inner liner.
进一步，所述转子叶片安装半径大于所述固定叶片安装半径，工作情况下转动不干涉。Further, the installation radius of the rotor blade is larger than the installation radius of the fixed blade, and rotation does not interfere in working conditions.
进一步，所述内嵌内胆内表面为喷涂氧化铝或氮化钛中一种陶瓷内衬，所述转子、所述转子叶片及所述固定叶片为全氧化铝、氧化锆或氮化钛其中一种陶瓷材质。Further, the inner surface of the inner liner is a ceramic lining of sprayed aluminum oxide or titanium nitride, and the rotor, the rotor blade and the fixed blade are all aluminum oxide, zirconium oxide or titanium nitride. A ceramic material.
进一步，所述定子与所述内嵌内胆之间设有夹层，可以存储冷却水，所述夹层与所述冷却水进口、所述冷却水出口相连通。Further, an interlayer is provided between the stator and the inner liner to store cooling water, and the interlayer is in communication with the cooling water inlet and the cooling water outlet.
本发明还涉及上述的微纳粉体精细加工方法生产的微纳粉体。The invention also relates to the micro-nano powder produced by the above-mentioned micro-nano powder fine processing method.
本发明具有如下优点：The present invention has the following advantages:
1.不受两种或多种颗粒之间热力学、化学反应可行性的制约，颗粒整形同时添加包覆的功能，通过调整转速以及整形时间来控制被整形颗粒的最终形态结果。叶轮转速在1000rpm-10000rpm之间，对于金属粉体、尤其是小颗粒金属粉体(微米级母颗粒平均粒径≤100μm)的颗粒的抛光整形以及包覆效果明显，可以实现增加球粒度，粉体流动性和松装密度的特性。1. Not restricted by the feasibility of thermodynamics and chemical reactions between two or more kinds of particles, particle shaping adds the function of coating at the same time, and the final shape of the shaped particles is controlled by adjusting the speed and shaping time. The impeller speed is between 1000rpm and 10000rpm. It has obvious polishing, shaping and coating effects for metal powders, especially small metal powders (average particle size of micron-level mother particles≤100μm), which can increase the size of the ball. The characteristics of body fluidity and bulk density.
2.整形装置内部表面为陶瓷结构。机体内壁可选择为喷涂氧化铝、氮化钛等陶瓷内衬，转子可以为全氧化铝、氧化锆或氮化钛等陶瓷材质。此类内结构耐磨、耐高温、耐腐蚀，对于粉体无污染。2. The internal surface of the shaping device is a ceramic structure. The inner wall of the machine can be made of ceramic linings such as sprayed alumina and titanium nitride, and the rotor can be made of ceramic materials such as all alumina, zirconia or titanium nitride. This kind of internal structure is wear-resistant, high-temperature resistant, corrosion-resistant, and has no pollution to the powder.
3.整形装置夹层通有冷却水，内部充满惰性气体，使装置可以加工易燃易 爆粉体，增加安全性，也防止材料与空气中的气体产生氧化反应，提升粉体物料纯度。3. The interlayer of the shaping device is filled with cooling water, and the interior is filled with inert gas, so that the device can process flammable and explosive powders, increasing safety, and preventing oxidation reactions between materials and gases in the air, and improving the purity of powder materials.
附图说明Description of the drawings
图中：In the figure:
1-定子；2-转子；3-密封盖；4-密封圈；5-转子叶片；6-固定叶片；7-内嵌内胆；8-冷却水进口；9-冷却水出口；10-进料口；11-出料口；12-保护气体入口；13-保护气体出口；14-转轴。1-stator; 2-rotor; 3-seal cover; 4-seal; 5-rotor blades; 6-fixed blades; 7-inline tank; 8-cooling water inlet; 9-cooling water outlet; 10-inlet Material port; 11-discharge port; 12-protective gas inlet; 13-protective gas outlet; 14-rotation shaft.
