CN115094393A - ZnO piezoelectric coating material capable of simultaneously exciting longitudinal-transverse waves and preparation method and application thereof - Google Patents

ZnO piezoelectric coating material capable of simultaneously exciting longitudinal-transverse waves and preparation method and application thereof Download PDF

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Publication number
CN115094393A
CN115094393A CN202210707500.3A CN202210707500A CN115094393A CN 115094393 A CN115094393 A CN 115094393A CN 202210707500 A CN202210707500 A CN 202210707500A CN 115094393 A CN115094393 A CN 115094393A
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piezoelectric coating
zno piezoelectric
zno
waves
substrate
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姜杨慧
杨兵
张俊
李敬雨
瓦西里·帕里诺维奇
曾晓梅
张翔宇
陈燕鸣
黄家辉
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Wuhan University WHU
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Wuhan University WHU
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10—Glass or silica
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B35/00—Screw-bolts; Stay-bolts; Screw-threaded studs; Screws; Set screws
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L5/00—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes
    • G01L5/24—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes for determining value of torque or twisting moment for tightening a nut or other member which is similarly stressed
    • G01L5/246—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes for determining value of torque or twisting moment for tightening a nut or other member which is similarly stressed using acoustic waves

Abstract

The invention provides a preparation method of a ZnO piezoelectric coating material capable of exciting longitudinal-transverse waves simultaneously, which comprises the steps of sequentially forming a bonding layer, a ZnO piezoelectric coating, a protective layer and an electrode layer on a substrate; the preparation method of the ZnO piezoelectric coating comprises the following steps: under the vacuum condition, forming a ZnO piezoelectric coating on the surface of the bonding layer by adopting a Zn target or a ZnO target through magnetron sputtering; in the magnetron sputtering, mixed gas of argon and oxygen is introduced; in the mixed gas, the flow ratio of argon to oxygen is 2: 1-1: 3. The invention also provides a ZnO piezoelectric coating material prepared based on the preparation method, and the ZnO piezoelectric coating presents different orientations on the surface of the matrix and has the characteristic of being excited by transverse waves and longitudinal waves of ultrasonic waves at the same time. The invention also provides an intelligent bolt, the surface of which is provided with the ZnO piezoelectric coating material, and the ZnO piezoelectric coating material can be excited by ultrasonic transverse waves and longitudinal waves at the same time, so that the calculation step of the pretightening force can be simplified, and the high-precision nondestructive measurement of the pretightening force of the bolt can be easily realized.

Description

ZnO piezoelectric coating material capable of simultaneously exciting longitudinal-transverse waves and preparation method and application thereof
Technical Field
The invention belongs to the technical field of coating materials, and particularly relates to a ZnO piezoelectric coating material capable of simultaneously exciting longitudinal waves and transverse waves, a preparation method of the ZnO piezoelectric coating material, and application of the coating material in manufacturing of intelligent bolts.
Background
Since the 80 s in the 20 th century, the ultrasonic pre-tightening force measuring technology has been used for detecting the axial stress of a threaded fastener, and the method has the advantages of small measuring error, high precision, good real-time performance, strong penetrating power and the like, is wide in application range, and still is a development direction of key attention at home and abroad at present. The method is based on the acoustoelastic theory, can utilize a piezoelectric material as an acoustoelectric conversion medium, and determines the stress value through processing and calculation of an echo signal. For a contact type ultrasonic stress measurement method, one method is to use an ultrasonic probe and a coupling agent to carry out measurement, but the measurement method is more complicated and needs to consider errors generated by the coupling agent and corrosion of a measured piece possibly caused by the coupling agent; and the piezoelectric ceramic plate is stuck on the detected piece, so that the method can avoid the problems of complicated operation and corrosion, but the influence of the adhesive on signal propagation and the stability of the adhesive in the service process of the fastener need to be considered, and the stuck piezoelectric ceramic plate has the problems of falling, cracking and the like. Therefore, it is of great value to develop a new type of ultrasonic transducer that can be perfectly combined with the bolt.
The film with the piezoelectric effect is simple in preparation method, high in stability and wide in applicability, and therefore is very suitable for being applied to the pretightening force detection direction. The coating with excellent ultrasonic excitation performance is directly deposited on the surface of the detected piece, so that the detected piece with the permanent following sensor can be obtained. The piezoelectric coating is directly deposited on the surface of the bolt, so that the intelligent bolt with the whole life cycle capable of being measured in situ on line can be prepared. The method can avoid all adverse effects caused by the coupling agent or the adhesive, and has the characteristics of quick and accurate measurement. At present, a sputtering type intelligent bolt technology capable of exciting longitudinal waves is developed at home and abroad and is applied to the fields of aerospace and the like, so that the high-precision measurement of the bolt pretightening force is realized. Besides the influence of the detection method on the result, the conversion calculation between the ultrasonic signal and the stress causes certain errors in the detection result.
