Research complex for formation and investigation of nanostructures and method to form nanostructures

FIELD: nanotechnologies.

SUBSTANCE: invention relates to the field of nanotechnologies and may be used to form nanostructures from evaporated microdrop by exposure to acoustic fields. Complex for formation of nanostructures comprises a nanostructures shaper, an optical microscope, a data display facility and information processing and complex control facility. The nanostructures shaper comprises a foundation and a source of shaping action, at the same time the foundation is formed as piezoelectric with the possibility to apply initial substrate on its surface, and the source of nanostructure-shaping action is represented by surface acoustic waves (SAW), besides, to develop a SAW line, a pair of interdigital transducers (IT) is located on the piezoelectric foundation with the possibility to excite the acoustic field between them, and the shaper is installed in the object area of the optical microscope, at the same time the axis of the microscope sighting is aligned relative to the foundation at the angle φ, besides, the complex also includes a generator of high-frequency oscillations and a wideband amplifier connected to it and to IT.

EFFECT: provision of universality as regards a class of objects exposed to nanostructuring.

12 cl, 1 dwg, 1 tbl

 

The invention relates to the field of nanotechnology, and is intended for the formation of nanostructures from evaporated droplets influence of acoustic field and study of their impact on the formation of nanostructures of different morphologies, as well as to study the source substrate, in particular colloidal solution, and the final morphology of the solid phase ensembles of nanostructures formed in the acoustic field.

Structured nanolayers (nanostructures) and apparatus for their manufacture may find application in modern high technologies in the development of nanostructured materials with tailored properties, and devices: micro - and nanosensors, chip, photonic crystals, and so on), as well as in biology and medicine. In addition, the study of the solid phase, resulting from drops after evaporation of the solvent, relevant physico-chemical analysis of the solution and, in particular, in medical diagnosis, as well as in the study of autowave processes of self-organization in organic and Bioorganic structures. These studies are interesting to establish patterns of crystallization solutions, including education fractal and dendritic structures, features of which are related to the drying and initial parameters of the solution in the straw.

Known enough t chelovecheski complex hardware complex for the formation and study of nanostructures in patent RU 2164718, 27.03.2001, in which the formation of nanostructures produced ion beams on the surface of semiconductor structures. Known complex patent DE 10055318, 20.12.2001, where the formation of nanostructures is the acoustic waves.

The disadvantages of the existing systems should be attributed to the limited capacity management process of formation, which, as a rule, associated with a certain job (regulated) initial conditions.

The present invention is the creation of a complex for the formation and study of nanostructures with advanced technology and functionality, allowing you to build and study the nanostructure of any class, regardless of their electrical or other characteristics.

The task is solved in that in the complex, including the driver nanostructures, optical microscope, a means of displaying information and a means of information processing and management, driver nanostructures comprises a base (substrate) and the source-forming impact, while the base is made of piezoelectric with the possibility of applying to the surface of the original substrate. Source forming nanostructure effects are surfactants (surface acoustic wave), and to create a line of surfactants on piezoelectric Eskom the basis posted a pair of IDT (interdigital transducers) with excitation between the acoustic field, and the driver is installed in the object plane of an optical microscope, while the axis of sight of the microscope is oriented relative to the base angle φ, in addition to the complex is entered generator of high frequency oscillations and coupled with it a broadband amplifier associated with the IDT.

Mentioned piezoelectric substrate can be made in the form of lithium niobate crystal size of not less than 10×10 mm2and IDT applied to the crystal by a photolithography method. Initial substrate can serve as a colloidal solution. The vehicle information display is executed in a digital camera, paired with an optical microscope and by means of information processing and management tool complex is PC. The complex additionally introduced the oscilloscope and the key, and one of IDT pairs is connected to one output of the amplifier, and the other IDT pairs is connected to the second output of the amplifier through first and second contacts of the key, and through the first and third contacts of the key to the second amplifier output is connected to the input of the oscilloscope, while the other input of the oscilloscope connected to a PC (personal computer). Driver nanostructures can be placed in a cell with an optically transparent window, the walls of which are lined inside absorbing acoustic waves in the material.

