CN1786684A - Spectrophotometer with controllable temp. sample chamber - Google Patents
Spectrophotometer with controllable temp. sample chamber Download PDFInfo
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- CN1786684A CN1786684A CN 200510061473 CN200510061473A CN1786684A CN 1786684 A CN1786684 A CN 1786684A CN 200510061473 CN200510061473 CN 200510061473 CN 200510061473 A CN200510061473 A CN 200510061473A CN 1786684 A CN1786684 A CN 1786684A
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Abstract
The invention discloses sample cell temperature controllable spectrophotometer. The wide spectrum light beam emitted from the light source is changed into one light wavelength light beam through binary modulation plate, monochromator, filter, and polarizer, and changed into detecting light shoot into photoelectric sensor through heating device. The heating device is fixed on rotatable specimen stage. The specimen stage is connected to detector tumbler by rotating shaft. The photoelectric sensor is at the other side of the tumbler. The tumbler is drove by stepper motor. Photometer is controlled by controller. The invention solves the problem that spectrophotometer cannot measure optics sample transmission reflectance characteristics at a certain constancy of temperature; or the transmission reflectance characteristics change with the temperature. It can apply in optical element with high using temperature demand, such as optical thin film transmission reflectance ratio measuring.
Description
Technical field
The present invention relates to the spectrophotometer of a kind of sample chamber Controllable Temperature.
Background technology
The transmissivity of optical element or reflectivity can be measured by spectrophotometer.Spectrophotometer is made up of lamp source, monochromator and detector etc.During work, the light beam that light source sends becomes single wavelength light behind monochromator, and the luminous energy after being reflected by optical element or by optical element by detector measurement list wavelength light then obtains optical element transmissivity or reflectivity.
The transmissivity of general optical element and reflectivity are considered to constant.This mainly is because general optical element uses at normal temperatures.Therefore out-of-control during the temperature of optical sample in spectrophotometer, be to change along with the variation of environment temperature.When the serviceability temperature of optical element and environment temperature differ big, its transmissivity and reflectivity will no longer be constant but in actual applications.Therefore particularly for some optical thin films, spectral-transmission favtor and the spectral-transmission favtor under the high temperature under the normal temperature have very big difference, need measure saturating, reflectivity under the actual serviceability temperature for these optical thin films that at high temperature use.In addition for some novel optical elements, as liquid crystal optical device etc., they saturating, reflectivity is responsive to variation of temperature, therefore need under some temperature, measure sample is constant.These optical properties under different temperatures can't be measured with conventional spectrophotometer.
Summary of the invention
The spectrophotometer that the purpose of this invention is to provide a kind of sample chamber Controllable Temperature.
The spectrophotometer of sample chamber Controllable Temperature: the broad-spectrum beam that sends from the lamp source, become monochromatic light wavelength light beam through double modulation dish, monochromator, optical filter, polarizer, become detection light through heating arrangement and inject photodetector; Heating arrangement is positioned on the rotatable sample stage, and sample stage links to each other with the detector pivoted arm by rotating shaft, and photodetector is at the opposite side of detector pivoted arm, and the detector pivoted arm is by step motor drive, and photometer is controlled by controller; Heating arrangement has the heating arrangement chassis, on the heating arrangement chassis, be connected with ceramic gasket, heated base in turn, be provided with heating tube, thermopair in heated base, ceramic gasket, the heated base outside are provided with heat shield, and thermopair, heating tube link to each other with heating controller respectively.
The present invention utilizes a heating arrangement to measure the relation curve of optical element between transmissivity, reflectivity and wavelength under different temperatures, different incidence angles degree, the different polarization state.Compare with existing spectrophotometer, when the invention solves actual use of optical element under high temperature uses thoroughly, the difficult problem of albedo measurement.In addition for some novel optical elements, as liquid crystal optical device etc., they saturating, reflectivity is responsive to variation of temperature, therefore need under some temperature, measure sample is constant.These optical properties under different temperatures can't be measured with conventional spectrophotometer.
Description of drawings
Fig. 1 is the spectrophotometer structural representation of sample chamber Controllable Temperature;
Fig. 2 is a thermal plafform configuration synoptic diagram of the present invention;
Fig. 3 is a heating control circuit synoptic diagram of the present invention;
Fig. 4 is a sonde rotary structural scheme of mechanism of the present invention;
Fig. 5 is a detector signal treatment circuit synoptic diagram of the present invention.
