CN1908625A - Time resolving two-dimensional laser light scattering apparatus with small and large angle - Google Patents
Time resolving two-dimensional laser light scattering apparatus with small and large angle Download PDFInfo
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- CN1908625A CN1908625A CN 200510012282 CN200510012282A CN1908625A CN 1908625 A CN1908625 A CN 1908625A CN 200510012282 CN200510012282 CN 200510012282 CN 200510012282 A CN200510012282 A CN 200510012282A CN 1908625 A CN1908625 A CN 1908625A
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Abstract
The related temporal resolution 2D laser optical scatterometer for large/small angle (20-90deg/0-20deg) comprises: a large angle detection system included two wide-aperture lens and a very sensitive array detector, a system central line fit to form some included angle with incidence light and detect the continual scattering signal in the range; a detection screen and another detector both on the incidence direction for scattering signal in small angle range. This invention can detect very poor signal or collects strong signal by screen imaging method.
Description
Technical field
The invention belongs to time resolution two-dimensional laser light scattering instrument field, be particularly related to and on an instrument, detect wide-angle (20～90 degree), and detect low-angle (0～20 degree), have the time resolution two-dimensional laser light scattering apparatus that the big angle Xiao Jiao of very high time resolution has both.
Background technology
The light scattering of superpolymer is to utilize superpolymer the scattering of light phenomenon to be studied a kind of research method of polymkeric substance inner structure situation, in high molecular solution of research and texture, play an important role, particularly to the behavioral study that is separated of blend, it is indispensable favourable instrument.At present, the input for the superpolymer light scattering mainly contains right spot method and photographic process.Solution light scattering instrument for example, detecting device generally is a photomultiplier, it has very high sensitivity, but the scattered signal of different angles is the detection positions by the rotation photomultiplier, angular detection can not get continuous light scattering signal one by one; And when need detecting the signal of a lot of angles, because the position of rotation detector to and fro, the temporal resolution of detection is very low.
And the input of low angle laser light scattering instrument commonly used, the main photographic process that adopts, at first imaging on screen of scattered signal, use the picture on CCD detecting device (camera or high-speed camera) the detection screen then, can detect the continuous scattered signal of certain angle scope, but,, can only detect very strong scattered signal because the sensitivity that detects is not high.And the angular range that detects little (generally being) less than 30 degree.
At the phase-splitting initial stage, need the angular range bigger (between 30～an angle of 90 degrees degree) of detection for blend polymer, or for the polyolefins blend, because refraction index differs very little, even the phase-splitting later stage, scattered signal is still very weak, just is difficult to detect with general light scattering device.For example: Chinese patent 96116432.8 disclosed technical schemes can only be carried out the detection of the laser light scattering at little angle, can not detect wide-angle, and detection sensitivity are not high.
Summary of the invention
The purpose of this invention is to provide a kind of wide-angle (20～90 degree) that on an instrument, both can detect, can detect the time resolution two-dimensional laser light scattering apparatus that the big angle Xiao Jiao of low-angle (0～20 degree) has both again.
The time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao of the present invention has both is made up of laser collimation system and detection system, and principal character is that detection system is divided into big angle detection system and two parts of little angle detection system.
The purpose of big angle of the present invention partial design is that design is a kind of highly sensitive, fast response and can control the pick-up unit of once finishing continuous light scattered signal in the wide range with digitized processing in real time.By wide-aperture camera lens, it can once detect the light scattering signal of about 60 degree angular ranges simultaneously; By the position of rotary table rotation detecting, can detect the light scattering signal of arbitrarily angled (0～90 degree).In order to guarantee that scattered light is not in the light by Re Tai and sample cell, the hot platform of design and sample cell adopt the hydraucone shape.
The purpose of little angle part design is the strong scattering light that can detect in the small angle range.
The big angle partial devices (is made up of one group of protruding and concave lens two identical wide- aperture camera lenses 14,13, both can collect the optical signalling of extensive angle, the image that obtains is also undistorted) and a very sensitive area array CCD detecting device composition that has shutter, two camera lens 14,13 back-to-back installations, the signal that camera lens 14 is collected, focused on once more on the big angle signal detector 12 by camera lens 13, gathered by big angle signal detector 12.Can receive the scattered light of (0～60 degree) in the wide range near the wide-aperture camera lens 14 of Re Tai and sample cell, after forming directional light, focused on the inductor of big angle signal detector by second identical high-aperture lenses 13 (can receive the scattered light of (0～60 degree) in the wide range), detected by detecting device.Like this, just can realize once detecting simultaneously continuous scattered signal in the wide range.
