WO2024045654A1 - Système et procédé de purification pour nanofils métalliques - Google Patents

Système et procédé de purification pour nanofils métalliques Download PDF

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Publication number
WO2024045654A1
WO2024045654A1 PCT/CN2023/090270 CN2023090270W WO2024045654A1 WO 2024045654 A1 WO2024045654 A1 WO 2024045654A1 CN 2023090270 W CN2023090270 W CN 2023090270W WO 2024045654 A1 WO2024045654 A1 WO 2024045654A1
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Prior art keywords
purification
metal nanowires
stage
storage tank
microfluidic
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PCT/CN2023/090270
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English (en)
Chinese (zh)
Inventor
詹世治
曾西平
靳世东
彭礼明
林仪珊
王海波
巫春荣
庄桂生
吴俊青
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深圳市华科创智技术有限公司
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Publication of WO2024045654A1 publication Critical patent/WO2024045654A1/fr

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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
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0545—Dispersions or suspensions of nanosized 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0547—Nanofibres or nanotubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Definitions

  • the invention relates to the technical field of nanomaterial preparation, and in particular to a purification system and purification method of metal nanowires.
  • Transparent conductive electrodes are one of the most important components in optoelectronic devices such as solar cells, light-emitting diodes, touch screens, and displays.
  • the material for transparent conductive electrodes currently widely used on the market is indium tin oxide.
  • indium tin oxide is relatively expensive and easily brittle under bending conditions, so it is not suitable for flexible electronic devices.
  • academic and industrial circles have successively developed flexible nanoconductive materials such as conductive polymers, carbon nanotubes, graphene, and metal nanowires. Among them, metal nanowires have attracted widespread attention due to their low cost, high performance, and ultra-flexibility.
  • metal nanoelectrodes is usually divided into the following steps: synthesis of metal nanowires, purification of metal nanowires, and preparation and coating of metal nanowire ink.
  • the performance of transparent electrodes based on metal nanowires mainly depends on Three processes: (1) the aspect ratio of the synthesized metal nanowires and the monodispersity of their size; (2) the purity of the nanowires, post-processing to remove nanorods, particles and polymers as surfactants ; (3) The uniformity of the conductive network when nanowire coating is used to form a film.
  • the purification of metal nanowires is a key step that determines the production cost and quality of metal nanowire ink.
  • the purity of metal nanowire purification mainly depends on the effectiveness of post-treatment to remove metal nanorods, metal nanoparticles and polymers as surfactants; traditional metal nanowire purification technologies include centrifugation, membrane filtration, and tangential flow. Methods, extraction methods, electrophoretic separation methods, etc. These methods have problems such as cumbersome operations, numerous steps, low purification efficiency, and require a lot of time and solvents.
  • excessive centrifugation can also cause the agglomeration of metal nanowires, which greatly affects The quality of metallic nanowire inks and the optoelectronic properties of transparent electrodes. Therefore, in order to further improve the quality of metal nanowires and reduce production costs for commercial applications, it is necessary to develop an efficient and fast method for large-scale automated purification of metal nanowires.
  • the present invention provides a purification system and purification method for metal nanowires, which use microfluidic technology through multi-stage purification to separate and obtain metal nanowires with a higher degree of purification.
  • a first aspect of the present invention provides a purification system for metal nanowires, including: a storage system, a multi-stage purification system and a control system;
  • the storage system is composed of multiple independent storage tanks, and different materials are stored in the multiple storage tanks;
  • the multi-stage purification system consists of a primary purification device, a secondary purification device and a tertiary purification device connected in sequence; the primary purification device is provided with a filter membrane, and the secondary purification device is provided with a sprinkler head.
  • the three-stage purification device is composed of a microfluidic purification tower. A plurality of glass microbead purification columns and a plurality of microfluidic chip purification columns are arranged in series in the microfluidic purification tower; different materials are stored in the storage system.
  • the tank is connected to various levels of purification devices through pipelines;
  • the control system includes multiple groups of control modules. Multiple groups of the control modules are electrically connected to the storage system and the multi-stage purification system. The control system controls the storage system to the multi-stage purification system through multiple groups of the control modules. , and material transfer between various levels of purification devices in a multi-stage purification system.
