CN110339992B - A kind of photoinduced ultrasonic transducer and preparation method thereof - Google Patents
A kind of photoinduced ultrasonic transducer and preparation method thereof Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- carbon nanotube
- nanotube array
- array film
- polydimethylsiloxane
- silicon wafer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 81
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 81
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 45
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 45
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 25
- 239000010703 silicon Substances 0.000 claims abstract description 25
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000005530 etching Methods 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- -1 polydimethylsiloxane Polymers 0.000 claims description 32
- 235000012431 wafers Nutrition 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000009489 vacuum treatment Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 235000013870 dimethyl polysiloxane Nutrition 0.000 abstract description 35
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 abstract description 13
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 3
- 238000009616 inductively coupled plasma Methods 0.000 abstract 2
- 238000004506 ultrasonic cleaning Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 57
- 239000012528 membrane Substances 0.000 description 7
- 238000003491 array Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000003384 imaging method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002071 nanotube Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002238 carbon nanotube film Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000009558 endoscopic ultrasound Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B8/00—Diagnosis using ultrasonic, sonic or infrasonic waves
- A61B8/12—Diagnosis using ultrasonic, sonic or infrasonic waves in body cavities or body tracts, e.g. by using catheters
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B8/00—Diagnosis using ultrasonic, sonic or infrasonic waves
- A61B8/44—Constructional features of the ultrasonic, sonic or infrasonic diagnostic device
- A61B8/4483—Constructional features of the ultrasonic, sonic or infrasonic diagnostic device characterised by features of the ultrasound transducer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B06—GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS IN GENERAL
- B06B—METHODS OR APPARATUS FOR GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS OF INFRASONIC, SONIC, OR ULTRASONIC FREQUENCY, e.g. FOR PERFORMING MECHANICAL WORK IN GENERAL
- B06B1/00—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Heart & Thoracic Surgery (AREA)
- Molecular Biology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Pathology (AREA)
- Radiology & Medical Imaging (AREA)
- Physics & Mathematics (AREA)
- Biomedical Technology (AREA)
- Veterinary Medicine (AREA)
- Medical Informatics (AREA)
- Biophysics (AREA)
- Surgery (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Gynecology & Obstetrics (AREA)
- Mechanical Engineering (AREA)
- Transducers For Ultrasonic Waves (AREA)
- Ultra Sonic Daignosis Equipment (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明公开一种光致超声换能器及其制备方法，该方法包括以下步骤：1)选取长方体形状的硅片并进行超声清洗；2)采用化学气相沉淀法在硅片上生长碳纳米管阵列膜；3)配置PDMS混合溶液；4)将配好的PDMS滴在碳纳米管阵列膜上使其在碳纳米管阵列顶部分散开；5)然后将滴有PDMS的碳纳米管阵列膜放置于真空环境下；6)抽完真空后在将碳纳米管阵列膜固化；7)待碳纳米管阵列膜固化后，将其从硅片上撕下后，采用感应耦合等离子体刻蚀法(ICP)对碳纳米管阵列膜进行刻蚀使其变薄厚度，使其达到预期的厚度。8)将脉冲激光做作用于减薄后的碳纳米管阵列膜后将会产生高频超声信号。本发明方法工艺简单，操作方便，制备的高频光声换能器性能良好。
The invention discloses a photo-induced ultrasonic transducer and a preparation method thereof. The method includes the following steps: 1) selecting a silicon wafer in the shape of a cuboid and performing ultrasonic cleaning; 2) using a chemical vapor deposition method to grow carbon nanotubes on the silicon wafer Array film; 3) Configure PDMS mixed solution; 4) Drop the prepared PDMS on the carbon nanotube array film to spread it on the top of the carbon nanotube array; 5) Then place the PDMS-dropped carbon nanotube array film on the In a vacuum environment; 6) after vacuuming, the carbon nanotube array film is cured; 7) after the carbon nanotube array film is cured, it is torn off from the silicon wafer, and the inductively coupled plasma etching method ( ICP) to etch the carbon nanotube array film to make it thinner to reach the desired thickness. 8) After the pulsed laser is applied to the thinned carbon nanotube array film, a high-frequency ultrasonic signal will be generated. The method of the invention has the advantages of simple process and convenient operation, and the prepared high-frequency photoacoustic transducer has good performance.