Because scattered light directly focuses on the detecting device by camera lens, rather than becomes phase by screen, therefore improved detection sensitivity greatly.
Because the angle of one-time detection is enough big, in experimentation, do not need to obtain the more information of wide range by the position of rotation detector, therefore improved temporal resolution greatly.
Big angle of the present invention detection system is installed on the adjutage of rotary table, and the center of rotary table is on the center line of detection system.Detected sample is placed in the sample cell that is sleeved in the hot platform, and hot platform is positioned at the rotary table center.When the rotation rotary table, pick-up unit is around the rotation center rotation like this, and the detection system center line just forms certain included angle, just scattering angle with incident light.So by the rotation rotary table, the light scattering signal that pick-up unit can detect arbitrarily angled (0～90 degree).
Little angle detection system is installed in along on the adjutage of incident light direction, and irradiate light is back imaging on screen to the sample, detects as little angle signal detecting device with a high-speed camera then.Before screen, increase an analyzer, the Hv that just can carry out crystallization, the detection of Vv image.
The time resolution two-dimensional laser light scattering apparatus parts that big angle Xiao Jiao of the present invention has both comprise laser instrument 1, diaphragm 2, optical filtering 3, polarizer 4, condenser 5, hot platform 6, screen 8, little angle signal detecting device 9, rotary table 10, the adjutage 11 of rotary table, big angle signal detector 12, camera lens 13 (is made up of one group of protruding and concave lens, both can collect the optical signalling of extensive angle, the image that obtains is also undistorted), camera lens 14 (is made up of one group of protruding and concave lens, both can collect the optical signalling of extensive angle, the image of acquisition is also undistorted), Xiao Jiao test section adjutage 15, optical table 16, adjustable height pole 17, the newel 18 of rotary table, sample cell 19.
One optical table 16 is equipped with laser instrument 1, diaphragm 2, optical filtering 3, polarizer 4, condenser 5, rotary table 10, Xiao Jiao test section adjutage 15 successively from the table top of optical table 16 1 ends;
Described laser instrument 1, diaphragm 2, optical filtering 3, polarizer 4, condenser 5 are mounted on the adjustable height pole 17; The laser instrument 1, diaphragm 2, optical filtering 3, polarizer 4 and the condenser 5 that are installed on the adjustable height pole 17 are formed the Lights section.
Single-revolution worktable 10, the center of rotary table 10 are equipped with the newel 18 of rotary table and the adjutage 11 of rotary table on rotary table 10 on the center line of detection system; Hot platform 6 is installed on the newel 18 of rotary table, be set with sample cell 19 in the hot platform 6, camera lens 14, camera lens 13 and big angle signal detector 12 are installed on the adjutage 11 of rotary table successively, wherein camera lens 14 is adjacent with sample cell 19 with hot platform 6, is camera lens 13 between big angle signal detector 12 and the camera lens 14.The adjutage 11 of rotary table 10, rotary table, big angle signal detector 12, camera lens 13 and camera lens 14 are formed the test section, big angle.
Described hot platform 6 and sample cell 19 are placed in the center of rotary table, and sample is placed in the sample cell 19.
One Xiao Jiao test section adjutage 15 is equipped with screen 8, little angle signal detecting device 9 successively on Xiao Jiao test section adjutage 15; Wherein, screen 8 is installed in the place ahead of rotary table 10.Xiao Jiao test section adjutage 15, screen 8, little angle signal detecting device 9, or add analyzer 7 and form the Xiao Jiao test section.Analyzer 7 can be selected to install or do not install according to the experiment situation.Analyzer 7 is mounted on the Xiao Jiao test section adjutage 15, and before screen 8, the laser that the center of analyzer 7 and laser instrument 1 send is at sustained height.
Described Xiao Jiao test section adjutage 15 is mounted in the another side of rotary table 10 on the incident light direction.
By regulating the height of adjustable height pole 17, make the center of diaphragm 2, optical filtering 3, polarizer 4, condenser 5, hot platform 6, sample cell 19, analyzer 7, screen 8, little angle signal detecting device 9, big angle signal detector 12, camera lens 13 and camera lens 14 and laser that laser instrument 1 sends at sustained height.
When big angle of the present invention detection system was rotated around rotation center, the detection system center line just formed certain included angle, just scattering angle with incident light.And wide-aperture camera lens can receive the scattered light in the wide range, like this, just can realize detecting simultaneously continuous scattered signal in the wide range.In the incident light direction, installation and measuring screen and another one detecting device can detect the strong scattered signal in small angle range simultaneously.Owing to can detect wide-angle very simultaneously, scattered signal continuously in the wide range, light scattering behavior that so just can the search time resolution can improve temporal resolution greatly, can detect very weak scattered signal.And, can adopt the method collection of screen imaging for strong scattered signal.
