CN112786777A - Preparation method of piezoelectric nanowire for passive self-energy supply and piezoelectric nanowire - Google Patents
Preparation method of piezoelectric nanowire for passive self-energy supply and piezoelectric nanowire Download PDFInfo
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Abstract
The invention belongs to the field of passive self-energy supply, and provides a preparation method of a piezoelectric nanowire for passive self-energy supply and the piezoelectric nanowire. The preparation method of the piezoelectric nanowire for passive self-power comprises the steps of sputtering a seed layer grown by the 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 passive self-powered piezoelectric nanowire.
Description
Technical Field
The invention belongs to the field of passive 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.
With the rapid development of the internet of things and wireless sensor networks and the miniaturization trend of the sensor volume, the inventor finds that the battery energy carried by the sensing system cannot meet the requirement of continuous working of the ubiquitous sensor in the internet of things.
In power supply systems, piezoelectric materials have undergone a progression from simple single crystal materials existing in nature to complex-structured composite materials. By the 90 s of the 20 th century, the state university of Bingzhou, USA developed novel relaxor ferroelectric single crystals, namely PMNT and PZNT, the strain capacity of which is more than 10 times of that of PZT ceramic and reaches 1% -7%, the electromechanical coupling coefficient is more than 92%, and the piezoelectric charge coefficient reaches more than 2000 pC/N. The single crystal piezoelectric material is a great breakthrough in the field of materials science. However, whether it isPMNT, PZNT are also PZT, PbO/Pb in piezoelectric material3O4The content of (A) is high and reaches more than 60 percent. Lead is one of the most harmful elements to the human body. Therefore, the traditional piezoelectric material cannot meet the development requirements of green environmental protection, 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 piezoelectric nanowire for passive self-power supply and the piezoelectric nanowire.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first aspect of the present invention provides a method for preparing a piezoelectric nanowire for passive self-power, comprising:
sputtering a seed layer grown by the ZnO nanowire on the 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 passive self-powered piezoelectric nanowire.
As an embodiment, before sputtering a seed layer for growing the ZnO nanowire on the substrate, the method further comprises: and cleaning the substrate.
In one embodiment, the substrate is a silicon wafer.
The silicon chip is the most core raw material for preparing the piezoelectric nanowire for passive 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 passive self-energy supply.
As an embodiment, the growth solution is composed of a liquid containing zinc nitrate and hexamethylenetetramine at predetermined 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 set by a person skilled in the art according to actual conditions.
In one embodiment, the piezoelectric layer electrode is made of a lead-free piezoelectric material.
As an embodiment, the lead-free piezoelectric material is prepared by the following steps:
uniformly mixing and grinding various raw materials, carrying out solid-phase reaction at a set temperature, and synthesizing piezoelectric ceramics;
finely vibrating, uniformly mixing and grinding the pre-sintered piezoelectric ceramic powder;
adding a binder to form the powder into particles with a preset density;
pressing the prepared granules into a blank with required prefabricated size;
removing the binder added during granulation from the blank;
sealing and sintering the blank at a set temperature to form porcelain;
grinding the fired product to the required finished product size;
arranging an upper conductive electrode on the set ceramic surface;
the internal electric domains of the ceramic are aligned, so that the ceramic has piezoelectric properties.
The performance of leadless acoustic vibration piezoelectric transduction material can be optimized through the above mode to this embodiment, realizes that piezoelectric material satisfies green and integrates, miniaturized development demand to components and parts.
The second aspect of the present invention provides a passive self-powered piezoelectric nanowire, which includes 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.
In one embodiment, the substrate is a silicon wafer.
As an embodiment, the growth solution is composed of a liquid containing zinc nitrate and hexamethylenetetramine at predetermined concentrations.
As an embodiment, the piezoelectric layer electrode is made of a lead-free piezoelectric material, and the preparation process includes:
uniformly mixing and grinding various raw materials, carrying out solid-phase reaction at a set temperature, and synthesizing piezoelectric ceramics;
finely vibrating, uniformly mixing and grinding the pre-sintered piezoelectric ceramic powder;
adding a binder to form the powder into particles with a preset density;
pressing the prepared granules into a blank with required prefabricated size;
removing the binder added during granulation from the blank;
sealing and sintering the blank at a set temperature to form porcelain;
grinding the fired product to the required finished product size;
arranging an upper conductive electrode on the set ceramic surface;
the internal electric domains of the ceramic are aligned, so that the ceramic has piezoelectric properties.
The invention has the beneficial effects that:
(1) the preparation method of the piezoelectric nanowire for passive self-energy supply is simple and convenient to operate, low in preparation cost and easy for 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 the semiconductor characteristic and the piezoelectric characteristic at the same time, and the unique structure causes polarization charges to be generated on the inner surface and the outer surface of the bent nanowire, so that the passive self-powered effect is realized.
(3) The piezoelectric layer electrode is made of the lead-free piezoelectric material, so that the performance of the lead-free acoustic vibration piezoelectric transduction material is optimized, and the piezoelectric material meets the development requirements of environmental protection and integration and miniaturization of components.