A large number of researches show that when the stress is detected by using a transverse wave and longitudinal wave combined method, except for constants related to the self performance and the geometric shape of a material, the real-time load of the bolt can be obtained under the condition of not calibrating the original stress only by measuring the flight time and the initial temperature of the longitudinal wave transverse wave of the bolt in a no-load state and simultaneously solving an eight-order polynomial. The method can reduce the number of compensation factors, simplify the detection steps and improve the measurement accuracy. Therefore, if a piezoelectric coating which is directly deposited on the surface of the part and can simultaneously excite transverse-longitudinal waves can be prepared, the development of the ultrasonic part stress measurement technology can be greatly promoted.
At present, the piezoelectric coating capable of simultaneously exciting transverse waves and longitudinal waves mainly comprises ZnO and AlN, both materials are in a hexagonal wurtzite structure, and the performance of the piezoelectric coating for generating the piezoelectric effect completely depends on the crystal orientation of the piezoelectric coating without polarization. The ZnO piezoelectric material has high piezoelectric coefficient and electromechanical coupling coefficient K 2 The ZnO coating has the advantages of high performance, capability of growing on various substrates, low epitaxial growth temperature requirement, and easier control of stoichiometry and texture, so that the ZnO coating with stronger piezoelectric effect and easier obtainment can be selected as the acoustoelectric conversion layer for exciting the ultrasound. When the ZnO thin film grows along the C-axis direction and has high crystalline quality, ultrasonic longitudinal waves are easily excited, and the most basic condition for exciting transverse waves is that the direction of an applied electric field is perpendicular to the propagation direction of acoustic waves and has a direct relationship with the crystalline orientation of the film layer. There have been many studies on the excitation of pure longitudinal waves or pure transverse waves by ZnO piezoelectric thin films, but there has been no report on the simultaneous excitation of transverse waves and longitudinal waves.
Based on this, a ZnO piezoelectric coating material capable of simultaneously exciting transverse waves and longitudinal waves is provided, so that the ZnO piezoelectric coating material can better meet the application requirements in the technical field of ultrasonic measurement of part stress, the accurate nondestructive measurement of parts is realized, and the technical problem to be solved is urgently needed.
Disclosure of Invention
The invention aims to provide a preparation method of a ZnO piezoelectric coating material which has simple process, is easy to adjust, meets the requirement of industrial mass production and can simultaneously excite longitudinal waves and transverse waves.
The other purpose of the invention is to provide a ZnO piezoelectric coating material capable of simultaneously exciting ultrasonic longitudinal-transverse mixed waves.
The invention also aims to provide the intelligent bolt which is provided with the special piezoelectric coating, can be excited by ultrasonic transverse waves and longitudinal waves at the same time, can simplify the calculation step of the pretightening force, improves the measurement accuracy and is easy to realize the high-precision measurement of the pretightening force of the bolt.
The technical scheme adopted by the invention for realizing one of the purposes is as follows: the preparation method of the ZnO piezoelectric coating material capable of simultaneously exciting longitudinal waves and transverse waves is provided, wherein a bonding layer, a ZnO piezoelectric coating, a protective layer and an electrode layer are sequentially formed on a substrate;
the preparation method of the ZnO piezoelectric coating comprises the following steps: under the vacuum condition, forming a ZnO piezoelectric coating on the surface of the bonding layer by adopting a Zn target or a ZnO target through magnetron sputtering; in the magnetron sputtering, mixed gas of argon and oxygen is introduced; in the mixed gas, the flow ratio of argon to oxygen is 2: 1-1: 3.
In the invention, the ZnO piezoelectric coating formed by adopting the magnetron sputtering method can be carried out at lower temperature, power and air pressure based on the magnetron sputtering method, and the prepared film material comprises most of metals and compounds, and has the advantages of higher sputtering efficiency and high film bonding force, and the film thickness or other properties can be regulated and controlled by adjusting preparation parameters, so that the method is more flexible, is suitable for preparing films with larger areas, and the like.
Further, the preparation method of the ZnO piezoelectric coating also comprises the following steps: and in the magnetron sputtering, the position of the substrate from the center to the edge of the target material is adjusted, so that the substrate is over against the center of the target material or the position of the substrate relative to the target material is away from the center of the target material by a certain distance. The distance between the position of the substrate relative to the target and the center of the target is 0-60 mm. Preferably, the distance may be 5mm, 10mm, 15mm, 20mm, 25mm, 30mm, 35mm, 40mm, 45mm, 50mm, 55mm, or the like.
