CN114477271A - Digital controllable printing SnO2Method for fabricating semiconductor nanowires - Google Patents
Digital controllable printing SnO2Method for fabricating semiconductor nanowires Download PDFInfo
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- CN114477271A CN114477271A CN202210319768.XA CN202210319768A CN114477271A CN 114477271 A CN114477271 A CN 114477271A CN 202210319768 A CN202210319768 A CN 202210319768A CN 114477271 A CN114477271 A CN 114477271A
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- 239000002070 nanowire Substances 0.000 title claims abstract description 76
- 238000007639 printing Methods 0.000 title claims abstract description 27
- 239000004065 semiconductor Substances 0.000 title claims abstract description 23
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 26
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 20
- FWPIDFUJEMBDLS-UHFFFAOYSA-L tin(II) chloride dihydrate Chemical compound O.O.Cl[Sn]Cl FWPIDFUJEMBDLS-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims description 13
- 238000010041 electrostatic spinning Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- 238000003491 array Methods 0.000 abstract description 8
- 230000010354 integration Effects 0.000 abstract description 4
- 238000000137 annealing Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 230000000946 synaptic effect Effects 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 230000003956 synaptic plasticity Effects 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002964 excitative effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 230000001242 postsynaptic effect Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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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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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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Abstract
The invention relates to a digital controllable printing SnO2A method of semiconducting nanowires. The method comprises the steps of taking N, N-dimethylformamide as a solvent and polyvinylpyrrolidone and stannous chloride dihydrate as solutes, stirring to obtain a precursor solution, and then printing SnO by utilizing an electric fluid jet printing device2Nanowire array, and finally high-temperature annealing to prepare long, continuous, uniformly-arranged and digitally-controllable SnO2And (4) nanowire arrays. The invention solves the problem of the traditional SnO2The problems of short size and disorder in nanowire synthesis can be solved, and SnO with orderly arrangement and controllable digital codes can be obtained2Nanowire arrays, suitable for more types of devices, such as: transistors, semiconductor gas sensors, etc. The invention truly realizes SnO2The digital code of the nanowire printing is controllable, and has important significance for large-scale integration and array.
Description
The technical field is as follows:
the invention belongs to the field of advanced material manufacturing, and particularly relates to digital controllable printing SnO2A method of semiconducting nanowires.
Background art:
tin dioxide (SnO)2) As a typical wide bandgap n-type semiconductor, it has the advantages of high electron mobility and good chemical stability, and is widely used in many fields such as transparent conductive materials, semiconductor gas sensors, lithium batteries, and solar cells.
The microstructure and the geometric appearance of the tin dioxide are regulated and controlled by nanocrystallizing the tin dioxide, so that the nano-sized tin dioxide with more excellent photoelectric performance is obtained and has been widely researched and reported. Up to now, the common one-dimensional SnO2The preparation method of the nano material comprises the following steps: the hydrothermal method, the coprecipitation method, the sol-gel method, the traditional electrostatic spinning method and the like can not obtain long and continuous nanowires, and the traditional electrostatic spinning method can obtain continuous nanowires but has disorder and uncontrollable orientation, so that the SnO is limited2Further application of the nano material.
The invention content is as follows:
the invention aims to provide a digital controllable printing SnO aiming at the defects in the prior art2A method of semiconducting nanowires. The method comprises the steps of taking N, N-dimethylformamide as a solvent and polyvinylpyrrolidone and stannous chloride dihydrate as solutes, stirring to obtain a precursor solution, and then printing SnO by utilizing an electric fluid jet printing device2Nanowire array, and finally high-temperature annealing to prepare long, continuous, uniformly-arranged and digitally-controllable SnO2And (4) nanowire arrays. The invention solves the problem of the traditional SnO2The problems of short size and disorder in nanowire synthesis can be solved, and SnO with orderly arrangement and controllable digital codes can be obtained2Nanowire arrays, suitable for more types of devices, such as: transistors, semiconductor gas sensors, etc. The invention truly realizes SnO2The digital code of the nanowire printing is controllable, and has important significance for large-scale integration and array.
