CN108147418B - SiO in parallel arrangement2Nanowire and method for preparing same - Google Patents

SiO in parallel arrangement2Nanowire and method for preparing same Download PDF

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CN108147418B
CN108147418B CN201711426036.6A CN201711426036A CN108147418B CN 108147418 B CN108147418 B CN 108147418B CN 201711426036 A CN201711426036 A CN 201711426036A CN 108147418 B CN108147418 B CN 108147418B
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sio
substrate
temperature
reaction source
reaction
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CN108147418A (en
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杨喜宝
吕航
王莉丽
李波欣
陈双龙
董恩来
赵景龙
刘秋颖
姚震
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Bohai University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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Abstract

The invention describes a parallel arrangement of SiO2The preparation method of the nanowire takes SiO nanometer powder as a reaction source in the whole process, the SiO nanometer powder reacts in a high-temperature area of a one-dimensional high-temperature tube furnace in a low vacuum environment, and the SiO nanometer powder is deposited on a low-temperature area of a silicon wafer substrate along with the circulation of protective gas. SiO prepared by the method2The nano-wires have parallel arrangement structure, and have important academic significance and application for developing new fields of material performance due to unique novel structure.

Description

SiO in parallel arrangement2Nanowire and method for preparing same
Technical Field
The invention relates to a parallel arrangement of SiO2A nano wire and a preparation method thereof, belonging to the technical field of three-dimensional nano materials.
Background
In recent years, the development of material preparation technology is rapid, especially in the field of nano science and technology, and the development of material preparation technology is advanced, so that a new place in the field of materials is opened up. SiO 22As a traditional electric insulating material, the nano-wire is also the most important basic material in the semiconductor process, the preparation technology of the nano-wire has important reference value in the application prospect of the fields of integrated circuits and solar cells, and has potential application in mesoscopic physical research and nano devices, for example, the nano-wire can be used for manufacturing one-dimensional quantum transistors, light emitting diodes and the like. In addition, as typical silicon-based nanomaterials, the amounts thereofThe combination of the sub-size limiting effect and the unique photoelectric characteristics of the elements of the same type has wide application prospect in the aspects of biomedicine and the integrated electronic field of nano devices. And, SiO2The nano material has peculiar properties of high purity, low density, high specific surface area, good dispersibility, excellent mechanical property and optical property, and is widely applied to products in various industries such as high polymer composite materials, catalyst carriers, electronic packaging materials, rubber, plastics, papermaking, sealants, high-grade fillers, coatings and the like. At present, the preparation of nano-structure materials with high yield, good crystallinity, uniform size and optical adjustability is still the key point of the current research stage, and has important scientific significance for the development and optimization of nano-devices.
The current methods for preparing nano-structured materials such as nano-wires, nano-rods and the like are various, such as a laser ablation method, a liquid phase deposition method, chemical vapor deposition and a thermal evaporation method. However, at present, for parallel arrangement of SiO2The preparation work of the nano-wire is not reported temporarily, the performance and the application of the nano-wire are not well proved, and the thermal evaporation method is utilized to prepare the parallel arrangement SiO2The nano wire has low cost and novel product structure, and has important reference value for the development of the field of nano material preparation. In addition, SiO aims at the problems of poor dispersibility, low stability, uncontrollable size, uneven appearance and the like in the preparation research of the silicon nano material2The preparation research of the parallel arrangement nano-wires has important significance for the optimization of the preparation process of the silicon-based nano-material.
Disclosure of Invention
For solving the existing SiO2The invention prepares a novel parallel SiO by a thermal evaporation method with safety, no pollution and low cost2A nanowire.
SiO in parallel arrangement2The preparation method of the nanowire comprises the following steps.
The first step is as follows: pretreating a substrate Si wafer, performing ultrasonic treatment by using acetone, and cleaning by using plasma water. The quartz boat was cleaned with alcohol.
The second step is that: placing SiO nano powder as a reaction source into one end of a quartz boat, then placing a processed substrate Si sheet into the quartz boat to ensure that the processed substrate Si sheet is above the reaction source and is not contacted with the reaction source, and then placing the quartz boat filled with the substrate and the reaction source into a high-temperature tube furnace filled with Ar protective gas.
The third step: the temperature in the furnace is raised to the proper temperature for the reaction source to react, and the temperature is kept for 2-3 hrs. After the reaction is finished, the temperature in the furnace is reduced to low temperature and the furnace is taken out, and then the growth of white floccules, namely the SiO which is arranged in parallel and is 1, on the substrate is found2A nanowire.
The substrate is a Si sheet and is compatible with related process devices.