The inventor finds that besides the ZnO piezoelectric coating which can excite different ultrasonic signal waves can be prepared by adjusting the flow ratio of argon to oxygen to be 2: 1-1: 3, the multi-orientation growth of the ZnO coating can be influenced by adjusting the position of the substrate relative to the center to the edge of the target. When the two methods are used in combination, a better excitation waveform can be obtained. For example, when the flow ratio of argon to oxygen is controlled to be 1:3 and the distance between the position of the substrate relative to the target and the center of the target is 30mm, compared with the condition that the substrate is directly opposite to the center of the target, the prepared piezoelectric coating can realize multi-orientation growth, shows that good ultrasonic longitudinal-transverse mixed waves can be excited, and has good performance when being applied to accurate measurement of bolt pretightening force in industry.
Furthermore, in the invention, specific parameters in the magnetron sputtering process are optimally selected by combining the application performance of the ZnO piezoelectric coating to be prepared, and the vacuum degree is set to be 4 multiplied by 10 -3 Pa, temperature of 50-200 ℃, sputtering pressure of 1-3 Pa, sputtering power of 550-700W, and magnetismAnd controlling the sputtering time to be 1-5 h under the magnetron sputtering condition so as to realize better regulation and control on the growth orientation of the ZnO film.
Preferably, the target material for sputtering is a ZnO ceramic target or a Zn target material with the purity of 99.99%, the diameter of the target material is 150mm, and the thickness of the target material is 5 mm. The target base distance (the vertical distance between the target material and the bolt substrate) is adjusted depending on the kind and diameter of the substrate. For example: when the substrate is a bolt with the diameter of 15mm and the length of 50mm or a stainless steel plate with the thickness of 0.77mm, the distance between the target and the bolt substrate is preferably 70 mm; when the substrate is a bolt having a diameter of 35mm, the distance between the target and the bolt substrate is preferably 110 mm.
In some preferred embodiments, the flow ratio of argon to oxygen in the mixed gas is 2:1 to 1: 2. The magnetron sputtering conditions are as follows: the sputtering temperature is 50-150 ℃, the target base distance is 60-100 mm, and the vacuum degree is 4 multiplied by 10 3 Pa～8×10 3 Pa, the sputtering pressure is 1-3 Pa, the sputtering power is 500-700W, the sputtering time is 3-5 h, and the deposition position of the matrix is 0-30 mm away from the center of the target. Under the condition, the temperature is low, the crystallinity is reduced, and columnar crystals are thick and large and are easy to exhibit multi-orientation growth; along with the reduction of the content of argon in the argon-oxygen ratio, the content of oxygen is increased, so that the sputtering rate is reduced, the coating thickness is reduced, the density is reduced, and multi-orientation growth is easy to present; as the deposition location changes, the orientation of the coating changes. Under the conditions of the argon-oxygen ratio and the magnetron sputtering, the deposited coating can realize the excitation of longitudinal-transverse mixed waves.
In some preferred embodiments, the flow ratio of argon to oxygen in the mixed gas is 1: 3. The magnetron sputtering conditions are as follows: sputtering at 200 deg.C and target base distance of 110mm, and vacuumizing to 4 × 10 -3 Pa, sputtering pressure of 2.5Pa, sputtering power of 550W, sputtering time of 5h, and deposition position of the substrate at a distance of 0-60mm from the center of the target. Under the above conditions, ultrasonic longitudinal-transverse waves can be excited due to the change of orientation during the deposition of the coating caused by the change of position.
In some preferred embodiments, the preparation method of the ZnO piezoelectric coating material for simultaneously exciting longitudinal-transverse waves comprises the following steps:
s1, carrying out plasma etching on the substrate in an argon environment at the temperature of 150-200 ℃;
s2, depositing a Cr bonding layer on the substrate surface treated in the step S1 under the conditions of 0.5-1 Pa and 50-250V of bias voltage;
s3, depositing for 1-5 hours at 50-200 ℃ on the surface of the Cr bonding layer under 1-3 Pa, adjusting the flow ratio of argon to oxygen to be 2: 1-1: 3, and the relative position of the target and the substrate to be 0-60mm to obtain the ZnO piezoelectric coating;
s4, depositing SiO on the surface of the ZnO piezoelectric coating under the current condition of 1-2 Pa and 0-80A 2 Or a high entropy alloy protective layer;
s5, depositing a Ti electrode layer on the surface of the protective layer under the conditions of 0.25-1 Pa, 0-100V bias voltage and 0-80A current, and obtaining the ZnO piezoelectric coating material capable of simultaneously exciting longitudinal waves and transverse waves.
In the technical scheme, firstly, the surface of the bolt matrix is subjected to plasma etching technology to remove oxides and pollutants on the surface of the bolt, so that the oxides on the surface can be thoroughly removed, and the adhesive force of the coating is improved; secondly, Cr is used as a bonding layer, so that the bonding force between the piezoelectric coating and the substrate is improved, and the problem of poor bonding between the piezoelectric coating and the substrate is solved; thirdly, the growth direction of the ZnO coating is converted into multi-orientation growth from a single (002) crystal face by controlling the flow ratio of argon to oxygen in the preparation process of the ZnO piezoelectric layer, and then the ZnO coating capable of exciting different ultrasonic signals is prepared; finally, SiO which has good insulativity and is easy to prepare is prepared on the surface of the piezoelectric coating 2 Or high-entropy alloy with high resistance and excellent high-temperature performance is used as a protective layer; on the surface of the protective layer, Ti with good conductivity and strong corrosion resistance is selected as an electrode layer, and finally the ZnO piezoelectric coating material capable of exciting ultrasonic signal waves of longitudinal and transverse mixed waves is obtained.
