CN2162652Y - Small angle laser scattering instrument system - Google Patents

Small angle laser scattering instrument system Download PDF

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Publication number
CN2162652Y
CN2162652Y CN 93202023 CN93202023U CN2162652Y CN 2162652 Y CN2162652 Y CN 2162652Y CN 93202023 CN93202023 CN 93202023 CN 93202023 U CN93202023 U CN 93202023U CN 2162652 Y CN2162652 Y CN 2162652Y
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parts
screw
high molecular
small angle
molecular polymer
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CN 93202023
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刘文耀
盛京
王锡颖
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Tianjin University
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Tianjin University
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Abstract

The utility model discloses a small angle laser scattering instrument system for high molecular polymer. The instrument is composed of a laser, a neutral filter combined component, a sample table component, a measured polymer sample slide glass, an analyser, an optical imaging lens combined component, a CCD camera, a reception visual-field adjustment combined component, a prism refraction component, etc. The small angle laser scattering instrument system can be used for studying the morphology, structure and orientation of polymer to determine crystallization morphology and size, and can be used for the phase structure and phase separation of multiphase polymer hierarchy. The small angle laser scattering instrument system can be used for on-line measurement. The small angle laser scattering instrument system has the advantages of high speed and convenient fabrication of samples during the process of measurement. The small angle laser scattering instrument system can be used for studying the molecule movement, molecular weight, gelatin course of the polymer if matched with some accessories.