图1为本发明的颗粒整形机示意图；Figure 1 is a schematic diagram of the particle shaping machine of the present invention;
图2为叶轮转子侧视图；Figure 2 is a side view of the impeller rotor;
图3为密封盖侧视图；Figure 3 is a side view of the sealing cover;
图4为铝粉覆氢化锆处理前后电镜照片(图4-a为氢化锆粉体，图4-b为铝粉体，图4-c为铝粉覆氢化锆复合粉体)；Figure 4 is an electron microscope photo of aluminum powder coated with zirconium hydride before and after treatment (Figure 4-a is zirconium hydride powder, Figure 4-b is aluminum powder, Figure 4-c is aluminum powder coated zirconium hydride composite powder);
图5为铜粉覆铝处理前后电镜照片(图5-d为处理前混合粉体，图5-e为处理后复合粉体)。Figure 5 is the electron microscope photos before and after the copper powder coating aluminum treatment (Figure 5-d is the mixed powder before treatment, and Figure 5-e is the composite powder after treatment).
具体实施方式Detailed ways
以下结合附图对本发明的内容作进一步说明。The content of the present invention will be further described below in conjunction with the accompanying drawings.
纳米级子颗粒与微米级母颗粒为非金属矿物粉体、金属粉体、有机高分子粉体中的一种或多种；微纳粉体加工时间范围为0.5min-60min，纳米级子颗粒的粒径范围为0.1nm-10μm，微米级母颗粒的粒径范围为0.5μm-1000μm，各成分比例(重量比)：纳米级子颗粒/微米级母颗粒在0.1％-50％之间；Nano-scale sub-particles and micro-scale mother particles are one or more of non-metallic mineral powder, metal powder, and organic polymer powder; the processing time of micro-nano powders ranges from 0.5 min to 60 min, and nano-scale sub-particles The particle size range is 0.1nm-10μm, the particle size range of micron-level mother particles is 0.5μm-1000μm, and the proportion of each component (weight ratio): nano-level daughter particles/micron-level mother particles are between 0.1%-50%;
优选设计为，加工粉体为金属粉体时，所选微米级母颗粒粉体平均粒径≤100μm。The preferred design is that when the processed powder is a metal powder, the average particle size of the selected micron-level mother particle powder is less than or equal to 100 μm.
加工方法是将纳米级子颗粒与微米级母颗粒加入整形装置，利用机械冲击研磨法对粉体颗粒处理，得到微纳粉体，加工过程为：The processing method is to add nano-scale sub-particles and micro-scale mother particles to the shaping device, and use mechanical impact grinding to process the powder particles to obtain micro-nano powder. The processing process is:
1.颗粒整形：纳米级子颗粒与微米级母颗粒通过进料口进入整形装置，经过 高速叶片及高速气流冲击，将不规则的颗粒通过高速物理冲击整形成球形、类球形的颗粒；1. Particle shaping: Nano-sized sub-particles and micron-sized mother particles enter the shaping device through the feed inlet, and are impacted by high-speed blades and high-speed airflow to shape irregular particles into spherical or quasi-spherical particles through high-speed physical impact;
装置内通入的高速气流为惰性气体流，优选设计为，惰性气体可为氦气、氮气或氩气其中一种；The high-speed gas flow introduced into the device is an inert gas flow, and it is preferably designed such that the inert gas can be one of helium, nitrogen or argon;
高速叶片转速在1000rpm-10000rpm之间；The speed of high-speed blades is between 1000rpm-10000rpm;
2.颗粒包覆：纳米级子颗粒在高速运动的情况下，冲击微米级母颗粒表面，并以附着、嵌入或铆焊的方式与微米级母颗粒表面结合，经过颗粒整形过程包覆于微米级母颗粒表面。2. Particle coating: When the nano-scale child particles are moving at high speed, they impact the surface of the micron-level mother particles, and are combined with the surface of the micron-level mother particles by adhesion, embedding or riveting, and then they are coated on the micron after the particle shaping process. Grade mother particle surface.
以上加工过程的两部分为相同条件下，同时发生；加工过程中，采用水冷的方式间接为物料降温。The two parts of the above processing process happen at the same time under the same conditions; in the processing process, water cooling is used to indirectly cool the material.