Embodiment
As shown in Figure 1, 2, the broad-spectrum beam that sends from lamp source 1 becomes monochromatic light wavelength light beam through double modulation dish 2, monochromator 3, optical filter 4, polarizer 5, becomes detection light through heating arrangement 9 and injects photodetector 12; Heating arrangement 9 is positioned on the rotatable sample stage 10, and sample stage 10 links to each other with detector pivoted arm 14 by rotating shaft, and photodetector 12 is at the opposite side of detector pivoted arm 14, and detector pivoted arm 14 drives by stepper motor 13, and photometer is controlled by controller; Heating arrangement 9 has heating arrangement chassis 9.4, on heating arrangement chassis 9.4, be connected with ceramic gasket 9.3, heated base 9.2 in turn, in heated base 9.2, be provided with heating tube 9.5, thermopair 9.6, ceramic gasket 9.3, heated base 9.2 outsides are provided with heat shield 9.1, and thermopair 9.6, heating tube 9.5 link to each other with heating controller 19 respectively.Photodetector 12 is provided with photomultiplier 12.1, ead sulfide detector 12.2 and integrating sphere 12.3.Controller is provided with probe control module 16 and system control module 15, and system control module 15 links to each other with computing machine 18 through I/O card 17.Lamp source 1 has metal halogen tungsten thing lamp 1.1 and deuterium lamp 1.2.
As shown in Figure 3, the transformer 19.1 that heating controller 19 connects successively, silicon controlled power modulation module 19.8, heating tube 19.7, thermopair 19.2, advance signal processing module 19.6, microprocessor module 19.5, RS232 mouth 19.4, microprocessor module 19.5 links to each other with nixie display 19.3.
As shown in Figure 4, photodetector 12 has bedplate 12.4, on bedplate 12.4, be provided with stepper motor 13, drive worm screw 13.3 by stepper motor 13, worm screw 13.3 is fixed on the worm screw seat 13.4, and worm screw 13.3 is joined with worm gear 13.2, worm gear 13.2 is fixed on worm gear seat 13.1, worm screw seat 13.4 worm gear seats 13.1 are separately fixed on the bedplate 12.4, and worm gear 13.2 drives pivoted arm 14 and rotates, and pivoted arm 14 opposite sides are provided with photodetector 12.
As shown in Figure 5, probe control module 16 has high-pressure modular 12.4, photomultiplier 12.1, advance signal processing module 16.8, signal selection module 16.7, program control amplification module 16.6, AD acquisition module 16.5, microprocessor module 16.4, the RS232 mouth 16.3 that connects successively, microprocessor module 16.4 is connected with modulation module 16.2, AD acquisition module 16.5 in turn, and microprocessor module 16.4 is connected with thermostatic control module 12.3, ead sulfide detector 12.2, advance signal processing module 16.1, signal selection module 16.7 in turn.
Hereinafter with reference to accompanying drawing, work control procedure of the present invention is described.
Lamp source 1 comprises two light emitting sources: metal halogen tungsten lamp 1.1, a deuterium lamp 1.2 cover this spectrophotometric whole measure spectrum.When being operated near infrared and visible region, beam splitting arrangement 1.3 stops the 1.1 emergent light outgoing of metal halogen tungsten lamp simultaneously from the emergent light of deuterium lamp 1.2; When being operated in ultraviolet region, beam splitting arrangement 1.3 stops deuterium lamp 1.2 emergent light outgoing simultaneously from the emergent light of metal halogen tungsten lamp 1.1.The light source emergent light is through double modulation dish 2 modulation, and monochromator 3 is selected, and through 4 filtering of color chips rotating disk, and is biased into polarized light by 5 of polarizers, incides sample 8.Sample 8 is positioned over a certain constant temperature of heating maintenance on the heating arrangement 9; Heating arrangement 9 is fixed on the rotatable sample stage 10 simultaneously, regulates control incident light incident angle.Light beam transmitted light beam 11 and folded light beam 7 by sample are collected by the integrating sphere in the photodetector 12 12.3, photomultiplier 12.1 is received in the light signal of ultraviolet and visible region and is converted into electric signal, ead sulfide detector 12.2 is received in the light signal of near infrared region and is converted into electric signal, and this electric signal is converted into digital signal through probe control module 16 and sends into computing machine 18.Remove sample 8, directly the single wavelength light beam 6 that comes out from monochromator is surveyed to collect at the detector of zones of different by corresponding work and is converted into digital signal and sends into computing machine 18.18 pairs of input signals of computing machine are handled, and the light intensity of folded light beam 7 obtains the reflectivity of sample 8 divided by the light intensity of single wavelength light beam 6; The light intensity of transmitted light 11 obtains the transmissivity of sample 8 divided by the light intensity of single wavelength light 6.Obtain the relation curve between optical element transmissivity, reflectivity and the wavelength under different temperatures, different incidence angles degree, the different polarization state at last.The computer control whole test process comprises that light source selects, the monochromator conversion, and optical filter is selected, and the polarization direction is regulated, the control of heating arrangement temperature, the sample stage angular adjustment, the position adjustments of photodetector and selection, and data processing is equal to the step and carries out.