Description
技术领域technical field
本发明涉及超声技术领域，更具体地，涉及一种光致超声换能器及其制备方法。The invention relates to the field of ultrasonic technology, and more particularly, to a photo-induced ultrasonic transducer and a preparation method thereof.
背景技术Background technique
凭借安全便捷、价格低廉、实时性好等优点，医学超声在临床疾病诊断与治疗中一直发挥着重要作用。作为超声产生与接收的关键部件，超声换能器一直是国内外研究的热点。传统超声换能器是电驱动器件，依靠材料的压电与逆压电特性，实现“电”与“声”之间的能量和信息的交互。随着人们对光致超声效应的认识与研究逐渐深入，光致超声薄膜的概念被提出。光致超声薄膜属于光驱动器件，依靠脉冲激光照射光致超声材料产生超声信号，结合光纤技术可接收与解读超声回波信号。就成像而言，与传统压电型器件相比，光致超声薄膜单元尺寸易小于100μm而且每个单元间没有串扰的影响，也不用考虑电连接问题，因此其在内窥式超声成像、特别是在高密度阵列研制方面具有很大的优势，但就成像的角度考虑光致超声换能器的频率还需进一步提高，而换能器的厚度对其频率特性的影响是比较明显的，但现有的旋涂法制备的光致超声换能器很难将光致超声换能器做薄，而传统的提拉法制备的光致超声换能器又存在技术限制，制备的膜均匀性较差。With the advantages of safety, convenience, low price, and good real-time performance, medical ultrasound has always played an important role in the diagnosis and treatment of clinical diseases. As a key component of ultrasonic generation and reception, ultrasonic transducers have always been a research hotspot at home and abroad. Traditional ultrasonic transducers are electrically driven devices, relying on the piezoelectric and inverse piezoelectric properties of materials to realize the interaction of energy and information between "electricity" and "sound". With the deepening of people's understanding and research on the photoinduced ultrasonic effect, the concept of photoinduced ultrasonic thin film was proposed. The photo-induced ultrasonic film is a light-driven device. It relies on the pulsed laser to irradiate the photo-induced ultrasonic material to generate ultrasonic signals. Combined with optical fiber technology, it can receive and interpret the ultrasonic echo signals. In terms of imaging, compared with traditional piezoelectric devices, the unit size of photoinduced ultrasound thin film is easily smaller than 100 μm, and there is no influence of crosstalk between each unit, and there is no need to consider the problem of electrical connection. Therefore, it is especially suitable for endoscopic ultrasound imaging. It has great advantages in the development of high-density arrays, but from the perspective of imaging, the frequency of photoinduced ultrasonic transducers needs to be further improved, and the thickness of the transducer has an obvious influence on its frequency characteristics, but The photoultrasonic transducer prepared by the existing spin coating method is difficult to make the photoultrasonic transducer thin, while the photoultrasonic transducer prepared by the traditional pulling method has technical limitations, and the prepared film is uniform. poor.
发明内容SUMMARY OF THE INVENTION
针对现有技术的缺陷，本发明的目的在于解决光致超声换能器制备过程中换能器厚度不可控、频率不高、结构微型化及微型化后涂膜不均匀的技术问题。In view of the defects of the prior art, the purpose of the present invention is to solve the technical problems of uncontrollable transducer thickness, low frequency, structure miniaturization and uneven coating film after miniaturization during the preparation process of the photoinduced ultrasonic transducer.
为实现上述目的，第一方面，本发明提供一种光致超声换能器的制备方法，包括以下步骤：In order to achieve the above object, in the first aspect, the present invention provides a preparation method of a photo-induced ultrasonic transducer, comprising the following steps:
在硅片上利用化学气相沉积法生长碳纳米管阵列膜；Growth of carbon nanotube array films on silicon wafers by chemical vapor deposition;
配置聚二甲基硅氧烷混合液，所述混合液包括聚二甲基硅氧烷和固化剂；configure a polydimethylsiloxane mixed liquid, the mixed liquid includes polydimethylsiloxane and a curing agent;
将聚二甲基硅氧烷混合液滴在所述碳纳米管阵列膜的表面，并待其铺满整个碳纳米管阵列膜表面，等待其在真空环境下固化，所述碳纳米管阵列和固化的聚二甲基硅氧烷构成处理后的碳纳米管阵列膜；The polydimethylsiloxane mixture is dropped on the surface of the carbon nanotube array film, and it is spread over the entire surface of the carbon nanotube array film, waiting for it to be cured in a vacuum environment, the carbon nanotube array and The cured polydimethylsiloxane constitutes the treated carbon nanotube array film;
从硅片上取下所述处理后的碳纳米管阵列膜，并对所述处理后的碳纳米管阵列膜进行刻蚀使其厚度达到预设厚度，得到光致超声换能器。The treated carbon nanotube array film is removed from the silicon wafer, and the treated carbon nanotube array film is etched so that the thickness reaches a preset thickness to obtain a photo-induced ultrasonic transducer.
