CN109850843B - Batch preparation method of suspended nanowire manipulator - Google Patents
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Abstract
The invention discloses a batch preparation method of suspended nanowire manipulators, which comprises the following steps: preparing a nanowire array growing on the edge of a slope step defined by photoetching based on an IPSLS (Internet protocol Security language) growth mode, then spin-coating a layer of oxygen resin colloid on a substrate on which silicon nanowires grow, carrying out photoetching pattern operation, removing an amorphous silicon medium layer on the surface of the substrate by wet etching, enabling an epoxy resin colloid film sticking the nanowire array to suspend on the surface of a solution, fully replacing the epoxy resin colloid film with ethanol, and then utilizing a drying technology to prepare the self-assembled suspended nanowire manipulator array. The invention utilizes the transfer technology and the critical point drying technology to transfer the nanowire array to the photoetched self-supporting substrate, eliminates the influence of the surface tension of the solution, keeps the original appearance of the nanowire manipulator, and finally obtains the operable suspended nanowire manipulator array, which can be widely applied to various fields of nano robots, biomedical cell detection, biosensors and the like.
Description
Technical Field
The invention relates to a batch preparation method of a suspended nanowire manipulator, which can be flexibly applied to the acquisition or detection of biological cells or micro structures, semiconductor sensing devices and other fields.
Background
The crystal silicon or related semiconductor nano-wire (Nanowire) is an important material for developing a new generation of high-performance large-area thin-film electronic device, and has very great application potential in the fields of novel flexible sensing, biomedical sensing and detection and logic storage. The nanowire structure with the diameter ranging from 10 nm to 100nm is prepared on the basis of a top-down electron beam direct writing (EBL) technology, the excellent characteristics of various novel nanowire functional devices are verified, but the nanowire structure is difficult to be applied in a large scale all the time due to the preparation cost, the high price, the low yield and other factors. In contrast, by means of Self-assembly (Self-assembly) nanowire growth catalyzed by nano-metal droplets, crystalline silicon, germanium and various alloy semiconductor nanowires with the diameter of below hundred nanometers can be prepared in a large scale, and the growth of the nanowires can be accurately controlled. However, most of the suspended nanowires prepared by the commonly adopted vapor-liquid-solid (VLS) growth mode are vertical random arrays, and reliable and low-cost positioning integration in the current planar electronic process is difficult to realize directly.
In order to reliably prepare a crystal silicon nanowire structure with programmable morphology, the applicant originally proposed a planar solid-liquid-solid (IPSLS) growth mode: amorphous silicon is used as a precursor, and the crystalline silicon nanowire structure grows by absorbing the amorphous silicon by low-melting-point metal indium and tin nanoparticles. Meanwhile, based on the method, a simple unilateral step defined on the planar substrate can be used as a guide, and the metal liquid drop moves along the step edge under the attraction of amorphous silicon covered by the step edge, so that the nanowire grows on the step edge, and the positioning and shaping growth of the planar nanowire is realized. Based on a traditional gas-liquid-solid (VLS) growth mechanism, the vertical random nanowires can obtain suspended nano linear structures in a plane only through ultrasonic and drying steps, and the nanowire structures with any shapes defined by the planar solid-liquid-solid (IPSLS) growth mechanism can be stressed by the surface tension of a solution in the transferring and drying processes, so that the originally defined shapes are changed and even broken, and the success rate of transferring the suspended nanowire manipulator array is greatly reduced. For the research and application fields related to biomedical NEMS, this increases the difficulty of obtaining and detecting the cell or DNA sequence structure in the organism, and hinders the further development of NEMS in the biochemical aspect of accurate and rapid analysis of cells, DNA and proteins and other biological components, and the technical development of related products.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides a batch preparation method of a suspended nanowire manipulator, which is characterized in that a nanowire array is transferred to a photoetched self-supporting substrate by utilizing a transfer technology and a critical point drying technology, the influence of the surface tension of a solution is eliminated, the original appearance of the nanowire manipulator is maintained, and finally, an operable suspended nanowire manipulator array is obtained and can be widely applied to various fields of nano robots, cell detection of biomedicine, biosensors and the like.
The technical scheme is as follows: in order to achieve the purpose, the invention adopts the technical scheme that:
a batch preparation method of suspended nanowire manipulators comprises the following steps: preparing a nanowire array growing on the edge of a slope step defined by photoetching based on an IPSLS (Internet protocol Security language) growth mode, then spin-coating a layer of oxygen resin colloid on a substrate on which silicon nanowires grow, carrying out photoetching pattern operation, removing an amorphous silicon medium layer on the surface of the substrate by wet etching, enabling an epoxy resin colloid film sticking the nanowire array to suspend on the surface of a solution, fully replacing the epoxy resin colloid film with ethanol, and then utilizing a drying technology to prepare the self-assembled suspended nanowire manipulator array.
