CN112786777B - Preparation method of piezoelectric nanowire for non-self-energy supply and piezoelectric nanowire - Google Patents
Preparation method of piezoelectric nanowire for non-self-energy supply and piezoelectric nanowire Download PDFInfo
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Abstract
The invention belongs to the field of passive self-power supply, and provides a preparation method of a piezoelectric nanowire for passive self-power supply and the piezoelectric nanowire. The preparation method of the passive self-powered piezoelectric nanowire comprises the steps of sputtering a seed layer grown by ZnO nanowire on a substrate; reacting the ZnO nanowire growth solution with a seed layer, and growing ZnO nanowires on the seed layer; after the reaction is finished, cleaning the seed layer and the ZnO nanowire; and preparing a piezoelectric layer electrode on the upper layer of the ZnO nanowire by adopting a plasma sputtering process, and finally obtaining the piezoelectric nanowire without self-supply.
Description
Technical Field
The invention belongs to the field of non-self-energy supply, and particularly relates to a preparation method of a piezoelectric nanowire for passive self-energy supply and the piezoelectric nanowire.
Background
The statements in this section merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Along with the high-speed development of the internet of things and the wireless sensor network and the miniaturization trend of the sensor volume, the inventor discovers that the battery energy carried by the sensor system can not meet the requirement of uninterrupted operation of the ubiquitous sensor in the internet of things.
In power supply systems, piezoelectric materials have undergone a development history from simple single crystal materials found in nature to complex-structured composite materials. By the 90 th century of the 20 th century, new relaxation ferroelectric single crystals, namely PMNT and PZNT, are developed by the state university of Binzhou, U.S. and have strain capacity more than 10 times that of PZT ceramics, reach 1% -7%, electromechanical coupling coefficient more than 92% and piezoelectric charge coefficient more than 2000 pC/N. Single crystal piezoelectric materials are a major breakthrough in the field of materials. However, pbO/Pb in piezoelectric materials, whether PMNT, PZNT or PZT 3 O 4 The content of the (C) is very high and reaches more than 60 percent. Lead is one of the most serious elements to the human body. Therefore, the conventional piezoelectric material cannot meet the development requirements of green environmental protection, and integration and miniaturization of components.
Disclosure of Invention
In order to solve at least one technical problem in the background art, the invention provides a preparation method of a passive self-powered piezoelectric nanowire and the piezoelectric nanowire, which have the advantages of low preparation cost, simple and convenient operation, easy large-area growth, capability of obtaining the piezoelectric nanowire without external power supply and self-powered.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a first aspect of the present invention provides a method for preparing a passive self-powered piezoelectric nanowire, comprising:
sputtering a seed layer grown by ZnO nano wires on a substrate;
reacting the ZnO nanowire growth solution with a seed layer, and growing ZnO nanowires on the seed layer;
after the reaction is finished, cleaning the seed layer and the ZnO nanowire;
and preparing a piezoelectric layer electrode on the upper layer of the ZnO nanowire by adopting a plasma sputtering process, and finally obtaining the piezoelectric nanowire without self-supply.
As an embodiment, before sputtering the seed layer for growing the ZnO nanowires on the substrate, the method further comprises: the substrate is cleaned.
As one embodiment, the substrate is a silicon wafer.
The silicon chip is a raw material for preparing the most core of the piezoelectric nanowire for non-self-energy supply, so that the nanowire has both semiconductor characteristics and piezoelectric characteristics, and the unique structure causes polarization charges to be generated on the inner surface and the outer surface of the bent nanowire, thereby realizing the effect of non-self-energy supply.
As one embodiment, the growth solution is composed of a liquid containing zinc nitrate and hexamethylenetetramine at a predetermined concentration.
The growth solution is used for enabling the nanowires to grow from the seed layer, and the seed layer can be a ZnO film or a structural film which is set by a person skilled in the art according to practical situations.
As one embodiment, the piezoelectric layer electrode is made of a lead-free piezoelectric material.
As an embodiment, the preparation process of the lead-free piezoelectric material comprises the following steps:
mixing the raw materials uniformly, grinding, and performing solid phase reaction at a set temperature to synthesize piezoelectric ceramics;
uniformly vibrating and mixing the presintered piezoelectric ceramic powder, and grinding;
adding an adhesive to enable the powder to form particles with preset density;
pressing the granulated material into blanks with required prefabricated sizes;
removing the binder added during granulation from the blank;
sealing and sintering the blank into porcelain at a set temperature;
grinding the burnt product to the required finished product size;
setting a conductive electrode on the set ceramic surface;
the internal electric domains of the ceramic are arranged in an oriented manner, so that the ceramic has piezoelectric performance.