And placing quartz boats downwards on the polished surface of the substrate Si wafer, arranging the quartz boats one by one at intervals without contacting with a reaction source, and then placing the quartz boats into a tube furnace to ensure that a sample smoothly grows on the Si substrate.
In the third step, the reaction temperature range of the reaction source is 1140-1160 ℃, and the deposition temperature range of the white flocculent product is 1120-1150 ℃. The experiment setting deposition temperature is 20 ℃ lower than the reaction temperature, so that the sample is ensured to be smoothly deposited on the substrate, and the experiment loss is avoided.
Argon as protective gas is introduced along the opening direction (clockwise direction) of the small quartz tube, and the flow is 80-90ml/min, so that the smooth growth of experimental products is ensured, and the experimental loss can be reduced to the minimum.
The reaction time is 2-3 hrs. And after the reaction is finished, the temperature in the furnace is reduced to room temperature, the argon bottle is closed, and the sample is taken out, so that the sample is found to have white deposition. The growth of the parallel nanowires is not influenced.
Prepared parallel arrangement of SiO2The nano-wire has a diameter of 0.3-0.5 micrometer and a length of more than 100 micrometers. The nanowires are free of other impurities, deposited uniformly on the substrate, and arranged in parallel.
The method has the advantages of no pollution, simple operation, safe flow, low cost, no other impurities and high purity of experimental samples. The method has low requirement on a deposition substrate, has simple reaction process, and can realize the purpose of being applied to Si sheets or other materialsThe in-situ growth is convenient for being compatible with various integration processes. The parallel arrangement of the SiO of the invention2The method for growing the nanowires has the advantages of high yield, simple process, environmental protection and safety, and has very important prospect application in the fields of medicine, optics, microelectronics and the like.
Drawings
FIG. 1 and FIG. 2 show the preparation of SiO in parallel arrangement2SEM images of nanowires wherein the nanowires have a diameter of 0.3-0.5 microns and a length greater than 100 microns.
FIG. 3 is a diagram of SiO arranged in parallel2EDX spectrum diagram of nanowire, wherein peaks are all shown to come from amorphous SiO2。
FIG. 4 is a diagram of growing SiO in parallel arrangement on a Si substrate2Raman scattering spectrum of the nanowire at 484 cm-1The vibration peak of (A) is derived from SiO2Bending vibration of the middle oxygen atom in the Si-O-Si bond, and is located at 315 cm-1Nearby vibration peaks are also due to typical SiO2And (5) vibrating.
FIG. 5 is a diagram of growing SiO in parallel arrangement on a Si substrate2PL spectrum of the nanowire.
Detailed Description
First embodiment of the invention preparation of SiO in parallel arrangement2The method of the nanowire is realized by the following steps.
Step one, pretreating a substrate Si wafer, performing ultrasonic treatment by using acetone, and cleaning by using plasma water. The quartz boat was cleaned with alcohol.
And secondly, placing the SiO nano powder serving as a reaction source into one end of a quartz boat, then placing the processed substrate Si sheet into the quartz boat to ensure that the processed substrate Si sheet is above the reaction source and is not in contact with the reaction source, and then placing the quartz boat filled with the substrate and the reaction source into a high-temperature tube furnace filled with Ar protective gas.
And step three, raising the temperature in the furnace to the appropriate temperature of the reaction source required to react, and preserving the temperature for 2 hrs. After the reaction is finished, the temperature in the furnace is reduced to low temperature and the furnace is taken out, and then the growth of white floccules, namely the SiO which is arranged in parallel and is 1, on the substrate is found2A nanowire.
In the second embodiment, the substrate is a Si wafer, a quartz wafer or a high temperature substrate, and is compatible with related process devices.
In the third specific embodiment, quartz boats are placed downwards on the polished surface of the substrate Si wafer, are arranged at intervals one by one and are not contacted with a reaction source, and then are placed into a tube furnace to ensure that a sample can grow on the Si substrate smoothly.
In the fourth specific implementation mode and the third step, the reaction temperature range of the reaction source is 1140-1160 ℃, and the deposition temperature range of the white flocculent product is 1120-1150 ℃. The experiment setting deposition temperature is 20 ℃ lower than the reaction temperature, so that the sample is ensured to be smoothly deposited on the substrate, and the experiment loss is avoided.
In the fifth concrete implementation mode, the argon gas as the protective gas is introduced along the opening direction (clockwise direction) of the small quartz tube, and the flow rate is 80-90ml/min, so that the smooth growth of the experimental product is ensured, and the experimental loss can be reduced to the minimum.
In the sixth embodiment, the reaction time is 2-3 hrs. And after the reaction is finished, the temperature in the furnace is reduced to room temperature, the argon bottle is closed, and the sample is taken out, so that the sample is found to have white deposition. The growth of the parallel nanowires is not influenced.
Seventh embodiment, prepared parallel arrangement of SiO2The nano-wire has a diameter of 0.3-0.5 micrometer and a length of more than 100 micrometers. The nanowires are free of other impurities, deposited uniformly on the substrate, and arranged in parallel.