Description

Small angle laser scattering instrument system
The utility model belongs to the high molecular polymer surveying instrument.
Little angle laser light scattering instrument, report is arranged in the prior art, China Chinese Academy of Sciences chemistry LS-I type photographic process laser small angle scattering instrument of developing comes recording light dispersion image information by photographic plate, (" modern analytical technique---the application in superpolymer ", P388-389, Shanghai science tech publishing house, 1987,2) this instrumental sensitivity is low, is difficult to obtain more accurate light intensity distributions data as quantitative examination, analytical cycle is long, poor repeatability; Changchun Applied Chemistry Research Inst., Chinese Academy of Sciences develops JSY-390 type laser light scattering photometer, scanning diaphragm is spiral of Archimedes shape (" modern analytical technique---the application in superpolymer ", P389, Shanghai science tech publishing house, 1987,2), University Of Tianjin develops one-dimensional scanning formula laser small angle scattering instrument, scanister is fibre bundle scanning dispersion image (" modern analytical technique---the application in superpolymer, P390.Shanghai science tech publishing house, 1987,2).The Beijing Chemical Engineering College develops the quick scanister of little angle laser light scattering, and the scanning diaphragm of employing is fan-shaped slit (" modern analytical technique---the application in superpolymer ", P390-391, Shanghai science tech publishing house, 1987,2).The common drawback of three kinds of instruments is that the machining precision of claimed apparatus is very high with the scattered light intensity under the mechanical system scanning different angles, and sweep velocity is unhappy, and analysis precision is poor, and analytical cycle is long, can not carry out performance analysis; Professor R.SStein presides over the low-angle light scattering optical multichannel analyzer of development, is to form array with the optical diode of most amounts to come receiving scattered light strong, and electric scanning is 500 passages nearly, transmitting digitized scattering strength [ A.Wasiak, D, Peiffer and R.S Stein, J, Polym, Sci; Letter Ed, 14,381(1976) ].But this analyzer is an experimental provision of building on the optical bench of laboratory, no instrumentation is because of adopting hyperchannel and multiple diode receiving array, the extremely difficult homogenization of receptivity, signal Processing is brought difficulty, and the A/D conversion links that reaches hundreds of passages simultaneously also can be because of the too complicated difficulty that causes.
The purpose of this utility model is to overcome the shortcoming that existing little angle laser light scattering instrument exists, and provides intelligentized miniature little angle laser system to be used for scientific research and production.
The utility model is the intelligentized little angle of an a kind of accurate photoelectricity laser light scattering instrument, has the scattering image Treatment Analysis software systems of perfect in shape and function.Little angle of the present utility model laser light scattering instrument system works theory diagram is as follows:
Figure 932020232_IMG2
1-laser instrument among the figure, 2-neutral filter combiner, 3-polarizer parts, 4-sample stage (worktable) parts, the tested polymer samples slide glass of 5-, 6-analyzer, 7-optical imagery camera lens combiner, combiner, M are regulated in 8-CCD video camera and reception visual field 1, M 2, M 3-be respectively prism refractive power parts.Principle of work is that the single-mode laser bundle that sends when laser instrument 1 is through M 1After the neutral filter combiner, has the luminous energy of accurate quantification, by the polarizer 3, through M 2Be mapped to the sample 5 a certain positions that put on sample stage 4, at this moment by sample incident light is carried out Rayleigh scattering, form dispersion image, this dispersion image is received by ccd video camera 8 through imaging lens group 7 with after picking up inclined to one side device 6, and send into computing machine and carry out analyzing and processing, handle the multiple structural parameters that draw polymkeric substance or blend as calculated.In the instrument course of work from the 3 and 6 different polarization configurations that can obtain scattering image.As H VAnd V VScattering image.
The utility model is the intelligentized little angle of the accurate photoelectricity laser light scattering instrument of a microminiaturization, has good optical system, precision is governor motion and objective table flexibly, receive scattering image by high sensitivity and high-resolution ccd video camera, and cooperate quick image collection card, can be quick, continuously, in real time image is carried out processing, analysis meters such as conversion, enhancing, level and smooth, recovery, identification and calculate the series of structure parameters of relevant superpolymer and blend.The utility model is equipped with the form that the 2-D data disposal system can be used for studying polymkeric substance, structure and orientation, calculate the size and the form of crystallization, the phase structure of research heterogeneous system and being separated and can be carried out on-line measurement, and speed is fast, sample is manufactured simply, be used some annexes, also can study molecular motion, polymer molecular weight and heavy glue process etc.