详细介绍整形装置结构：The structure of the shaping device is introduced in detail:
如图1所示，整形装置包括：定子1、转子2、密封盖3、密封圈4、转子叶片5、固定叶片6、内嵌内胆7、冷却水进口8、冷却水出口9、进料口10、出料口11、保护气体入口12、保护气体出口13、转轴14。As shown in Figure 1, the shaping device includes: stator 1, rotor 2, sealing cover 3, sealing ring 4, rotor blades 5, fixed blades 6, embedded liner 7, cooling water inlet 8, cooling water outlet 9, and feed Port 10, discharge port 11, protective gas inlet 12, protective gas outlet 13, and rotating shaft 14.
如图1所示，定子1为圆柱状壳体，端面中心处开设有通孔安装转轴14；转子2为圆盘状结构，中心处连接转轴14；转子2、转子叶片5及固定叶片6均处于内嵌内胆7中；定子1外壳开设有通孔安装冷却水进口8、冷却水出口9；定子1与内嵌内胆7中间形成夹层可存储冷却水，并与内嵌内胆7开设4组相对应通孔，安装进料口10、出料口11、保护气体入口12、保护气体出口13。As shown in Figure 1, the stator 1 is a cylindrical shell with a through hole at the center of the end face to install the shaft 14; the rotor 2 is a disc-shaped structure, and the center is connected to the shaft 14; the rotor 2, the rotor blades 5 and the fixed blades 6 are all It is in the built-in liner 7; the stator 1 shell is provided with through-holes to install the cooling water inlet 8 and the cooling water outlet 9; the stator 1 and the embedded liner 7 form an interlayer to store the cooling water, and are opened with the built-in liner 7 There are 4 sets of corresponding through holes, and the inlet 10, the outlet 11, the protective gas inlet 12, and the protective gas outlet 13 are installed.
如图2所示，转子2一侧沿旋转圆周方向均匀分布8个转子叶片5，另一侧中心处与转轴14连接。As shown in FIG. 2, 8 rotor blades 5 are evenly distributed along the rotation circumferential direction on one side of the rotor 2, and the center of the other side is connected with the rotating shaft 14.
如图3所示，密封盖3沿圆周方向均匀分布8个固定叶片6，密封圈4与内嵌内胆7开设有相对应固定叶片6的异形孔；转子叶片5安装半径大于固定叶片6安装半径，工作情况下转动不干涉；As shown in Figure 3, the sealing cover 3 evenly distributes 8 fixed blades 6 along the circumferential direction. The sealing ring 4 and the inner liner 7 are provided with special-shaped holes corresponding to the fixed blades 6; the installation radius of the rotor blades 5 is larger than that of the fixed blades 6. Radius, rotation does not interfere under working conditions;
整形装置内部表面为陶瓷结构，优选设计为，内嵌内胆7内表面为喷涂氧化铝或氮化钛中一种陶瓷内衬，转子2、转子叶片5及固定叶片6为全氧化铝、氧 化锆或氮化钛其中一种陶瓷材质。The internal surface of the shaping device is a ceramic structure, preferably designed such that the inner surface of the inner liner 7 is sprayed with a ceramic lining of alumina or titanium nitride, and the rotor 2, the rotor blade 5 and the fixed blade 6 are all alumina, oxidized One of the ceramic materials of zirconium or titanium nitride.
具体加工流程：Specific processing flow:
1.准备阶段。依据粉体物料产品要求，分别选取子、母颗粒平均粒径合适的粉体，计算成分组成比，并将配好的粉体机械搅拌混合；装置通入惰性气体，接通外部冷却水循环，并通电启动装置。1. Preparation stage. According to the requirements of the powder material product, select the powder with the appropriate average particle size of the child and mother particles respectively, calculate the composition ratio, and mechanically stir and mix the prepared powder; the device is filled with inert gas, connected to the external cooling water cycle, and Power-on start device.
2.加工阶段。当装置转子叶轮达到设计转速时，将混合粉体物料通过进料口推入装置内部，开始加工。2. Processing stage. When the rotor impeller of the device reaches the design speed, the mixed powder material is pushed into the device through the feed port to start processing.
3.收集检验阶段。当加工时间到达设计时间，关闭装置电源，保持冷却水循环直至内部物料降至室温后关闭，打开出料口倾倒出初步加工的粉体物料；将粉体物料送至分拣机进行分拣，并对分拣后的产品进行抽样微观检测，符合设计标准表示一次完整加工完成。3. Collection and inspection stage. When the processing time reaches the design time, turn off the power supply of the device, keep the cooling water circulating until the internal materials drop to room temperature and then turn off, open the discharge port to pour out the preliminary processed powder materials; send the powder materials to the sorter for sorting, and Sampling and micro-testing the sorted products, meeting the design standard means that a complete processing is completed.
