CN114570938A - Method for digitally and controllably printing Ag nanowires - Google Patents
Method for digitally and controllably printing Ag nanowires Download PDFInfo
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- CN114570938A CN114570938A CN202210245776.4A CN202210245776A CN114570938A CN 114570938 A CN114570938 A CN 114570938A CN 202210245776 A CN202210245776 A CN 202210245776A CN 114570938 A CN114570938 A CN 114570938A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000007639 printing Methods 0.000 title claims abstract description 29
- 239000002070 nanowire Substances 0.000 claims abstract description 53
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 23
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 18
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 18
- KZJPVUDYAMEDRM-UHFFFAOYSA-M silver;2,2,2-trifluoroacetate Chemical compound [Ag+].[O-]C(=O)C(F)(F)F KZJPVUDYAMEDRM-UHFFFAOYSA-M 0.000 claims abstract description 17
- JIDMEYQIXXJQCC-UHFFFAOYSA-L copper;2,2,2-trifluoroacetate Chemical compound [Cu+2].[O-]C(=O)C(F)(F)F.[O-]C(=O)C(F)(F)F JIDMEYQIXXJQCC-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000012046 mixed solvent Substances 0.000 claims abstract description 12
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007921 spray Substances 0.000 claims abstract description 4
- 239000000758 substrate Substances 0.000 claims description 15
- 238000010041 electrostatic spinning Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 10
- 230000010354 integration Effects 0.000 abstract description 3
- 238000000137 annealing Methods 0.000 abstract description 2
- 239000002042 Silver nanowire Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 239000011295 pitch Substances 0.000 description 6
- 238000003491 array Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 238000004917 polyol method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a method for digitally and controllably printing Ag nanowires. The method comprises the steps of dissolving polyvinylpyrrolidone, copper trifluoroacetate and silver trifluoroacetate by using N, N-dimethylformamide and tetrahydrofuran as a mixed solvent to obtain a precursor solution, then printing an Ag nanowire array by utilizing an electro-fluidic spray printing device, and finally annealing at a high temperature to prepare the long and continuous Ag nanowire array with uniform arrangement and controllable digital codes. The method solves the problems of short size and disorder in the traditional Ag nanowire preparation, can obtain the Ag nanowire array which is orderly arranged and digitally controllable, opens up a new path for the preparation of the Ag nanowire, and has important significance for further application of large-scale controllable integration of the Ag nanowire and the like.
Description
The technical field is as follows:
the invention belongs to the field of advanced material manufacturing, and particularly relates to a method for digitally controllable printing of Ag nanowires.
The background art comprises the following steps:
with the progress of science and technology, optoelectronic devices are developed towards miniaturization, lightness and foldability, and a new generation of flexible conductive materials is widely researched. Among them, Ag nanowires have excellent bending resistance, high mechanical strength, good reliability, and excellent chemical stability, have been widely studied, and are considered as one of the most promising flexible conductive materials. In addition, the Ag nanowire plays an important role in biosensing, optical fibers and solar cells, and is one of the research hotspots in the field of the current nano materials.
There are many methods for preparing Ag nanowires, which can be mainly classified into physical methods, chemical methods, and the like according to their types, and the common methods include: template method, hydrothermal method, polyol method, self-assembly method, electrochemical method, and the like. However, most of the Ag nanowires prepared by the method are short, discontinuous and uncontrollable in orientation, and continuous and orderly-arranged Ag nanowire arrays cannot be prepared, which seriously limits the further application of the Ag nanowires in the fields of flexible electronic devices, optical fibers and the like.
The invention content is as follows:
the invention aims to provide a method for digitally and controllably printing Ag nanowires, aiming at the defects in the current Ag nanowire preparation technology. The method comprises the steps of dissolving polyvinylpyrrolidone, copper trifluoroacetate and silver trifluoroacetate by using N, N-dimethylformamide and tetrahydrofuran as a mixed solvent to obtain a precursor solution, printing an Ag nanowire array by using an electro-fluidic spray printing device, and finally annealing at high temperature to prepare the Ag nanowire array which is long and continuous, is uniformly arranged and is digitally controllable. The method solves the problems of short size and disorder in the traditional Ag nanowire preparation, can obtain the Ag nanowire array which is orderly arranged and digitally controllable, opens up a new path for the preparation of the Ag nanowire, and has important significance for further application of large-scale controllable integration of the Ag nanowire and the like.