The second technical scheme adopted for achieving the purpose of the invention is as follows: the ZnO piezoelectric coating material which is prepared based on one of the purposes of the invention and can simultaneously excite longitudinal waves and transverse waves is provided, and the ZnO piezoelectric coating presents different orientations on the surface of a substrate and comprises (002) crystal planes and (102) diffraction crystal planes. Wherein, the (002) crystal face is the preferred growth crystal face of the ZnO coating and is easy to excite ultrasonic longitudinal waves, the (102) crystal face is the crystal face grown by regulation, and the ZnO piezoelectric coating with the crystal face has the capability of exciting ultrasonic transverse waves.
Preferably, the thickness of the ZnO piezoelectric coating is 5-20 micrometers.
Preferably, the thickness of the bonding layer is 250-1000 nanometers.
Preferably, the thickness of the protective layer is 1-5 microns.
Preferably, the thickness of the electrode layer is 2-10 micrometers.
The invention realizes the third technical scheme that the purpose is realized by: the intelligent bolt comprises the ZnO piezoelectric coating material which simultaneously excites longitudinal-transverse waves.
In the invention, ZnO piezoelectric coating materials capable of simultaneously exciting longitudinal-transverse waves are deposited on the surfaces of the bolts or the stainless steel sheets, so that the surfaces of the bolts or the stainless steel sheets have the performance of simultaneously exciting ultrasonic longitudinal-transverse waves. When the bolt pre-tightening force of the intelligent bolt is measured, the stress can be detected by a method combining transverse waves and longitudinal waves, the number of compensation factors is effectively reduced, the detection steps are simplified, and meanwhile, the measurement accuracy is improved. Meanwhile, the intelligent bolt provided by the invention also effectively avoids complicated operation, falling off of the piezoelectric ceramic piece and adverse effects of the coupling agent and the adhesive on the substrate, and can realize online permanent measurement in the whole period without corrosion and with high precision.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the ZnO piezoelectric coating material capable of exciting longitudinal-transverse waves simultaneously provided by the invention is characterized in that the ZnO piezoelectric coating is prepared by utilizing radio frequency magnetron sputtering, and the piezoelectric coating material capable of exciting different ultrasonic waveforms is prepared by adjusting the flow ratio of argon and oxygen introduced in the magnetron sputtering process. In addition, different ultrasonic waveforms can be optimized by adjusting different positions of the substrate relative to the target material, and the ZnO piezoelectric coating material capable of simultaneously exciting ultrasonic longitudinal-transverse waves can be prepared. The preparation method provided by the invention has the advantages of simple and feasible process and wide adaptability, and provides important value for the field of novel ultrasonic transducers.
(2) According to the ZnO piezoelectric coating material capable of simultaneously exciting longitudinal waves and transverse waves, the ZnO piezoelectric coating presents different orientations on the surface of a substrate, comprises a (002) crystal plane and a (102) diffraction crystal plane, and has the characteristic of being simultaneously excited by the transverse waves and the longitudinal waves of ultrasonic waves. In addition, the ZnO piezoelectric coating material capable of exciting longitudinal-transverse waves simultaneously provided by the invention also comprises a bonding layer, a protective layer and an electrode layer, so that the corrosion of the coating to a base material and the falling-off of the coating from the surface of the base can be effectively avoided, the failure of a sensor is avoided, and the long-period measurement is facilitated.