According to the purpose complex which should excite the acoustic field capacity, necessary to transfer the nanoparticles inside the drops of solvent on the substrate at distances of the order of the spatial period of the emerging patterns. The optimal base material (substrate) of the substrate is a piezoelectric material is lithium niobate, with large values of the coefficients of the piezoelectric effect, and therefore, when applying IDT directly to the substrate it will effectively be excited surface acoustic wave.

This should be a continuous monitoring of the amplitude of a sound wave and its frequency to control the drying rate drops and the characteristics of the formed films. For these purposes, but also for automatic recording and archiving of control values generated by the structure of the complex digital input oscilloscope is able to transmit measurement results to the PC.

For further analysis of the research it is also necessary to have a constant visual control of the dynamics of the processes in the formation of nanostructures in the field of surfactants. For this purpose the installation used a digital optical microscope with a resolution, enabling real-time to monitor the formation of nanostructures and record experimental data in the PC, and coupled with him a digital camera for discrete fix the AI observations.

The angle of sight of the microscope φ in the case of one-dimensional structures are selected from those considerations that the emerging patterns (as they are in this case parallel to the IDT electrodes) were perpendicular to the plane containing the incident light beam and the normal to the substrate, have been made from the point of incidence of the beam. In the case of two-dimensional structures of the substrate rotate in a horizontal plane at φ=45° right or left relative to the previous case. The change in the angle of sight is carried out manually controls an optical microscope.

For the formation of nanostructures with the desired spatial period is necessary to excite a standing surface acoustic waves on the declared substrate coated with it a drop of the solution containing nanoparticles. The spatial period of nanostructures equal to half the wavelength of the surfactant, which, in turn, is determined by the spatial period of the IDT and the saw velocity in the substrate. It is the spatial period of nanostructures defines the requirement for the frequency generator. So, for the formation of nanostructures with a period of from 120 to 12 μm on a substrate of lithium niobate frequency should be changed from 5 to 150 MHz. The generator together with the amplifier in the process of formation of nanostructures under the influence of acoustic fields should provide at IDT line SAS variable visocica totoe voltage amplitude in the range (0.5 to 10) volts. Preliminary experiments conducted by the authors of the present invention showed that the intensity of excited when this surfactant is sufficient for the formation of nanostructured films of a drop of the colloidal solution prior to evaporation (for aqueous solutions of the characteristic time of 10-20 minutes for the alcohol - much less). Feeding a high frequency signal with amplitude of more than 10 volts undesirable because of possible interelectrode electrical breakdown and destruction of the IDT. Changing the frequency of the oscillator in the frequency range (15-150) MHz supplied to the IDT line surfactants allows on a substrate of lithium niobate to create an ordered nanostructured films with a period equal to half the wavelength of the surfactant (120-12 μm). When this generator to create the structure of a given period should provide for a time greater than the time of formation of nanostructured films of a drop of the colloidal solution prior to evaporation (for aqueous solutions of the characteristic time of 10-20 minutes for the alcohol - much less), the relative frequency stability (∆F/f)≤10-5.

Frequency generator that specifies the spatial period corresponds to the frequency of the applied IDT. As a rule, on one substrate is applied no more than three pairs of IDT with different frequencies. Thus, in the course of the study, the frequency generator may optionally be treason is and discrete in the frequency range, given inflicted IDT.

Because the standard high-frequency generators have typically low output power in a specified frequency range, you must be able to amplify the amplitude of the high frequency signal to the level of 10 V, the complex is entered broadband amplifier with a given operating band amplification.

To control the frequency and amplitude of the induced signal, the system provides for the use of a digital oscilloscope with a recording signal to a personal computer for further analysis. The choice of the oscilloscope was determined by the need to record and monitor incoming and passing the signals on line surfactants. The parameters of the signal, the control IDT, determined the bandwidth of the oscilloscope as not less than 150 MHz with a sampling rate of at least 2 GHz.