可选地，当聚二甲基硅氧烷混合液铺满整个碳纳米管阵列膜表面后，进行真空处理，使聚二甲基硅氧烷均匀分布在碳纳米管阵列膜之间，将碳纳米管阵列膜内的空气抽干净，对聚二甲基硅氧烷混合液进行热固化或者光固化。Optionally, after the polydimethylsiloxane mixture is spread over the entire surface of the carbon nanotube array membrane, vacuum treatment is performed to make the polydimethylsiloxane evenly distributed between the carbon nanotube array membranes, and the carbon nanotube array membranes are The air in the nanotube array film is evacuated, and the polydimethylsiloxane mixed solution is thermally cured or photocured.
可选地，通过如下步骤配置聚二甲基硅氧烷混合液：Optionally, configure the polydimethylsiloxane mixture through the following steps:
按预设比例分别加入聚二甲基硅氧烷和固化剂，得到聚二甲基硅氧烷混合液。The polydimethylsiloxane and the curing agent are respectively added in a preset proportion to obtain a polydimethylsiloxane mixed solution.
可选地，在硅片上利用化学气相沉积法生长碳纳米管阵列膜，具体包括如下步骤：Optionally, the carbon nanotube array film is grown on the silicon wafer by chemical vapor deposition, which specifically includes the following steps:
在C2H4、H2和/或He的混合物中使用高温化学气相沉积法来制备碳纳米管阵列膜。Carbon nanotube array films were prepared using high temperature chemical vapor deposition in a mixture of C 2 H 4 , H 2 and/or He.
可选地，对所述处理后的碳纳米管阵列膜进行刻蚀，具体包括如下步骤：Optionally, etching the treated carbon nanotube array film specifically includes the following steps:
采用CF4、Ar和/或O2作为刻蚀气体对处理后的碳纳米管阵列膜进行刻蚀。The treated carbon nanotube array film is etched by using CF 4 , Ar and/or O 2 as etching gas.
可选地，在硅片上利用化学气相沉积法生长碳纳米管阵列膜之前，包括如下步骤：Optionally, before the carbon nanotube array film is grown on the silicon wafer by chemical vapor deposition, the following steps are included:
对硅片依次通过丙酮、酒精、去离子水超声清洗，将其表面清洗干净。The silicon wafer was ultrasonically cleaned with acetone, alcohol, and deionized water in turn to clean the surface.
第二方面，本发明提供一种光致超声换能器，包括：碳纳米管阵列膜和聚二甲基硅氧烷；所述聚二甲基硅氧烷均匀固化在碳纳米管阵列膜的表面。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 cured on the carbon nanotube array film surface.
第三方面，本发明提供一种基于上述第一方面提供的光致超声换能器的制备方法制备得到的光致超声换能器。In a third aspect, the present invention provides a photo-induced ultrasonic transducer prepared based on the method for preparing a photo-induced ultrasonic transducer provided in the first aspect.
总体而言，通过本发明所构思的以上技术方案与现有技术相比，具有以下有益效果：In general, compared with the prior art, the above technical solutions conceived by the present invention have the following beneficial effects:
1)本发明提供的光致超声换能器及其制备方法，根据碳纳米管热导的各项异性特点，轴向热导更高；采用碳纳米管阵列作为制备光致超声换能器的材料能有效提高轴向热导，改善光致超声换能器的光声转化效率。1) The photo-induced ultrasonic transducer provided by the present invention and the preparation method thereof, according to the anisotropic characteristics of the thermal conductivity of carbon nanotubes, the axial thermal conductivity is higher; the carbon nanotube array is used as the preparation method of the photo-induced ultrasonic transducer. The material can effectively increase the axial thermal conductivity and improve the photo-acoustic conversion efficiency of the photo-induced ultrasonic transducer.