  • the microfluidic chip purification column includes multiple microfluidic chips connected in series.
  • the width of the microchannel in the microfluidic chip is 10-500 ⁇ m and the depth is 5-300 ⁇ m.
  • the glass microbead purification column The size of the glass microbeads in the column is 1-30 ⁇ m; preferably, the width of the microchannel in the microfluidic chip is 50 ⁇ m and the depth is 30 ⁇ m, and the size of the glass microbeads in the glass bead purification column is 25 ⁇ m.
  • Microfluidic chips are mainly composed of micron-level channels and chambers. Taking advantage of the laminar flow characteristics of fluids in microchannels, the diffusion speeds of metal nanowires, particles and other impurities are not consistent. Through the series connection of chips, the fluid path can be extended. thereby manipulating the separation of metal nanowires and impurities.
  • the storage tanks of the storage system include metal nanowire slurry storage tanks, desorbent storage tanks, ultrapure water storage tanks and pure water storage tanks.
  • the metal nanowire original slurry storage tank, the desorbent storage tank and the primary purification device are connected through pipelines, and the ultrapure water storage tank and the sprinkler head of the secondary purification device are connected through Pipe connections.
  • a plurality of metering pumps are arranged between the storage tank and the purification devices at each level, and the control system controls the material transfer process and the material transfer amount through the metering pumps.
  • the purification system also includes an enrichment device. After the metal nanowires are purified by the multi-stage purification system, they enter the enrichment device from the three-stage purification device, thereby obtaining the purified metal nanowire suspension; specifically, the Enrichment device microcentrifuge.
  • a mixing device is connected between the secondary purification device and the tertiary purification device, and the mixing device is connected to the pure water storage tank through a metering pump.
  • the mixing device is mainly used to dilute the secondary purification products entering the three-stage purification device so that they can flow out of the purification column.
  • a second aspect of the present invention provides a method for purifying metal nanowires using the above-mentioned purification system for metal nanowires, including the following steps:
  • Three-stage purification add pure water to the secondary purification product to obtain a dilution, place the dilution in a microfluidic tower for separation, collect the separated products, and centrifuge for enrichment to obtain a metal nanowire purification solution.
  • the desorbent described in step (1) is selected from the group consisting of methyl acetate, ethyl acetate, propyl acetate, acetone, methyl butanone, methyl isobutyl ketone, chlorobenzene, dichlorobenzene, and methylene chloride. , pentane, hexane, octane, benzene, toluene, xylene, chloroform, carbon tetrachloride, trichlorethylene, tetrachlorethylene, trichloropropane, dichloroethane, kerosene, petroleum ether or Several kinds.
  • metal nanowires are nanowires of gold, silver, copper, iron, aluminum, nickel, tin and their oxides.
  • step (1) the dosage ratio of metal nanowire slurry to desorbent is 1: (2-3), the stirring speed is 50-100r/min, and the stirring time is 10-15min.
  • step (2) the ultrapure water spray speed is 50-1000 mL/min, and the spray time is 3-5 min.
  • the microfluidic tower in step (3) is the microfluidic tower in the aforementioned metal nanowire purification system of the present invention, and the outflow rate of the diluent in the microfluidic tower is 50 to 100 ml/min. , at this flow rate, it is possible to ensure purification quality and achieve mass production at the same time.
  • Metal nanowires prepared based on chemical template methods or other methods because metal nanowires are made of gold It is obtained by the continuous deposition of nanoparticles on the surface of the template (usually an organic carrier), so the surface of the prepared metal nanowires is usually attached with an organic carrier, and due to the incomplete deposition of the metal nanoparticles, the prepared metal nanowire slurry It also contains impurities such as nanorods and nanoparticles.
  • the purification system and purification method of the present invention adopt multi-stage step-by-step purification.
  • the primary purification is desorption purification.
  • the desorbent is used to stir and mix the metal nanowire original slurry to separate the metal nanowires from the organic carriers attached to their surfaces.
  • Secondary purification is elution purification, which uses ultrapure water for spraying and uses ultrapure water to entrain and take away water-soluble impurities such as additives in the preparation process of metal nanowires.