According to the embodiment, the performance of the lead-free acoustic vibration piezoelectric transduction material can be optimized through the mode, and the piezoelectric material meets the development requirements of green and environment protection and integration and miniaturization of components.
A second aspect of the present invention provides a passive self-powered piezoelectric nanowire comprising a substrate, a seed layer, a ZnO nanowire, and a piezoelectric layer electrode;
the seed layer is sputtered on the substrate;
the ZnO nanowire grows on the seed layer and is obtained by reacting a ZnO nanowire growth solution with the seed layer;
the piezoelectric layer electrode is prepared by adopting a plasma sputtering process and is arranged on the upper layer of the ZnO nanowire.
As one embodiment, the substrate is a silicon wafer.
As one embodiment, the growth solution is composed of a liquid containing zinc nitrate and hexamethylenetetramine at a predetermined concentration.
As an implementation mode, the preparation material of the piezoelectric layer electrode is a lead-free piezoelectric material, and the preparation process comprises the following steps:
mixing the raw materials uniformly, grinding, and performing solid phase reaction at a set temperature to synthesize piezoelectric ceramics;
uniformly vibrating and mixing the presintered piezoelectric ceramic powder, and grinding;
adding an adhesive to enable the powder to form particles with preset density;
pressing the granulated material into blanks with required prefabricated sizes;
removing the binder added during granulation from the blank;
sealing and sintering the blank into porcelain at a set temperature;
grinding the burnt product to the required finished product size;
setting a conductive electrode on the set ceramic surface;
the internal electric domains of the ceramic are arranged in an oriented manner, so that the ceramic has piezoelectric performance.
The beneficial effects of the invention are as follows:
(1) The preparation method of the passive self-powered piezoelectric nanowire is simple and convenient to operate, low in preparation cost and easy for the large-area growth of the ZnO nanowire;
(2) The piezoelectric layer electrode is prepared on the upper layer of the ZnO nanowire by adopting a plasma sputtering process, so that external power supply is not needed, the nanowire has semiconductor characteristics and piezoelectric characteristics, and the unique structure causes polarized charges to be generated on the inner surface and the outer surface of the bent nanowire, thereby realizing the effect of no self-energy supply.
(3) The preparation material of the piezoelectric layer electrode adopts the lead-free piezoelectric material, optimizes the performance of the lead-free acoustic vibration piezoelectric transduction material, and realizes the development requirements of the piezoelectric material on green environmental protection, integration and miniaturization of components.
Additional aspects of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a flow chart of a method for preparing a passive self-powered piezoelectric nanowire in accordance with an embodiment of the present invention;
fig. 2 is a schematic diagram of a passive self-powered piezoelectric nanowire structure according to an embodiment of the present invention.
Detailed Description
The invention will be further described with reference to the drawings and examples.
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
In the present invention, terms such as "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "side", "bottom", etc. refer to an orientation or a positional relationship based on that shown in the drawings, and are merely relational terms, which are used for convenience in describing structural relationships of various components or elements of the present invention, and do not denote any one of the components or elements of the present invention, and are not to be construed as limiting the present invention.
In the present invention, terms such as "fixedly attached," "connected," "coupled," and the like are to be construed broadly and refer to either a fixed connection or an integral or removable connection; can be directly connected or indirectly connected through an intermediate medium. The specific meaning of the terms in the present invention can be determined according to circumstances by a person skilled in the relevant art or the art, and is not to be construed as limiting the present invention.
Example 1
Referring to fig. 1, the method for preparing the piezoelectric nanowire for power supply without source of the present embodiment includes:
step 1: sputtering seed layer for growing ZnO nano-wire on the substrate.
In an implementation, before sputtering the seed layer for growing the ZnO nanowire on the substrate, the method further comprises: the substrate is cleaned.
In this embodiment, the substrate is a silicon wafer.
The silicon chip is a raw material for preparing the most core of the piezoelectric nanowire for non-self-energy supply, so that the nanowire has both semiconductor characteristics and piezoelectric characteristics, and the unique structure causes polarization charges to be generated on the inner surface and the outer surface of the bent nanowire, thereby realizing the effect of non-self-energy supply.
Specifically, the silicon wafer can be cleaned by adopting a silicon wafer cleaning agent. The components of the silicon wafer cleaning agent belong to the prior art, and are not described in detail herein.