2)本发明提供的光致超声换能器及其制备方法，通过ICP刻蚀可以有效控制光致超声换能器的厚度，进而控制光致超声换能器的频率特性。2) In the photo-ultrasonic transducer and the preparation method thereof provided by the present invention, the thickness of the photo-ultrasonic transducer can be effectively controlled by ICP etching, thereby controlling the frequency characteristics of the photo-ultrasonic transducer.
3)本发明提供的光致超声换能器及其制备方法，将碳纳米管阵列膜做在光纤端面上可实现光致超声换能器的微型化特点。3) In the photo-induced ultrasonic transducer and the preparation method thereof provided by the present invention, the carbon nanotube array film is made on the end face of the optical fiber to realize the miniaturization feature of the photo-induced ultrasonic transducer.
附图说明Description of drawings
图1是本发明提供的光致超声换能器的制备方法流程图；Fig. 1 is the flow chart of the preparation method of the photoultrasonic transducer provided by the present invention;
图2是本发明制备的碳纳米管阵列膜的结构示意图；Fig. 2 is the structural representation of the carbon nanotube array film prepared by the present invention;
图3是本发明在碳纳米管阵列膜上涂PDMS的示意图；Fig. 3 is the schematic diagram of the present invention coating PDMS on carbon nanotube array film;
图4是本发明制备的固化后的碳纳米管阵列膜和PDMS的结构示意图；4 is a schematic structural diagram of the cured carbon nanotube array film and PDMS prepared by the present invention;
图5(a)是本发明制备的无衬底的碳纳米管阵列膜的三维结构示意图；Figure 5(a) is a schematic diagram of the three-dimensional structure of the substrate-free carbon nanotube array film prepared by the present invention;
图5(b)是本发明制备的无衬底的碳纳米管阵列膜的截面示意图；Figure 5(b) is a schematic cross-sectional view of the substrate-free carbon nanotube array film prepared by the present invention;
图6是本发明制备的经过ICP刻蚀后的碳纳米管阵列膜的结构示意图。FIG. 6 is a schematic structural diagram of a carbon nanotube array film prepared by the present invention after ICP etching.
具体实施方式Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。此外，下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
图1是本发明提供的光致超声换能器的制备方法流程图；如图1所示，包括如下步骤：Fig. 1 is the flow chart of the preparation method of photoinduced ultrasonic transducer provided by the present invention; As shown in Fig. 1, comprises the following steps:
S101，在硅片上利用化学气相沉积法生长碳纳米管阵列膜；S101, growing a carbon nanotube array film on a silicon wafer by chemical vapor deposition;
S102，配置聚二甲基硅氧烷混合液，所述混合液包括聚二甲基硅氧烷和固化剂；S102, configure a polydimethylsiloxane mixed solution, the mixed solution includes polydimethylsiloxane and a curing agent;
S103，将聚二甲基硅氧烷混合液滴在所述碳纳米管阵列膜的表面，并待其铺满整个碳纳米管阵列膜表面，等待其在真空环境下固化，所述碳纳米管阵列和固化的聚二甲基硅氧烷构成处理后的碳纳米管阵列膜；S103, drop the polydimethylsiloxane mixture on the surface of the carbon nanotube array film, and wait for it to be spread over the entire surface of the carbon nanotube array film, and wait for it to be cured in a vacuum environment. The array and cured polydimethylsiloxane constitute the treated carbon nanotube array film;
S104，从硅片上取下所述处理后的碳纳米管阵列膜，并对所述处理后的碳纳米管阵列膜进行刻蚀使其厚度达到预设厚度，得到光致超声换能器。S104 , the treated carbon nanotube array film is removed from the silicon wafer, and the treated carbon nanotube array film is etched so that its thickness reaches a preset thickness to obtain a photo-induced ultrasonic transducer.
阵列膜进行刻蚀使其厚度达到预设厚度，得到光致超声换能器。The array film is etched to make its thickness reach a preset thickness to obtain a photo-induced ultrasonic transducer.