(3) According to the intelligent bolt provided by the invention, the ZnO piezoelectric coating material which simultaneously excites longitudinal waves and transverse waves is arranged on the surface of the intelligent bolt, so that ultrasonic transverse waves and longitudinal waves can be simultaneously excited, the calculation step of the pre-tightening force can be simplified, the measurement accuracy is improved, and the high-precision measurement of the pre-tightening force of the bolt is easy to realize. The ZnO piezoelectric coating material has high binding force with a bolt substrate, can ensure that a piezoelectric functional coating can work stably for a long time on the surfaces of various alloy bolts, and reduces the possibility of failure of the piezoelectric functional coating. In addition, the preparation technology and equipment of the ZnO piezoelectric coating material are closer to those of the existing industrial equipment, the batch production of industrial production is easy to realize, the processing efficiency is higher, and the production cost of manufacturers can be greatly reduced.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus for preparing a ZnO piezoelectric coating material for simultaneously exciting longitudinal-transverse waves according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a ZnO piezoelectric coating material capable of simultaneously exciting longitudinal waves and transverse waves prepared by the preparation method provided by the invention;
FIG. 3 is an XRD pattern of coatings deposited at different deposition locations for coatings made in accordance with examples 4-6 of the present invention;
FIG. 4 is a comparison of surface topography and cross-sectional topography of different ultrasonic waves excitable at different deposition locations made by examples 4-6 of the present invention;
FIG. 5 is a graph of the ultrasonic signal of the coating produced in example 1 of the present invention;
FIG. 6 is a graph of ultrasonic signals at different deposition locations made in example 3 of the present invention;
FIG. 7 is a graph of ultrasonic signals of different deposition locations made in examples 4-6 of the present invention;
wherein, 1-radio frequency magnetron sputtering (RF); 2-ZnO/Zn target material; 3-bolt sample; 4-etching source; 5-a sample holder; 6-a workpiece holder; 7-a heater; 8-an air exhaust port; 9-furnace door; 10-a substrate; 11-Cr bond coat; 12-ZnO piezoelectric coating; 13-a protective layer; 14-electrode layer.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
A preparation method of a ZnO piezoelectric coating for an intelligent bolt capable of simultaneously exciting longitudinal waves and transverse waves comprises the following steps: controlling the distance between the target material and the bolt substrate (diameter is 15mm) to be 70mm, and vacuumizing to 7 x 10 at 150 DEG C -3 Pa, introducing 50sccm argon (purity 99.99%), starting a bias voltage and arc power supply, performing plasma etching on the substrate under the conditions of-150V, duty ratio 80%, air pressure 1.0Pa and current 80A, removing impurities attached to the surface of the substrate, and improving the bonding force of the film layer and the substrate. After the etching is finished, a layer of bonding layer Cr is prepared on the bolt substrate, so that the internal stress can be eliminated, the bonding force between the coating and the substrate is increased, and the thickness of the bonding layer is about 500 nm. After the bonding layer was prepared, it was evacuated to 7X 10 at 150 deg.C -3 Pa, controlThe position of the bolt is opposite to the center of the ZnO target, mixed gas of argon (with the purity of 99.99%) and oxygen (with the purity of 99.99%) is introduced, the flow ratio of the argon to the oxygen is 2:1, until the air pressure in the cavity is 2.5Pa, the deposition position is 10mm away from the center of the target, a radio frequency power supply is started, the sputtering power is 700W, and the sputtering time is 4.5 h. After the ZnO piezoelectric coating is prepared, preparing SiO on the surface of the piezoelectric coating 2 Or a protective layer of a high entropy alloy and an electrode layer of Ti. After the preparation is finished, the bolt is naturally cooled to room temperature, and the intelligent bolt capable of exciting different ultrasonic waves is obtained.
Example 2
A preparation method of a ZnO piezoelectric coating for an intelligent bolt capable of simultaneously exciting longitudinal waves and transverse waves comprises the following steps: controlling the distance between the target material and the bolt substrate (diameter is 15mm) to be 70mm, and vacuumizing to 7 x 10 at 200 DEG C -3 Pa, introducing 50sccm argon (purity 99.99%), starting a bias voltage and an arc power supply, performing plasma etching on the substrate under the conditions of-150V, duty ratio 80%, air pressure 0.5Pa and current 70A, removing impurities attached to the surface of the substrate, and improving the bonding force of the film layer and the substrate. After the etching is finished, a layer of bonding layer Cr is prepared on the bolt substrate, so that the internal stress can be eliminated, the bonding force between the coating and the substrate is increased, and the thickness of the bonding layer is about 500 nm. After the bonding layer was prepared, it was evacuated to 6X 10 at 100 deg.C -3 Pa, controlling the position of the bolt to be opposite to the center of the ZnO target, introducing mixed gas of argon (with the purity of 99.99%) and oxygen (with the purity of 99.99%), wherein the flow ratio of the argon to the oxygen is 1:1, until the air pressure in the cavity is 2.8Pa, the deposition position is 30mm away from the center of the target, starting a radio frequency power supply, the sputtering power is 550W, and the sputtering time is 5 h. After the ZnO piezoelectric coating is prepared, preparing SiO on the surface of the piezoelectric coating 2 Or a protective layer of a high entropy alloy and an electrode layer of Ti. After the preparation is finished, the bolt is naturally cooled to room temperature, and the intelligent bolt capable of exciting different ultrasonic waves is obtained.
Example 3
In the preparation method, the preparation methods of plasma etching, a Cr binding layer, a protective layer and an electrode layer are the same as those in the embodiment 2The same is true. The difference is that the preparation of the ZnO piezoelectric coating comprises the following steps: controlling the distance between the target material and a stainless steel substrate (with the thickness of 0.77mm) to be 70mm, and vacuumizing to 8 x 10 at 65 DEG C -3 Pa, controlling the position of the stainless steel plate to face 15mm of the center of the ZnO target, introducing mixed gas of argon (with the purity of 99.99%) and oxygen (with the purity of 99.99%), wherein the flow ratio of the argon to the oxygen is 1:2, turning on a radio frequency power supply until the air pressure in the cavity is 2.0Pa, and the sputtering power is 700W and the sputtering time is 4 h. And after the ZnO piezoelectric coating is prepared, preparing a protective layer and an electrode layer on the surface of the piezoelectric coating. And after the preparation is finished, naturally cooling to room temperature to obtain the coating which is prepared on the surface of the stainless steel matrix and can excite ultrasonic longitudinal-transverse waves.