Advantages of 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 incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a flow chart of a method for fabricating piezoelectric nanowires for passive self-power application according to 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 is further described with reference to the following figures and examples.
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. 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 invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In the present invention, terms such as "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "side", "bottom", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only terms of relationships determined for convenience of describing structural relationships of the parts or elements of the present invention, and are not intended to refer to any parts 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 connected", "connected", and the like are to be understood in a broad sense, and mean either a fixed connection or an integrally connected or detachable connection; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be determined according to specific situations by persons skilled in the relevant scientific or technical field, and are not to be construed as limiting the present invention.
Example one
Referring to fig. 1, the method for preparing a passive self-powered piezoelectric nanowire of this embodiment includes:
step 1: and sputtering a seed layer for growing the ZnO nanowire on the substrate.
In the specific implementation, before sputtering a seed layer for growing the ZnO nanowires on the substrate, the method further comprises: and cleaning the substrate.
In this embodiment, the substrate is a silicon wafer.
The silicon chip is the most core raw material for preparing the piezoelectric nanowire for passive 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 passive self-energy supply.
Specifically, the silicon wafer can be cleaned by using a silicon wafer cleaning agent. The components of the silicon wafer cleaning agent belong to the prior art, and are not detailed here.
It should be noted here that in other embodiments, supercritical CO may also be used2As a solvent, and comprises the following components in percentage by mass: 20% of isomeric fatty alcohol alkoxylates as surfactant; 20% of alkylolamide phosphate; 0.1% of glycolic acid as a complexing agent; 15% of ethylene glycol alkyl ether and 5% of deionized water, and cleaning the silicon wafer. The cleaning solution is green and environment-friendly, has no pollution, has strong detergency, is 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 to grow the ZnO nanowire on the seed layer.
In a specific implementation, the growth solution is composed of a liquid containing zinc nitrate and hexamethylenetetramine in predetermined 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 set by a person skilled in the art according to actual conditions.
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 in the air at 500-510 ℃ for 2-2.5h to become the patterned ZnO film which is used as a seed layer for preparing the ZnO nanowire.
And step 3: and after the reaction is finished, cleaning the seed layer and the ZnO nanowire.
In an implementation, the seed layer and the ZnO nanowires may be rinsed with deionized water.
It can be understood here that, those skilled in the art can select corresponding cleaning solutions to clean the seed layer and the ZnO nanowires according to actual situations, so as to improve the semiconductor performance of the ZnO nanowires.
And 4, 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 passive self-powered piezoelectric nanowire.
In 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 performing solid phase reaction at a set temperature to synthesize the piezoelectric ceramic.
Dry or wet milling is generally used. The small batch can adopt a dry grinding method, and the large batch can adopt a stirring ball milling or airflow crushing method, so that the efficiency is higher.
Wherein, the raw material can be set to be perovskite structure, tungsten bronze structure or bismuth layer structure according to the actual situation by the skilled person.
In other embodiments, three elements of Sb, Bi and Hf can be doped in the lead-free piezoelectric ceramic at the same time, and the uneven distribution of chemical components on a microscopic scale is realized, so that a nano domain structure with ultrahigh ferroelectric activity is constructed, and the level of the lead-containing ceramic is reached.
Before the step, the method also comprises the steps of pretreatment of the raw materials, impurity removal and moisture removal, and then weighing various raw materials according to the formula proportion, wherein a small amount of additives are placed in the middle of the large materials.
This procedure directly affects the sintering conditions and the properties of the final product.
Step 4.2: and finely vibrating, uniformly mixing and grinding the pre-sintered piezoelectric ceramic powder.
Wherein, the preburning piezoelectric ceramic powder is finely vibrated, uniformly mixed and ground, and a foundation is laid for the uniformity and the performance of the finished ceramic.
Step 4.3: the binder is added to form the powder into granules of a predetermined density.
It should be noted that the granulation process in this step can be performed manually, but the method is inefficient and efficient by using spray granulation.
Step 4.4: pressing the prepared granules into a blank with required prefabricated size;
step 4.5: removing the binder added during granulation from the blank;
step 4.6: sealing and sintering the blank at a set temperature to form porcelain;
step 4.7: grinding the fired product to the required finished product size;
step 4.8: arranging an upper conductive electrode on the set ceramic surface;
step 4.9: the internal electric domains of the ceramic are aligned, so that the ceramic has piezoelectric properties.
The performance of leadless acoustic vibration piezoelectric transduction material can be optimized through the above mode to this embodiment, realizes that piezoelectric material satisfies green and integrates, miniaturized development demand to components and parts.
The preparation method of the piezoelectric nanowire for passive self-power supply 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 at the same time, 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 passive self-energy supply.
Example two
Referring to fig. 2, the passive self-energizing piezoelectric nanowire of the present embodiment includes a substrate 1, a seed layer 2, a ZnO nanowire 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 the most core raw material for preparing the piezoelectric nanowire for passive 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 passive 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 in predetermined 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 set by a person skilled in the art according to actual conditions.
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 in the air at 500-510 ℃ for 2-2.5h to become the patterned ZnO film which is used as a seed layer for preparing the ZnO nanowire.