可选地，当聚二甲基硅氧烷混合液铺满整个碳纳米管阵列膜表面后，进行真空处理，使聚二甲基硅氧烷均匀分布在碳纳米管阵列膜之间，将碳纳米管阵列膜内的空气抽干净，对聚二甲基硅氧烷混合液进行热固化或者光固化。Optionally, after the polydimethylsiloxane mixture is spread over the entire surface of the carbon nanotube array membrane, vacuum treatment is performed to make the polydimethylsiloxane evenly distributed between the carbon nanotube array membranes, and the carbon nanotube array membranes are The air in the nanotube array film is evacuated, and the polydimethylsiloxane mixed solution is thermally cured or photocured.
可选地，通过如下步骤配置聚二甲基硅氧烷混合液：Optionally, configure the polydimethylsiloxane mixture through the following steps:
按预设比例分别加入聚二甲基硅氧烷和固化剂，得到聚二甲基硅氧烷混合液。The polydimethylsiloxane and the curing agent are respectively added in a preset proportion to obtain a polydimethylsiloxane mixed solution.
可选地，在硅片上利用化学气相沉积法生长碳纳米管阵列膜，具体包括如下步骤：Optionally, the carbon nanotube array film is grown on the silicon wafer by chemical vapor deposition, which specifically includes the following steps:
在C2H4、H2和/或He的混合物中使用高温化学气相沉积法来制备碳纳米管阵列膜。Carbon nanotube array films were prepared using high temperature chemical vapor deposition in a mixture of C 2 H 4 , H 2 and/or He.
可选地，对所述处理后的碳纳米管阵列膜进行刻蚀，具体包括如下步骤：Optionally, etching the treated carbon nanotube array film specifically includes the following steps:
采用CF4、Ar和/或O2作为刻蚀气体对处理后的碳纳米管阵列膜进行刻蚀。The treated carbon nanotube array film is etched by using CF 4 , Ar and/or O 2 as etching gas.
可选地，在硅片上利用化学气相沉积法生长碳纳米管阵列膜之前，包括如下步骤：Optionally, before the carbon nanotube array film is grown on the silicon wafer by chemical vapor deposition, the following steps are included:
对硅片依次通过丙酮、酒精、去离子水超声清洗，将其表面清洗干净。The silicon wafer was ultrasonically cleaned with acetone, alcohol, and deionized water in turn to clean the surface.
本发明提供了一种高频光致超声换能器制备方法，采用ICP刻蚀技术，对碳纳米管阵列膜进行减薄，使其厚度在微米量级，从而产生一个几十MHz的高频超声信号。The invention provides a preparation method for a high-frequency photo-induced ultrasonic transducer. The ICP etching technology is used to thin the carbon nanotube array film so that the thickness is in the order of microns, thereby generating a high-frequency ultrasonic signal of tens of MHz. .
为实现上述目的，按照本发明，提供了一种高频光致超声换能器制备方法，该方法包括以下步骤：In order to achieve the above object, according to the present invention, a method for preparing a high-frequency photo-induced ultrasonic transducer is provided, and the method comprises the following steps:
1)选取长方体形状的硅片，其中，所述硅片长为1cm，宽为1cm；1) Select a cuboid-shaped silicon wafer, wherein the silicon wafer is 1 cm long and 1 cm wide;
2)将硅片依次通过丙酮、酒精、去离子水超声清洗，将其表面清洗干净，以便更好的在其表面生长碳纳米管阵列膜，然后用化学气相沉淀法在其表面生长厚度约为100μm的碳纳米管阵列膜，如图2所示。2) The silicon wafer is ultrasonically cleaned with acetone, alcohol, and deionized water in turn, and its surface is cleaned so as to better grow a carbon nanotube array film on its surface, and then chemical vapor deposition is used. 100μm carbon nanotube array film, as shown in Figure 2.
3)配置PDMS，加2g的PDMS于烧杯中，然后再加入0.2g的固化剂。3) Prepare PDMS, add 2g of PDMS to the beaker, and then add 0.2g of curing agent.
4)如图3所示，将配置好的PDMS滴在碳纳米管阵列膜表面并待其铺满整个膜表面，然后进行真空处理30min，使PDMS均匀分布在碳纳米管阵列之间，并使膜内的空气抽干净，最后将其放于90℃环境中加热0.5h，使其固化，其结构如图4所示。4) As shown in Figure 3, drop the configured PDMS on the surface of the carbon nanotube array film and wait for it to cover the entire film surface, and then perform vacuum treatment for 30 minutes, so that the PDMS is evenly distributed between the carbon nanotube arrays, and the The air in the membrane was evacuated, and finally it was heated at 90°C for 0.5h to cure it. The structure is shown in Figure 4.
