WO2021232647A1 - 一种宏量提纯金属基纳米线的装置及方法 - Google Patents
一种宏量提纯金属基纳米线的装置及方法 Download PDFInfo
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- WO2021232647A1 WO2021232647A1 PCT/CN2020/117145 CN2020117145W WO2021232647A1 WO 2021232647 A1 WO2021232647 A1 WO 2021232647A1 CN 2020117145 W CN2020117145 W CN 2020117145W WO 2021232647 A1 WO2021232647 A1 WO 2021232647A1
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- filter
- metal
- stirring
- nanowires
- macro
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- 239000002070 nanowire Substances 0.000 title claims abstract description 59
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 50
- 239000002184 metal Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000000746 purification Methods 0.000 title claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 64
- 238000001914 filtration Methods 0.000 claims abstract description 27
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 21
- 239000002904 solvent Substances 0.000 claims description 21
- 239000012528 membrane Substances 0.000 claims description 19
- 239000011148 porous material Substances 0.000 claims description 16
- 238000002347 injection Methods 0.000 claims description 12
- 239000007924 injection Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 8
- 239000012452 mother liquor Substances 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 claims description 2
- 239000012156 elution solvent Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000002042 Silver nanowire Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000009295 crossflow filtration Methods 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
- B04B7/00—Elements of centrifuges
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
- B04B5/00—Other centrifuges
- B04B5/12—Centrifuges in which rotors other than bowls generate centrifugal effects in stationary containers
-
- 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
Definitions
- the invention relates to the field of nano-material preparation, in particular to a device and method for macro-purifying metal-based nanowires.
- the polyol method is most commonly used at present (using PVP as a capping agent and high-boiling ethylene glycol as a solvent and reducing agent) to obtain metal nanowires with suitable size and aspect ratio.
- PVP a capping agent
- high-boiling ethylene glycol as a solvent and reducing agent
- metal nanowires with suitable size and aspect ratio have better mechanical and optoelectronic properties. Therefore, based on this theory, a lot of research work is devoted to improving the synthesis method to prepare metal nanowires with ultra-long-diameter ratio.
- the currently reported methods for preparing metal nanowires with ultra-long-diameter ratios have inherent shortcomings, such as complex processes and cumbersome steps, which are not conducive to large-scale and reproducible preparation in actual production.
- improving the photoelectric performance of the transparent electrode by increasing the aspect ratio also has side effects.
- the diameter of the metal nanowire reduces the actual conductive coverage area in the transparent electrode, which is detrimental to charge collection in optoelectronic devices.
- Another method is to improve the photoelectric performance of metal nanowires from the source without changing the aspect ratio of the metal nanowires. Impurities such as non-conductive polymer PVP, metal nanoparticles, nano short rods and so on that wrap the metal nanowires are removed by purification. Conventional centrifugal washing is the most commonly used method. However, this method is inefficient and takes a long time. Excessive centrifugation can also cause metal nanowires to agglomerate.
- the dynamic stirring centrifugal filtration device includes:
- the dynamic stirring centrifugal filter device includes: a filter base, a solution injection system, a filter cylinder, and a filtrate outflow system;
- the filter cylinder includes a filter frame, a stirring device, and a filter membrane; the filter membrane includes a first filter area, a second filter area, and a third filter area in the vertical direction.
- the first filter area, the second filter area The inward included angle between any two of the filter area and the third filter area is less than 180 degrees, and a plurality of filter holes are distributed on the first filter area, the second filter area and the third filter area.
- the first filter area, the second filter area, and the third filter area are at an angle to each other, which will increase the filter area of the filter membrane and improve the filter efficiency.
- the direction toward the stirring paddle is an inward direction.
- the pore sizes of the filter holes on the first filter zone, the second filter zone and the third filter zone are different.
- the pore size of the first filtration region is 100 nm-1 ⁇ m, and/or the pore size of the second filtration region is 1 ⁇ m-5 ⁇ m, and/or the pore size of the third filtration region is 5 ⁇ m-20 ⁇ m.
- the stirring device includes an electric motor and a stirring paddle connected with the electric motor.
- the filtering device includes a stirring paddle selected from one of a single-screw stirring paddle, a double-screw stirring paddle, a single-hole stirring paddle, and a porous stirring paddle.
- the stirring device includes an electric motor and a stirring paddle connected with the electric motor.
- the solution injection system injects the replacement solvent during the stirring and filtration to ensure that the concentration of the metal-based nanowires in the stirring centrifugal filter cylinder is relatively stable during the filtration process, and the filtrate flows out of the collection system to collect the filtered by-products.
- a method for purifying metal-based nanowires using the above-mentioned macro-purifying metal-based nanowire device includes the following steps:
- the metal-based nanowires are: gold, silver, copper, iron, aluminum, nickel, tin, and the foregoing metal oxides.
- the diluent is selected from one or more of ethanol, isopropanol, alcohol, distilled water, acetone, n-hexane, and ethyl acetate.
- the dilution concentration of the metal-based nanowire mother liquor in S1 is 0.2 mg/mL-1.2 mg/mL.
- the stirring speed is 300-1200 revolutions/min.
- the filtration pressure comes from the centrifugal force generated when the liquid is stirred, which can be controlled by the stirring speed;
- the three filter membranes are fixed on the filter tank through the framework of the filter tank, which has a larger filter area compared with the traditional filter and improves the filtration efficiency;
- the shear force generated by the stirring can clean the surface of the filter membrane, prevent nanowires from gathering and blocking the filter pores of the filter membrane, reducing subsequent filtration efficiency and continuous filtration capacity.