Thus, the inventive complex is different technological simplicity and allows the flexibility to change the parameters of the acoustic field on the nanostructures during their formation and research. The complex allows to form nanostructures, acting on objects of any class that has mass, regardless of the presence or absence of electric charge or magnetic moment, or other features.

The functional scheme of a research complex for the formation of the tion and study of nanostructures, appended to the description, position 1 is the shaper of nanostructures comprising a substrate 2 coated with her pair of IDT (positions 3 and 4), the position of the 5 - generator of high-frequency signals, the output of which is connected to the input of a broadband amplifier 6. The first output of the amplifier is connected to VSP, and the second output - or VSP through 1st and 2nd contacts key 7, or through the 1st and 3rd contacts key 4 to one input of the oscilloscope 8. The imaging unit 1 is placed in the subject field of an optical microscope 9, through which the digital camera 10 is connected to a personal computer 11, which simultaneously means of information processing and vehicle control.

The operation of the complex will be clear from the description of the method of forming nanostructures, which is the second object of the present invention associated with the first single inventive concept and aimed at solving the same technical problem.

Known methods of forming nanostructures, for example, the influence of electric and magnetic fields (patent DE 102004032451, 26.01.2006, FR 289728, 17.08.2007), suitable for impact on structures with certain properties. The basis of most methods of obtaining ordered ensembles of nanoparticles on the process of self-organization of nanoparticles into one-, two - and three-dimensional structure, the nature of the data for open non-equilibrium systems, where can be formed of a dissipative structure due to irreversible processes with phase transition. Such processes are directly implemented in the evaporating on a solid substrate nano - or micro-drops of a certain solution, which is dispersed nanoparticles or molecules of another substance. Control of this process and its result (in the form of the morphology of the resulting structure of the ensemble of nanoparticles) are usually either to changes in initial conditions (the type of solvent and solute, the size of the drops, the properties of the substrate), or the change of kinetic factors (for example, changing the mode of evaporation). This severely limited the mechanisms of dynamic impact on the system and the process (i.e. when changing certain parameters, the system essentially remains unchanged).

For the formation of structured films or coatings are sometimes used substrate with pre-formed on them relief, which has a structuring effect on damage on top of the relief layer of the nanoparticles. Known methods of forming such relief by laser lithography [Xia D., S.Brueck S. Lithographically directed deposition of silica nanoparticles using spin coating. // J. Vac. Sci. Technol. In 22 (6), 3415, 2004]. Typical dimensions of a relief when it is determined by the wavelength of the photons, and for common types of laser have order is OK 1 μm. This is a disadvantage: it is necessary to create the topography of the substrate with the smaller details (holes, grooves). For structuring the substrate is also used a method of plasma etching (reactive-ion etching RIE) [D. Xia, D. Li, Z. Ku, Y. Luo, S.R.J. Brueck Top-Down Approaches to the Formation of Silica Nanoparticle Patterns. // Langmuir 2007, 23, 5377-5385]. The use of shorter-wavelength x-ray lasers is hampered by the high cost of the hardware.

A variation of the method of pattern formation is applied to the primary substrate layer of the nanoparticles. The roughness of the relief associated with the nature of the packaging, the size and shape of the nanoparticles. The secondary layer is applied on top of the first. The location of the secondary particles of the layer is determined by topography, formed the primary layer, and the degree of its fixing to the substrate, because the application of the secondary layer can create the conditions for the mobility of the first layer and a movement of its molecules in the process of forming the secondary layer. However, obtaining well-ordered primary layer itself is quite complex technological task.

Thus, methods of structuring the substrate is not enough universal or involve the use of expensive equipment.

The technical problem solved by the present invention in part, the contest is the action scene of the method of forming nanostructures, is achieving its universality class of objects exposed nanostructuring, in combination with technological ease of implementation.

Known methods of forming nanostructures, including pre-create on a substrate of some relief methods plasma etching and laser and electron lithography. Creating an ordered layer on the surface of the substrate is a complex technological problem. In addition, these methods have limited universal or involve the use of expensive equipment.