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 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 performing solid phase reaction at a set temperature to synthesize the piezoelectric ceramic.
Dry or wet milling is generally used. The small batch can adopt a dry grinding method, and the large batch can adopt a stirring ball milling or airflow crushing method, so that the efficiency is higher.
Wherein, the raw material can be set to be perovskite structure, tungsten bronze structure or bismuth layer structure according to the actual situation by the skilled person.
In other embodiments, three elements of Sb, Bi and Hf can be doped in the lead-free piezoelectric ceramic at the same time, and the uneven distribution of chemical components on a microscopic scale is realized, so that a nano domain structure with ultrahigh ferroelectric activity is constructed, and the level of the lead-containing ceramic is reached.
Before the step, the method also comprises the steps of pretreatment of the raw materials, impurity removal and moisture removal, and then weighing various raw materials according to the formula proportion, wherein a small amount of additives are placed in the middle of the large materials.
This procedure directly affects the sintering conditions and the properties of the final product.
Step 4.2: and finely vibrating, uniformly mixing and grinding the pre-sintered piezoelectric ceramic powder.
Wherein, the preburning piezoelectric ceramic powder is finely vibrated, uniformly mixed and ground, and a foundation is laid for the uniformity and the performance of the finished ceramic.
Step 4.3: the binder is added to form the powder into granules of a predetermined density.
It should be noted that the granulation process in this step can be performed manually, but the method is inefficient and efficient by using spray granulation.
Step 4.4: pressing the prepared granules into a blank with required prefabricated size;
step 4.5: removing the binder added during granulation from the blank;
step 4.6: sealing and sintering the blank at a set temperature to form porcelain;
step 4.7: grinding the fired product to the required finished product size;
step 4.8: arranging an upper conductive electrode on the set ceramic surface;
step 4.9: the internal electric domains of the ceramic are aligned, so that the ceramic has piezoelectric properties.
The performance of leadless acoustic vibration piezoelectric transduction material can be optimized through the above mode to this embodiment, realizes that piezoelectric material satisfies green and integrates, miniaturized development demand to components and parts.
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 at the same time, 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 passive self-energy supply.
The piezoelectric layer electrode of the embodiment is made of the lead-free piezoelectric material, so that the performance of the lead-free acoustic vibration piezoelectric transduction material is optimized, and the piezoelectric material meets the development requirements of environmental protection, integration and miniaturization of components.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a piezoelectric nanowire for passive self-power supply is characterized by comprising the following steps:
sputtering a seed layer grown by the ZnO nanowire on the 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 passive self-powered piezoelectric nanowire.
2. The method of claim 1, wherein the step of sputtering a seed layer for ZnO nanowire growth on the substrate further comprises: and cleaning the substrate.
3. The method of making passive self-powered piezoelectric nanowires of claim 1, wherein the substrate is a silicon wafer.
4. The method of claim 1, wherein the growth solution is composed of a liquid containing zinc nitrate and hexamethylenetetramine at predetermined concentrations.
5. The method of manufacturing passive self-powered piezoelectric nanowires of claim 1, wherein the piezoelectric layer electrode is made of a lead-free piezoelectric material.
6. The method for preparing the passive self-powered piezoelectric nanowire as claimed in claim 5, wherein the lead-free piezoelectric material is prepared by the following steps:
uniformly mixing and grinding various raw materials, carrying out solid-phase reaction at a set temperature, and synthesizing piezoelectric ceramics;
finely vibrating, uniformly mixing and grinding the pre-sintered piezoelectric ceramic powder;
adding a binder to form the powder into particles with a preset density;
pressing the prepared granules into a blank with required prefabricated size;
removing the binder added during granulation from the blank;
sealing and sintering the blank at a set temperature to form porcelain;
grinding the fired product to the required finished product size;
arranging an upper conductive electrode on the set ceramic surface;
the internal electric domains of the ceramic are aligned, so that the ceramic has piezoelectric properties.
7. The piezoelectric nanowire for the passive self-power supply is characterized by 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.
8. The passive self-powered piezoelectric nanowire of claim 7, wherein the substrate is a silicon wafer.
9. The passive, self-powered piezoelectric nanowire of claim 7, wherein the growth solution is comprised of a liquid containing a predetermined concentration of zinc nitrate and hexamethylenetetramine.
10. The passive self-powered piezoelectric nanowire of claim 7, wherein the piezoelectric layer electrode is made of a lead-free piezoelectric material by a process comprising:
uniformly mixing and grinding various raw materials, carrying out solid-phase reaction at a set temperature, and synthesizing piezoelectric ceramics;
finely vibrating, uniformly mixing and grinding the pre-sintered piezoelectric ceramic powder;
adding a binder to form the powder into particles with a preset density;
pressing the prepared granules into a blank with required prefabricated size;
removing the binder added during granulation from the blank;
sealing and sintering the blank at a set temperature to form porcelain;
grinding the fired product to the required finished product size;
arranging an upper conductive electrode on the set ceramic surface;
the internal electric domains of the ceramic are aligned, so that the ceramic has piezoelectric properties.
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