The general structure of little angle of the present utility model laser light scattering instrument system is shown in accompanying drawing 1 and accompanying drawing 2.Shown in Figure 2 is the A-A sectional view of Fig. 1 instrument general view.The part that each numeral is represented respectively among Fig. 1 and Fig. 2 is: 1-instrument base plate, 2-instrument stand, 3-plate washer, the 4-set collar, the 5-leading screw, the 6-set collar, 7-sells (2 * 8), the 8-end cap, 9-screw (M3 * 10) (10), 10-planker, (2 of 11-side plates, make with the HT20-40 material), 12-flat board (making) with the LY-11 material, 13-hole glass (making), 14-top cover (making) with the HT20-40 material with K9 glass, the 15-scale, the 16-scale frame, 17-screw (M5 * 8) (3), 18-gamma camera, the 19-prism holder, the 20-slide block, 21-tooth bar, 22-guide rail, the 23-gear shaft, the 24-planker, 25-binding (the HT20-40 material is made), the fastening shell of 26-, 27-screw (M2 * 5) (4), 28-connecting plate (2), 29-prism, 30-frequency modulated light sheet, 31-screw (M5 * 12) (3), 32-screw (M4 * 10) (16), 33-pin hole, 34-camshaft, the 35-gear shaft, the 36-support, 37-screw (M4 * 12) (30), 38-screw (M4 * 12) (2), the 39-polarizer, the 40-trim ring, 41-geared sleeve, 42-sleeve, the 43-support, the 44-support, 45-axle, 46-light-balancing filter framework (7), the 47-support, the 48-support, 49-prism holder (2), 50-laser instrument, 51-side top board (HT20-40 material system) (2), 52-screw (M6 * 7) (4), 53-gear, 54-cam (3), 55-cam (3), the 56-guide rail, 57-slide block, 58-tooth bar, the 59-gear shaft, 60-screw (M3 * 10) (5), 61-handwheel, 62-end cap, the 63-guide wheel, the 64-slide block, 65-electric furnace, 66-lens set (ZF6+QK3), the 67-lens barrel, the 68-trim ring, 69-lens barrel, 70-analyzer, the 71-trim ring, the 72-CCD gamma camera.
Accompanying drawing 3 is the H with the PE of the production of the utility model instrument and digitized certain sample VAnd V VScattering image, accompanying drawing 4 are the H that draw through after a series of image processings and the Karhunen-Loeve transformation VTwo principal component axis of scattering image, it indicates the orientation conditions of sample, accompanying drawing 5(a) be this H VThe 2-D intensity distribution of image (b) is this visual 3-D intensity distribution.Accompanying drawing 6 be different component blend LDPE+PCBR during in position angle μ=60 ° intensity distributions relatively (to H VScattering image), when analytical calculation, the principal component angle in the Karhunen-Loeve transformation of cooperation Fig. 4 just can estimate the size parameter of spherocrystal.Accompanying drawing 7 be the blend LDPE+PCBR of different component during in position angle μ=60 ° intensity distributions relatively (to V VDispersion image), by comparative analysis computing, can estimate the correlation distance of blend, density fluctuation coefficient and phase structure thereof etc. to Fig. 6 and Fig. 7.
Sample stage parts of the present utility model are by part plate washer 3, set collar 4, leading screw 5, set collar 6, pin (2 * 8) 7, end cap 8, screw (M3 * 10) 9(10), planker 10, guide rail 56, slide block 57, tooth bar 58, gear shaft 59, screw (M3 * 10) 60(5), handwheel 61, end cap 62, guide rail 63, slide block 64, electric furnace 65 constitutes, and two-layer up and down guide rail is a quadrature, can finish the position adjustments of sample scattering point, adjusting ultimate range is 30mm, and maximum nonstraightness error is 10 μ m/30mm; Imaging lens and analyzer parts are by part lens set 66, lens barrel 67, and trim ring 68, lens barrel 69, analyzer 70, trim ring 71 constitutes, the cemented doublet that lens set is made by QK3 and ZF6, disappearing image is poor, and is last because the maximum error that spherical aberration produced is δ Hmax=0.01868; The refracting prisms parts are by part connecting plate 28, prism 29, frequency modulated light sheet 30, screw (M5 * 12) 31(3), screw (M4 * 10) 32(16) constitute, prism dimensions is 25 * 25mm 2, precision is 1 a minute/45; Polarizer rotary part is by part gear shaft 35, support 36, screw (M4 * 12) 37(30), screw (M4 * 12) 38(2), polarizer 39, trim ring 40, geared sleeve 41, sleeve 42, support 43 constitutes, these parts cooperate with imaging len and analyzer parts, scalable scattering image configuration: H VAnd V VConfiguration.Play the non-perpendicularity (H of inclined to one side and analyzing axis V) less than 0.1 ° (6 '), misalignment (V V) less than 1 ° (6 '); Parts are regulated in the neutral filter combination, by camshaft 34, and cam 54 and 55, part support 44, axle 45, light-balancing filter framework 46, support 47 constitutes, and can form 16 grades of compound transmitance scopes 0.22%-9。15% is adjustable, with the primary optical axis non-perpendicularity be 40 μ m/16 levels; CCD gamma camera and reception are wished the field control parts by part slide block 20, tooth bar 21, guide rail 22, gear shaft 23, planker 24 and the CCD gamma camera of putting thereon 72 constitute, and the guide rail maximum moving distance is 110mm, precision is 20 μ m/110mm, and CCD gamma camera resolution is 512 * 580, and sensitivity is 0.2Lux adapts to 0 ° of-15 ° of angle of range of scatter angles.