Example 4
A preparation method of a ZnO piezoelectric coating for an intelligent bolt capable of simultaneously exciting longitudinal waves and transverse waves comprises the following steps: controlling the distance between the target material and a bolt substrate (the diameter is 35mm) to be 110mm, and vacuumizing to 7 x 10 at 200 DEG C -3 Pa, introducing 50sccm argon (purity 99.99%), starting a bias voltage and an arc power supply, performing plasma etching on the substrate under the conditions of-150V, duty ratio 80%, air pressure 0.5Pa and current 70A, removing impurities attached to the surface of the substrate, and improving the bonding force of the film layer and the substrate. After the etching is finished, a layer of bonding layer Cr is prepared on the bolt substrate, so that the internal stress can be eliminated, the bonding force between the coating and the substrate is increased, and the thickness of the bonding layer is about 500 nm. After the bonding layer was prepared, it was evacuated to 4X 10 at 200 deg.C -3 Pa, controlling the position of the bolt to be opposite to the center of the ZnO target, introducing mixed gas of argon (with the purity of 99.99%) and oxygen (with the purity of 99.99%), enabling the flow ratio of the argon to the oxygen to be 1:3, enabling the pressure in the cavity to be 2.5Pa, starting a radio frequency power supply, and enabling the sputtering power to be 550W and the sputtering time to be 5 h. After the ZnO piezoelectric coating is prepared, preparing SiO on the surface of the piezoelectric coating 2 Or a protective layer of a high entropy alloy and an electrode layer of Ti. And after the preparation is finished, naturally cooling to room temperature to obtain the intelligent bolt capable of exciting different ultrasonic waves.
Example 5
A method for preparing a ZnO piezoelectric coating for an intelligent bolt capable of simultaneously exciting longitudinal waves and transverse waves,the method comprises the following steps: controlling the distance between the target material and the bolt substrate (diameter is 35mm) to be 110mm, and vacuumizing to 7 x 10 at 200 DEG C -3 Pa, introducing 50sccm argon (purity 99.99%), starting a bias voltage and arc power supply, performing plasma etching on the substrate under the conditions of-150V, duty ratio 80%, air pressure 0.5Pa and current 70A, removing impurities attached to the surface of the substrate, and improving the bonding force of the film layer and the substrate. After the etching is finished, a layer of bonding layer Cr is prepared on the bolt substrate, so that the internal stress can be eliminated, the bonding force between the coating and the substrate is increased, and the thickness of the bonding layer is about 500 nm. After the bonding layer was prepared, it was evacuated to 4X 10 at 200 deg.C -3 Pa, controlling the position of the bolt to be 30mm away from the center facing the ZnO target, introducing mixed gas of argon (with the purity of 99.99%) and oxygen (with the purity of 99.99%), wherein the flow ratio of the argon to the oxygen is from 1:3, the pressure in the cavity is 2.5Pa, starting a radio frequency power supply, the sputtering power is 550W, and the sputtering time is 5 h. After the ZnO piezoelectric coating is prepared, preparing SiO on the surface of the piezoelectric coating 2 Or a protective layer of a high entropy alloy and an electrode layer of Ti. After the preparation is finished, the bolt is naturally cooled to room temperature, and the intelligent bolt capable of exciting different ultrasonic waves is obtained.
Example 6
A preparation method of a ZnO piezoelectric coating for an intelligent bolt capable of simultaneously exciting longitudinal waves and transverse waves comprises the following steps: controlling the distance between the target material and the bolt substrate (diameter is 35mm) to be 110mm, and vacuumizing to 7 x 10 at 200 DEG C -3 Pa, introducing 50sccm argon (purity 99.99%), starting a bias voltage and arc power supply, performing plasma etching on the substrate under the conditions of-150V, duty ratio 80%, air pressure 0.5Pa and current 70A, removing impurities attached to the surface of the substrate, and improving the bonding force of the film layer and the substrate. After the etching is finished, a layer of bonding layer Cr is prepared on the bolt substrate, so that the internal stress can be eliminated, the bonding force between the coating and the substrate is increased, and the thickness of the bonding layer is about 500 nm. After the bonding layer was prepared, it was evacuated to 4X 10 at 200 deg.C -3 Pa, controlling the position of the bolt to be 60mm away from the center opposite to the ZnO target material, introducing mixed gas of argon (with the purity of 99.99%) and oxygen (with the purity of 99.99%), wherein the flow ratio of the argon to the oxygen is from 1:3, and opening the chamber until the air pressure in the chamber is 2.5PaStarting a radio frequency power supply, wherein the sputtering power is 550W, and the sputtering time is 5 h. After the ZnO piezoelectric coating is prepared, preparing SiO on the surface of the piezoelectric coating 2 Or a protective layer of a high entropy alloy and an electrode layer of Ti. After the preparation is finished, the bolt is naturally cooled to room temperature, and the intelligent bolt capable of exciting different ultrasonic waves is obtained.