The principle is as follows: the invention adopts a tubular heating furnace device, SiO is used as a reaction raw material under the condition of Ar protective gas, the temperature of the tubular furnace is kept at 1140-1160 ℃ for 2-3hrs, and a substrate is placed in a lower temperature region in a reaction cavity. The substrate was pretreated by sonication in acetone solution followed by deionized water rinsing. The parallel arrangement of nanowires prepared on the substrate requires that the flow of Ar is controlled to be 80-90 ml/min.
The invention will be further illustrated with reference to the following specific examples.
The first embodiment.
0.5g of SiO nano powder is used as a reaction source and put at the bottom of a quartz boat, and an n-type (111) Si sheet is used as a baseThe bottom is arranged in a quartz boat, then the quartz boat is arranged in a quartz cavity of the horizontal tube furnace, and the positions of the reaction source and the substrate are adjusted to ensure that the position of the reaction source is in a high-temperature area of the tube furnace and the position of the substrate is in a relatively low-temperature area. Before heating, argon with the flow rate of 90ml/min is introduced into the system to remove air impurities in the reaction system, then the tubular furnace is heated to 1150 ℃ and is kept at the temperature for 2 hrs, after the system is cooled to room temperature in an argon environment, a white floccule is found to grow on a region of 1130-. FIG. 3 is a diagram of SiO arranged in parallel2EDX spectrum diagram of nanowire, wherein peaks are all shown to come from amorphous SiO2. FIG. 4 is a Si substrate and SiO arranged in parallel2Raman scattering spectrum of the nanowire at 484 cm-1The vibration peak of (A) is derived from SiO2Bending vibration of the middle oxygen atom in the Si-O-Si bond, and is located at 315 cm-1Nearby vibration peaks are also due to typical SiO2And (5) vibrating. FIG. 5 is a PL photoluminescence spectrum of a sample illustrating that the sample has superior luminescence properties, wherein luminescence at around 560 nm and 660 nm is primarily due to oxygen vacancies generated during sample preparation.
Example two.
0.7g of SiO nano powder is used as a reaction source and is placed at the bottom of a quartz boat, an n-type (111) Si sheet is used as a substrate and is placed in the quartz boat together, then the quartz boat is placed in a quartz cavity of a horizontal tube furnace, and the positions of the reaction source and the substrate are adjusted, so that the position of the reaction source is in a high-temperature area of the tube furnace, and the position of the substrate is in a relatively low-temperature area. Before heating, introducing argon with the flow rate of 80 ml/min into the system to remove air impurities in the reaction system, then heating the tubular furnace to 1140 ℃ and preserving the temperature for 2 hrs, after the system is cooled to room temperature in an argon environment, finding that white floccules grow in a 1120-1130 ℃ region on a Si substrate, and observing that parallel nanowires with the diameter of 0.3-0.5 microns grow.
Example three.
0.6g of SiO nano powder is used as a reaction source and is placed at the bottom of a quartz boat, an n-type (111) Si sheet is used as a substrate and is placed in the quartz boat together, then the quartz boat is placed in a quartz cavity of a horizontal tube furnace, and the positions of the reaction source and the substrate are adjusted, so that the position of the reaction source is in a high-temperature area of the tube furnace, and the position of the substrate is in a relatively low-temperature area. Before heating, argon with the flow rate of 90ml/min is introduced into the system to remove air impurities in the reaction system, then the tubular furnace is heated to 1145 ℃ and is kept at the temperature for 3hrs, after the system is cooled to room temperature in an argon environment, a white floccule is found to grow in the 1125-DEG and 1135-DEG region on the Si substrate, and the parallel arrangement nano-wires with the diameter of 0.4-0.5 micron are found to grow.
Example four.
0.5g of SiO nano powder is used as a reaction source and is placed at the bottom of a quartz boat, an n-type (111) Si sheet is used as a substrate and is placed in the quartz boat together, then the quartz boat is placed in a quartz cavity of a horizontal tube furnace, and the positions of the reaction source and the substrate are adjusted, so that the position of the reaction source is in a high-temperature area of the tube furnace, and the position of the substrate is in a relatively low-temperature area. Before heating, argon with the flow rate of 90ml/min is introduced into the system to remove air impurities in the reaction system, then the tubular furnace is heated to 1140 ℃ and is kept at the temperature for 2 hrs, after the system is cooled to room temperature in an argon environment, a white floccule is found to grow in a 1120-1130 ℃ region on a Si substrate, and the parallel arrangement nanowires with the diameter of 0.5 micron are found to grow.
Example five.
0.5g of SiO nano powder is used as a reaction source and is placed at the bottom of a quartz boat, an n-type (111) Si sheet is used as a substrate and is placed in the quartz boat together, then the quartz boat is placed in a quartz cavity of a horizontal tube furnace, and the positions of the reaction source and the substrate are adjusted, so that the position of the reaction source is in a high-temperature area of the tube furnace, and the position of the substrate is in a relatively low-temperature area. Before heating, argon with the flow rate of 85 ml/min is introduced into the system to remove air impurities in the reaction system, then the tubular furnace is heated to 1160 ℃ and is kept at the temperature for 2 hrs, after the system is cooled to room temperature in an argon environment, a white floccule is found to grow in the 1140-1150 ℃ region on the Si substrate, and the growth of parallel arranged nanowires on a sample is observed, wherein the diameter of the nanowires is 0.3-0.4 micron.