实施例1Example 1
氢化锆是一种核反应慢化剂，铝材在用于核反应堆构件时为了避免反应堆对构件的影响，应用上述方法及装置将氢化锆微粒包覆于铝粉颗粒表面，加工条件如下：Zirconium hydride is a nuclear reaction moderator. When aluminum is used in nuclear reactor components, in order to avoid the impact of the reactor on the components, the above methods and devices are used to coat the surface of aluminum powder particles with zirconium hydride particles. The processing conditions are as follows:
氢化锆微粒与铝粉颗粒的(质量比)比例：5％；The (mass ratio) ratio of zirconium hydride particles to aluminum powder particles: 5%;
氢化锆微粒的平均粒径：58nm；Average particle size of zirconium hydride particles: 58nm;
铝粉颗粒的平均粒径：43μm；Average particle size of aluminum powder particles: 43μm;
保护气体成分为：氮气；The protective gas composition is: nitrogen;
高速叶片的转速为：5500rpm；The speed of the high-speed blade is: 5500rpm;
加工时间：8min。Processing time: 8min.
如图4所示，图4-a中氢化锆微粒粉体与图4-b铝粉经过加工，氢化锆微粒包覆于铝粉颗粒表面，形成图4-c中类麻团状包覆，有效地提升铝材性能。As shown in Figure 4, the zirconium hydride particle powder in Figure 4-a and the aluminum powder in Figure 4-b are processed, and the zirconium hydride particles are coated on the surface of the aluminum powder particles to form a hemp-like coating in Figure 4-c. Effectively improve the performance of aluminum.
实施例2Example 2
铜作为原材料有着优异的导电性和加工性，有着多种用途，但是铜的易腐蚀性和易氧化性常常给应用带来局限。为解决该类问题，应用上述方法及装置，在铜粉颗粒的外部包覆一层铝，加工条件如下:As a raw material, copper has excellent electrical conductivity and processability, and has a variety of uses. However, the corrosion and oxidation properties of copper often limit the application. In order to solve this type of problem, the above method and device are used to coat a layer of aluminum on the outside of the copper powder particles. The processing conditions are as follows:
铝粉颗粒与铜粉颗粒的(质量比)比例：30％；The ratio of aluminum powder particles to copper powder particles (mass ratio): 30%;
铝粉颗粒的平均粒径：1μm；Average particle size of aluminum powder particles: 1μm;
铜粉颗粒的平均粒径：22μm；Average particle size of copper powder particles: 22μm;
保护气体成分为：氮气；The protective gas composition is: nitrogen;
高速叶片的转速为：6800rpm；The speed of the high-speed blade is: 6800rpm;
加工时间：22min。Processing time: 22min.
如图5所示，图5-d中铝粉、铜粉混合颗粒经过加工形成图5-e中外部包裹铝的核壳结构复合颗粒，可以降低外界对铜粉的腐蚀性，达到减缓铜氧化速度的目的。As shown in Figure 5, the mixed particles of aluminum powder and copper powder in Figure 5-d are processed to form composite particles with a core-shell structure in Figure 5-e that are wrapped with aluminum, which can reduce the external corrosiveness of copper powder and reduce copper oxidation. The purpose of speed.
上述详细说明是针对本发明其中之一可行实施例的具体说明，该实施例并非用以限制本发明的专利范围，凡未脱离本发明所为的等效实施或变更，均应包含于本发明技术方案的范围内。The above detailed description is a specific description of one of the possible embodiments of the present invention. This embodiment is not intended to limit the patent scope of the present invention. Any equivalent implementation or modification that does not deviate from the present invention should be included in the present invention. Within the scope of technical solutions.

