CN110339992B - Photoinduced ultrasonic transducer and preparation method thereof - Google Patents
Photoinduced ultrasonic transducer and preparation method thereof Download PDFInfo
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- CN110339992B CN110339992B CN201910570950.0A CN201910570950A CN110339992B CN 110339992 B CN110339992 B CN 110339992B CN 201910570950 A CN201910570950 A CN 201910570950A CN 110339992 B CN110339992 B CN 110339992B
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- A61B8/44—Constructional features of the ultrasonic, sonic or infrasonic diagnostic device
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Abstract
The invention discloses a photoinduced ultrasonic transducer and a preparation method thereof, wherein the method comprises the following steps: 1) selecting a cuboid silicon wafer and carrying out ultrasonic cleaning; 2) growing a carbon nano tube array film on a silicon wafer by adopting a chemical vapor deposition method; 3) preparing a PDMS mixed solution; 4) dropping the prepared PDMS on the carbon nano tube array film to enable the PDMS to be dispersed at the top of the carbon nano tube array; 5) then placing the carbon nanotube array film dripped with PDMS in a vacuum environment; 6) after the vacuum pumping is finished, curing the carbon nano tube array film; 7) after the carbon nanotube array film is solidified and torn off from the silicon wafer, the carbon nanotube array film is etched by an inductive coupling plasma etching method (ICP) to be thinned, so that the carbon nanotube array film reaches the expected thickness. 8) The pulse laser is used for generating a high-frequency ultrasonic signal after the thinned carbon nano tube array film is acted. The method has simple process and convenient operation, and the prepared high-frequency photoacoustic transducer has good performance.
Description
Technical Field
The invention relates to the technical field of ultrasound, in particular to a photoinduced ultrasonic transducer and a preparation method thereof.
Background
By virtue of the advantages of safety, convenience, low price, good real-time property and the like, medical ultrasound plays an important role in clinical disease diagnosis and treatment all the time. As a key component for generating and receiving ultrasound, an ultrasound transducer has been a hot spot of research at home and abroad. Traditional ultrasonic transducers are electrically driven devices that rely on the piezoelectric and inverse piezoelectric properties of materials to achieve energy and information interaction between "electricity" and "sound". With the understanding and research on the photo-induced ultrasonic effect, the concept of the photo-induced ultrasonic film is proposed. The photoinduced ultrasonic film belongs to an optical drive device, irradiates an photoinduced ultrasonic material by pulse laser to generate an ultrasonic signal, and can receive and interpret an ultrasonic echo signal by combining an optical fiber technology. In terms of imaging, compared with a traditional piezoelectric device, the size of a photoinduced ultrasonic thin film unit is easily smaller than 100 micrometers, no influence of crosstalk exists between every two units, and no electric connection problem needs to be considered, so that the photoinduced ultrasonic thin film unit has great advantages in endoscopic ultrasonic imaging, particularly in the aspect of high-density array development, the frequency of a photoinduced ultrasonic transducer needs to be further improved in terms of imaging, the influence of the thickness of the transducer on the frequency characteristic of the transducer is obvious, but the photoinduced ultrasonic transducer prepared by the existing spin coating method is difficult to thin, the photoinduced ultrasonic transducer prepared by the traditional pulling method has technical limitations, and the uniformity of a prepared film is poor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to solve the technical problems of uncontrollable transducer thickness, low frequency, miniaturized structure and uneven coating after miniaturization in the preparation process of the photoinduced ultrasonic transducer.
In order to achieve the above object, in a first aspect, the present invention provides a method for manufacturing a photo-induced ultrasonic transducer, including the steps of:
growing a carbon nano tube array film on a silicon chip by using a chemical vapor deposition method;
preparing polydimethylsiloxane mixed liquor, wherein the mixed liquor comprises polydimethylsiloxane and a curing agent;
dripping the dimethyl silicone polymer mixture on the surface of the carbon nano tube array membrane, and waiting for the dimethyl silicone polymer mixture to be fully paved on the surface of the whole carbon nano tube array membrane and be solidified in a vacuum environment, wherein the carbon nano tube array and the solidified dimethyl silicone polymer form the processed carbon nano tube array membrane;
and taking the processed carbon nano tube array film off the silicon wafer, and etching the processed carbon nano tube array film to enable the thickness of the processed carbon nano tube array film to reach a preset thickness, so as to obtain the photoinduced ultrasonic transducer.
Optionally, after the polydimethylsiloxane mixed solution is paved on the surface of the whole carbon nanotube array film, vacuum treatment is performed to uniformly distribute the polydimethylsiloxane among the carbon nanotube array films, air in the carbon nanotube array film is pumped out completely, and the polydimethylsiloxane mixed solution is subjected to thermal curing or photo-curing.