Claims (1)

1. SiO in parallel arrangement2The preparation method of the nanowire is characterized by comprising the following steps: the prepared nanowires are uniformly distributed, are arranged in a parallel structure, and do not contain a catalyst:
the method comprises the following steps:
the first step is as follows: pretreating a substrate Si wafer, performing ultrasonic treatment by using acetone, cleaning by using plasma water, and cleaning a quartz boat by using alcohol;
the second step is that: placing SiO nano powder as a reaction source into one end of a quartz boat, then placing a polished surface of a processed substrate Si wafer downwards into the quartz boat, ensuring that the substrate Si wafer is arranged above the reaction source at intervals one by one and is not contacted with the reaction source, and then placing the quartz boat filled with the substrate and the reaction source into a high-temperature tube furnace filled with Ar protective gas, wherein the argon flow is 80-90 mL/min;
the third step: raising the temperature in the furnace to the adaptive temperature of the reaction source to be reacted, preserving the heat for 2-3hrs, after the reaction is finished, reducing the temperature in the furnace to low temperature, taking out the furnace, and finding that white floccules growing on the substrate are the SiO arranged in parallel2The nanowire, wherein the reaction temperature range of the reaction source is 1140-1160 ℃, and the deposition temperature range for generating the white floccule is 1120-1150 ℃.
CN201711426036.6A 2017-12-26 2017-12-26 SiO in parallel arrangement2Nanowire and method for preparing same Expired - Fee Related CN108147418B (en)

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CN111717921B (en) * 2020-06-29 2022-01-28 中国科学院过程工程研究所 SiO (silicon dioxide)xNanowire, preparation method thereof and application of nanowire as lithium ion battery cathode
CN113800939B (en) * 2021-08-30 2023-02-28 华中科技大学 Nano fiber SiO 2 Porous ceramic material and preparation method thereof

Citations (2)

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CN104016359A (en) * 2014-06-27 2014-09-03 四川大学 Conical amorphous SiO2 nanowires and preparation method thereof
CN106276922A (en) * 2016-08-10 2017-01-04 渤海大学 A kind of intersecting vertical SiO2nanometer rods and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104016359A (en) * 2014-06-27 2014-09-03 四川大学 Conical amorphous SiO2 nanowires and preparation method thereof
CN106276922A (en) * 2016-08-10 2017-01-04 渤海大学 A kind of intersecting vertical SiO2nanometer rods and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
沉积温度对热蒸发法制备SiO2一维纳米材料的影响;吕航 等;《人工晶体学报》;20171031;第46卷;第2-3节 *

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