The invention has the beneficial effects as follows that owing to can detect very in the polarizers of big angle scope scattered signal continuously simultaneously, light scattering behavior that so just can the search time resolution can improve temporal resolution greatly; And can detect very weak scattered signal and scattered signal at any angle, for being separated of research blend polymer, the initial stage that particularly is separated has important use to be worth; Simultaneously because its very strong light detection sensitivity, can study the behavior that is separated that the polyolefins refraction index differs very little blend polymer.
The phase-splitting than strong scattering intensity can be studied in little angle part, can also study the behavior of crystallization, orientation.
The present invention is further described below in conjunction with drawings and Examples.
Description of drawings
Fig. 1. the principle schematic of the time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao of the present invention has both.
Fig. 2 is the principle schematic of test section, big angle when the incident light direction of schematic diagram shown in Figure 1.
Fig. 3 is the principle schematic of test section, big angle when rotary table rotation θ spends of schematic diagram shown in Figure 1.
Fig. 4. the apparatus structure synoptic diagram of the time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao of the present invention has both.
Fig. 5. carry out polyolefin blends (PES/PEB=30/70) the time resolution result that research institute gets that is separated with the big angle part of Fig. 1 and laser light scattering instrument shown in Figure 4.(a) the time resolution image that is separated, unit is minute among the figure; (b) be the two-dimensional representation of the light distribution of this image.
Fig. 6. carry out the result of polyolefin (PEH) crystallization gained, (a) Hv image with the little angle part of Fig. 1 and laser light scattering instrument shown in Figure 4; (b) Vv image.
Fig. 7. carry out the time resolution polyolefin result that research institute gets that is separated with the little angle part of Fig. 1 and laser light scattering instrument shown in Figure 4.(a) the time resolution image (PES/PEB=50/50) that is separated, unit is minute among the figure; (b) be three-dimensional (intensity, Scattering of Vector, the time) expression of the light distribution of this image.
Reference numeral
1. laser instrument 2. diaphragms 3. optical filterings
4. polarizer 5. condensers 6. hot platforms
7. analyzer 8. screens 9. little angle signal detecting devices
10. the adjutage 12. big angle signal detectors of rotary table 11. rotary tables
13,14. camera lenses, 15. Xiao Jiao test section adjutage 16. optical tables
17. newel 19. sample cells of adjustable height pole 18. rotary tables
θ. angle
Embodiment
Embodiment 1
See also Fig. 1 and Fig. 4.Rotary table 10 is installed on the optical table 16.One side at rotary table 10 is laser instrument 1 (532 nanometers, 17 milliwatts), diaphragm 2, optical filtering 3, polarizer 4, the condenser 5 that is installed in respectively on the adjustable height pole 17, and adjustable height pole 17 is installed on the optical table 16, forms the Lights section.
Another side at rotary table 10 is a Xiao Jiao test section adjutage 15 along the incident light direction, on Xiao Jiao test section adjutage 15, analyzer 7, screen 8, little angle signal detecting device 9 is installed successively.Wherein, analyzer 7 is installed in the place ahead of rotary table 10, and screen 8 is between analyzer 7 and little angle signal detecting device 9.Xiao Jiao test section adjutage 15, analyzer 7, screen 8, little angle signal detecting device 9 are formed the Xiao Jiao test section.
The hot platform 6 of toroidal is installed on the newel 18 of rotary table 10, in the hot platform 6 of toroidal, be set with the sample cell 19 of toroidal, on the adjutage 11 of the single-revolution worktable of rotary table 10, big angle signal detector 12 is installed, (two camera lenses 13 are identical high-aperture lenses with 14 to camera lens 13 with camera lens 14, form by one group (3 convex lens and concavees lens) respectively, can receive the light of 0～60 degree angular range, carried out the processing of optical parallaxs such as achromatism, make the image of acquisition not have distortion, two back-to-back installations of camera lens), wherein camera lens 14 is adjacent with sample cell 19 with hot platform 6, is camera lens 13 between big angle signal detector 12 and the camera lens 14.The adjutage 11 of rotary table 10, rotary table, big angle signal detector 12, camera lens 13 and camera lens 14 are formed the test section, big angle.
By regulating the height of adjustable height pole 17, make the center of diaphragm 2, optical filtering 3, polarizer 4, condenser 5, Re Tai and sample cell 6, analyzer 7, screen 8, little angle signal detecting device 9, big angle signal detector 12, camera lens 13 and camera lens 14 and laser that laser instrument 1 sends at sustained height.