Heated base 9.2 in the heating arrangement 9 is a copper billet, the centre through hole passes through test beams, heated base 9.2 back sides are that annular groove is used to place circular heating tube 9.5, and circular heating tube 9.5 one sides are close to heated base 9.2 copper billets, and heated base is heated up rapidly.Sample 8 usefulness spring leafs are fixed on heated base 9.2 fronts, thermopair 9.6 probes go deep into heated base 9.2 test heated base heating-up temperatures from the side, circular heating tube 9.5, thermopair 9.6 form the temperature control loop with heating controller 19, a certain constant temperature control is spent to Celsius 250 from room temperature.Wherein by proofreading and correct the temperature difference of sample 8 and heated base 9.2, the temperature of heating controller 19 control samples 8.Heated base 9.2 links to each other with heating arrangement chassis 9.4 by ceramic gasket 9.3, plays heat-blocking action.Whole heating arrangement 9 is fixedly mounted on the specimen rotating holder 10 by heating arrangement chassis 9.4.Whole in addition heating arrangement 9 outer covers one heat shield 9.1, heat shield 9.1 hollow plug asbestos make heating arrangement 9 and sample chamber isolated, in case the heat that heating arrangement 9 produces damages the sample chamber miscellaneous part.Wherein heating tube 9.5 centers are insulating material, and stainless steel outer packed material, interlayer are the resistance heating wire, not only play heating but also make the resistance heating wire play insulating effect each other.This heating tube is operated under the safe voltage scope, and is safe and reliable.
The circuit of constant temperature heating device 9 and control procedure are used for silicon controlled power modulation module NZK01 (19.8) is normal for changing the 220V alternating current input power supplying into the 42V direct-current input power supplying by transformer B1 (19.1).Silicon controlled power modulation module NZK01 (19.8) is controlled by microprocessor module MSP202 (19.5) by pin 4-20mA IN+ and 4-20mA IN-.Set a certain temperature controlling signal and input to microprocessor module MSP202 (19.5) by computing machine 18, start heating tube JR400 (19.7) heating by silicon controlled power modulation module NZK01 (19.8).In the heating process, thermopair K400 (19.7) surveys heating-up temperature constantly and is converted into electric signal, be sent to advance signal processing module AMP203 (19.6) for gathering, and feed back in microprocessor module MSP202 (19.5) by OUT+ and OUT-, thereby the output power of control heating tube JR400 (19.7), regulate the sample heating-up temperature, and keep constant temperature.Microprocessor passes through CLK, DATA, three pin output temperatures of GND information, and goes up demonstration sample temperature at nixie display LED04 (19.3).This processor receives image data, and the gained forms data is 3 bytes, is sent to computing machine 18 by RS232 mouth COM2 (19.4) and handles.
Whole sonde rotary mechanism is fixed on the bedplate 12.4, and rotating mechanism drives worm screws 13.3 by stepper motor 13, worm gear 13.2, thus drive revoliving arm 14 around sample stage 10 rotations, make photodetector 12 survey reflected light 7 and transmitted light 11 light intensity.Adopt lambert's body diffusion integrating sphere efficiently, cooperate the turnover light path, and photomultiplier 12.1 and ead sulfide detector 12.2 constitute a broad spectrum (ultraviolet/visible/near infrared) and incident light are changed insensitive Photodetection system among a small circle in incident direction.The size of this integrating sphere through repetition test, adopts the integrating sphere effect of diameter little 40 to 150mm best with to survey the photosignal power obtain closely related, has not only guaranteed signal intensity but also has guaranteed the insensitivity of incident angle of light.