FIG. 1 shows an apparatus used in an embodiment of the present invention, in which a vacuum chamber is surrounded by furnace walls, and the size of the vacuum chamber is 600X600 mm. The vacuum chamber is provided with an extraction opening 8, and the vacuum pumping unit performs vacuum pumping on the vacuum chamber through the extraction opening 8. The heaters 7 are arranged at the upper two corners of the vacuum chamber, the heating power is 25 kilowatts, and the heating efficiency is improved; the lower two corners of the vacuum chamber are etching sources 4, which can remove impurities on the surface of the substrate and ensure the cleanness of the substrate surface.
The ZnO target 2 is arranged on the furnace wall and connected with a radio frequency magnetron sputtering (RF)1 together, the sputtering power can be adjusted, the back of the ZnO target 2 faces the furnace door 9, the front of the ZnO target is a sample 3, the sample is placed on a sample rack 5, and the sample rack is arranged on a workpiece rack 6. The position of the sample 4 on the sample holder 5 can be divided into a position a opposite to the target center a, a position b spaced 30mm apart from the center a, and a position c spaced 60mm apart from the center a and 30mm apart from the center b. The layout greatly increases the plasma density in the vacuum chamber, the workpiece is completely immersed in the plasma, and the deposition rate, hardness and adhesive force of the coating are greatly improved. Because the target structure is optimized, the magnetic field distribution is more uniform, the etching of the magnetron sputtering target surface is uniform, and the uniformity of the coating is improved.
Fig. 2 is a schematic structural diagram of a ZnO piezoelectric coating material simultaneously exciting longitudinal-transverse waves prepared in an embodiment of the present invention, and it can be seen from the diagram that a component gradient exists on the coating structure, so that the structural stability can be better increased, and a thicker piezoelectric coating can be deposited. Comprises a Cr bonding layer 11, a ZnO piezoelectric coating 12 and SiO sequentially deposited on the surface of a substrate 10 2 Or a high-entropy alloy protective layer 13 and a Ti electrode layer 14 with high resistance.
FIG. 3 is an XRD pattern of the coating deposited under different deposition positions of the coatings prepared in examples 4-6 of the present invention, and it can be seen from the XRD pattern that the orientation of the ZnO coating on the substrate changes to multi-orientation growth from the process of the substrate facing the center to the edge of the target, and the intensity of the diffraction peak (102) becomes larger and larger.
FIG. 4 is a comparison of the surface profile and the cross-sectional profile of different deposition locations with different ultrasonic waves, which are obtained in examples 4-6 of the present invention, and it can be seen that when the ratio of argon to oxygen is 1:3 and the deposition locations are different, the particles at the edge of the deposition locations are irregular, the surface roughness is larger, and the growth liquid of the columnar crystals is larger and more irregular.
FIG. 5 is a graph showing ultrasonic signals of the coating obtained in example 1 of the present invention, and it can be seen that ultrasonic longitudinal waves and transverse waves appear on the bolt.
FIG. 6 is a graph of ultrasonic signals of a coating produced in example 3 of the present invention, showing ultrasonic longitudinal and transverse waves on a stainless steel substrate.
FIG. 7 is a graph of ultrasonic signals obtained from examples 4-6 of the present invention at different argon to oxygen ratios and different deposition locations, as is evident from the graph: when the argon-oxygen ratio is 1:3, the longitudinal wave and the transverse wave obtained by excitation have higher intensity. Further, on the premise that the argon-oxygen ratio is fixed, along with the fact that the deposition position is gradually far away from the sputtering center, the signal intensity of the transverse wave is gradually increased, the signal intensity of the longitudinal wave is gradually reduced, generally speaking, the signal intensities of the longitudinal wave and the transverse wave are relatively balanced when the deposition position is 30mm, when the deposition position is located at the sputtering edge, the excited ultrasonic waveform is mainly pure transverse wave, and only a small number of longitudinal waves with lower intensity exist.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made without departing from the spirit and scope of the invention.

Claims (10)

1. A preparation method of ZnO piezoelectric coating material capable of exciting longitudinal-transverse waves simultaneously is characterized in that a binding layer, a ZnO piezoelectric coating, a protective layer and an electrode layer are sequentially formed on a substrate;
the preparation method of the ZnO piezoelectric coating comprises the following steps: under the vacuum condition, forming a ZnO piezoelectric coating on the surface of the bonding layer by adopting a Zn target or a ZnO target through magnetron sputtering; introducing mixed gas of argon and oxygen in the magnetron sputtering; in the mixed gas, the flow ratio of argon to oxygen is 2: 1-1: 3.
