CN117784105A - Ultrasonic sensing device and manufacturing method thereof - Google Patents
Ultrasonic sensing device and manufacturing method thereof Download PDFInfo
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- CN117784105A CN117784105A CN202211142701.XA CN202211142701A CN117784105A CN 117784105 A CN117784105 A CN 117784105A CN 202211142701 A CN202211142701 A CN 202211142701A CN 117784105 A CN117784105 A CN 117784105A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000010410 layer Substances 0.000 claims abstract description 119
- 239000010445 mica Substances 0.000 claims abstract description 88
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 88
- 239000002346 layers by function Substances 0.000 claims abstract description 69
- 239000000758 substrate Substances 0.000 claims abstract description 67
- 239000000463 material Substances 0.000 claims description 39
- 239000002994 raw material Substances 0.000 claims description 32
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 21
- 229910002115 bismuth titanate Inorganic materials 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 229920003023 plastic Polymers 0.000 claims description 13
- 239000004033 plastic Substances 0.000 claims description 13
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 8
- 229910052721 tungsten Inorganic materials 0.000 claims description 8
- 239000010937 tungsten Substances 0.000 claims description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 7
- 239000013077 target material Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 239000010955 niobium Substances 0.000 claims description 6
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 4
- 238000004544 sputter deposition Methods 0.000 claims description 4
- 238000011109 contamination Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 16
- 238000012360 testing method Methods 0.000 description 9
- 229910052697 platinum Inorganic materials 0.000 description 8
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 7
- 229910052737 gold Inorganic materials 0.000 description 7
- 239000010931 gold Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 229940068984 polyvinyl alcohol Drugs 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000012085 test solution Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 2
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- -1 polydimethylsiloxane Polymers 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01S—RADIO DIRECTION-FINDING; RADIO NAVIGATION; DETERMINING DISTANCE OR VELOCITY BY USE OF RADIO WAVES; LOCATING OR PRESENCE-DETECTING BY USE OF THE REFLECTION OR RERADIATION OF RADIO WAVES; ANALOGOUS ARRANGEMENTS USING OTHER WAVES
- G01S7/00—Details of systems according to groups G01S13/00, G01S15/00, G01S17/00
- G01S7/52—Details of systems according to groups G01S13/00, G01S15/00, G01S17/00 of systems according to group G01S15/00
- G01S7/521—Constructional features
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Computer Networks & Wireless Communication (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Radar, Positioning & Navigation (AREA)
- Remote Sensing (AREA)
- Transducers For Ultrasonic Waves (AREA)
Abstract
The invention belongs to the technical field of sensing, in particular relates to an ultrasonic sensing device and a manufacturing method thereof, and aims to solve the technical problems that an existing piezoelectric ultrasonic sensing device is difficult to attach a special-shaped structure and cannot work normally at a higher temperature. The manufacturing method of the ultrasonic sensing device comprises the following steps: providing a mica substrate; forming a bottom electrode layer on a mica substrate; forming a piezoelectric functional layer on the bottom electrode layer; a top electrode layer is formed on the piezoelectric functional layer, the top electrode layer being not in contact with the bottom electrode layer. The flexible high-temperature-resistant ultrasonic sensing device is formed by utilizing good flexibility and high melting point of mica, so that the device can be well attached to a curved surface of a special-shaped structure, the signal acquisition capacity of the ultrasonic sensing device is improved, and the device can work for a long time under a high-temperature condition, so that the application range of the ultrasonic sensing device is wider.
Description
Technical Field
The embodiment of the invention relates to the technical field of sensing, in particular to an ultrasonic sensing device and a manufacturing method thereof.
Background
An ultrasonic sensing device is an electronic component that converts vibration signals into electrical signals. The ultrasonic sensing device is usually a hard sensor, and the hard sensor adopts inorganic materials such as piezoelectric ceramics, aluminum nitride, zinc oxide and the like, and the materials have higher piezoelectric coefficients and wider piezoelectric response ranges. However, the high hardness and low toughness of the materials make the hard sensor often have a rigid end face, and the problem that a special-shaped structure is difficult to apply is caused, especially the hard sensor and the curved surface of the special-shaped structure often only can realize point contact or line contact, so that acquisition of fault signals or defect signals is affected, and missed judgment and erroneous judgment are easily caused.