Claims (10)

  1. 一种微纳粉体精细加工方法，其特征在于：所述方法是将纳米级子颗粒与微米级母颗粒加入整形装置，利用机械冲击研磨法对所述纳米级子颗粒和所述微米级母颗粒处理，得到所述微纳粉体，所述微纳粉体加工时间范围为0.5min-60min，所述纳米级子颗粒的粒径范围为0.1nm-10μm，所述微米级母颗粒的粒径范围为0.5μm-1000μm，各成分比例(重量比)：所述纳米级子颗粒/所述微米级母颗粒在0.1％-50％之间；A fine processing method of micro-nano powder, which is characterized in that: the method is to add nano-scale child particles and micro-scale mother particles into a shaping device, and use a mechanical impact grinding method to treat the nano-scale child particles and the micron-level mother particles. Particle processing to obtain the micro-nano powder, the processing time of the micro-nano powder ranges from 0.5 min to 60 min, and the particle size of the nano-scale daughter particles ranges from 0.1 nm to 10 μm. The diameter range is 0.5 μm-1000 μm, and the ratio of each component (weight ratio): the nano-scale daughter particles/the micron-scale mother particles are between 0.1% and 50%;
    加工过程为：The processing process is:
    (1)颗粒整形：所述纳米级子颗粒与微米级母颗粒通过进料口进入整形装置，经过高速叶片及高速气流冲击，将不规则的颗粒通过高速物理冲击整形成球形、类球形的颗粒；(1) Particle shaping: The nano-sized sub-particles and micron-sized mother particles enter the shaping device through the feed port, and are impacted by high-speed blades and high-speed airflow, and irregular particles are shaped into spherical or quasi-spherical particles through high-speed physical impact. ；
    (2)颗粒包覆：所述纳米级子颗粒在高速运动的情况下，冲击所述微米级母颗粒表面，并以附着、嵌入或铆焊的方式与所述微米级母颗粒表面结合，经过所述颗粒整形过程包覆于所述微米级母颗粒表面；(2) Particle coating: The nano-sized child particles impact the surface of the micron-level mother particles under the condition of high-speed movement, and are combined with the surface of the micron-level mother particles by adhesion, embedding or riveting. The particle shaping process covers the surface of the micron-level mother particles;
    加工过程中，采用水冷的方式间接为物料降温。During the processing, water cooling is used to indirectly cool the material.
  2. 根据权利要求1所述一种微纳粉体精细加工方法，其特征在于，所述颗粒整形和颗粒包覆过程为相同条件下，同时发生。The fine processing method of micro-nano powder according to claim 1, wherein the particle shaping and particle coating processes occur simultaneously under the same conditions.
  3. 根据权利要求1所述一种微纳粉体精细加工方法，其特征在于，所述高速气流为惰性气体流。The method for fine processing of micro-nano powders according to claim 1, wherein the high-speed gas flow is an inert gas flow.
  4. 根据权利要求1所述一种微纳粉体精细加工方法，其特征在于，所述纳米级子颗粒与微米级母颗粒为非金属矿物粉体、金属粉体或有机高分子粉体中的一种或多种；对于所述金属粉体，微米级母颗粒粉体平均粒径≤100μm。The method for fine processing of micro-nano powders according to claim 1, wherein the nano-scale sub-particles and micro-scale mother particles are one of non-metallic mineral powder, metal powder or organic polymer powder. One or more kinds; for the metal powder, the average particle size of the micron-level mother particle powder is less than or equal to 100 μm.
  5. 根据权利要求1所述一种微纳粉体精细加工方法，其特征在于，所述高速叶片转速在1000rpm-10000rpm之间。The fine processing method of micro-nano powder according to claim 1, wherein the speed of the high-speed blade is between 1000 rpm and 10000 rpm.