5)碳纳米管阵列膜完全固化后，将其从硅衬底上撕下来。无衬底的碳纳米管阵列膜结构如图5(a)和图5(b)所示。然后采用ICP刻蚀技术将碳纳米管阵列膜减薄，减薄后的结构如图6所示。5) After the carbon nanotube array film is completely cured, it is torn off from the silicon substrate. The structure of the substrate-free carbon nanotube array film is shown in Fig. 5(a) and Fig. 5(b). Then, the carbon nanotube array film is thinned by ICP etching technology, and the thinned structure is shown in FIG. 6 .
优选地，步骤2)中所述碳纳米管阵列的制备，是通过在C2H4/H2/He(775℃)的混合物中使用高温化学气相沉积来制备的。Preferably, the carbon nanotube arrays in step 2) are prepared by using high temperature chemical vapor deposition in a mixture of C 2 H 4 /H 2 /He (775°C).
优选地，步骤5)中所述ICP刻蚀，是采用CF4、Ar和O2作为刻蚀气体对碳纳米管阵列膜进行刻蚀的，但不限于这个气体成分。Preferably, in the ICP etching in step 5), CF 4 , Ar and O 2 are used as etching gases to etch the carbon nanotube array film, but it is not limited to this gas composition.
优选地，步骤5)中所述对碳纳米管阵列膜进行减薄，使碳纳米管阵列膜的厚度控制在10μm，但不限于这个厚度。Preferably, the carbon nanotube array film is thinned as described in step 5), so that the thickness of the carbon nanotube array film is controlled at 10 μm, but not limited to this thickness.
本发明提供了高频光致超声换能器制备工艺流程。其工艺流程简单，不仅制备了碳纳米管阵列和PDMS膜，而且采用ICP刻蚀技术对碳纳米管膜进行减薄，使其厚度控制在微米量级。The invention provides a process flow for preparing a high-frequency photo-induced ultrasonic transducer. The process flow is simple, not only the carbon nanotube array and the PDMS film are prepared, but also the carbon nanotube film is thinned by ICP etching technology, so that the thickness is controlled in the order of microns.
在一个具体的实施例中，实例步骤如下：In a specific embodiment, the example steps are as follows:
1)切片，切取长为1cm，宽1cm的硅片；1) Slice, cut a silicon wafer with a length of 1cm and a width of 1cm;
2)洗片，将切好的硅片进行清洗，首先用丙酮超声清洗10min，然后用乙醇超声清洗10min，最后用去离子水超声清洗10min。然后通过在C2H4/H2/He(775℃)的混合物中使用高温化学气相沉积来制备碳纳米管阵列膜2) Washing the wafers, cleaning the cut silicon wafers, first ultrasonically cleaned with acetone for 10 min, then ultrasonically cleaned with ethanol for 10 min, and finally ultrasonically cleaned with deionized water for 10 min. Carbon nanotube array films were then prepared by using high temperature chemical vapor deposition in a mixture of C2H4/H2/He (775°C)
3)配置PDMS，加2g的PDMS于烧杯中，然后再加入0.2g的固化剂。3) Prepare PDMS, add 2g of PDMS to the beaker, and then add 0.2g of curing agent.
4)将配置好的PDMS滴在碳纳米管阵列膜表面并待其铺满整个膜表面，然后进行真空处理30min，使PDMS均匀分布在碳纳米管阵列之间，并使膜内的空气抽干净，最后将其放于90℃环境中加热0.5h。4) Drop the prepared PDMS on the surface of the carbon nanotube array film and wait for it to cover the entire film surface, and then perform vacuum treatment for 30 minutes, so that the PDMS is evenly distributed between the carbon nanotube arrays, and the air in the film is evacuated. , and finally it was heated at 90°C for 0.5h.
5)碳纳米管阵列膜完全固化后，将其从硅衬底上撕下来，采用ICP刻蚀技术将碳纳米管阵列膜减薄，以CF4、Ar和O2作为刻蚀气体，使碳纳米管阵列膜的厚度控制在10μm左右。 5 ) After the carbon nanotube array film is completely cured, it is torn off from the silicon substrate, and the carbon nanotube array film is thinned by ICP etching technology . The thickness of the nanotube array film is controlled at about 10 μm.