The technical problem solved by the present invention regarding the method of forming nanostructures is achieving its universality class of objects exposed nanostructuring, in combination with technological ease of implementation.

The task is solved in that in the method of forming nanostructures, including the impact on the substrate containing the nanoparticles and the solvent and placed on a substrate, according to the invention on the surface of the substrate excite the acoustic wave, and carry out the ordering of the particles due to the acoustic treatment of the particles and the substrate, and the solvent is subjected to drying by forced convection, due to shaking of the nanoparticles in the process of drying process is of Italia intensify the process and increase the mobility of the nanoparticles. When the excitation of standing acoustic waves ordering of the particles is carried out by grouping them in locations corresponding to the alternating nodes or antinodes of the standing wave, and when excited by a traveling acoustic waves provide directional movement of the nanoparticles within the substrate. In the process of formation of nanostructures exercise intensity acoustic waves, and changing the wavelength, including discrete in the frequency range determined by a specific nanostructure. With the aim of eliminating the mode of formation of parasitic streams or increase the viscosity of the solvent, or reduce the thickness of the droplet on the substrate, or reduce the amplitude of the acoustic effects, or perform these actions simultaneously.

The proposed method for the formation of nanostructures, unveiled in NP claims, it is implemented using the open in n.p.1 claims complex for the formation of nanostructures.

An important feature of the inventive method is that sonic and ultrasonic waves are able to penetrate into the medium that is opaque to other radiations, including opaque water and other solutions or suspensions, emulsions, liquid ceramics, polymers, molten metals and semiconductors. At the same time, the acoustic waves have a gentle impact is s, allowing them to apply for organic substances, including biomaterials and biological tissues.

The inventive method allows to:

- to form a one-dimensional or two-dimensional periodic structure with a spatial period equal to half the wavelength of the surfactant, by providing periodic pressure field in the standing wave mode. The pressure field has the character of alternating nodes and antinodes. When this occurs, the splitting of the ensemble of particles lying separately on the group or region with depleted or enriched with number of particles,

to reduce the likelihood of spurious streams erode formed structure

- to intensify the process of interaction of the particles during formation of the nanostructures due to the forced convection of the solvent and the acoustic treatment of the particles and the substrate. Thus due to the shaking of the nanoparticles in the drying process increases their mobility, and hence the probability of achieving the provisions of the minimum energy corresponding to an ordered, dense packaging

- to organize the directed transport of nanoparticles in the mode traveling wave solution, enabling you to move the particles from one substrate to another.

The claimed method also allows you to create clusters of nanoparticles of a given shape and size, paramashiva the ü and fragment aggregates of nanoparticles, to embed the nanoparticles from the liquid phase in a matrix of another material, to create structures with gradient distribution of density and size of the nanoparticles, in a contactless manner to transport the nanoparticles in a predetermined path, to manage the processes of diffusion and evaporation of liquid droplets.

The table shows the comparative characteristics of methods of forming nanostructures in microcaps and thin films of colloidal solution.

The claimed complex and the method can be used to form nanostructures of evaporated droplets influence of acoustic field and study of their impact on the formation of nanostructures of different morphologies, as well as to study the initial colloidal solution (substrate) and the final morphology of the solid phase ensembles of nanostructures formed in the acoustic field.

1. Complex formation of nanostructures, including driver nanostructures, optical microscope, a means of displaying information and a means of information processing and management of complex, characterized in that the driver of the nanostructures comprises a base and a source forming impact, while the base is made of piezoelectric with the possibility of applying to the surface of the source substrate, and the source of f is mirowska nanostructure effects are surface acoustic wave (saw), and to create a line of surfactants on the piezoelectric base placed a pair of interdigital transducers (IDT) with excitation between the acoustic field and the imaging unit is installed in the object plane of an optical microscope, while the axis of sight of the microscope is oriented relative to the base angle φ, in addition to the complex is entered generator of high frequency oscillations and coupled with it a broadband amplifier associated with the IDT.