Claims (7)

1, a kind of high molecular polymer surveying instrument, with laser as light source, the instrument that is characterised in that of the present utility model is provided with sample stage parts, imaging len and analyzer parts, folding is as component prism, polarizer rotary part, parts are regulated in the neutral filter combination, and parts are regulated in CCD gamma camera and reception visual field.
2, high molecular polymer surveying instrument according to claim 1 is characterized in that the sample stage parts by plate washer 3, set collar 4, leading screw 5, set collar 6, pin (2 * 8) 7, end cap 8, screw (M3 * 10) 9, planker 10, guide rail 56, slide block 57, tooth bar 58, gear shaft 59, screw (M3 * 10) 60, handwheel 61, end cap 62, guide rail 63, slide block 64, electric furnace 65 constitutes.Two-layer up and down guide rail is a quadrature, can finish the position adjustments of sample scattering point, and adjusting ultimate range is 30mm, and maximum nonstraightness error is 10 μ m/30mm.
3, high molecular polymer surveying instrument according to claim 1, it is characterized in that imaging len and analyzer parts are made of lens set 66, lens barrel 67, trim ring 68, lens barrel 69, analyzer 70, trim ring 71, wherein lens are cemented doublets of being made by QK3 and ZF6, disappearing image is poor, and is last because the maximum error δ that spherical aberration produced Hmax=0.01868.
4, high molecular polymer surveying instrument according to claim 1, it is characterized in that folding as component prism by connecting plate 28, prism 29, frequency modulated light sheet 30, screw (M5 * 12) 31 and screw (M4 * 10) 32 constitutes, wherein prism dimensions is 25 * 25mm 2, precision is 1 a minute/45.
5, high molecular polymer surveying instrument according to claim 1, it is characterized in that polarizer rotary part by gear shaft 35, support 36, screw (M4 * 12) 37, screw (M4 * 12) 38, polarizer 39, trim ring 40, geared sleeve 41, sleeve 42, support 43 constitutes, and these parts cooperate with imaging len and analyzer parts, scalable scattering image H VAnd V vConfiguration rises partially and the non-perpendicularity (H of analyzing axis V) less than 0.1 ° (6 '), misalignment (V V) less than 0.1 ° (6 ').
6, high molecular polymer surveying instrument according to claim 1, it is characterized in that neutral filter combination adjusting parts are by camshaft 34, cam 54 and 55, support 44, axle 45, light-balancing filter framework 46, support 47 constitutes, it is adjustable to form 16 grades of compound transmitance scope 0.22%-9.15%, with the primary optical axis non-perpendicularity be 40 μ m/16 levels.
7, high molecular polymer surveying instrument according to claim 1, it is characterized in that the CCD gamma camera and receive the visual field regulating parts by slide block 20, tooth bar 21, guide rail 22, gear shaft 23, planker 24 and ccd video camera thereon 72 constitute, its middle guide maximum moving distance is 110mm, precision is 20 μ m/110mm, and (CCD gamma camera resolution is 512 * 580, and sensitivity is 0.2Lux, adapting to range of scatter angles is 0-15 ° of angle.)
CN 93202023 1993-01-18 1993-01-18 Small angle laser scattering instrument system Expired - Fee Related CN2162652Y (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105181724A (en) * 2015-10-21 2015-12-23 吉林大学 In-situ rotary fiber sample platform based on X-ray small-angle scatterometer
CN107014319A (en) * 2017-04-05 2017-08-04 中国计量大学 A kind of spatial vertical degree detection method of worm-gear speed reducer drive axle seat axially bored line
CN108318454A (en) * 2018-03-28 2018-07-24 山东大学 A kind of small angle laser light scattering instrument and characterizing method with the controllable sample cell of temperature, pressure

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105181724A (en) * 2015-10-21 2015-12-23 吉林大学 In-situ rotary fiber sample platform based on X-ray small-angle scatterometer
CN105181724B (en) * 2015-10-21 2017-11-21 吉林大学 Fiber based on low-angle scattering of X-rays instrument specimen rotating holder in situ
CN107014319A (en) * 2017-04-05 2017-08-04 中国计量大学 A kind of spatial vertical degree detection method of worm-gear speed reducer drive axle seat axially bored line
CN107014319B (en) * 2017-04-05 2019-02-12 中国计量大学 A kind of spatial vertical degree detection method of worm-gear speed reducer drive axle seat axially bored line
CN108318454A (en) * 2018-03-28 2018-07-24 山东大学 A kind of small angle laser light scattering instrument and characterizing method with the controllable sample cell of temperature, pressure
US11067505B2 (en) 2018-03-28 2021-07-20 Shandong University Small angle laser scatterometer with temperature-pressure-controllable sample cell and characterization method
CN108318454B (en) * 2018-03-28 2022-11-04 山东大学 Small-angle laser scattering instrument with temperature and pressure controllable sample cell and characterization method

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