In particular, in the field of nondestructive testing, a rigid sensor used for ultrasonic guided wave detection generally comprises a single or array sensing unit with a fixed shape and size, and the sensing unit mostly adopts lead zirconate titanate piezoelectric ceramics. The degree of fit of the hard sensor to the special-shaped structure is low, so that the hard sensor cannot fully acquire the defect acoustic signals. In addition, the curie temperature of the hard sensor is mostly lower than 500 ℃, and the operating temperature is lower. For example, lead zirconate titanate piezoelectric ceramics have a curie temperature point around 300 ℃ and an operating temperature range of-25 ℃ to +80 ℃, and when the ambient temperature exceeds 100 ℃, the piezoelectric performance of the hard sensor is greatly reduced, and if the ambient temperature exceeds the curie temperature, the ferroelectric and piezoelectric properties of the hard sensor are lost and are not recoverable.
For this reason, a flexible and high temperature resistant ultrasonic sensing device is required.
Disclosure of Invention
In view of the above problems, embodiments of the present invention provide an ultrasonic sensing device and a method for manufacturing the same, which are used for applying a special-shaped structure and can work under a high temperature condition.
In order to achieve the above object, the embodiment of the present invention provides the following technical solutions:
in a first aspect, an embodiment of the present invention provides a method for manufacturing an ultrasonic sensing device, including:
providing a mica substrate;
forming a bottom electrode layer on the mica substrate;
forming a piezoelectric functional layer on the bottom electrode layer;
a top electrode layer is formed on the piezoelectric functional layer, the top electrode layer being free of contact with the bottom electrode layer.
In some possible embodiments, providing a mica substrate includes:
thinning the mica by mechanical stripping to form a mica substrate with a preset thickness;
and cleaning the mica substrate to reduce pollution on the mica substrate.
In some possible embodiments, the mica comprises fluorogenic mica, the predetermined thickness being less than or equal to 100 μm;
and/or cleaning the mica substrate to reduce contamination on the mica substrate includes:
washing the mica substrate by using absolute ethyl alcohol;
and placing the cleaned mica substrate into an oven for drying.
In some possible embodiments, forming a bottom electrode layer on the mica substrate comprises:
and depositing and forming the bottom electrode layer on the mica substrate by utilizing magnetron sputtering, wherein the thickness of the bottom electrode layer is less than or equal to 10 mu m.
In some possible embodiments, the shielding gas during the magnetron sputtering includes argon, the vacuum degree is 0.04-0.06 mbar, and the voltage is 40-60V.
In some possible embodiments, forming a piezoelectric functional layer on the bottom electrode layer includes:
preparing raw materials according to the material of the piezoelectric functional layer, and grinding the raw materials for the first time to mix the raw materials;
presintering the raw materials after the first grinding to enable all components of the raw materials to react;
grinding the presintered raw materials for the second time to form material powder;
adding a binder into the material powder, and forming under the preset pressure condition;
performing plastic discharge and sintering on the formed material powder to form a piezoelectric functional layer target;
and forming the piezoelectric function layer on the bottom electrode layer by utilizing the piezoelectric function layer target material.
In some possible embodiments, the material of the piezoelectric functional layer includes bismuth titanate doped with at least one of sodium, calcium, tungsten, and niobium;
and/or the first grinding is ball milling, and the ball milling time is 4-6 hours;
and/or the binder comprises polyvinyl alcohol, and the preset pressure is 50-150 MPa;
and/or the temperature during plastic discharge is 400-500 ℃, the temperature is raised to 1000-1100 ℃ at the speed of 1.5-2.5 ℃/min after plastic discharge, and the temperature is kept for sintering for 9-11 hours;
and/or, after the sintering, carrying out surface treatment on the sintered and formed material powder to form the piezoelectric functional layer target;
and/or the piezoelectric functional layer is formed by magnetron sputtering by the target material of the piezoelectric functional layer, wherein the protective gas in the magnetron sputtering is argon, and the sputtering power is 55-70W.
