CN1220871C - Real time monitoring device for nanometer particle diameter during nanometer material preparation using sol-gel method - Google Patents

Real time monitoring device for nanometer particle diameter during nanometer material preparation using sol-gel method Download PDF

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CN1220871C
CN1220871C CN 03110985 CN03110985A CN1220871C CN 1220871 C CN1220871 C CN 1220871C CN 03110985 CN03110985 CN 03110985 CN 03110985 A CN03110985 A CN 03110985A CN 1220871 C CN1220871 C CN 1220871C
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optical fiber
absorption spectrometer
signal output
output optical
processing system
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CN1521496A (en
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孔祥贵
单桂晔
安利民
王新
曾庆辉
费晓方
刘益春
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Changchun Institute of Optics Fine Mechanics and Physics of CAS
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Changchun Institute of Optics Fine Mechanics and Physics of CAS
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Abstract

The present invention relates to a nanometer particle diameter real-time monitoring device in the nanometer material preparation of a sol-gel method, which belongs to the technical field of plasmid monitoring. A light source of the present invention and the end surface of an introducing optical fiber are arranged on a front focal point and a back focal point of an optical fiber coupling; a coupling for signal output optical fiber is connected with an absorption spectrometer and a signal processing system; the other ends of the input optical fiber and the output optical fiber are arranged in a sol-gel reaction chamber, and the end surfaces of the other ends of the input optical fiber and the output optical fiber are opposite to guarantee that an optical signal passing through the introducing optical fiber can totally enter the output optical fiber. The signal output optical fiber transmits the optical signal received from the introducing optical fiber to a detector CCD of the absorption spectrometer; after the optical signal received by the detector CCD, data processing is carried out by the absorption spectrometer and the signal processing system to give data to be measured. The present invention can monitor particle diameters of particles in real time and control reaction conditions, and has the advantages of simple structure, easy realization, time saving, labour saving and resource saving.

Description

Prepare in the nano material the nanometer particle size real-time monitoring device in sol-gel process
Technical field: the invention belongs to plasmid monitoring technical field in the system, relate to the real time monitoring of nano particle diameter, specifically a kind of nanometer particle size real-time monitoring device in the sol-gel process material preparation.
Background technology: nanometer technology is a hot fields of current scientific research, and the preparation of nano material is the important foundation of Nano-technology Development.Sol-gel process is a kind of common method in the nanometer technology of preparing.If can in this method, carry out the real-time monitoring and the control of particle diameter to nano particle, determine the size of nano particle and the relation of its character, be a significant contribution to the perfect of nanometer technology of preparing.
The size of monitoring particle diameter all adopts timing sampling usually, carries out the size of absorption spectrum or other method and commercial measurement nanometer particle size then, and then determines the preparation condition of control particle diameter.This method, promptly time-consuming, effort is wasted resource again, the more important thing is that preparation condition can not real-time quantitative control.
The device that sol-gel prepares nanometer is very simple, and its main body is a sol gel reaction chamber, has gas on the reaction chamber and feeds mouth, sample import and export and temperature control inlet.Kind difference according to the preparation nanometer can distinguishingly design, if any process need heat, be equipped with heating apparatus; When the needs that and for example have lead to special gas, will open blow vent or the like on the top of flask more.The method of monitoring particle diameter and technology have multiple, and absorption spectrum method is comparatively commonly used, and instrument and equipment is seen everywhere.But also there is not at present one fixing, unified to prepare in the nano material the nanometer particle size method of real-time, still do not have such device of monitoring particle diameter in real time in the sol-gel preparation system both at home and abroad in sol-gel process.
Summary of the invention: the present invention organically combines sol gel reaction device and light guide optical fiber, be connected with small-sized absorption spectrum test macro, purpose provide a kind of in the sol-gel process material preparation particle diameter real-time monitoring device to nano particle, can be implemented in the sol-gel process material preparation real-time monitoring and control to the nanoparticle particle diameter.
The present invention is by light source 8, and optical fiber coupler 9 imports optical fiber 5, signal output optical fibre 6, and absorption spectrometer and signal processing system 7, optical fiber coupler 10 constitutes.Light source 8 is that a wavelength coverage is the wideband light source of 200nm~1 μ m, and optical fiber coupler 9 is one group of optics compound lens.Light signal in the signal output optical fibre 6 is delivered in the absorption spectrometer, carries out signal Processing and is shown on the display by delivering to CCD receiver in the spectrometer and data handling system after the spectrometer beam split.
Import in the optical fiber 5 for the broadband light that light source 8 is sent enters fully, light source 8 is placed on the front focus of optical fiber coupler 9, and the outer face 11 that imports optical fiber 5 is just in time on the back focus of optical fiber coupler 9.Signal output optical fibre 6 is sending the entrance slit of absorption spectrometer and signal processing system 7 to so that light signal delivered to carry out beam split in the spectrometer and signal data is handled from importing light signal that optical fiber 5 receives through fiber coupler 10, demonstrates the numerical value of nano particle diameter and corresponding relation curve etc. on display.The other end that imports optical fiber 5 and signal output optical fibre 6 places in the sol gel reaction chamber 1, the end face 13 that imports the end face 12 of optical fiber 5 and signal output optical fibre 6 is corresponding, guarantees by the light signal behind the optical excitation nano particle of importing optical fiber 5 to greatest extent in the entering signal output optical fibre 6.
The present invention is to be undertaken by importing optical fiber 5 and signal output optical fibre 6 to the real-time monitoring of nanometer particle size.When nano particle reacted in reactor 1, the light that light source 8 is sent was imported as light signal by an end face 11 that imports optical fiber 5, is in the nano particle that imports between optical fiber 5 end faces 12 and signal output optical fibre 6 end faces 13 in the provocative reaction device 1.The end face 13 of signal output optical fibre 6 in reactor 1 collected spectral signal and exported absorption spectrometer and the data handling system 7 that is connected to outer end 14 to.The data handling system of absorption spectrometer and data handling system 7 is according to the relation of absorption spectrum intensity and particle diameter, can be with the numerical value instant playback of particle diameter in display screen.The relation of absorption spectrum intensity and particle diameter is expressed from the next:
Figure C0311098500041
Wherein, second is the quantum confinement energy, and the 3rd is the coulomb interaction energy, and the 4th is relevant modified value, R *Be equivalent Reed fort constant.
The present invention utilizes the light signal that imports optical fiber 5 and signal output optical fibre 6 signs, by absorption spectrometer and data handling system 7 light signal is treated as data, provide the particle size of nano particle in the sol gel reaction chamber 1, realize monitoring in real time, and can control such as temperature, concentration and time isosol-gel reaction condition according to the result of real-time monitoring.The present invention is simple in structure, is easy to realize, and is time saving and energy saving, saves resource.
Description of drawings: Fig. 1 is a structural representation of the present invention.1 is the sol gel reaction chamber among the figure, and 2 gases feed mouth, and 3 samples are imported and exported, 4 temperature control inlet, 5 import optical fiber, 6 signal output optical fibres, 7 absorption spectrometers and signal processing system, 8 light sources, optical fiber coupler 9,11,12 is the both ends of the surface of light source importing optical fiber 5, the end face of 13 signal output optical fibres 6, the outer end of 14 signal output optical fibres 6,10 optical fiber couplers.
Embodiment:
In absorption spectrometer of the present invention and the signal processing system 7, adopt the absorption spectrometer of measuring grain graininess commonly used, ready-made product is arranged.Signal processing system comprises photoelectric commutator, data processor, display etc., also is common equipment therefor.
The used absorption spectrometer of the present invention itself has light source, light source 8 can be with the light source on the absorption spectrometer, need be installed in fixture of optical fiber coupler 9 usefulness the specimen holder front end of absorption spectrometer this moment, and the outer face 11 that imports optical fiber 5 is fixed on the specimen holder.Can utilize existing absorption spectrometer like this, carry out little change and just can finish task proposed by the invention.