Behind laser process diaphragm 2, optical filtering 3, polarizer 4 and the condenser 5 that sends in the laser instrument 1, shine on the sample in hot platform 6 and the sample cell 19, the detected device of the scattered light that sends receives.Pick-up unit is divided into two parts, and we are referred to as big angle detection system and little angle detection system.
Introduce the big angle detection system earlier, as shown in Figure 2.
, form directional light and focused on the big angle signal detector 12 by camera lens 13 again through behind the camera lens 14 by the scattered light behind the sample, gathered by big angle signal detector 12.Because camera lens 14 can be collected the light of about 60 degree angular ranges, big angle signal detector 12 collects the scattered signal in the respective angles scope in can be at one time.
The big angle detection system comprises camera lens 14, and camera lens 13 and big angle signal detector 12 are installed on the adjutage 11 of rotary table.The center of rotary table 10 is on the center line of detection system, and like this, when rotation rotary table 10 rotated around rotation center, the anglec of rotation was exactly the center of big angle detection system and the angle of incident light, angle θ as shown in Figure 3.Suppose θ=45 degree, then the angle of detectable scattered light is 15～75 degree.So,, just can collect the scattered signal in 0～90 degree scope by rotation rotary table 10.
In Fig. 3, when becoming θ=45 with incident light, the detection system center line spends, and sensing range is 15～75 degree, and hot platform 6 and sample cell 19 rotations 22.5 degree can guarantee that so hot platform and sample cell can not stop scattered light.
Because the scattered light in the 60 degree angular ranges can be received simultaneously, so temporal resolution is enhanced greatly.Directly imaging on detecting device of scattered light, detection sensitivity improves greatly.Employing face town CCD can obtain the more data amount as detecting device, and data accuracy improves.
Introduce little angle detection system again.
By the imaging on screen 8 of the scattered light behind the sample, little angle signal detecting device 9 is high speed video recording equipments, the record by imaging on the screen can be got off.Increase analyzer 7 before screen, can detect Hv, the Vv image is used for the research of crystallization.Also analyzer 7 can be installed, be used for the research of the very high phase-splitting of scattered light intensity.
Carry out polyolefin blends (PES/PEB=30/70) with the big angle part of above-mentioned laser light scattering instrument and be separated time resolution result that research institute gets as shown in Figure 5; With the little angle part of above-mentioned laser light scattering instrument, analyzer 7 has been installed, the result who carries out polyolefin (PEH) crystallization gained is as shown in Figure 6; Carry out time resolution polyolefin blends (PES/PEB=50/50) research that is separated with the little angle part of above-mentioned laser light scattering instrument, analyzer 7 is not installed, the result of gained as shown in Figure 7.
Claims (10)
1. time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao has both comprises adjutage (11), big angle signal detector (12), camera lens (13), camera lens (14), Xiao Jiao test section adjutage (15), optical table (16), adjustable height pole (17), the newel (18) of rotary table, the sample cell (19) of laser instrument (1), diaphragm (2), optical filtering (3), polarizer (4), condenser (5), hot platform (6), screen (8), little angle signal detecting device (9), rotary table (10), rotary table; It is characterized in that:
One optical table (16) is equipped with laser instrument (1), diaphragm (2), optical filtering (3), polarizer (4), condenser (5), rotary table (10), Xiao Jiao test section adjutage (15) successively from the table top of optical table (16) one ends;
Single-revolution worktable (10), the center of rotary table (10) are equipped with the newel (18) of rotary table and the adjutage (11) of rotary table on rotary table (10) on the center line of detection system; On the newel (18) of rotary table, hot platform (6) is installed, is set with sample cell (19) in the hot platform (6); Camera lens (14), camera lens (13) and big angle signal detector (12) are installed on the adjutage (11) of rotary table successively, and wherein camera lens (14) is adjacent with sample cell (19) with hot platform (6);
One Xiao Jiao test section adjutage (15) is equipped with screen (8), little angle signal detecting device (9) successively on Xiao Jiao test section adjutage (15); Wherein, screen (8) is installed in the place ahead of rotary table (10);
Described hot platform and sample cell are placed in the center of rotary table; Described camera lens (14) is back-to-back installation with camera lens (13).
2. the time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao according to claim 1 has both, it is characterized in that: described on Xiao Jiao test section adjutage (15), and at the preceding analyzer (7) that is equipped with of screen (8), analyzer (7), the laser that the center of screen (8) and little angle signal detecting device (9) and laser instrument (1) send is at sustained height.