The technical scheme of the invention is as follows:
a method of digitally controllable printing of Ag nanowires, the method comprising the steps of:
(1) mixing N, N-dimethylformamide and tetrahydrofuran to prepare a mixed solvent;
wherein, N-dimethylformamide: the mass ratio of tetrahydrofuran is 1-2: 1;
(2) dissolving polyvinylpyrrolidone, copper trifluoroacetate and silver trifluoroacetate in the prepared mixed solvent, stirring and dissolving for 1-24 hours at normal temperature to obtain a precursor solution;
wherein, the mass ratio is that silver trifluoroacetate: copper trifluoroacetate ═ 3-4:1, silver trifluoroacetate: 1-2:1 of polyvinylpyrrolidone, wherein the mass fraction of polyvinylpyrrolidone in the precursor solution is 7-15%;
(3) printing the precursor solution into a nanowire array by utilizing an electro-fluidic spray printing device;
the electrostatic spinning parameters of the process are as follows: the electrostatic spinning voltage is 1-1.5kV, the distance from the syringe needle to the substrate is 1-5mm, the liquid outlet quantity of the syringe needle is 1-100nL/min, and the substrate moving speed is 250-1000 mm/s;
(4) heating the nanowire array in a muffle furnace, calcining for 30-60 minutes at the temperature of 300-400 ℃, and cooling to obtain the Ag nanowire;
the Ag nanowire has the diameter of 700-5000nm, the length of 1 mm-20 cm and the interval of 100 mu m-1 cm.
The heating speed of the nanowire is 2-10 ℃/min, and the cooling speed is 2-10 ℃/min.
The essential characteristics of the invention are as follows:
the invention realizes the preparation of the long, straight and continuous Ag nano-wire with the centimeter grade by a digital controllable printing technology. In the prior art, methods such as a polyol method, a hydrothermal method, an autonomous loading method and the like are generally adopted for preparing the Ag nanowires, the length of the Ag nanowires prepared by the methods is hundreds of microns or even lower, and the Ag nanowires obtained by the traditional spinning technology for preparing the Ag nano materials are disordered.
According to the invention, through a large amount of researches, the Ag nano material is successfully prepared by printing under the low voltage of 1-1.5 kV. In the preparation process, the substrate for receiving the nanowires runs at the speed of 250-1000mm/s, and the originally bent and disordered nanowires are straightened through high-speed motion; meanwhile, polyvinylpyrrolidone with enhanced viscosity and a copper component with higher boiling point and low content are added into the precursor solution, so that the phenomena of breakage and agglomeration of the nanowires in the printing process and the calcining process are avoided.
The invention has the beneficial effects that:
the invention can regulate and control parameters such as the movement speed of the substrate, the distance between the syringe needle and the substrate and the like under a smaller spinning voltage, and prepare continuous and orderly Ag nanowires and arrays thereof. The energy consumption of the electrostatic spinning process is reduced, the safety is improved, the digital controllable printing of the Ag nano wires is realized, and the length and the orientation of the Ag nano wires and the distance between the wires can be adjusted. The problems of shortness and disorder in the current Ag nanowire preparation process are effectively solved, and a new idea is provided for the preparation of the Ag nanowire. The concrete expression is as follows:
1. the voltage for printing the silver nanowires is only 1kV, which is far less than the spinning voltage (20kV) in the silver nanowire preparation process in the prior art, so that the energy consumption is greatly reduced;
2. the invention can obtain long, straight and continuous silver nanowires, the length of which can reach 20cm without breaking and bending (the length of the Ag nanowire reaches the centimeter level can be seen by combining with figure 6), while the silver nanowires obtained by the current technology such as a hydrothermal method and a glycol method are short and about hundred microns level, while the reported silver nanowires in the traditional electrostatic spinning are disordered although the silver nanowires are long in length; (see comparison of FIGS. 1 and 4.)