In some possible embodiments, forming a top electrode layer on the piezoelectric functional layer, the top electrode layer not in contact with the bottom electrode layer, comprises:
and depositing and forming the top electrode layer on the piezoelectric functional layer by utilizing magnetron sputtering.
The manufacturing method of the ultrasonic sensing device provided by the embodiment of the invention has at least the following advantages:
according to the manufacturing method of the ultrasonic sensing device, the bottom electrode layer, the piezoelectric functional layer and the top electrode layer are sequentially formed on the mica substrate, the mica substrate is used as a support, and the flexible high-temperature-resistant ultrasonic sensing device is formed by using good flexibility and high melting point of mica, so that the flexible high-temperature-resistant ultrasonic sensing device can be well attached to a curved surface of a special structure, the signal acquisition capability of the ultrasonic sensing device is improved, and the ultrasonic sensing device can work for a long time under the high-temperature condition, so that the application range of the ultrasonic sensing device is wider.
In a second aspect, an embodiment of the present invention provides an ultrasonic sensing device formed by the manufacturing method as described above, including: the piezoelectric ceramic comprises a mica substrate, a bottom electrode layer formed on the mica substrate, a piezoelectric functional layer arranged on the bottom electrode layer, and a top electrode layer arranged on the piezoelectric functional layer, wherein the top electrode layer is not contacted with the bottom electrode layer.
In some possible embodiments, the material of the piezoelectric functional layer includes bismuth titanate doped with sodium, calcium, tungsten, and niobium;
and/or the bottom electrode layer is provided with a first leading-out end, the top electrode is provided with a second leading-out end, at least part of the second leading-out end is positioned on the mica substrate, and the second leading-out end and the first leading-out end are arranged in a dislocation mode.
The ultrasonic sensing device provided by the embodiment of the invention has at least the following advantages:
the ultrasonic sensing device provided by the embodiment of the invention comprises a mica substrate, a bottom electrode layer, a piezoelectric functional layer and a top electrode layer which are sequentially arranged, and the flexible high-temperature-resistant ultrasonic sensing device is formed by utilizing good flexibility and high melting point of mica so as to be applied with a special-shaped structure and can work under a high-temperature condition.
In addition to the technical problems, technical features constituting the technical solutions, and beneficial effects caused by the technical features of the technical solutions described above, other technical problems that can be solved by the ultrasonic sensing device and the manufacturing method thereof, other technical features included in the technical solutions, and beneficial effects caused by the technical features provided by the embodiments of the present invention will be described in further detail in the detailed description of the present invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method of fabricating an ultrasonic sensing device in an embodiment of the invention;
FIG. 2 is a schematic diagram of a bottom electrode layer formed according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of a piezoelectric functional layer according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of an embodiment of the present invention after forming a top electrode layer;
fig. 5 is a diagram of a process for fabricating a piezoelectric functional layer target in an embodiment of the present invention.
Reference numerals illustrate:
10-mica substrate;
20-a bottom electrode layer;
30-a piezoelectric functional layer;
40-top electrode layer.
Detailed Description
The sensor in the related art is difficult to attach a special-shaped structure and cannot work normally at a higher temperature, and therefore, the embodiment of the invention provides a manufacturing method of an ultrasonic sensing device, wherein a bottom electrode layer, a piezoelectric functional layer and a top electrode layer which are stacked are sequentially formed on a mica substrate, and the flexible high-temperature-resistant ultrasonic sensing device is formed by using good flexibility and high melting point of mica so as to attach the special-shaped structure and can work at a high temperature.
In order to make the above objects, features and advantages of the embodiments of the present invention more comprehensible, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
An embodiment of the present invention provides a method for manufacturing an ultrasonic sensing device, referring to fig. 1, fig. 1 is a method for manufacturing an ultrasonic sensing device in an embodiment of the present invention, which specifically includes the following steps:
step S100: a mica substrate is provided.