The technical scheme adopted by the invention is as follows:
digital controllable printing SnO2A method of semiconducting nanowires, the method comprising the steps of:
(1) dissolving polyvinylpyrrolidone and stannous chloride dihydrate in N, N-dimethylformamide, and stirring and dissolving for 0.5-24 hours at normal temperature to obtain a precursor solution;
wherein, polyvinylpyrrolidone: the mass ratio of the stannous chloride dihydrate is 1:1-3: 1; in the precursor solution, the mass fraction of polyvinylpyrrolidone is 10-20%;
(2) absorbing the precursor solution into an injector, and printing the precursor solution into a nanowire array by using electrofluid spray printing equipment;
the electrostatic spinning parameters of the process are as follows: the electrostatic spinning voltage is 1-2kV, the distance from the syringe needle to the substrate is 2-7mm, the liquid outlet quantity of the syringe needle is 10-100nL/min, and the substrate movement speed is 0.1-1 m/s;
(3) heating the obtained nanowire array in a muffle furnace, calcining at 400-550 ℃ for 30-120min, and cooling to obtain SnO2A semiconductor nanowire array;
the heating speed of the nanowire is 2-10 ℃/min, and the cooling speed is 2-10 ℃/min.
The diameter of the obtained nanowire is 100-5000nm, the length is 1 mm-20 cm, and the interval is 100 mu m-1 cm.
The essential characteristics of the invention are as follows:
the invention realizes the preparation of the long, straight and continuous tin dioxide nano-wire with the centimeter grade by the digital controllable printing technology. In the prior art, the preparation of the tin dioxide nanowire usually comprises a hydrothermal method, a coprecipitation method, a sol-gel method and other methods, the length of the tin dioxide nanowire prepared by the methods is hundreds of microns or even lower, and the spinning technology of the tin dioxide material has large voltage (10kV-25kV) in operation and disordered obtained nanowires due to the reasons that the distance between an injector needle and a substrate in spinning is too large and the like.
Through a large amount of research, the invention realizes the low-voltage printing of tin dioxide material under 1-2 kV. In the preparation process, the substrate for receiving the nanowires runs at the speed of 0.1-1 m/s, and the originally bent and disordered nanowires are straightened through high-speed motion; meanwhile, polyvinylpyrrolidone is added into the precursor solution to enhance the toughness, so that the nanowire is prevented from being broken in the printing process.
The invention has the beneficial effects that:
according to the method, continuous and orderly SnO can be prepared by regulating and controlling parameters such as electrostatic spinning voltage, substrate movement speed, needle liquid outlet amount and the like2The nanowire array has the advantages that the arrangement mode of the nanowires, the trend of a single nanowire and the distance between the nanowires are digitally controllable, so that the problem of one-dimensional SnO is effectively solved2The problems of short, discontinuous and disordered nano-wires are SnO2Large scale arrays and integration of nanowires provide the potential. The concrete embodiment is as follows:
1. the voltage for printing the tin dioxide nanowire is only 1kV, which is far less than the spinning voltage (about 9 kV-25kV) in the preparation process of the tin dioxide nanowire in the prior art, so that the energy consumption is greatly reduced;
2. the invention can obtain long, straight and continuous tin dioxide nano-wires, the length of which can reach 20cm without breaking and bending (the distance between wires can reach 100 mu m), while the tin dioxide nano-wires in the prior art are short, short and disordered, and the length is about tens of microns; (in conjunction with FIGS. 1 and 5 and 6, it can be seen that the tin dioxide nanowires prepared in the present invention are long, straight and continuous, while other techniques are short, disorderly)
3. The method can prepare the array of the tin dioxide nanowires, which is not available in other technologies and provides support for large-scale integration and array. The representation of fig. 2 shows that the three tin dioxide nanowires are regularly, straightly and continuously arranged, and the array is successfully realized, so that the array of the electronic device taking the tin dioxide nanowires as the semiconductor can be realized, and the method has wide application scenes in large-scale arrays of tin dioxide nanowire devices.