It should be noted here that in other embodiments, supercritical CO may also be employed 2 The solvent is prepared from the following components in percentage by mass: 20% of an isopolyol alkoxylate as surfactant; 20% alkyl alcohol amide phosphate; 0.1% glycolic acid as complexing agent; and cleaning the silicon wafer by 15% of glycol alkyl ether and 5% of deionized water. The cleaning liquid is environment-friendly, pollution-free, strong in detergency and convenient to store, and is suitable for cleaning semiconductor silicon wafer materials.
Step 2: and reacting the ZnO nanowire growth solution with the seed layer, and growing ZnO nanowires on the seed layer.
In a specific implementation, the growth solution is composed of a liquid containing zinc nitrate and hexamethylenetetramine at preset concentrations.
The growth solution is used for enabling the nanowires to grow from the seed layer, and the seed layer can be a ZnO film or a structural film which is set by a person skilled in the art according to practical situations.
For example: the silicon wafer substrate can contain a silicon oxide layer, a patterned ZnS film can be deposited by electron beam evaporation, and then the patterned ZnS film is oxidized for 2-2.5 hours at 500-510 ℃ in air to become a patterned ZnO film which is used as a seed layer for preparing ZnO nanowires.
Step 3: and after the reaction is finished, cleaning the seed layer and the ZnO nanowire.
In a specific implementation, deionized water may be used to rinse the seed layer and the ZnO nanowires.
It is understood herein that the skilled artisan can select the corresponding cleaning solution to clean the seed layer and the ZnO nanowires according to the actual situation, so as to improve the semiconductor performance of the ZnO nanowires.
Step 4: and preparing a piezoelectric layer electrode on the upper layer of the ZnO nanowire by adopting a plasma sputtering process, and finally obtaining the piezoelectric nanowire without self-supply.
In a specific implementation, the piezoelectric layer electrode is made of a lead-free piezoelectric material.
Specifically, the preparation process of the lead-free piezoelectric material comprises the following steps:
step 4.1: mixing the raw materials, grinding, and solid-phase reacting at a set temperature to synthesize the piezoelectric ceramic.
Dry milling or wet milling is generally employed. The method of dry grinding can be adopted in small batches, and the method of stirring ball milling or jet milling can be adopted in large batches, so that the efficiency is high.
Among them, a person skilled in the art can set the raw material to be perovskite structure, tungsten bronze structure, bismuth layered structure, or the like according to the actual situation.
In other embodiments, three elements of Sb, bi and Hf can be doped in the leadless piezoelectric ceramic at the same time, so that the uneven distribution of chemical components on a microscopic scale is realized, and a nano domain structure with ultra-high ferroelectric activity is constructed, and the level of the lead-containing ceramic is reached.
Before this step, the method also comprises the steps of carrying out pretreatment of materials, removing impurities and moisture, and weighing various raw materials according to the formula proportion, wherein a small amount of additive is required to be placed in the middle of the large material.
This process directly affects the sintering conditions and the properties of the final product.
Step 4.2: and (3) uniformly mixing the presintered piezoelectric ceramic powder by fine vibration and grinding.
Wherein, the presintered piezoelectric ceramic powder is evenly vibrated and mixed, and the grinding is carried out, thus laying a foundation for consistent ceramic forming uniformity.
Step 4.3: the binder is added to form the powder into particles of a predetermined density.
The granulation process in this step may be performed manually but is inefficient, and the efficient method is spray granulation.
Step 4.4: pressing the granulated material into blanks with required prefabricated sizes;
step 4.5: removing the binder added during granulation from the blank;
step 4.6: sealing and sintering the blank into porcelain at a set temperature;
step 4.7: grinding the burnt product to the required finished product size;
step 4.8: setting a conductive electrode on the set ceramic surface;
step 4.9: the internal electric domains of the ceramic are arranged in an oriented manner, so that the ceramic has piezoelectric performance.
According to the embodiment, the performance of the lead-free acoustic vibration piezoelectric transduction material can be optimized through the mode, and the piezoelectric material meets the development requirements of green and environment protection and integration and miniaturization of components.
The preparation method of the passive self-powered piezoelectric nanowire is simple and convenient to operate, low in preparation cost and easy for large-area growth of the ZnO nanowire;
in the embodiment, the piezoelectric layer electrode is prepared on the upper layer of the ZnO nanowire by adopting a plasma sputtering process, so that external power supply is not needed, the nanowire has the semiconductor characteristic and the piezoelectric characteristic, and the unique structure causes polarized charges to be generated on the inner surface and the outer surface of the bent nanowire, so that the effect of no self-energy supply is realized.