Mica, as an inorganic material having a layered structure, can be regarded as a two-dimensional material when its thickness is thin, that is, its thickness is negligible. The mica has good flexibility, can be well attached to the curved surface of the special-shaped structure, and cannot be damaged due to deformation; and the glass has better transparency, the light transmittance is more than 80 percent, and the influence on light is small.
In addition, mica can also maintain chemical stability under high temperature conditions, where high temperature refers to a temperature greater than or equal to 300 ℃, as compared to organic polymers such as Polyimide (PI), polyvinyl alcohol (Polyvinyl Alcohol PVA), polydimethylsiloxane (Poly-Dimethyl Siloxane PDMS), and the like. In particular, mica can still maintain stability under 1100 ℃ conditions, so that the ultrasonic sensing device can withstand high temperatures.
In one possible implementation, providing a mica substrate may include: thinning the mica by mechanical peeling to form a mica substrate 10 having a predetermined thickness; the mica substrate 10 is cleaned to reduce contamination on the mica substrate 10.
Specifically, mica is peeled layer by layer using tweezers to form a mica substrate 10 having a predetermined thickness; and cleaning the mica substrate 10 by using absolute ethyl alcohol, and drying the cleaned mica substrate 10 in an oven. Wherein, the mica substrate 10 can be cleaned by absolute ethyl alcohol for 2-3 times, and then the cleaned mica substrate 10 is put into a blast air temperature box for drying, the drying temperature is 80 ℃, and the drying time is 1 hour. Preferably, the predetermined thickness may be less than or equal to 100 μm to ensure that the mica substrate 10 is flexible and not easily damaged, and the mica may be smooth fluorine crystal mica.
Step S200: a bottom electrode layer is formed on the mica substrate.
The thickness of the bottom electrode layer 20 is less than or equal to 10 μm to avoid the bottom electrode layer 20 from falling off the mica substrate 10. Referring to fig. 2, the bottom electrode layer 20 may be deposited on the mica substrate 10 using magnetron sputtering, for example, the bottom electrode layer 20 may be formed on the mica substrate 10 using a direct current magnetron sputtering method.
Preferably, the material of the bottom electrode layer 20 may be platinum or gold, and the platinum or gold may be used to make the bottom electrode layer 20 have good conductivity, and reduce oxide formation of the bottom electrode layer 20 under high temperature condition, so as to ensure conductivity of the bottom electrode layer 20 under high temperature condition. The material of the bottom electrode layer 20 is not limited, and may be titanium, nickel, or the like.
Specifically, platinum or gold is mounted on a radio frequency magnetron sputtering apparatus, and a bottom electrode layer 20 is sputtered on the mica substrate 10. The shielding gas during magnetron sputtering comprises argon, the vacuum degree is 0.04-0.06 mbar, the voltage is 40-60V, for example, the vacuum degree can be 0.05mbar, and the voltage can be 50V, so that the bottom electrode layer 20 with a relatively flat surface and a relatively good structure is obtained.
Step S300: a piezoelectric functional layer is formed on the bottom electrode layer.
Referring to fig. 3, a piezoelectric functional layer 30 is formed on the bottom electrode layer 20 through a magnetron sputtering process, wherein the magnetron sputtering target is bismuth titanate doped with at least one of sodium, calcium, tungsten, and niobium prepared based on a solid phase reaction method. The bismuth titanate has better high-temperature performance, namely the bismuth titanate has higher Curie temperature and mechanical performance, and ensures the stable operation of the ultrasonic sensing device under the high-temperature condition. The piezoelectric performance of the bismuth titanate can be improved by doping the bismuth titanate, and the high sensitivity of the ultrasonic sensing device under the high-temperature working condition can be ensured.