6)将脉冲激光作用于碳纳米管阵列膜将会产生一个高频超声信号。6) Applying a pulsed laser to the carbon nanotube array film will generate a high frequency ultrasonic signal.
本领域的技术人员容易理解，以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。Those skilled in the art can easily understand that the above are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention, etc., All should be included within the protection scope of the present invention.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910570950.0A CN110339992B (en) | 2019-06-28 | 2019-06-28 | A kind of photoinduced ultrasonic transducer and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910570950.0A CN110339992B (en) | 2019-06-28 | 2019-06-28 | A kind of photoinduced ultrasonic transducer and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110339992A CN110339992A (en) | 2019-10-18 |
| CN110339992B true CN110339992B (en) | 2020-09-08 |
Family
ID=68177274
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910570950.0A Expired - Fee Related CN110339992B (en) | 2019-06-28 | 2019-06-28 | A kind of photoinduced ultrasonic transducer and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110339992B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111112035B (en) * | 2019-12-25 | 2021-02-09 | 华中科技大学 | Transceiver-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 | A kind of photoinduced ultrasonic transducer based on halide perovskite material and preparation method thereof |
| CN117920556B (en) * | 2024-01-25 | 2024-10-01 | 华中科技大学 | A photo-induced ultrasonic transducer for opening the blood-brain barrier and a preparation method thereof |
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 |
-
2019
- 2019-06-28 CN CN201910570950.0A patent/CN110339992B/en not_active Expired - Fee Related
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110339992A (en) | 2019-10-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110339992B (en) | A kind of photoinduced ultrasonic transducer and preparation method thereof | |
| CN109433571B (en) | Flexible photoultrasonic thin film transducer and preparation method thereof | |
| Chang et al. | Candle soot nanoparticles-polydimethylsiloxane composites for laser ultrasound transducers | |
| CN105958956B (en) | A kind of thin film bulk acoustic wave resonator and preparation method thereof | |
| CN103130178B (en) | Capacitance type micromachined ultrasonic transducer manufacture method and subject information acquisition device | |
| CN111009496B (en) | A kind of semiconductor substrate with high thermal conductivity and preparation method thereof | |
| CN106209001B (en) | Thin-film bulk acoustic wave resonator based on single-crystal lithium niobate flakes and preparation method thereof | |
| CN110862088A (en) | Preparation method of silicon nanoneedle array with ultra-high depth-to-width ratio | |
| CN103011181A (en) | Stripping-transplanting method of silicon dioxide nanowire array | |
| CN106209002A (en) | A kind of novel thin film bulk acoustic wave resonator and preparation method thereof | |
| CN101463182A (en) | Microfine piezoelectric ceramics array structure composite material and preparation thereof | |
| CN107474267A (en) | A kind of photic ultrasonic membrane and preparation method thereof | |
| CN104655261A (en) | Capacitive ultrasonic sensor and manufacturing method thereof | |
| CN114665005A (en) | D33Mode ferroelectric single crystal film piezoelectric vibration sensor and preparation method thereof | |
| CN103337449A (en) | Method for transplanting silicon nanowire array and preparing simple device thereof | |
| CN113182157A (en) | Flexible piezoelectric ultrasonic transducer | |
| CN114497352B (en) | Piezoelectric material layer with microstructure array, preparation method and application thereof | |
| CN108910868A (en) | A method of preparing graphene dendrite on an insulating substrate | |
| CN102247164A (en) | Method for manufacturing high-frequency acoustic self-focusing spherical probe | |
| CN110954570B (en) | Method for stripping two-dimensional material grown on sapphire substrate by temperature control bubbling | |
| CN110040722B (en) | Method for preparing graphene bubbles | |
| CN116639694A (en) | Vibrating diaphragm material, preparation method and acoustic wave sensor | |
| CN111485230B (en) | A kind of preparation method of zinc oxide thick film for ultrasonic transducer | |
| CN114584092A (en) | Preparation method of diamond simple harmonic oscillator | |
| CN106653952B (en) | A kind of preparation method of the middle infrared antireflective micro-structure of silicon |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200908 Termination date: 20210628 |