Further, the method specifically comprises the following steps:
1) using crystalline silicon, glass or a metal film covered by a dielectric layer as a substrate, and depositing an amorphous dielectric layer (such as amorphous silicon oxide SiO2, silicon nitride SiNx and the like) on the substrate by using one or more film deposition techniques;
2) the required plane pattern is realized by utilizing a photoetching technology, the step position of a slope guide channel is defined, and then a dielectric layer is etched by utilizing an Inductively Coupled Plasma (ICP) etching or reactive plasma etching (RIE) technology; c can be used in the etching process4F8、CF4、SF6And (or mixed gas thereof) and other reactive gases with different steep characteristics and surface passivation characteristics are etched to form the slope side wall.
3) Depositing a metal (such as indium, tin and the like) catalyst layer at the middle part of the slope step by utilizing the technologies such as photoetching technology, thermal evaporation or electron beam evaporation and the like to be used as a starting point of the catalytic nanowire, and then processing a metal catalyst deposited on the surface of the substrate in advance in a reducing gas plasma atmosphere (such as hydrogen plasma in PECVD at the temperature of 200-500 ℃) to reduce the metal catalyst into catalytic metal nano liquid drops;
4) reducing the temperature below the melting point of the metal catalyst and suitable for depositing amorphous silicon, depositing a layer of amorphous silicon film as a precursor, raising the temperature to a suitable temperature, activating catalytic metal droplets, absorbing an amorphous silicon medium in the annealing process, and simultaneously separating out a crystalline silicon nanowire at the rear end of the amorphous silicon film, so as to guide the growth of the planar silicon nanowire (the remaining amorphous silicon can be selectively etched by hydrogen plasma or corresponding etching processes such as ICP (inductively coupled plasma), RIE (reactive ion etching), and the like, and the silicon nanowire is reserved);
the diameter of the nanowire growing on the slope surface is larger than that of the amorphous film precursor layer remaining on the slope surface, the diameter is usually 2-3 times of the thickness of the film, in the same etching processes such as ICP (inductively coupled plasma), RIE (reactive ion etching) and the like, the etching rate of the amorphous layer is usually higher than that of the crystalline nanowire channel, and the amorphous layer on the slope surface can be selectively (or sacrifice the thickness of a small amount of crystalline silicon channel) removed.
5) Directly spin-coating a layer of epoxy resin colloid, such as novolac epoxy resin colloid SU8, on the surface of the sample, and performing photolithography to expose the manipulator structure to form a self-supporting organic film with openings;
6) separating the epoxy resin colloid film adhered with the nanowire structure from the substrate by utilizing a wet etching technology, and floating on the surface of a hydrofluoric acid solution after the epoxy resin colloid film adhered with the nanowire structure is separated from the substrate to form a suspended nanowire manipulator structure array;
7) transferring the epoxy resin colloid film adhered with the suspended nanowire array from the hydrofluoric acid solution to ethanol for full replacement; because the surface tension of the solution can drag the nanowire structure to deform or even break, the suspended nanowire structure array after transfer is put into a supercritical drying instrument for drying, the influence of the surface tension of the solution is eliminated through a critical point drying method, the original appearance of the nanowire manipulator is kept, and the suspended nanowire manipulator in batches is obtained finally.
The suspended nanowire manipulator structure prepared by the invention realizes magnetic field driving under the condition of introducing a magnetic field with proper strength and direction, and can be applied to various occasions such as acquisition or detection of biological cells or micro structures. The suspended nanowire manipulator structure obtained by growing the silicon nanowire has good semiconductor characteristics under the condition of current introduction, is free from the interference of environmental factors, avoids the problems of parasitic effect and the like, and can be applied to the field of semiconductor integrated circuits based on the characteristics.
Preferably, the thickness of the metal catalyst layer is within the range of 1-300 nm.
Preferably, the diameter distribution of the metal nanoparticles in the guide channel can be controlled within the range of 10-1000nm by controlling the process parameters such as the treatment reaction time, the temperature, the power, the gas pressure and the like, and the diameter distribution of the metal nanoparticles obeys the normal distribution rule. In the PECVD equipment, the processing power density is between 1mW/cm2 and 10W/cm2, and the air pressure is between 1Pa and 100 Torr.
Preferably, the step 5) specifically comprises: at the temperature lower than the melting point of the catalytic metal liquid drop, covering one or more amorphous thin film precursor layers (such as amorphous silicon a-Si, amorphous germanium a-Ge, amorphous carbon a-C or amorphous alloy layers thereof and heterogeneous lamination (such as a-Ge/a-Si) structures) corresponding to the components of the nanowire to be grown on the surface by PECVD, CVD or PVD deposition technology, wherein the thickness of the amorphous thin film layer can be regulated and controlled by process parameters such as reaction time, temperature, power, air pressure and the like, and the thickness distribution of the amorphous thin film layer is 2-500 nm.