It will be appreciated that the piezoelectric functional layer 30 may be bismuth titanate doped with sodium or bismuth titanate doped with sodium and calcium. Preferably, the piezoelectric functional layer 30 in the embodiment of the present invention is made of bismuth titanate doped with tungsten, and the molecular formula thereof may be Bi 4 Ti 2.94 W 0.06 O 12 The high temperature and the piezoelectric performance of the composite material are good.
Step S400: a top electrode layer is formed on the piezoelectric functional layer, the top electrode layer being not in contact with the bottom electrode layer.
Referring to fig. 4, an exemplary top electrode layer 40 may be deposited on the piezoelectric functional layer 30 using magnetron sputtering. Preferably, the top electrode layer 40 may be made of a metal such as platinum or gold, so that the top electrode layer 40 has good electrical conductivity, and oxide generated by the top electrode layer 40 under high temperature condition is reduced, so as to ensure electrical conductivity of the top electrode layer 40 under high temperature condition.
Specifically, platinum or gold is mounted on a radio frequency magnetron sputtering device, and a top electrode layer 40 is sputtered on the piezoelectric functional layer 30. The shielding gas during magnetron sputtering comprises argon, the vacuum degree is 0.04-0.06 mbar, the voltage is 40-60V, for example, the vacuum degree can be 0.05mbar, and the voltage can be 50V, so that the top electrode layer 40 with a relatively flat surface and a relatively good structure is obtained.
The material of the top electrode layer 40 is not limited in this embodiment, and may be nickel or the like. The material of the top electrode layer 40 may be the same as that of the bottom electrode layer 20, for example, both are platinum; the material of the top electrode layer 40 may also be different from the material of the bottom electrode layer 20, for example, the material of the top electrode layer 40 is platinum and the material of the bottom electrode layer 20 is gold.
In summary, in the manufacturing method of the ultrasonic sensing device according to the embodiment of the invention, the bottom electrode layer 20, the piezoelectric functional layer 30 and the top electrode layer 40 which are stacked are sequentially formed on the mica substrate 10, and the flexible high-temperature-resistant ultrasonic sensing device is formed by utilizing good flexibility and high melting point of mica, so that on one hand, the flexible high-temperature-resistant ultrasonic sensing device can be well attached to a curved surface of a special-shaped structure, the signal acquisition capability of the ultrasonic sensing device is improved, and on the other hand, the ultrasonic sensing device can also work for a long time under a high-temperature condition, so that the application range of the ultrasonic sensing device is wider.
In some possible embodiments, forming the piezoelectric functional layer on the bottom electrode layer may specifically include the steps of:
step S301: the raw materials are prepared according to the material of the piezoelectric functional layer, and are ground for the first time so as to be mixed.
Specifically, the raw material is selected according to the molecular formula of the piezoelectric functional layer 30, and the raw material may be a metal oxide containing a formulation element or a compound which can be heated to become an oxide. Exemplary materials for the piezoelectric functional layer 30 are bismuth titanate doped with tungsten, which may be Bi 4 Ti 2.94 W 0.06 O 12 The raw materials may include titanium dioxide (TiO 2 ) Bismuth trioxide (Bi) 2 O 3 ) And tungsten trioxide (WO) 3 )。
After the raw materials are selected, the raw material ratio is calculated according to the molecular formula of the piezoelectric functional layer 30, and the raw materials of corresponding mass are weighed, such as ingredients in the step shown in fig. 5. To ensure accurate weighing, after the raw materials are selected, the raw materials are placed in a blast air incubator and dried, for example, for 1 hour, before weighing.
And grinding the weighed raw materials for the first time to fully mix the raw materials so as to ensure that the raw materials can fully react in the subsequent process. Wherein the first grinding is ball milling, and the ball milling time is 4-6 hours. Such as the first ball milling in the step shown in fig. 5. Illustratively, absolute ethyl alcohol is used as a ball milling medium, raw materials are ball-milled in a ball mill for 4-6 hours, and the raw materials are dried after ball milling is finished. The first drying in the step shown in fig. 5.
Step S302: the raw materials after the first grinding are presintered to react the components of the raw materials.