Claims (2)

1, a kind ofly prepares in the nano material the nanometer particle size real-time monitoring device in sol-gel process, it is characterized in that by light source (8) optical fiber coupler (9) imports optical fiber (5), signal output optical fibre (6), absorption spectrometer and signal processing system (7) and optical fiber coupler (10) constitute; One end face (11) of light source (8) and importing optical fiber (5) is placed on the front focus and back focus of optical fiber coupler (9), one end (14) of signal output optical fibre (6) is by optical fiber coupler (10), link to each other with detecting device on the absorption spectrometer of absorption spectrometer and signal processing system (7), the other end that imports optical fiber (5) and signal output optical fibre (6) places in the so-gel reaction chamber (1), the end face (12) of importing optical fiber (5) and the end face (13) of signal output optical fibre (6) are corresponding, make by in the whole entering signal output optical fibres (6) of light signal energy that import optical fiber (5); The light that light source (8) sends is through optical fiber coupler (9), focus on the end face (11) that imports optical fiber (5), and enter in the lead-in light fibre (5), after importing optical fiber (5), pass nano particle the reaction chamber (1) from its end face (12), in end face (13) the entering signal output optical fibre (6) of signal output optical fibre (6), behind signal output optical fibre (6), send detector C CD on the absorption spectrometer of absorption spectrometer and signal processing system (7) to by optical fiber coupler (10), behind the detector C CD receiving optical signals, signal processing system by absorption spectrometer and signal processing system (7) becomes numeral to light signal, provides the particle size of the nano particle in the reactor (1).
2, according to claim 1ly prepare in the nano material the nanometer particle size real-time monitoring device in sol-gel process, it is characterized in that light source (8) is that a wavelength coverage is the wideband light source of 200nm~1 μ m, optical fiber coupler (9) is one group of optics compound lens, optical fiber coupler (10) be one the coupling element that connects together of the detector C CD on the absorption spectrometer in signal output optical fibre 6 and absorption spectrometer and the signal processing system 7.
CN 03110985 2003-01-30 2003-01-30 Real time monitoring device for nanometer particle diameter during nanometer material preparation using sol-gel method Expired - Fee Related CN1220871C (en)

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CN102252945B (en) * 2011-06-03 2013-11-27 上海理工大学 Particle measurement device and method based on fiber coupling
CN103529643B (en) * 2012-07-05 2017-01-18 中国科学院物理研究所 Nano graphical system and light response characteristic detection device thereof
CN104677789B (en) * 2015-03-05 2018-01-26 江苏苏净集团有限公司 A kind of nano particle counting and detecting device and detection method
CN106404623B (en) * 2016-08-29 2019-04-05 南开大学 Suspended Sedimentation Concentration monitors system and monitoring method
CN111272615B (en) * 2020-02-21 2024-03-08 陕西佰傲再生医学有限公司 Gel particle size distribution detection method

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