  6. 根据权利要求1-5中任一项所述的一种微纳粉体精细加工方法进行微纳粉体精细加工的装置，其包括：定子(1)、转子(2)、密封盖(3)、密封圈(4)、转子叶片(5)、固定叶片(6)、内嵌内胆(7)、冷却水进口(8)、冷却水出口(9)、进料口(10)、出料口(11)、保护气体入口(12)、保护气体出口(13)、转轴(14)；A device for fine processing of micro/nano powder according to any one of claims 1 to 5, comprising: a stator (1), a rotor (2), and a sealing cover (3) , Sealing ring (4), rotor blades (5), fixed blades (6), built-in liner (7), cooling water inlet (8), cooling water outlet (9), inlet (10), discharge Port (11), protective gas inlet (12), protective gas outlet (13), rotating shaft (14);
    所述定子(1)为圆柱状壳体，端面中心处开设有通孔安装所述转轴(14)，内部嵌套所述内嵌内胆(7)；The stator (1) is a cylindrical shell, a through hole is opened at the center of the end face to install the rotating shaft (14), and the inner liner (7) is nested inside;
    所述定子(1)外壳开设有通孔安装所述冷却水进口(8)及所述冷却水出口(9)；The stator (1) shell is provided with a through hole to install the cooling water inlet (8) and the cooling water outlet (9);
    所述定子(1)外壳与所述内嵌内胆(7)开设有4组相对应通孔，安装所述进料口(10)、所述出料口(11)、所述保护气体入口(12)及所述保护气体出口(13)；The stator (1) shell and the inner liner (7) are provided with 4 sets of corresponding through holes, and the inlet (10), the outlet (11), and the protective gas inlet are installed. (12) and the protective gas outlet (13);
    所述转子(2)为圆盘状结构；The rotor (2) is a disc-shaped structure;
    所述密封盖(3)上沿圆周方向均匀分布8个所述固定叶片(6)；Eight fixed blades (6) are evenly distributed along the circumferential direction on the sealing cover (3);
    其特征在于，所述密封圈(4)为圆片状，安装于所述密封盖(3)与所述内嵌内胆(7)之间，并与所述内嵌内胆(7)开设有相对应所述固定叶片(6)的异形孔；所述内嵌内胆(7)侧端面中心处开设有通孔安装所述转轴(14)；所述转子(2)一侧中心处连接所述转轴(14)，另一侧沿旋转圆周方向均匀设置有8个所述转子叶片(5)；所述固定叶片(6)、所述转子(2)及所述转子叶片(5)均处于所述内嵌内胆(7)的空腔中。It is characterized in that the sealing ring (4) is in the shape of a disc, and is installed between the sealing cover (3) and the embedded liner (7), and is opened with the embedded liner (7) There is a special-shaped hole corresponding to the fixed blade (6); a through hole is opened at the center of the side end surface of the inner liner (7) to install the rotating shaft (14); the rotor (2) is connected at the center of one side On the other side of the rotating shaft (14), eight rotor blades (5) are uniformly arranged along the rotation circumferential direction; the fixed blades (6), the rotor (2) and the rotor blades (5) are all It is located in the cavity of the embedded inner liner (7).
  7. 根据权利要求6所述的一种微纳粉体精细加工装置，其特征在于，所述内嵌内胆(7)内表面为喷涂氧化铝或氮化钛中一种陶瓷内衬，所述转子(2)、所述转子叶片(5)及所述固定叶片(6)为全氧化铝、氧化锆或氮化钛其中一种陶瓷材质。The micro-nano powder fine processing device according to claim 6, characterized in that the inner surface of the inner liner (7) is a ceramic lining of sprayed alumina or titanium nitride, and the rotor (2) The rotor blade (5) and the fixed blade (6) are made of ceramic material of one of alumina, zirconia or titanium nitride.
  8. 根据权利要求6所述的一种微纳粉体精细加工装置，其特征在于，所述转子叶片(5)安装半径大于所述固定叶片(6)安装半径，工作情况下转动不干涉。The micro-nano powder fine processing device according to claim 6, characterized in that the installation radius of the rotor blade (5) is larger than the installation radius of the fixed blade (6), and rotation does not interfere in working conditions.
  9. 根据权利要求6所述的一种微纳粉体精细加工装置，其特征在于，所述定子(1)与所述内嵌内胆(7)之间设有夹层，所述夹层与所述冷却水进口(8)、所述冷却水出口(9)相连通。The micro-nano powder fine processing device according to claim 6, characterized in that, an interlayer is provided between the stator (1) and the embedded inner liner (7), and the interlayer and the cooling The water inlet (8) and the cooling water outlet (9) are communicated.
  10. 一种由权利要求1-5中任一项所述的微纳粉体精细加工方法生产的微纳粉体。A micro-nano powder produced by the micro-nano powder fine processing method according to any one of claims 1-5.
PCT/CN2019/117250 2019-11-05 2019-11-11 Fine processing method and device for preparing micro/nano powder WO2021088098A1 (en)

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