Specifically, the raw materials after the first grinding are put into a crucible, and the crucible is put into a high-temperature furnace to be presintered at a proper temperature and a proper heat preservation time, so that the components of the raw materials fully react, and the presintering is performed in the step shown in fig. 5. Illustratively, the temperature in the high temperature furnace may be 850 ℃, and the heat preservation time is 2 hours, that is, the raw materials after the first grinding are pre-burned in the high temperature furnace at 850 ℃ for 2 hours.
Step S303: and grinding the presintered raw materials for the second time to form material powder.
Illustratively, the preset raw materials are ball-milled and crushed in absolute ethyl alcohol by using a ball mill, and are subjected to drying treatment to form material powder, such as second ball milling and second drying in the steps shown in fig. 5.
Step S304: and adding a binder into the material powder, and forming under the preset pressure condition.
In one possible implementation, the material powder is granulated by adding a binder, applying a preset pressure using a tablet press, and shaping in a die, such as the granulation in the step shown in fig. 5. Wherein, the binder can be polyvinyl alcohol (Poly Vinyl Alcohol, PVA for short), the concentration of the polyvinyl alcohol can be 7 percent, and the preset pressure is 50-150 MPa.
Step S305: and (3) performing plastic discharge and sintering on the formed material powder to form the piezoelectric functional layer target.
And (3) sequentially carrying out plastic discharging and sintering on the formed material powder, wherein the temperature during plastic discharging is 400-500 ℃, the temperature is raised to 1000-1100 ℃ at the speed of 1.5-2.5 ℃/min after plastic discharging, and the material powder is subjected to heat preservation and sintering for 9-11 hours, such as plastic discharging and sintering in the steps shown in fig. 5. Illustratively, the molded material powder is placed in a low temperature furnace and is subjected to plastic discharge at 450 ℃ for 2 hours; then the temperature is raised to 1050 ℃ at the speed of 2 ℃/min, and the temperature is kept for sintering for 10 hours.
In order to obtain the piezoelectric functional layer target material with better quality, the sintered material powder is subjected to surface treatment to reduce the surface roughness of the piezoelectric functional layer target material, so that the piezoelectric functional layer target material has lower surface roughness to facilitate subsequent processing, such as surface treatment in the step shown in fig. 5. In short, the piezoelectric functional layer target is obtained after material proportioning, ball milling, drying, presintering, ball milling, drying, granulating, plastic discharging, sintering and surface treatment.
Step S306: and forming a piezoelectric functional layer on the bottom electrode layer by using the piezoelectric functional layer target.
In some possible implementations, the piezoelectric functional layer target forms the piezoelectric functional layer 30 on the bottom electrode layer 20 by magnetron sputtering, wherein the shielding gas is argon gas and the sputtering power is 55-70W. Specifically, the piezoelectric functional layer target is mounted on a radio frequency magnetron sputtering device, and the piezoelectric functional layer 30 is formed on the bottom electrode layer 20 by sputtering.
A second aspect of the embodiment of the present invention provides an ultrasonic sensing device, which is formed by the above-mentioned manufacturing method, referring to fig. 4, and includes: the piezoelectric ceramic comprises a mica substrate 10, a bottom electrode layer 20 formed on the mica substrate 10, a piezoelectric functional layer 30 arranged on the bottom electrode layer 20, and a top electrode layer 40 arranged on the piezoelectric functional layer 30, wherein the top electrode layer 40 is not contacted with the bottom electrode layer 20.
Wherein, the material of the mica substrate 10 can be fluorine crystal mica, and the thickness of the mica substrate 10 can be less than or equal to 100 μm, so that the mica substrate has better flexibility. The thickness of the bottom electrode layer 20 is less than or equal to 10 μm to avoid the bottom electrode layer 20 from falling off the mica substrate 10. The bottom electrode layer 20 and the top electrode layer 40 may be metal layers with good conductivity, and the material may be platinum or gold, which has good stability under high temperature conditions.