2. The complex according to claim 1, characterized in that the said piezoelectric base is made in the form of lithium niobate crystal size of not less than 10×10 mm2and IDT applied to the crystal by a photolithography method.

3. The complex according to claim 1, characterized in that as the initial substrate used colloidal solution.

4. The complex according to claim 1, characterized in that the means of displaying information is a digital camera coupled with an optical microscope and by means of information processing.

5. The complex according to claim 1, characterized in that the means for the management of complex serves as a personal computer (PC).

6. The complex according to claim 1, characterized in that it additionally introduced the oscilloscope and the key, and one of IDT pairs is connected to one output of the amplifier, and the other IDT pairs is connected to the second output of the amplifier cher the C of the first and second contacts of the key, and through the first and third contacts of the key to the second amplifier output is connected to the input of the oscilloscope, while the other input of the oscilloscope connected to a PC.

7. The complex according to claim 1, characterized in that the driver nanostructures placed in a cell with an optically transparent window, the walls of which are lined inside absorbing acoustic waves in the material.

8. The method of forming nanostructures, including the impact on the substrate containing the nanoparticles and the solvent and placed on the substrate, characterized in that the surface of the substrate excite the acoustic wave and carry out the ordering of the nanoparticles due to the acoustic treatment of the particles and the substrate, and the solvent is subjected to drying by forced convection.

9. The method according to claim 8, characterized in that excite a standing acoustic wave and the ordering of the nanoparticles is carried out by grouping them in locations corresponding to the alternating nodes or antinodes of the standing wave.

10. The method according to claim 8, characterized in that excite a traveling acoustic wave and carry out the directed movement of nanoparticles within the substrate.

11. The method according to claim 8, characterized in that in the process of formation of nanostructures exercise intensity acoustic waves and wavelengths, including discrete.

12. The method of claim 8, distinguish the different topics that or increase the viscosity of the solvent, or reduce the thickness of the droplet on the substrate, or reduce the amplitude of the acoustic wave, or perform these actions simultaneously.



 

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19 cl, 7 ex

FIELD: chemistry.

SUBSTANCE: method of producing modified inorganic oxygen-containing granular material involves the following steps: a) preparing a mixture of an aqueous suspension of inorganic oxygen-containing granular material and alkoxylated alcohol of formula where R1 is C1-C8-alkyl or phenyl, C4-C8-cycloalkyl or phenyl, R2 is a hydrogen atom or methyl, and n is an integer from 1 to 5; b) optional addition of a first resin and/or precursor of the first resin; c) adding a mixture of one or more cross-linking agents containing one or more elements selected from a group comprising Si, Al, Ti, Zr, B, Zn, Sn and V; d) optional addition of a second resin and/or precursor of the second resin to the obtained mixture. Water is optionally removed from the mixture at least partially before or during step b), c) or d) or after step d). Also, the precursor of the first resin can be converted to the first resin before, during or after step c) and/or the precursor of the second resin can be converted to the second resin after step d).

EFFECT: invention increases environmental safety and simplifies production of modified inorganic oxygen-containing granular material which is well compatible with resins.

11 cl, 4 tbl, 37 ex

FIELD: carbon materials.

SUBSTANCE: weighed quantity of diamonds with average particle size 4 nm are placed into press mold and compacted into tablet. Tablet is then placed into vacuum chamber as target. The latter is evacuated and after introduction of cushion gas, target is cooled to -100оС and kept until its mass increases by a factor of 2-4. Direct voltage is then applied to electrodes of vacuum chamber and target is exposed to pulse laser emission with power providing heating of particles not higher than 900оС. Atomized target material form microfibers between electrodes. In order to reduce fragility of microfibers, vapors of nonionic-type polymer, e.g. polyvinyl alcohol, polyvinylbutyral or polyacrylamide, are added into chamber to pressure 10-2 to 10-4 gauge atm immediately after laser irradiation. Resulting microfibers have diamond structure and content of non-diamond phase therein does not exceed 6.22%.

EFFECT: increased proportion of diamond structure in product and increased its storage stability.

2 cl

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