2. The method for preparing the ZnO piezoelectric coating according to claim 1, wherein the method for preparing the ZnO piezoelectric coating further comprises the following steps: and in the magnetron sputtering, adjusting the position of the substrate relative to the center to the edge of the target material to ensure that the distance between the position of the substrate relative to the target material and the center of the target material is 0-60 mm.
3. The method according to claim 2, wherein the magnetron sputtering is performed under a vacuum of 4X 10 and a target pitch of 60 to 110mm -3 Pa～7×10 -3 Pa, the sputtering temperature is 50-200 ℃, the sputtering pressure is 1-3 Pa, the sputtering power is 550-700W, and the sputtering time is 1-5 h.
4. The method of claim 3, comprising the steps of:
s1, carrying out plasma etching on the substrate in an argon environment at the temperature of 150-200 ℃;
s2, depositing a Cr bonding layer on the substrate surface treated in the step S1 under the bias conditions of 0.5-1 Pa and 50-250V;
s3, at the temperature of 50-200 ℃, depositing for 1-5 hours on the surface of the Cr bonding layer at 1-3 Pa, adjusting the flow ratio of argon to oxygen to be 2: 1-1: 3, adjusting the distance between the substrate and the target to be 0-60mm, and preparing a ZnO piezoelectric coating;
s4, depositing SiO on the surface of the ZnO piezoelectric coating under the current condition of 1-2 Pa and 0-80A 2 Or a high entropy alloy protective layer;
s5, depositing a Ti electrode layer on the surface of the protective layer under the conditions of 0.25-1 Pa, 0-100V bias voltage and 0-80A current to obtain the ZnO piezoelectric coating material capable of simultaneously exciting longitudinal-transverse waves.
5. A ZnO piezoelectric coating material capable of exciting longitudinal waves and transverse waves simultaneously prepared by the preparation method according to any one of claims 1 to 4, wherein the ZnO piezoelectric coating presents different orientations on the surface of a substrate, and comprises (002) crystal planes and (102) diffraction crystal planes.
6. The ZnO piezoelectric coating material capable of simultaneously exciting longitudinal and transverse waves according to claim 5, wherein the thickness of the ZnO piezoelectric coating is 5-20 micrometers.
7. The ZnO piezoelectric coating material capable of exciting longitudinal waves and transverse waves simultaneously according to claim 5, wherein the thickness of the bonding layer is 250-1000 nanometers.
8. The ZnO piezoelectric coating material capable of exciting longitudinal waves and transverse waves simultaneously according to claim 5, wherein the thickness of the protective layer is 1-5 micrometers.
9. The ZnO piezoelectric coating material capable of simultaneously exciting longitudinal waves and transverse waves according to claim 5, wherein the thickness of the electrode layer is 2-10 micrometers.
10. A smart bolt comprising a ZnO piezoelectric coating material according to any one of claims 5 to 9 which simultaneously excites longitudinal-transverse waves.
CN202210707500.3A 2022-06-21 2022-06-21 ZnO piezoelectric coating material capable of simultaneously exciting longitudinal-transverse waves and preparation method and application thereof Pending CN115094393A (en)

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Citations (4)

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Publication number Priority date Publication date Assignee Title
JPS6321298A (en) * 1986-07-10 1988-01-28 Murata Mfg Co Ltd Production of thin film of piezoelectric zinc oxide crystal
JPH11295281A (en) * 1998-04-08 1999-10-29 Toshiba Tungaloy Co Ltd Ultrasonic transducer for measurement
JP2008182515A (en) * 2007-01-25 2008-08-07 Doshisha Ultrasonic transducer
CN111537132A (en) * 2020-04-20 2020-08-14 中物院成都科学技术发展中心 Axial pretightening force double-wave measurement method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6321298A (en) * 1986-07-10 1988-01-28 Murata Mfg Co Ltd Production of thin film of piezoelectric zinc oxide crystal
JPH11295281A (en) * 1998-04-08 1999-10-29 Toshiba Tungaloy Co Ltd Ultrasonic transducer for measurement
JP2008182515A (en) * 2007-01-25 2008-08-07 Doshisha Ultrasonic transducer
CN111537132A (en) * 2020-04-20 2020-08-14 中物院成都科学技术发展中心 Axial pretightening force double-wave measurement method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YANGHUI JIANG ET AL: ""ZnO piezoelectric coatings used for the ultrasonic excitation of longitudinal-transverse waves and their application for smart bolts"", 《JOURNAL OF VACUUM SCIENCE & TECHNOLOGY B》, vol. 40, no. 4, pages 0430021 - 0430029, XP012266163, DOI: 10.1116/6.0001845 *

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