  • the third-level purification is microfluidic purification. First, in the glass bead purification column, the solute moves vertically downward and diffuses in an undirected manner. The metal nanowires are difficult to enter the micropores of the glass beads due to their large diameter.
  • the moving speed is relatively fast. Impurities such as metal nanoparticles are small in size and will continue to diffuse into the micropores of the glass beads, resulting in a slower moving speed.
  • the metal nanowires flow out of the glass bead purification column first. ; The metal nanowires that flow out are still mixed with other impurities, and are then placed in a microfluidic chip purification column.
  • the microfluidic chip has micro-sized channels inside. In the microchannels, the fluid will form a well-defined multi-layered structure. Phase parallel flow (laminar flow). At this time, diffusion becomes the main way of mass transfer at the microscale.
  • the diffusion rates are also different, thereby achieving the separation of metal nanowires from other impurities, and by extending their For the diffusion path, multiple groups of microfluidic chips are used in series to further amplify the separation effect and ultimately achieve the purification of metal nanowires.
  • the purification system of metal nanowires of the present invention has simple parts and equipment structures, and low system construction cost; purification is carried out step by step through a multi-stage purification system, and the primary purification uses a desorbent to separate the metal nanowires from the organic carrier.
  • the secondary purification spray removes water-soluble impurities.
  • the third-stage purification uses glass bead purification columns to amplify the separation effect, and uses microfluidic chips to provide microchannels. Laminar flow and differential diffusion are used in the microchannels to separate metal nanowires from other impurities. the final separation.
  • the use of multi-stage automatic purification can improve the purification speed and quality, and achieve mass production of high-purity metal nanowires.
  • the metal nanowire purification system of the present invention also includes a metering pump, a mixing device and an enrichment device on the basis of a storage tank, various levels of purification devices and a control system. It can be built into a fully automated purification system and saves money. Reduce labor costs, improve system stability, and ensure the success rate of the purification process.
  • the purification method of metal nanowires of the present invention adopts desorption-elution-microfluidic purification
  • conventional solvents are used as the desorbent, and only one desorption and washing process is required, which does not waste a large amount of solvent, thereby reducing raw material costs and saving time; and only ultrapure water is used in the elution stage and microfluidic purification stage. and pure water, no new organic solvents will be introduced; microfluidic technology is used for further separation. Due to the differential flow of fluids in the microchannel, the separation effect can be significantly improved and higher purity metal nanowires can be obtained.
  • Figure 1 is a schematic diagram of the purification system of the present invention
  • Figure 2 is a schematic diagram of the microfluidic purification tower of the present invention.
  • Figure 3 is a schematic diagram of the microfluidic chip of the present invention.
  • Figure 4 is a TEM image of the purified silver nanowires obtained in Example 1 of the present invention.
  • Figure 5 is a TEM image of the purified silver nanowires obtained in Comparative Example 1 of the present invention.
  • the purification system of metal nanowires of the present invention includes: a storage system 100, a multi-stage purification system and a control system 800; the storage system 100 is composed of multiple independent storage tanks. Different materials are stored in the material tank; the multi-stage purification system consists of a primary purification device 300, a secondary purification device 400 and a tertiary purification device 600 connected in sequence; the primary purification device 300 is equipped with a filter membrane, and the secondary purification device 400 is equipped with a filter membrane.
  • a shower head is provided, and the three-stage purification device 600 is composed of a microfluidic purification tower.
  • a plurality of glass microbead purification columns 610 and a plurality of microfluidic chip purification columns 620 are arranged in series in the microfluidic purification tower; a storage system Different storage tanks within 100 are connected to various levels of purification devices through pipelines; the control system 800 includes multiple sets of control modules, and the multiple sets of control modules are electrically connected to the storage system 100 and the multi-level purification system.
  • the control system 800 controls the The module controls the material transfer from the storage system 100 to the multi-stage purification system and between various purification devices in the multi-stage purification system.
  • the purification system of metal nanowires of the present invention includes multi-stage purification devices, corresponding to different purification operations, and is provided with a storage system to store materials required for each level of purification operations, and is also provided with a control system to regulate the internal contents of each device. Material transportation and control of the purification conditions of each purification process, thereby realizing the automation of the entire purification process.