Example two
Referring to fig. 2, the non-self-powered piezoelectric nanowire of the present embodiment includes a substrate 1, a seed layer 2, znO nanowires 3, and a piezoelectric layer electrode 4.
Wherein the seed layer 2 is sputtered on the substrate 1;
in this embodiment, the substrate is a silicon wafer.
The silicon chip is a raw material for preparing the most core of the piezoelectric nanowire for non-self-energy supply, so that the nanowire has both semiconductor characteristics and piezoelectric characteristics, and the unique structure causes polarization charges to be generated on the inner surface and the outer surface of the bent nanowire, thereby realizing the effect of non-self-energy supply.
The ZnO nanowire 3 grows on the seed layer 2 and is obtained by reacting a ZnO nanowire growth solution with the seed layer;
in a specific implementation, the growth solution is composed of a liquid containing zinc nitrate and hexamethylenetetramine at preset concentrations.
The growth solution is used for enabling the nanowires to grow from the seed layer, and the seed layer can be a ZnO film or a structural film which is set by a person skilled in the art according to practical situations.
For example: the silicon wafer substrate can contain a silicon oxide layer, a patterned ZnS film can be deposited by electron beam evaporation, and then the patterned ZnS film is oxidized for 2-2.5 hours at 500-510 ℃ in air to become a patterned ZnO film which is used as a seed layer for preparing ZnO nanowires.
The piezoelectric layer electrode 4 is prepared by adopting a plasma sputtering process and is arranged on the upper layer of the ZnO nanowire.
In a specific implementation, the piezoelectric layer electrode is made of a lead-free piezoelectric material.
Specifically, the preparation process of the lead-free piezoelectric material comprises the following steps:
step 4.1: mixing the raw materials, grinding, and solid-phase reacting at a set temperature to synthesize the piezoelectric ceramic.
Dry milling or wet milling is generally employed. The method of dry grinding can be adopted in small batches, and the method of stirring ball milling or jet milling can be adopted in large batches, so that the efficiency is high.
Among them, a person skilled in the art can set the raw material to be perovskite structure, tungsten bronze structure, bismuth layered structure, or the like according to the actual situation.
In other embodiments, three elements of Sb, bi and Hf can be doped in the leadless piezoelectric ceramic at the same time, so that the uneven distribution of chemical components on a microscopic scale is realized, and a nano domain structure with ultra-high ferroelectric activity is constructed, and the level of the lead-containing ceramic is reached.
Before this step, the method also comprises the steps of carrying out pretreatment of materials, removing impurities and moisture, and weighing various raw materials according to the formula proportion, wherein a small amount of additive is required to be placed in the middle of the large material.
This process directly affects the sintering conditions and the properties of the final product.
Step 4.2: and (3) uniformly mixing the presintered piezoelectric ceramic powder by fine vibration and grinding.
Wherein, the presintered piezoelectric ceramic powder is evenly vibrated and mixed, and the grinding is carried out, thus laying a foundation for consistent ceramic forming uniformity.
Step 4.3: the binder is added to form the powder into particles of a predetermined density.
The granulation process in this step may be performed manually but is inefficient, and the efficient method is spray granulation.
Step 4.4: pressing the granulated material into blanks with required prefabricated sizes;
step 4.5: removing the binder added during granulation from the blank;
step 4.6: sealing and sintering the blank into porcelain at a set temperature;
step 4.7: grinding the burnt product to the required finished product size;
step 4.8: setting a conductive electrode on the set ceramic surface;
step 4.9: the internal electric domains of the ceramic are arranged in an oriented manner, so that the ceramic has piezoelectric performance.
According to the embodiment, the performance of the lead-free acoustic vibration piezoelectric transduction material can be optimized through the mode, and the piezoelectric material meets the development requirements of green and environment protection and integration and miniaturization of components.
In the embodiment, the piezoelectric layer electrode is prepared on the upper layer of the ZnO nanowire by adopting a plasma sputtering process, so that external power supply is not needed, the nanowire has the semiconductor characteristic and the piezoelectric characteristic, and the unique structure causes polarized charges to be generated on the inner surface and the outer surface of the bent nanowire, so that the effect of no self-energy supply is realized.