3. The method can prepare the silver nanowire array, which is not available in other technologies and provides support for large-scale integration and array. (As can be seen by combining the representation of FIG. 2, the three silver nanowires are arranged regularly, long and continuous, and the array is successfully realized)
Description of the drawings:
fig. 1 is an SEM picture of Ag nanowires in example 1;
FIG. 2 is an SEM photograph of an Ag nanowire array of example 1;
FIG. 3 is an I-V characteristic curve of the Ag nanowire array of example 1;
fig. 4 is an SEM picture of Ag nanowires prepared in the prior art;
FIG. 5 is SEM pictures of nanowire arrays obtained in examples 2 and 3 with different pitches; wherein, fig. 5a is an SEM picture of the Ag nanowire array with a pitch of 1mm prepared in example 2, and fig. 5b is a picture of the Ag nanowire array with a pitch of 0.25mm prepared in example 3;
fig. 6 is a schematic view of an optical mirror of a single length of the Ag nanowire array prepared in example 1.
The specific implementation mode is as follows:
the invention is illustrated below with reference to examples, without thereby restricting the invention to the scope of the examples.
Example 1:
(1) mixing N, N-dimethylformamide with the mass ratio of 1: mixing tetrahydrofuran to prepare a mixed solvent;
(2) dissolving polyvinylpyrrolidone, copper trifluoroacetate and silver trifluoroacetate in the prepared mixed solvent, stirring and dissolving for 12 hours at normal temperature to obtain a precursor solution, wherein the mass ratio of the copper trifluoroacetate to the silver trifluoroacetate is 1:3, the mass ratio of the silver trifluoroacetate to the polyvinylpyrrolidone is 2:1, and the mass concentration fraction of the polyvinylpyrrolidone is 9%;
(3) absorbing the precursor solution into an injector, printing the precursor solution into a nanowire array by using an electrofluid Jet printing device (E-Jet), controlling the voltage of electrostatic spinning to be 1.3kV, the distance between a syringe needle and a substrate to be 4mm, controlling the liquid outlet amount of the needle to be 50nL/min, and controlling the movement speed of the substrate to be 300 mm/s;
(4) and (3) placing the prepared Ag nanowire array in a muffle furnace to be heated for 0.5 hour at 350 ℃, wherein the heating speed is 3 ℃/min, and the cooling speed is 3 ℃/min.
As can be seen from fig. 1, the Ag nanowires have uniform thickness, are long and continuous, and are not bent, which indicates that we successfully prepare long, straight and continuous Ag nanowires; as can be seen from fig. 2, the three Ag nanowires are arranged neatly, oriented in the same direction and highly parallel, which indicates that we successfully prepare an Ag nanowire array; the length of the Ag nanowire can be calculated to reach 1cm through the ruler in FIG. 6, which shows that we successfully prepare the nanowire in the centimeter level; fig. 3 is an I-V characteristic curve chart of the Ag nanowire prepared in example 1 under the 4200 test, and it can be found that the I-V characteristic curve of the Ag nanowire array has good linearity in the range of 0-50V, and the current increases in equal proportion with the increase of the voltage, indicating that the Ag nanowire array has good conductivity.
Fig. 4 is an SEM image of the Ag nanowires prepared by the conventional electrospinning technique, and it can be found that the prepared Ag nanowires are intricately coiled, have uncontrollable orientation, and are difficult to integrate into an array, and the Ag nanowire arrays of the present invention are long and continuous, and are aligned and have controllable orientation, as compared with fig. 1 and fig. 2.
Example 2:
(1) mixing N, N-dimethylformamide with a mass ratio of 1.5: 1: mixing tetrahydrofuran to prepare a mixed solvent;
(2) dissolving polyvinylpyrrolidone, copper trifluoroacetate and silver trifluoroacetate in the prepared mixed solvent, stirring and dissolving for 12 hours at normal temperature to obtain a precursor solution, wherein the mass ratio of copper trifluoroacetate to silver trifluoroacetate is 1:3.5, the mass ratio of silver trifluoroacetate to polyvinylpyrrolidone is 2:1, and the mass concentration fraction of polyvinylpyrrolidone is 10%;
(3) sucking the precursor solution into an injector, printing the precursor solution into a nanowire array by using an electrofluid Jet printing device (E-Jet), controlling the voltage of electrostatic spinning to be 1.2kV, the distance between a syringe needle and a substrate to be 4mm, controlling the liquid outlet amount of the needle to be 100nL/min, controlling the movement speed of the substrate to be 400mm/s, and controlling the single transverse movement distance of the substrate to be 1 mm;
(4) and (3) placing the prepared Ag nanowire array in a muffle furnace to be heated for 0.5 hour at 350 ℃, wherein the heating speed is 3 ℃/min, and the cooling speed is 3 ℃/min.