  • each group of control modules is used to control the purification process in the primary purification device, the secondary purification device and the tertiary purification device respectively, and optionally includes a signal collection module, a signal analysis module and an execution module according to different objects;
  • the signal collection module is used to collect status information in each purification device, such as material volume, etc.
  • the signal analysis module is connected to the output end of the signal collection module, and compares the status information collected by the signal collection module with the preset threshold. If If the signals match, the corresponding response strategy is activated and instructions are output.
  • the execution module is connected to the output end of the signal analysis module and is used to execute the instructions output by the signal analysis module.
  • Specific coping strategies include, when the required transportation volume of a material reaches a set threshold, shut down the transportation of this material and start the transportation of the next material at the same time, start the corresponding material stirring and heating operations after all set materials are transported, etc.
  • the microfluidic purification tower contains a plurality of glass microbead purification columns 610 and microfluidic chip purification columns 620 arranged in series.
  • the diluted solution is separated in the microfluidic purification tower after passing through multiple glass bead purification columns 610 and multiple microfluidic chip purification columns 620.
  • the microfluidic chip purification column 620 includes multiple microfluidic chips connected in series. 621, in which each microfluidic chip 621 is set horizontally to avoid the effect of gravity on the inner layer of the microfluidic chip. The influence of flow characteristics ensures the separation effect.
  • the width of the microchannel in the microfluidic chip 621 is 50 ⁇ m and the depth is 30 ⁇ m, and the size of the glass beads in the glass bead purification column 610 is 25 ⁇ m.
  • the storage tank 110 of the storage system 100 includes a metal nanowire slurry storage tank 111 , a desorbent storage tank 112 , an ultrapure water storage tank 113 and a pure water storage tank 114 .
  • the metal nanowire slurry storage tank 111 and the desorbent storage tank 112 are connected to the primary purification device 300 through pipelines, and the ultrapure water storage tank 113 is connected to the sprinkler head of the secondary purification device 400 through pipelines. .
  • multiple metering pumps 200 are provided between the storage tank 110 and the purification devices at each level.
  • the control system 800 controls the material transfer process and the material transfer amount through the metering pumps 200;
  • Purification System It also includes an enrichment device 700. After the metal nanowires are purified by the multi-stage purification system, they enter the enrichment device 700 from the three-stage purification device 600, thereby obtaining the purified metal nanowire suspension; the secondary purification device 400 and the three-stage purification device 400.
  • a mixing device 500 is also connected between the first-stage purification devices 600 , and the mixing device 500 and the pure water storage tank 114 are connected through a metering pump 200 .
  • the primary purification device 300 is connected to the metal nanowire slurry storage tank 111 and the desorbent storage tank 112 to obtain the materials required for primary purification (desorption purification), and transfers the primary purification product to the secondary purification device 400.
  • the secondary purification device 400 is connected to the ultrapure water storage tank 113 to obtain the materials required for secondary purification (elution purification), and transfers the secondary purification product to the mixing device 500, which is connected to the pure water storage tank 113.
  • 114 is connected to obtain the materials required for the third-stage purification (microfluidic purification), and the diluted liquid is sent to the third-level purification device 600. After the third-level purification device 600 completes the purification, the purified product is sent to the enrichment device 700 to obtain the metal. Nanowire purification solution.
  • the purification method of metal nanowires using the above purification system includes the following steps:
  • the purification system used in this embodiment is basically the same as that in Embodiment 1, except that the width of the microchannel in the microfluidic chip 621 in the three-stage purification device 600 is 20 ⁇ m and the depth is 10 ⁇ m. The size of the glass beads is 10 ⁇ m.
  • the purification method of metal nanowires using this purification system includes the following steps:
  • the purification system used in this embodiment is basically the same as that in Embodiment 1, except that the width of the microchannel in the microfluidic chip 621 in the three-stage purification device 600 is 200 ⁇ m and the depth is 100 ⁇ m. The size of the glass beads is 30 ⁇ m.
  • the purification method of metal nanowires using this purification system includes the following steps:
  • the specific operation mode of the metal nanowire purification system of the present invention is as follows:
  • Raw material preparation Add metal nanowire slurry, desorbent, ultrapure water and pure water to the corresponding storage tanks 110 of the storage system 100 respectively.