The circuit and the control procedure of photodetector 12 are as described below, the wavelength coverage of ead sulfide detector PBS (12.2) is made as 800～1500nm, thermostatic control module HTK201 (12.3) is controlled by microprocessor module MSP201 (16.4) by pin A2, A3, thereby working temperature and the bias voltage of accurately controlling PBS are constant, the signal that PBS produces is sent to advance signal processing module AMP202 (16.1) and amplifies, and amplifying signal is selected module XHK201 (16.7) through pin OUT2 input signal.The wavelength coverage of photomultiplier PMT (12.1) is made as 200～800nm; microprocessor module MSP201 (16.4) is by high pressure amplitude and the break-make of pin A0, A1 control high-pressure modular WG956 (12.4); thereby accurately control the working voltage of PMT; when opening the sample chamber door; high pressure cuts off automatically, effectively protects PMT.The signal that PMT produces is sent to advance signal processing module AMP202 (16.8) and amplifies, and amplifying signal is selected module XHK201 (16.7) through pin OUT1 input signal.Signal selection module XHK201 (16.7) is selected by microprocessor module MSP201 (16.4) control by D6, D7, three tunnel effective input signal: IN1 (PMT), IN2 (PBS), IN3 (GND), the data of being gathered when selecting IN3 can return to zero to circuit.Program control amplification module CKA201 (16.6) contains 6 road control line D (0 ~ 5), and programme-controlled gain is respectively 1,2,4,8,16,32,64,128,256, by programme-controlled gain to main signal, thus the acquisition precision of raising AD acquisition module AD201 (16.5).When gathering main signal, in order to deduct instant background at any time, present embodiment has designed the structure of coaxial double modulation dish 2 especially, the number of teeth is respectively 6 and 12, the double wedge phase place of 6 fluted discs is corresponding to main signal, and the groove phase place is corresponding to the bias light signal, and AD acquisition module AD201 (16.5) is sent in the light lotus root pulse of 6 fluted discs after treatment, gather main signal during pulse high level, gather the bias light signal during pulses low.The double wedge phase place of 12 fluted discs just is centered at the phase place of main signal or bias light signal, and high double wedge light lotus root pulse AD-START directly controls AD and gathers sequential, and high level is opened and gathered, and low level is closed collection.Double modulation dish signals collecting is finished by chopper wheel optoelectronic switch 1 and chopper wheel optoelectronic switch 2 respectively.Microprocessor module MSP201 (16.4) rewrites the AD acquisition rate by data line D (0 ~ 7), is defaulted as 40us/ time.Disturb in order effectively to suppress power frequency, modulating frequency is elected 50 hertz as.The data that AD acquisition module AD201 (16.5) gathers directly are sent to the P5 mouth of microprocessor module MSP201 (16.4), this processor is 16 risc instruction set MCU structures, receive image data and carry out digital anti-interference filtration and processing, data after the processing (16 system) are carried out binary-coded decimal conversion and compression again, the gained forms data is 3 bytes, is sent to computing machine 18 by RS232 mouth COM1 (16.3) and handles.
Above-mentioned only is illustrative, but not is restricted person.Anyly do not break away from spirit of the present invention and category, and, all should be contained in the claim scope of the present invention its equivalent modifications of carrying out or change.
Claims (7)
1. the spectrophotometer of a sample chamber Controllable Temperature, it is characterized in that the broad-spectrum beam that sends from lamp source (1), become monochromatic light wavelength light beam (6) through double modulation dish (2), monochromator (3), optical filter (4), polarizer (5), become detection light through heating arrangement (9) and inject photodetector (12); Whole heating arrangement (9) is positioned on the rotatable sample stage (10), sample stage (10) links to each other with detector pivoted arm (14) by rotating shaft, photodetector (12) is at the opposite side of detector pivoted arm (14), detector pivoted arm (14) drives by stepper motor (13), and photometer is controlled by controller; Heating arrangement (9) has heating arrangement chassis (9.4), on heating arrangement chassis (9.4), be connected with ceramic gasket (9.3), heated base (9.2) in turn, in heated base (9.2), be provided with heating tube (9.5), thermopair (9.6), ceramic gasket (9.3), heated base (9.2) outside are provided with heat shield (9.1), and thermopair (9.6), heating tube (9.5) link to each other with heating controller (19) respectively.