In some possible embodiments, the piezoelectric functional layer 30 is made of bismuth titanate doped with sodium, calcium, tungsten and niobium, and the bismuth titanate has good high-temperature performance, i.e. the bismuth titanate has high curie temperature and mechanical performance, so as to ensure stable operation of the ultrasonic sensing device under high-temperature conditions. The piezoelectric performance of the bismuth titanate can be improved by doping the bismuth titanate, and the high sensitivity of the ultrasonic sensing device under the high-temperature working condition can be ensured.
In some possible embodiments, the bottom electrode layer 20 has a first lead-out and the top electrode layer 40 has a second lead-out, at least a portion of which is located on the mica substrate 10, and the second lead-out is offset from the first lead-out.
Specifically, the bottom electrode layer 20 includes a first body and a first lead-out terminal connected to the first body, the top electrode layer 40 has a second body and a second lead-out terminal connected to the second body, and the piezoelectric functional layer 30 is disposed between the first body and the second body, so that the first body and the second body are insulated from each other, and the first lead-out terminal and the second lead-out terminal are arranged in a dislocation manner, so that the bottom electrode layer 20 and the top electrode layer 40 are isolated from each other.
The first body and the first lead-out end are both located on the mica substrate 10, the piezoelectric functional layer 30 covers at least the first body, and at least part of the first lead-out end is exposed, that is, the piezoelectric functional layer 30 covers the first body and may also cover part of the first lead-out end. The second body is located on the piezoelectric functional layer 30, the second lead-out end is at least partially located on the mica substrate 10, and the second lead-out end and the first lead-out end are arranged in a staggered mode. The orthographic projection of the piezoelectric functional layer 30 on the mica substrate 10 covers the orthographic projection of the first body on the mica substrate 10 and covers the orthographic projection of the second body on the mica substrate 10, so that the contact of the bottom electrode layer 20 and the top electrode layer 40 can be avoided.
In summary, the ultrasonic sensing device in the embodiment of the invention comprises a mica substrate 10, a bottom electrode layer 20, a piezoelectric functional layer 30 and a top electrode layer 40 which are sequentially arranged, and the flexible high-temperature-resistant ultrasonic sensing device is formed by utilizing good flexibility and high melting point of mica so as to be attached with a special-shaped structure and can work under a high-temperature condition.
In the corrosion-resistant test method provided by the embodiment of the invention, a sample to be detected and a test solution are provided, wherein the sample to be detected comprises a test surface; mounting a sample to be detected in the sample clamp, wherein the test surface is exposed in the first through hole; placing a test solution into a test container, and installing a sample clamp, a reference electrode and an auxiliary electrode; after the temperature is raised to the test temperature, the test solution is filled with test gas, and the test surface is subjected to corrosion resistance test. The isolation effect of the non-test surface of the sample to be detected is improved through the sample clamp, so that the accuracy of the test result is improved.
In this specification, each embodiment or implementation is described in a progressive manner, and each embodiment focuses on a difference from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other.
It will be appreciated by those skilled in the art that in the present disclosure, the terms "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," etc. refer to an orientation or positional relationship based on that shown in the drawings, which is merely for convenience of description and to simplify the description, and do not indicate or imply that the system or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore the above terms should not be construed as limiting the present invention.
In the description of the present specification, reference is made to "one embodiment," "some embodiments," "an exemplary embodiment," "an example," "a particular instance," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. A method of making an ultrasonic sensing device, comprising:
providing a mica substrate;
forming a bottom electrode layer on the mica substrate;
forming a piezoelectric functional layer on the bottom electrode layer;
a top electrode layer is formed on the piezoelectric functional layer, the top electrode layer being free of contact with the bottom electrode layer.
2. The method of making of claim 1, wherein providing a mica substrate comprises:
thinning the mica by mechanical stripping to form a mica substrate with a preset thickness;
and cleaning the mica substrate to reduce pollution on the mica substrate.