Has the advantages that: compared with the prior art, the batch preparation method of the suspended nanowire manipulator provided by the invention has the following advantages: 1. under the guidance of slope nano steps, the nanowires grow on the slope in parallel, the growth direction is determined by the whole trend of the slope, and the key problem that the growth morphology of the nanowires cannot be controlled by gas-liquid-solid (VLS) growth semiconductor nanowires is solved;
2. transferring the nanowire array to a photoetched self-supporting substrate by utilizing a transfer technology and a critical point drying technology, eliminating the influence of the surface tension of a solution, keeping the original appearance of the nanowire manipulator, and finally obtaining an operable suspended nanowire manipulator array, wherein the technology is completely compatible with the basic technology of large-area thin-film electronic devices, and an additional high-precision photoetching technology is not required to be introduced;
3. meanwhile, the suspended nanowire has higher relaxivity, so that a key implementation technology is provided for developing a new generation of nano-electromechanical system (NEMS), the operation similar to the opening and closing of tweezers is realized, various microorganisms are obtained under the driving of voltage and a magnetic field, and the manipulator has certain flexibility and operability;
4. the suspended nanowire manipulator can realize the acquisition and detection of biological cells and the application of a new generation of micro-nano sensing device (such as a biochip), which is particularly important for the sensing technology in the field of biomedical cells.
5. In addition, the technology is expected to help reduce the interference of substrate noise (such as parasitic capacitance) on the CMOS integrated circuit, improve the efficiency and reliability of the system, and can be applied to the design and test of the semiconductor large-scale integrated circuit.
Drawings
FIG. 1 is a schematic structural diagram of a suspended nanowire manipulator array prepared according to the present invention;
fig. 2 is a schematic view of a preparation process of a batch nanowire manipulator array provided by the present invention, which respectively includes: a. etching to form a guide step, b, depositing a catalytic metal layer, c, growing a silicon nanowire, d, spin-coating SU8 for photoetching, e, wet etching, transferring and drying to form a suspended structure, and f, obtaining a nanowire manipulator structure which can be used for obtaining a tiny object;
fig. 3 is a schematic diagram of a process for realizing magnetic field driving by the nanowire manipulator structure obtained in the invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and examples.
As shown in fig. 2, a method for preparing a batch suspended nanowire manipulator, which is a method for transferring a self-assembled nano manipulator array to a flexible substrate by using a colloidal material to obtain and detect a micro object, wherein the preparation process comprises the following steps:
1) using crystalline silicon, glass or a metal film covered by a dielectric layer as a substrate, and depositing an amorphous dielectric layer (such as amorphous silicon oxide SiO2, silicon nitride SiNx and the like) on the substrate by using one or more film deposition technologies;
2) the required plane pattern is realized by utilizing a photoetching technology, the step position of a slope guide channel is defined, and a dielectric layer is etched by utilizing an Inductively Coupled Plasma (ICP) etching or reactive plasma etching (RIE) technology;
3) depositing a metal indium catalyst layer (with the thickness of 20-40 nm) at one end of the slope step at the middle part of the slope step by utilizing photoetching positioning and thermal evaporation technology to serve as a growth starting point of the nanowire, loading a sample into a PECVD (plasma enhanced chemical vapor deposition) cavity, and carrying out hydrogen plasma treatment at high temperature to convert the catalytic metal layer covered on the slope guide channel on the side wall into separated indium nanoparticles;
4) reducing the temperature to 100-160 ℃, covering an amorphous silicon film (20-100 nm) precursor layer on the surface of a PECVD system, and then properly increasing the temperature to enable indium nanoparticles to be re-melted, starting to absorb amorphous silicon at the front end and separate out a crystalline silicon nanowire structure at the rear end, wherein the nanowires grow in parallel on the slope by virtue of the guiding action of slope nano steps and are guided to move along the whole slope;
5) the residual amorphous precursor layer can be selectively etched and removed in the PECVD cavity through hydrogen plasma;
the diameter of the nanowire growing on the slope surface is larger than that of the amorphous film precursor layer remaining on the slope surface, the diameter is usually 2-3 times of the thickness of the film, in the same etching processes such as ICP (inductively coupled plasma), RIE (reactive ion etching) and the like, the etching rate of the amorphous layer is usually higher than that of the crystalline nanowire channel, and the amorphous layer on the slope surface can be selectively (or sacrifice the thickness of a small amount of crystalline silicon channel) removed.