Description of the drawings:
FIG. 1 is SnO of example 12SEM pictures of semiconductor nanowires;
FIG. 2 is SnO of example 12SEM pictures of semiconductor nanowire arrays;
FIG. 3 is SnO prepared based on example 12The electrical performance diagram of the short-time synaptic plasticity of the semiconductor nanowire synaptic electronic device under the conditions that the source electrode is grounded and the drain electrode voltage is 0.1V;
FIG. 4 shows the hydrothermal method for preparing SnO in the prior art2SEM pictures of nanobelts;
FIG. 5 shows growing SnO in the prior art2SEM pictures of nanowires;
FIG. 6 is SnO of example 22An optical microscope picture of the semiconductor nanowire array;
FIG. 7 is SnO of example 32Optical microscopy pictures of semiconductor nanowire array lengths;
the specific implementation mode is as follows:
the invention is illustrated below with reference to examples, but the invention is not limited thereby within the scope of the examples.
Example 1
(1) Dissolving stannous chloride dihydrate and polyvinylpyrrolidone in a mass ratio of 3:4 in N, N-dimethylformamide, and stirring for 6 hours at normal temperature to prepare a precursor solution; wherein the mass concentration fraction of the polyvinylpyrrolidone is 12.5%;
(2) 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 electrostatic spinning voltage to be 1.2kV, the distance between a syringe needle and a substrate to be 5mm, setting the liquid outlet quantity of the needle to be 30nL/min, and setting the substrate movement speed to be 1000 mm/s;
(3) the nanowire array obtained by the preparation method is placed in a muffle furnace to be heated for 1.5 hours at the temperature of 500 ℃, the heating speed is 3 ℃/min, and the cooling speed is 3 ℃/min.
FIG. 1 is SnO of example 12SEM picture of semiconductor nanowire, it can be seen that SnO2The semiconductor nanowire is long and continuous, and the situation of fracture does not occur; FIG. 2 is SnO of example 12SEM picture of semiconductor nanowire array, visible SnO2The lines of the nanowire array are uniformly arranged, and the line spacing is uniform. FIG. 3 is SnO prepared based on example 12Semiconductor device and method for manufacturing the sameThe short-time synaptic plasticity electrical performance of the synaptic electronic device of the nanowire is shown in the figure, wherein the source electrode of the synaptic electronic device is grounded, the drain electrode voltage of the synaptic electronic device is 0.1V, and when a stimulation with the size of 2V and the duration of 50ms is applied to the gate electrode, the excitatory postsynaptic current of the synaptic electronic device is detected to be about 12 muA, which indicates that the synaptic electronic device has better short-time synaptic plasticity performance.
FIGS. 4 and 5 are SnO prepared using current technology2SEM picture of the nanowire shows that SnO prepared by the nanowire2The disordered, short and discontinuous characteristics of the nanowires, and the comparison of fig. 1 and 2 can prove that the technology can print a continuous and orderly nanowire array.
Example 2
(1) Dissolving stannous chloride dihydrate and polyvinylpyrrolidone in a mass ratio of 1:2 in N, N-dimethylformamide, and stirring at normal temperature for 12 hours to prepare a precursor solution, wherein the mass concentration fraction of the polyvinylpyrrolidone is 15%;
(2) 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 electrostatic spinning voltage to be 1kV, the distance between a syringe needle and a substrate to be 3mm, setting the liquid outlet amount of the needle to be 30nL/min, and setting the substrate movement speed to be 500 mm/s;
(3) the nanowire array obtained by the preparation method is placed in a muffle furnace to be heated for 1 hour at the temperature of 400 ℃, the heating speed is 2 ℃/min, and the cooling speed is 2 ℃/min.
Example 2 a long, straight, continuous array of tin dioxide semiconductor nanowires was successfully prepared, the basic shape of which is similar to that of example 1 and will not be described in detail herein, except that the spacing between the arrays of tin dioxide nanowires was 100 μm, as can be seen in fig. 6.