3. the time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao according to claim 1 has both is characterized in that: described hot platform and sample cell are the hydraucone shapes.
4. the time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao according to claim 1 and 2 has both is characterized in that: described Xiao Jiao test section adjutage (15) is mounted in the another side of rotary table (10) on the incident light direction.
5. the time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao according to claim 1 has both is characterized in that: described camera lens (14) is two identical wide-aperture camera lenses with camera lens (13).
6. the time resolution two-dimensional laser light scattering apparatus that has both of big angle Xiao Jiao according to claim 1 or 5, it is characterized in that: described camera lens (13), camera lens (14) by one group protruding and concavees lens form, both can collect the optical signalling of extensive angle, the image of acquisition is also undistorted.
7. the time resolution two-dimensional laser light scattering apparatus that has both of big angle Xiao Jiao according to claim 1 or 5, it is characterized in that: described camera lens (13) and camera lens (14) can receive the scattered light in 0～60 degree wide range.
8. the time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao according to claim 6 has both is characterized in that: described camera lens (13) and camera lens (14) can receive the scattered light in 0～60 degree wide range.
9. the time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao according to claim 1 has both is characterized in that: described laser instrument (1), diaphragm (2), optical filtering (3), polarizer (4), condenser (5) are mounted on the adjustable height pole (17).
10. the time resolution two-dimensional laser light scattering apparatus that big angle Xiao Jiao according to claim 1 has both is characterized in that: the laser that the center of described diaphragm (2), optical filtering (3), polarizer (4), condenser (5), hot platform (6), sample cell (19), screen (8), little angle signal detecting device (9), big angle signal detector (12), camera lens (13) and camera lens (14) and laser instrument (1) send is at sustained height.
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| CNB2005100122828A CN100460861C (en) | 2005-08-01 | 2005-08-01 | Time resolving two-dimensional laser light scattering apparatus with small and large angle |
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| CNB2005100122828A CN100460861C (en) | 2005-08-01 | 2005-08-01 | Time resolving two-dimensional laser light scattering apparatus with small and large angle |
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| CN100460861C CN100460861C (en) | 2009-02-11 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207195A (en) * | 2013-04-08 | 2013-07-17 | 中国科学技术大学 | Combined device for small-angle and wide-angle X-ray scattering and experiment test method of combined device |
| CN104931388A (en) * | 2015-02-16 | 2015-09-23 | 青岛科技大学 | Rheological in-situ online test system integrating scattering and microscopy |
| WO2020000319A1 (en) * | 2018-06-28 | 2020-01-02 | 深圳市汇顶科技股份有限公司 | Scattering angle measuring device and scattering angle measuring method |
| CN111256816A (en) * | 2018-12-03 | 2020-06-09 | 北京世纪朝阳科技发展有限公司 | Scattered light signal intensity acquisition method and device |
| US11067505B2 (en) | 2018-03-28 | 2021-07-20 | Shandong University | Small angle laser scatterometer with temperature-pressure-controllable sample cell and characterization method |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5703692A (en) * | 1995-08-03 | 1997-12-30 | Bio-Rad Laboratories, Inc. | Lens scatterometer system employing source light beam scanning means |
| CN1066538C (en) * | 1996-07-16 | 2001-05-30 | 复旦大学 | Time-resolution laser optical scattering measuring system |
| WO2004077033A1 (en) * | 2003-02-28 | 2004-09-10 | Koninklijke Philips Electronics N.V. | A scatterometer and a method for inspecting a surface |
-
2005
- 2005-08-01 CN CNB2005100122828A patent/CN100460861C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207195A (en) * | 2013-04-08 | 2013-07-17 | 中国科学技术大学 | Combined device for small-angle and wide-angle X-ray scattering and experiment test method of combined device |
| CN103207195B (en) * | 2013-04-08 | 2015-01-14 | 中国科学技术大学 | Combined device for small-angle and wide-angle X-ray scattering and experiment test method of combined device |
| CN104931388A (en) * | 2015-02-16 | 2015-09-23 | 青岛科技大学 | Rheological in-situ online test system integrating scattering and microscopy |
| US11067505B2 (en) | 2018-03-28 | 2021-07-20 | Shandong University | Small angle laser scatterometer with temperature-pressure-controllable sample cell and characterization method |
| WO2020000319A1 (en) * | 2018-06-28 | 2020-01-02 | 深圳市汇顶科技股份有限公司 | Scattering angle measuring device and scattering angle measuring method |
| CN111256816A (en) * | 2018-12-03 | 2020-06-09 | 北京世纪朝阳科技发展有限公司 | Scattered light signal intensity acquisition method and device |
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