6) Directly spin-coating epoxy resin colloid on a substrate on which the nanowire grows, and transferring the nanowire to a colloid material with an opening by a photoetching technology and a wet etching technology;
7) the method comprises the steps of utilizing a wet etching technology to enable an epoxy resin colloid film adhered with a nanowire structure to be separated from a substrate, enabling the nanowire structure to float on the surface of a hydrofluoric acid solution and form a suspended nanowire manipulator structure array, transferring the epoxy resin colloid film adhered with the suspended nanowire array from the hydrofluoric acid solution to ethanol for sufficient replacement, placing the transferred suspended nanowire structure array into a supercritical drying instrument for sufficient drying, eliminating the influence of surface tension of the solution through a critical point drying method, keeping the original appearance of a nanowire manipulator, and finally obtaining the operable suspended nanowire manipulator array as shown in figure 1. As shown in fig. 3, under the condition of introducing a magnetic field with appropriate strength and direction, the device can be widely applied to the acquisition and detection of various biological cells or micro structures; the suspended nanowire manipulator structure obtained by growing the silicon nanowire has good semiconductor characteristics under the condition of current introduction, is free from the interference of environmental factors, avoids the problems of parasitic effect and the like, and can be applied to the field of semiconductor integrated circuits based on the characteristics.
The linear shape of the nanowire can be accurately programmed and designed through the design of the guide step, a programmable planar linear nanowire structure is grown, and the pattern design has operability; on the other hand, the nanowire manipulator is high in relaxation property when being suspended, the 'acquiring' operation is suitable for various objects, the 'opening' and 'closing' operations under voltage and magnetic fields are achieved, the application flexibility is high, and the range is wide.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (5)
1. A batch preparation method of suspended nanowire manipulators is characterized by comprising the following steps: preparing and obtaining a nanowire array growing on the edge of a slope step defined by photoetching based on an IPSLS plane solid-liquid solid growth mode, then spin-coating a layer of epoxy resin colloid on a substrate on which silicon nanowires grow, carrying out photoetching pattern operation, removing an amorphous silicon medium layer on the surface of the substrate by wet etching, enabling an epoxy resin colloid film sticking the nanowire array to suspend on the surface of a solution, fully replacing the epoxy resin colloid film with ethanol, and then utilizing a drying technology to prepare and obtain the self-assembled suspended nanowire manipulator array.
2. The batch preparation method of the suspended nanowire manipulator as claimed in claim 1, which comprises the following steps:
1) defining the position of a guide channel step on the substrate by utilizing a photoetching technology, and etching an amorphous silicon dielectric layer on the substrate by utilizing an inductive coupling plasma etching or reactive plasma etching technology to form the guide channel step;
2) in the middle part of the slope step, a metal catalyst layer is deposited in advance to be used as a starting point of the catalytic nanowire, and then the metal catalyst layer deposited in advance on the surface of the substrate is treated under the action of plasma of reducing gas at high temperature to be reduced into dispersed catalytic metal nano liquid drops;
3) reducing the temperature to be below the melting point of the metal catalytic liquid drop, depositing a layer of amorphous silicon film on the surface of the substrate to be used as a precursor, and raising the temperature to enable the metal catalytic liquid drop to be re-melted, so that the amorphous silicon medium is absorbed by the metal catalytic liquid drop in the annealing process and the crystalline silicon nanowire is separated out at the rear end of the metal catalytic liquid drop, thereby guiding the growth of the planar silicon nanowire;
4) directly spin-coating an epoxy resin colloid on a substrate on which a silicon nanowire grows, and carrying out photoetching to form a self-supporting organic film with an opening;
5) separating the epoxy resin colloid film adhered with the nanowire structure from the substrate by utilizing a wet etching technology, and floating the epoxy resin colloid film adhered with the nanowire structure on the surface of a hydrofluoric acid solution after the epoxy resin colloid film is separated from the substrate to form a suspended nanowire manipulator structure array;
6) transferring the epoxy resin colloid film adhered with the suspended nanowire array from a hydrofluoric acid solution to ethanol for full replacement, putting the transferred suspended nanowire structure array into a supercritical drying instrument for drying, eliminating the influence of the surface tension of the solution through a critical point drying method, keeping the original appearance of the nanowire manipulator, and finally obtaining the suspended nanowire manipulator in batches.
3. The batch preparation method of the suspended nanowire manipulator as claimed in claim 2, wherein the thickness of the metal catalyst layer is in a range of 1-300 nm.
4. The batch preparation method of the suspended nanowire manipulator as claimed in claim 2, wherein the diameter of the metal nanoparticle liquid drop is within a range of 10-1000 nm.
5. The batch preparation method of the suspended nanowire manipulator as claimed in claim 2, wherein the step 3) specifically comprises: and covering one or more amorphous film precursor layers corresponding to the components of the nanowire to be grown on the surface of the substrate by a CVD or PVD deposition technology at a temperature lower than the melting point of the catalytic metal droplet, wherein the covering thickness of each film layer on the slope surface is 2-500 nm.
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