Example 3
(1) Dissolving stannous chloride dihydrate and polyvinylpyrrolidone in a mass ratio of 1:1 in N, N-dimethylformamide, and stirring at normal temperature for 12 hours to prepare a precursor solution, wherein the mass concentration fraction of the polyvinylpyrrolidone is 10%;
(2) 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 electrostatic spinning voltage to be 1.5kV, the distance between a syringe needle and a substrate to be 6mm, setting the liquid outlet quantity of the needle to be 50nL/min, and setting the substrate movement speed to be 800 mm/s;
(3) the nanowire array obtained by the preparation method is placed in a muffle furnace to be heated for 1 hour at 550 ℃, the heating speed is 5 ℃/min, and the cooling speed is 5 ℃/min.
Example 3 a long, straight, continuous array of tin dioxide semiconductor nanowires was successfully prepared, the basic shape is similar to examples 1 and 2, and will not be described herein, except that the length of a single tin dioxide nanowire reaches the centimeter level, as can be seen from fig. 7.
The invention is not the best known technology.
Claims (4)
1. Digital controllable printing SnO2Method of semiconducting nanowires, characterized in that the method comprises the steps of:
(1) dissolving polyvinylpyrrolidone and stannous chloride dihydrate in N, N-dimethylformamide, and stirring and dissolving for 0.5-24 hours at normal temperature to obtain a precursor solution;
wherein, polyvinylpyrrolidone: the mass ratio of the stannous chloride dihydrate is 1:1-3: 1; in the precursor solution, the mass fraction of polyvinylpyrrolidone is 10-20%;
(2) absorbing the precursor solution into an injector, and printing the precursor solution into a nanowire array by using electrofluid spray printing equipment;
the electrostatic spinning parameters of the process are as follows: the electrostatic spinning voltage is 1-2kV, the distance from the syringe needle to the substrate is 2-7mm, the liquid outlet quantity of the syringe needle is 10-100nL/min, and the substrate movement speed is 0.1-1 m/s;
(3) heating the obtained nanowire array in a muffle furnace, calcining at 400-550 ℃ for 30-120min, and cooling to obtain SnO2A semiconductor nanowire array.
2. The digital controller of claim 1Printed SnO2The method of semiconductor nanometer wire is characterized in that the heating rate of the nanometer wire is 2-10 ℃/min, and the cooling rate is 2-10 ℃/min.
3. The digitally controllable printed SnO of claim 12The method of semiconductor nanometer line is characterized in that the diameter of the obtained nanometer line is 100-5000nm, the length is 1 mm-20 cm, and the interval is 100 μm-1 cm.
4. The digitally controllable printed SnO of claim 12Method for semiconductor nanowires, characterized in that the nanowires obtained are long straight and continuous (in the order of centimeters).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101183086A (en) * | 2007-12-12 | 2008-05-21 | 天津工业大学 | Preparation method of nanometer tin oxide fibre air-sensitive film |
| CN101792935A (en) * | 2010-01-22 | 2010-08-04 | 天津工业大学 | Aluminum oxide/tin oxide blending nano-fiber membrane and preparation method thereof |
| CN105603713A (en) * | 2015-11-13 | 2016-05-25 | 大连民族大学 | Preparation method and applications of SnO2/ZnO nano composite fiber material with coaxial heterostructure |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101183086A (en) * | 2007-12-12 | 2008-05-21 | 天津工业大学 | Preparation method of nanometer tin oxide fibre air-sensitive film |
| CN101792935A (en) * | 2010-01-22 | 2010-08-04 | 天津工业大学 | Aluminum oxide/tin oxide blending nano-fiber membrane and preparation method thereof |
| CN105603713A (en) * | 2015-11-13 | 2016-05-25 | 大连民族大学 | Preparation method and applications of SnO2/ZnO nano composite fiber material with coaxial heterostructure |
Non-Patent Citations (1)
| Title |
|---|
| CHANG-YEOUL KIM等: "Synthesis of One-Dimensional SnO2 Lines by Using Electrohydrodynamic Jet Printing for a NO Gas Sensor", 《JOURNAL OF THE KOREAN PHYSICAL SOCIETY》, vol. 68, no. 2, pages 357 - 362, XP035616644, DOI: 10.3938/jkps.68.357 * |
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Application publication date: 20220513 |