Optionally, preparing a polydimethylsiloxane mixed solution by the following steps:
and respectively adding polydimethylsiloxane and a curing agent according to a preset proportion to obtain polydimethylsiloxane mixed liquor.
Optionally, growing the carbon nanotube array film on the silicon wafer by using a chemical vapor deposition method, specifically including the following steps:
at C2H4、H2And/or He using a high temperature chemical vapor deposition method to prepare the carbon nanotube array film.
Optionally, etching the processed carbon nanotube array film specifically includes the following steps:
using CF4Ar and/or O2And etching the processed carbon nanotube array film as etching gas.
Optionally, before growing the carbon nanotube array film on the silicon wafer by using a chemical vapor deposition method, the method comprises the following steps:
and (3) ultrasonically cleaning the silicon wafer through acetone, alcohol and deionized water in sequence, and cleaning the surface of the silicon wafer.
In a second aspect, the present invention provides a photo-induced ultrasonic transducer comprising: a carbon nanotube array film and polydimethylsiloxane; the polydimethylsiloxane is uniformly solidified on the surface of the carbon nano tube array film.
In a third aspect, the present invention provides a photoinduced ultrasonic transducer prepared based on the preparation method of the photoinduced ultrasonic transducer provided in the first aspect.
Generally, compared with the prior art, the above technical solution conceived by the present invention has the following beneficial effects:
1) according to the photoinduced ultrasonic transducer and the preparation method thereof, the axial thermal conductivity is higher according to the anisotropic characteristic of the thermal conductivity of the carbon nano tube; the carbon nanotube array is used as a material for preparing the photoinduced ultrasonic transducer, so that the axial heat conduction can be effectively improved, and the photoacoustic conversion efficiency of the photoinduced ultrasonic transducer is improved.
2) According to the photoinduced ultrasonic transducer and the preparation method thereof, the thickness of the photoinduced ultrasonic transducer can be effectively controlled through ICP etching, and further the frequency characteristic of the photoinduced ultrasonic transducer is controlled.
3) The photoinduced ultrasonic transducer and the preparation method thereof provided by the invention have the advantage that the miniaturization characteristic of the photoinduced ultrasonic transducer can be realized by manufacturing the carbon nanotube array film on the end face of the optical fiber.
Drawings
FIG. 1 is a flow chart of a method for manufacturing a photo-induced ultrasonic transducer according to the present invention;
FIG. 2 is a schematic structural diagram of a carbon nanotube array film prepared according to the present invention;
FIG. 3 is a schematic view of PDMS coating on a carbon nanotube array film according to the present invention;
FIG. 4 is a schematic structural diagram of a cured carbon nanotube array film and PDMS prepared according to the present invention;
FIG. 5(a) is a schematic diagram of the three-dimensional structure of a substrate-free carbon nanotube array film prepared according to the present invention;
FIG. 5(b) is a schematic cross-sectional view of a substrate-less carbon nanotube array film prepared according to the present invention;
fig. 6 is a schematic structural diagram of the ICP etched carbon nanotube array film prepared according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
FIG. 1 is a flow chart of a method for manufacturing a photo-induced ultrasonic transducer according to the present invention; as shown in fig. 1, the method comprises the following steps:
s101, growing a carbon nano tube array film on a silicon chip by using a chemical vapor deposition method;
s102, preparing a polydimethylsiloxane mixed solution, wherein the mixed solution comprises polydimethylsiloxane and a curing agent;
s103, dripping the dimethyl silicone polymer mixture on the surface of the carbon nano tube array membrane, and waiting for the dimethyl silicone polymer mixture to be solidified in a vacuum environment after the dimethyl silicone polymer mixture is fully paved on the surface of the whole carbon nano tube array membrane, wherein the carbon nano tube array and the solidified dimethyl silicone polymer form the processed carbon nano tube array membrane;
and S104, taking down the processed carbon nano tube array film from the silicon wafer, and etching the processed carbon nano tube array film to enable the thickness of the processed carbon nano tube array film to reach a preset thickness, so as to obtain the photoinduced ultrasonic transducer.
And etching the array film to enable the thickness of the array film to reach a preset thickness, so as to obtain the photoinduced ultrasonic transducer.
Optionally, after the polydimethylsiloxane mixed solution is paved on the surface of the whole carbon nanotube array film, vacuum treatment is performed to uniformly distribute the polydimethylsiloxane among the carbon nanotube array films, air in the carbon nanotube array film is pumped out completely, and the polydimethylsiloxane mixed solution is subjected to thermal curing or photo-curing.