  • the desorbent is pre-prepared and added into the desorbent storage tank 112. The preparation of the desorbent can be as needed. Make component adjustments;
  • the control system 800 is used to transfer the metal nanowire slurry and desorbent from the storage system 100 to the primary purification device 300 through the metering pump 200 according to the pre-designed feeding sequence and raw material addition amount, and start stirring. After the stirring is completed, filtration is performed to obtain the primary purified product; the control system 800 transmits the primary purified product to the secondary purification device 400 and turns on the metering pump 200 connected to the ultrapure water storage tank 113. The ultrapure water flows from the sprinkler head according to the preset setting. The primary purified product is sprayed and cleaned at a certain speed, and the spray liquid overflows downward in real time.
  • the control system 800 transmits the secondary purified product to the mixing device 500 and turns on the The metering pump 200 connected to pure water adds a specified amount of pure water to dilute the secondary purified product and mix it evenly; the control system transmits the diluted secondary purified product to the third-level purification device 600, and in the third-level purification device 600, the diluted The liquid passes through the glass microbead purification column 610 and the microfluidic chip purification column 620 successively to collect the first outflow component. The control system 800 transfers the first outflow component to the enrichment device 700 for centrifugation. After completion, the metal nanowires are obtained. Purified solution. All the above steps are programmed in advance, and then the control system automatically completes the purification process under the preset program.
  • This comparative example uses purified silver nanowires obtained by conventional multiple elution methods. The specific steps are as follows:
  • the silver nanowire original slurry was washed three times with acetone to obtain purified silver nanowires, whose TEM image is shown in Figure 5.
  • the metal nanowires purified by the method of the present invention have higher purity and fewer small particle impurities; while the silver nanowires purified by three times of elution in Comparative Example 1 have obvious problems.
  • the content of silver nanoparticles and silver nanorods is high, and the purification effect is poor.
  • the purification system and purification method of metal nanowires provided in this application can automatically complete the purification process. chemical process, high purification efficiency, greatly shortened purification cycle, and can effectively remove impurities such as metal nanoparticles, metal nanorods and organic additives.
  • the purification effect is good, can be carried out on a large scale, and has good application value.

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Abstract

L'invention concerne un système et un procédé de purification de nanofils métalliques. Le système de purification comprend un système de stockage (100), un système de purification à étages multiples et un système de commande (800) ; le système de stockage (100) est constitué d'une pluralité de citernes de stockage mutuellement indépendantes (110) et le système de purification à étages multiples est constitué d'un dispositif de purification primaire (300), d'un dispositif de purification secondaire (400) et d'un dispositif de purification tertiaire (600) qui sont reliés en séquence ; une membrane filtrante est disposée dans le dispositif de purification primaire (300), une tête de pulvérisation est disposée dans le dispositif de purification secondaire (400), le dispositif de purification tertiaire (600) est formé par une tour de purification microfluidique et une pluralité de colonnes de purification à billes de verre (610) et une pluralité de colonnes de purification à copeaux microfluidiques (620) sont agencées en série dans la tour de purification microfluidique ; et le système de commande (800) commande le système de stockage (100) de façon à transporter des matières vers le système de purification à étages multiples et dans les dispositifs de purification à tous les étages dans le système de purification à étages multiples. Le système de purification utilise une purification à étages multiples, de telle sorte que la vitesse de purification peut être augmentée au maximum, la qualité de purification est assurée et des nanofils métalliques purifiés présentant une teneur en impuretés relativement faible sont obtenus.
PCT/CN2023/090270 2022-08-31 2023-04-24 Système et procédé de purification pour nanofils métalliques WO2024045654A1 (fr)

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CN111774187A (zh) * 2020-05-22 2020-10-16 深圳第三代半导体研究院 一种宏量提纯金属基纳米线的装置及方法
CN114178542A (zh) * 2021-12-10 2022-03-15 西安石油大学 一种银纳米线的制备方法
CN115415518A (zh) * 2022-08-31 2022-12-02 深圳市华科创智技术有限公司 一种金属纳米线的纯化系统及纯化方法

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