- the setting of filter membranes with different pore diameters is beneficial to extend the filter membrane The service life of the filter membrane is also realized repeatedly, and the cost is reduced;
- the solvent can be replaced by a variety of target solvents after the metal nanowires are concentrated through the solution injection system;
- the purification, concentration and solvent exchange of the nanowires can be realized in one step during stirring, which simplifies the post-treatment process.
- the invention of the device basically solves the core problems of cumbersome steps, complicated processes, and high cost faced by the current industrialized preparation and purification of metal nanowires.
- Figure 1 is a schematic diagram of an apparatus for macro-purification of metal-based nanowires.
- This embodiment provides a method for macro-purifying metal-based nanowires, and the experimental device is shown in FIG. 1.
- the first filter area has a filter pore size of 0.1 ⁇ m
- the second filter area has a filter pore size of 1 ⁇ m
- the third filter area filters
- the hole size is 10 ⁇ m
- the stirring speed is set at 500 revolutions per minute
- the double screw stirring paddle is used
- the rinsing solvent is set to ethanol.
- This embodiment provides a method for macro-purifying metal-based nanowires, and the experimental device is shown in FIG. 1.
- the first filter area has a filter pore size of 0.2 ⁇ m
- the second filter area has a filter pore size of 2 ⁇ m
- the third filter The size of the regional filter hole is 15 ⁇ m
- the stirring speed is set at 800 rpm
- a porous screw stirring paddle is used
- the rinsing solvent is set to isopropanol.
- This embodiment provides a method for macro-purifying metal-based nanowires, and the experimental device is shown in FIG. 1.
- the first filter area has a filter hole size of 0.5 ⁇ m
- the second filter area has a filter hole size of 5um
- the third filter area filters
- the pore size is 20 ⁇ m
- the stirring speed is set at 500 rpm
- a single-hole stirring paddle is used
- the rinsing solvent is set to distilled water.
- the process conditions and raw materials used in this comparative example are the same as those in Example 1, except that the filter membrane is installed on the stirring filter rod in a vertical direction.
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
序号 | 浓缩浓度 | 所需时间 |
实施例1 | 5mg mL -1 | 40min |
对比例1 | 5mg mL -1 | 150min |
Claims (9)
- 一种宏量提纯金属基纳米线的装置,包括动态搅拌离心过滤装置,其特征在于,所述动态搅拌离心过滤装置包括:溶液注入系统、过滤缸、滤液流出系统;所述过滤缸包括过滤骨架、搅拌装置和过滤膜;所述过滤膜在垂直方向上依次包括第一过滤区、第二过滤区和第三过滤区,所述第一过滤区、所述第二过滤区和所述第三过滤区任意两个之间向内夹角小于180度,所述第一过滤区、所述第二过滤区和所述第三过滤区上分布有多个过滤孔。
- 如权利要求1所述的一种宏量提纯金属基纳米线的装置,其特征在于,所述第一过滤区、所述第二过滤区和所述第三过滤区上过滤孔的孔径大小不同。
- 如权利要求1所述的一种宏量提纯金属基纳米线的装置,其特征在于,所述第一过滤区域的孔径为100nm-1μm,和/或,所述第二过滤区域的孔径为1μm-5μm,和/或,所述第三过滤区域的孔径为5μm-20μm。
- 如权利要求1所述的一种宏量提纯金属基纳米线的装置,其特征在于,所述溶液注入系统在搅拌过滤时注入置换溶剂,以保证过滤过程中搅拌离心过滤缸内金属基纳米线浓度相对稳定,所述滤液流出收集系统收集滤出的副产物。
- 一种使用权利要求1-4任一所述的宏量提纯金属基纳米线装置的提纯金属基纳米线的方法,其特征在于,包括以下步骤:S1:使用稀释剂稀释金属基纳米线母液,并通过溶液注入系统注入过滤缸中;S2:以固定搅拌速度开启搅拌;搅拌时淋洗溶剂经溶液注入系统持续流入以补偿流走的滤液损失;S3:搅拌20-50min停止加入淋洗溶剂,继续搅拌浓缩溶液;S4:当浓缩溶液浓度达到1mg mL -1-15mg mL -1后,在过滤缸的底部收集纯化的浓缩液。
- 根据权利要求5所述的提纯纳米线的方法,其特征在于,所述金属基纳米线为:金、银、铜、铁、铝、镍、锡以及上述金属氧化物。
- 根据权利要求5所述的提纯纳米线的方法,其特征在于,所述稀释液选自 乙醇、异丙醇、酒精、蒸馏水、丙酮、正己烷、乙酸乙酯中的一种或几种。
- 根据权利要求5所述的提纯纳米线的方法,其特征在于,S1中金属基纳米线母液稀释浓度为0.2mg/mL-1.2mg/mL。
- 根据权利要求5所述的提纯纳米线的方法,其特征在于,所述搅拌速度为300-1200转/min。
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CN115283661A (zh) * | 2022-08-09 | 2022-11-04 | 北京化工大学 | 铜纳米线的纯化方法和由该方法制得的铜纳米线 |
CN115415518B (zh) * | 2022-08-31 | 2023-10-24 | 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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CN106493391B (zh) * | 2016-12-12 | 2019-05-17 | 中国科学技术大学 | 一种铜纳米线的提纯方法 |
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