Optionally, preparing a polydimethylsiloxane mixed solution by the following steps:
and respectively adding polydimethylsiloxane and a curing agent according to a preset proportion to obtain polydimethylsiloxane mixed liquor.
Optionally, growing the carbon nanotube array film on the silicon wafer by using a chemical vapor deposition method, specifically including the following steps:
at C2H4、H2And/or He using a high temperature chemical vapor deposition method to prepare the carbon nanotube array film.
Optionally, etching the processed carbon nanotube array film specifically includes the following steps:
using CF4Ar and/or O2And etching the processed carbon nanotube array film as etching gas.
Optionally, before growing the carbon nanotube array film on the silicon wafer by using a chemical vapor deposition method, the method comprises the following steps:
and (3) ultrasonically cleaning the silicon wafer through acetone, alcohol and deionized water in sequence, and cleaning the surface of the silicon wafer.
The invention provides a preparation method of a high-frequency photoinduced ultrasonic transducer, which adopts an ICP etching technology to thin a carbon nano tube array film to enable the thickness of the carbon nano tube array film to be in a micron order, thereby generating a high-frequency ultrasonic signal of dozens of MHz.
In order to achieve the above object, according to the present invention, there is provided a method for manufacturing a high frequency photoacoustic ultrasonic transducer, the method comprising the steps of:
1) selecting a cuboid silicon wafer, wherein the length of the silicon wafer is 1cm, and the width of the silicon wafer is 1 cm;
2) the silicon wafer is sequentially subjected to ultrasonic cleaning by acetone, alcohol and deionized water, the surface of the silicon wafer is cleaned, so that a carbon nanotube array film can be better grown on the surface of the silicon wafer, and then the carbon nanotube array film with the thickness of about 100 mu m is grown on the surface of the silicon wafer by a chemical vapor deposition method, as shown in figure 2.
3) PDMS was prepared, 2g of PDMS was added to the beaker, and 0.2g of curing agent was added.
4) As shown in fig. 3, the prepared PDMS is dropped on the surface of the carbon nanotube array film and spread over the entire film surface, then vacuum treatment is performed for 30min to uniformly distribute the PDMS between the carbon nanotube arrays, air in the film is pumped out, and finally the PDMS is heated in an environment at 90 ℃ for 0.5h to be cured, and the structure is shown in fig. 4.
5) And after the carbon nano tube array film is completely cured, tearing the carbon nano tube array film off the silicon substrate. The carbon nanotube array film structure without a substrate is shown in fig. 5(a) and 5 (b). And thinning the carbon nanotube array film by adopting an ICP (inductively coupled plasma) etching technology, wherein the thinned structure is shown in FIG. 6.
Preferably, the carbon nanotube array in step 2) is prepared by2H4/H2Prepared using high temperature chemical vapor deposition in a mixture of/He (775 ℃).
Preferably, the ICP etching in the step 5) adopts CF4Ar and O2 as etching gases for etching carbon nanotube array film, but not limited toAnd (4) dividing.
Preferably, the carbon nanotube array film is thinned in step 5), so that the thickness of the carbon nanotube array film is controlled to be 10 μm, but not limited to this thickness.
The invention provides a preparation process flow of a high-frequency photoinduced ultrasonic transducer. The method has simple process flow, not only prepares the carbon nanotube array and the PDMS film, but also thins the carbon nanotube film by adopting the ICP etching technology, so that the thickness of the carbon nanotube film is controlled in the micron order.
In one particular embodiment, the example steps are as follows:
1) slicing, namely cutting a silicon wafer with the length of 1cm and the width of 1 cm;
2) and (3) washing, namely washing the cut silicon wafer by using acetone ultrasonic cleaning for 10min, then using ethanol ultrasonic cleaning for 10min, and finally using deionized water ultrasonic cleaning for 10 min. The carbon nanotube array film was then prepared by using high temperature chemical vapor deposition in a mixture of C2H4/H2/He (775℃.)
3) PDMS was prepared, 2g of PDMS was added to the beaker, and 0.2g of curing agent was added.
4) Dropping the prepared PDMS on the surface of the carbon nano tube array film, performing vacuum treatment for 30min to uniformly distribute the PDMS among the carbon nano tube arrays, pumping out air in the film, and finally heating the film in an environment at 90 ℃ for 0.5 h.
5) Tearing off the carbon nanotube array film from the silicon substrate after the carbon nanotube array film is completely cured, thinning the carbon nanotube array film by adopting an ICP (inductively coupled plasma) etching technology, and using CF (CF)4Ar and O2As an etching gas, the thickness of the carbon nanotube array film was controlled to about 10 μm.