Example 3:
(1) mixing N, N-dimethylformamide with a mass ratio of 1.5: 1: mixing tetrahydrofuran to prepare a mixed solvent;
(2) dissolving polyvinylpyrrolidone, copper trifluoroacetate and silver trifluoroacetate in the prepared mixed solvent, stirring and dissolving for 12 hours at normal temperature to obtain a precursor solution, wherein the mass ratio of copper trifluoroacetate to silver trifluoroacetate is 1:3, the mass ratio of silver trifluoroacetate to polyvinylpyrrolidone is 1.5:1, and the mass concentration fraction of polyvinylpyrrolidone is 13%;
(3) sucking the precursor solution into an injector, printing the precursor solution into a nanowire array by using an electrofluid Jet printing device (E-Jet), controlling the voltage of electrostatic spinning to be 1.2kV, the distance between a syringe needle and a substrate to be 4mm, controlling the liquid outlet amount of the needle to be 30nL/min, controlling the movement speed of the substrate to be 400mm/s, and controlling the single transverse movement distance of the substrate to be 0.25 mm; (4) and (3) placing the prepared Ag nanowire array in a muffle furnace to be heated for 1 hour at 300 ℃, wherein the heating speed is 3 ℃/min, and the cooling speed is 3 ℃/min.
Fig. 5a is an SEM image of the Ag nanowire array with a pitch of 1mm prepared in example 2, and fig. 5b is an image of the Ag nanowire array with a pitch of 0.25mm prepared in example 3, and it can be found from fig. 5a and b that the present invention successfully achieves control of the pitch of the Ag nanowire array columns.
The invention is not the best known technology.
Claims (4)
1. A method for digitally controlled printing of Ag nanowires, characterized in that the method comprises the steps of:
(1) mixing N, N-dimethylformamide and tetrahydrofuran to prepare a mixed solvent;
wherein, N-dimethylformamide: the mass ratio of tetrahydrofuran is 1-2: 1;
(2) dissolving polyvinylpyrrolidone, copper trifluoroacetate and silver trifluoroacetate in the prepared mixed solvent, stirring and dissolving for 1-24 hours at normal temperature to obtain a precursor solution;
wherein, the mass ratio is that silver trifluoroacetate: copper trifluoroacetate ═ 3-4:1, silver trifluoroacetate: 1-2:1 of polyvinylpyrrolidone, wherein the mass fraction of polyvinylpyrrolidone in the precursor solution is 7-15%;
(3) printing the precursor solution into a nanowire array by utilizing an electro-fluidic spray printing device;
the electrostatic spinning parameters of the process are as follows: the electrostatic spinning voltage is 1-1.5kV, the distance from the syringe needle to the substrate is 1-5mm, the liquid outlet quantity of the syringe needle is 1-100nL/min, and the substrate moving speed is 250-1000 mm/s;
(4) and heating the Ag nanowire array in a muffle furnace, calcining at the temperature of 300-400 ℃ for 30-60 minutes, and cooling to obtain the Ag nanowire.
2. The method for controllable printing of Ag nano-wires according to claim 1, wherein the Ag nano-wires have a diameter of 700-5000nm, a length of 1 mm-20 cm and a spacing of 100 μm-1 cm.
3. The method for digitally and controllably printing Ag nanowires according to claim 1, wherein the nanowire is heated at a temperature rising speed of 2-10 ℃/min and cooled at a temperature falling speed of 2-10 ℃/min.
4. The method of digitally controllable printing of Ag nanowires according to claim 1, wherein the Ag nanowires are long straight and continuous.
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