3. The method of claim 2, wherein the mica comprises fluorogenic mica, the predetermined thickness being less than or equal to 100 μιη;
and/or cleaning the mica substrate to reduce contamination on the mica substrate includes:
washing the mica substrate by using absolute ethyl alcohol;
and placing the cleaned mica substrate into an oven for drying.
4. The method of making according to claim 1, wherein forming a bottom electrode layer on the mica substrate comprises:
and depositing and forming the bottom electrode layer on the mica substrate by utilizing magnetron sputtering, wherein the thickness of the bottom electrode layer is less than or equal to 10 mu m.
5. The method according to claim 4, wherein the shielding gas during the magnetron sputtering comprises argon gas, the vacuum degree is 0.04-0.06 mbar, and the voltage is 40-60V.
6. The method of any one of claims 1 to 5, wherein forming a piezoelectric functional layer on the bottom electrode layer comprises:
preparing raw materials according to the material of the piezoelectric functional layer, and grinding the raw materials for the first time to mix the raw materials;
presintering the raw materials after the first grinding to enable all components of the raw materials to react;
grinding the presintered raw materials for the second time to form material powder;
adding a binder into the material powder, and forming under the preset pressure condition;
performing plastic discharge and sintering on the formed material powder to form a piezoelectric functional layer target;
and forming the piezoelectric function layer on the bottom electrode layer by utilizing the piezoelectric function layer target material.
7. The method according to claim 6, wherein the piezoelectric functional layer is made of bismuth titanate doped with at least one of sodium, calcium, tungsten, and niobium;
and/or the first grinding is ball milling, and the ball milling time is 4-6 hours;
and/or the binder comprises polyvinyl alcohol, and the preset pressure is 50-150 MPa;
and/or the temperature during plastic discharge is 400-500 ℃, the temperature is raised to 1000-1100 ℃ at the speed of 1.5-2.5 ℃/min after plastic discharge, and the temperature is kept for sintering for 9-11 hours;
and/or, after the sintering, carrying out surface treatment on the sintered and formed material powder to form the piezoelectric functional layer target;
and/or the piezoelectric functional layer is formed by magnetron sputtering by the target material of the piezoelectric functional layer, wherein the protective gas in the magnetron sputtering is argon, and the sputtering power is 55-70W.
8. The method according to any one of claims 1 to 5, wherein a top electrode layer is formed on the piezoelectric functional layer, the top electrode layer being not in contact with the bottom electrode layer, comprising:
and depositing and forming the top electrode layer on the piezoelectric functional layer by utilizing magnetron sputtering.
9. An ultrasonic sensing device formed by the manufacturing method of any one of claims 1 to 8, the ultrasonic sensing device comprising: the piezoelectric ceramic comprises a mica substrate, a bottom electrode layer formed on the mica substrate, a piezoelectric functional layer arranged on the bottom electrode layer, and a top electrode layer arranged on the piezoelectric functional layer, wherein the top electrode layer is not contacted with the bottom electrode layer.
10. The ultrasonic sensing device of claim 9, wherein the piezoelectric functional layer comprises bismuth titanate doped with sodium, calcium, tungsten, niobium;
and/or the bottom electrode layer is provided with a first leading-out end, the top electrode layer is provided with a second leading-out end, at least part of the second leading-out end is positioned on the mica substrate, and the second leading-out end and the first leading-out end are arranged in a dislocation mode.
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| CN202211142701.XA CN117784105A (en) | 2022-09-20 | 2022-09-20 | Ultrasonic sensing device and manufacturing method thereof |
| PCT/CN2023/119347 WO2024061152A1 (en) | 2022-09-20 | 2023-09-18 | Ultrasonic sensing device and manufacturing method therefor |
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| CN106554202B (en) * | 2016-11-14 | 2019-09-27 | 山东大学 | A kind of bismuth laminated bismuth-sodium titanate high temperature piezoceramics and preparation method thereof |
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| CN110395768A (en) * | 2018-10-26 | 2019-11-01 | 济南大学 | A kind of preparation method of flexibility self poling ferrous acid bismuth-based thin films |
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