6) Applying pulsed laser to the carbon nanotube array film will generate a high frequency ultrasonic signal.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A method for preparing a photoinduced ultrasonic transducer is characterized by comprising the following steps:
growing a carbon nano tube array film on a silicon chip by using a chemical vapor deposition method;
preparing polydimethylsiloxane mixed liquor, wherein the mixed liquor comprises polydimethylsiloxane and a curing agent;
dripping the dimethyl silicone polymer mixture on the surface of the carbon nano tube array membrane, and waiting for the dimethyl silicone polymer mixture to be fully paved on the surface of the whole carbon nano tube array membrane and be solidified in a vacuum environment, wherein the carbon nano tube array and the solidified dimethyl silicone polymer form the processed carbon nano tube array membrane;
taking down the processed carbon nano tube array film from the silicon wafer, and etching the processed carbon nano tube array film to enable the thickness of the processed carbon nano tube array film to reach a preset thickness, so as to obtain the photoinduced ultrasonic transducer;
and after the polydimethylsiloxane mixed solution is paved on the surface of the whole carbon nano tube array membrane, carrying out vacuum treatment to ensure that the polydimethylsiloxane is uniformly distributed among the carbon nano tube array membranes, completely pumping air in the carbon nano tube array membranes, and carrying out thermal curing or photocuring on the polydimethylsiloxane mixed solution.
2. The method of manufacturing a photoacoustic ultrasound transducer according to claim 1, wherein the polydimethylsiloxane mixed solution is prepared by the steps of:
and respectively adding polydimethylsiloxane and a curing agent according to a preset proportion to obtain polydimethylsiloxane mixed liquor.
3. The method for manufacturing a photoinduced ultrasonic transducer according to claim 2, wherein the carbon nanotube array film is grown on the silicon wafer by using a chemical vapor deposition method, and the method specifically comprises the following steps:
at C2H4、H2And/or He using a high temperature chemical vapor deposition method to prepare the carbon nanotube array film.
4. The method for manufacturing a photoacoustic ultrasonic transducer according to claim 2, wherein the etching of the processed carbon nanotube array film specifically comprises the following steps:
using CF4Ar and/or O2And etching the processed carbon nanotube array film as etching gas.
5. The method for manufacturing a photoacoustic ultrasonic transducer according to claim 2, wherein before growing the carbon nanotube array film on the silicon wafer by chemical vapor deposition, the method comprises the following steps:
and (3) ultrasonically cleaning the silicon wafer through acetone, alcohol and deionized water in sequence, and cleaning the surface of the silicon wafer.
6. A photoinduced ultrasonic transducer prepared based on the preparation method of the photoinduced ultrasonic transducer as claimed in any one of claims 1 to 5.
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| CN111112035B (en) * | 2019-12-25 | 2021-02-09 | 华中科技大学 | Transmit-receive integrated all-optical ultrasonic transducer device and preparation method thereof |
| CN112604928B (en) * | 2020-12-17 | 2022-03-15 | 华中科技大学鄂州工业技术研究院 | Photoinduced ultrasonic transducer based on halogen perovskite material and preparation method thereof |
| CN117920556B (en) * | 2024-01-25 | 2024-10-01 | 华中科技大学 | Photo-induced ultrasonic transducer with opened facial blood brain barrier and preparation method thereof |
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| CN101948105A (en) * | 2010-08-25 | 2011-01-19 | 上海理工大学 | Method for preparing vertical array of high-purity single-walled carbon nanotubes |
| CN104787748A (en) * | 2015-04-28 | 2015-07-22 | 南京工业大学 | Preparation method of vertically-grown open carbon nanotube film |
| KR20190007312A (en) * | 2017-07-12 | 2019-01-22 | 성균관대학교산학협력단 | Method for manufacturing optoacoustic transmitter |
| CN109433571A (en) * | 2018-09-25 | 2019-03-08 | 中国科学院电工研究所 | Flexible photic Piezoelectric Thin Film Ultrasonic Transducers and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948105A (en) * | 2010-08-25 | 2011-01-19 | 上海理工大学 | Method for preparing vertical array of high-purity single-walled carbon nanotubes |
| CN104787748A (en) * | 2015-04-28 | 2015-07-22 | 南京工业大学 | Preparation method of vertically-grown open carbon nanotube film |
| KR20190007312A (en) * | 2017-07-12 | 2019-01-22 | 성균관대학교산학협력단 | Method for manufacturing optoacoustic transmitter |
| CN109433571A (en) * | 2018-09-25 | 2019-03-08 | 中国科学院电工研究所 | Flexible photic Piezoelectric Thin Film Ultrasonic Transducers and preparation method thereof |
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