The preparation material of the piezoelectric layer electrode adopts a lead-free piezoelectric material, optimizes the performance of the lead-free acoustic vibration piezoelectric transduction material, and realizes the development requirements of green and environment-friendly piezoelectric material on integration and miniaturization of components.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for preparing a passive self-powered piezoelectric nanowire, comprising:
sputtering a seed layer grown by ZnO nano wires on a substrate;
reacting the ZnO nanowire growth solution with a seed layer, and growing ZnO nanowires on the seed layer;
after the reaction is finished, cleaning the seed layer and the ZnO nanowire;
preparing a piezoelectric layer electrode on the upper layer of the ZnO nanowire by adopting a plasma sputtering process, and finally obtaining the piezoelectric nanowire without self-supply;
the substrate is a silicon wafer;
the preparation material of the piezoelectric layer electrode is a lead-free piezoelectric material;
the preparation process of the lead-free piezoelectric material comprises the following steps:
mixing the raw materials uniformly, grinding, and performing solid phase reaction at a set temperature to synthesize piezoelectric ceramics;
uniformly vibrating and mixing the presintered piezoelectric ceramic powder, and grinding;
adding an adhesive to enable the powder to form particles with preset density;
pressing the granulated material into blanks with required prefabricated sizes;
removing the binder added during granulation from the blank;
sealing and sintering the blank into porcelain at a set temperature;
grinding the burnt product to the required finished product size;
setting a conductive electrode on the set ceramic surface;
the internal electric domains of the ceramic are arranged in an oriented manner, so that the ceramic has piezoelectric performance.
2. The method of preparing a self-powered piezoelectric nanowire of claim 1, further comprising, prior to sputtering a seed layer on the substrate for growth of the ZnO nanowire: the substrate is cleaned.
3. The method of preparing non-self-powered piezoelectric nanowires of claim 1, wherein the growth solution is comprised of a liquid containing zinc nitrate and hexamethylenetetramine at predetermined concentrations.
4. The passive self-energized piezoelectric nanowire is characterized by comprising a substrate, a seed layer, znO nanowires and a piezoelectric layer electrode;
the seed layer is sputtered on the substrate;
the ZnO nanowire grows on the seed layer and is obtained by reacting a ZnO nanowire growth solution with the seed layer;
the piezoelectric layer electrode is prepared by adopting a plasma sputtering process and is arranged on the upper layer of the ZnO nanowire;
the substrate is a silicon wafer;
the preparation material of the piezoelectric layer electrode is a lead-free piezoelectric material, and the preparation process comprises the following steps:
mixing the raw materials uniformly, grinding, and performing solid phase reaction at a set temperature to synthesize piezoelectric ceramics;
uniformly vibrating and mixing the presintered piezoelectric ceramic powder, and grinding;
adding an adhesive to enable the powder to form particles with preset density;
pressing the granulated material into blanks with required prefabricated sizes;
removing the binder added during granulation from the blank;
sealing and sintering the blank into porcelain at a set temperature;
grinding the burnt product to the required finished product size;
setting a conductive electrode on the set ceramic surface;
the internal electric domains of the ceramic are arranged in an oriented manner, so that the ceramic has piezoelectric performance.
5. The passive self-powered piezoelectric nanowire of claim 4, wherein the substrate is a silicon wafer.
6. The passive self-energized piezoelectric nanowire of claim 4, wherein said growth solution is comprised of a liquid containing zinc nitrate and hexamethylenetetramine at predetermined concentrations.
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| CN101215172A (en) * | 2008-01-09 | 2008-07-09 | 华中科技大学 | Method for preparing bismuth sodium titanate base leadless piezoelectricity thick film |
| CN102249596A (en) * | 2011-03-25 | 2011-11-23 | 四川大学 | Niobate-series leadless piezoelectric ceramic-polymer three-phase composite material with high dielectric constant |
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| US8344597B2 (en) * | 2009-10-22 | 2013-01-01 | Lawrence Livermore National Security, Llc | Matrix-assisted energy conversion in nanostructured piezoelectric arrays |
| CN102646788B (en) * | 2012-04-19 | 2014-04-09 | 纳米新能源（唐山）有限责任公司 | Nano generator and manufacturing method thereof |
| US9193580B1 (en) * | 2013-11-01 | 2015-11-24 | University Of Florida Research Foundation, Inc. | Barium titanate nanowire their arrays and array based devices |
| CA2967004A1 (en) * | 2017-05-11 | 2018-11-11 | Dayan Ban | Cascade-type hybrid energy cells for driving wireless sensors |
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| CN101215172A (en) * | 2008-01-09 | 2008-07-09 | 华中科技大学 | Method for preparing bismuth sodium titanate base leadless piezoelectricity thick film |
| CN102249596A (en) * | 2011-03-25 | 2011-11-23 | 四川大学 | Niobate-series leadless piezoelectric ceramic-polymer three-phase composite material with high dielectric constant |
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