2. the spectrophotometer of a kind of sample chamber according to claim 1 Controllable Temperature, it is characterized in that described photodetector (12) has bedplate (12.4), on bedplate (12.4), be provided with stepper motor (13), drive worm screw (13.3) by stepper motor (13), worm screw (13.3) is fixed on the worm screw seat (13.4), worm screw (13.3) is joined with worm gear (13.2), worm gear (13.2) is fixed on worm gear seat (13.1), worm screw seat (13.4) is separately fixed on the bedplate (12.4) with worm gear seat (13.1), worm gear (13.2) drives pivoted arm (14) and rotates, and pivoted arm (14) opposite side is provided with photodetector (12).
3. the spectrophotometer of a kind of sample chamber according to claim 1 and 2 Controllable Temperature is characterized in that described photodetector (12) is provided with photomultiplier (12.1), ead sulfide detector (12.2) and integrating sphere (12.3).
4. the spectrophotometer of a kind of sample chamber according to claim 1 Controllable Temperature, it is characterized in that described controller is provided with probe control module (16) and system control module (15), system control module (15) links to each other with computing machine (18) through I/O card (17).
5. according to the spectrophotometer of claim 1 or 4 described a kind of sample chamber Controllable Temperature, it is characterized in that described probe control module (16) has the high-pressure modular (12.4) that connects successively, photomultiplier (12.1), advance signal processing module (16.8), signal selection module (16.7), program control amplification module (16.6), AD acquisition module (16.5), microprocessor module (16.4), RS232 mouth (16.3), microprocessor module (16.4) is connected with modulation module (16.2) in turn, AD acquisition module (16.5), microprocessor module (16.4) is connected with thermostatic control module (12.3) in turn, ead sulfide detector (12.2), advance signal processing module (16.1), signal selection module (16.7).
6. the spectrophotometer of a kind of sample chamber according to claim 1 Controllable Temperature, it is characterized in that transformer (19.1), silicon controlled power modulation module (19.8), heating tube (19.7), thermopair (19.2), advance signal processing module (19.6), microprocessor module (19.5), RS232 mouth (19.4) that described heating controller (19) connects successively, microprocessor module (19.5) links to each other with nixie display (19.3).
7. the spectrophotometer of a kind of sample chamber according to claim 1 Controllable Temperature is characterized in that described lamp source (1) has metal halogen tungsten thing lamp (1.1) and deuterium lamp (1.2).
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| CN 200510061473 CN100554936C (en) | 2005-11-08 | 2005-11-08 | The spectrophotometer of sample chamber Controllable Temperature |
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| CN 200510061473 CN100554936C (en) | 2005-11-08 | 2005-11-08 | The spectrophotometer of sample chamber Controllable Temperature |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102426129A (en) * | 2011-12-21 | 2012-04-25 | 中国计量学院 | Sample heating device used in integrating-sphere reflectivity measurement |
| CN105928906A (en) * | 2016-06-20 | 2016-09-07 | 中国工程物理研究院流体物理研究所 | Dynamic measuring system for material reflectivity changing with temperature and measuring method |
| CN109856071A (en) * | 2019-03-11 | 2019-06-07 | 西北核技术研究所 | A kind of spectrum on line diagnostic method and device |
| CN110044490A (en) * | 2019-05-21 | 2019-07-23 | 上海航天测控通信研究所 | A kind of fast switch type emissivity measurement device and measurement method |
| CN110118645A (en) * | 2019-04-19 | 2019-08-13 | 西北核技术研究所 | A kind of optical property integrated evaluating method of semielliptical reflecting surface |
| CN111122451A (en) * | 2020-01-16 | 2020-05-08 | 青海省药品检验检测院 | Volatile oil separation and determination device |
| CN112285042A (en) * | 2020-10-13 | 2021-01-29 | 上海中科航谱光电技术有限公司 | Spectrum detector and method for measuring transmission spectrum characteristics of optical material |
| CN113533229A (en) * | 2021-06-25 | 2021-10-22 | 华东师范大学 | Portable temperature control device of spectrophotometer |
| CN109781671B (en) * | 2019-03-11 | 2021-11-05 | 西北核技术研究所 | Transmission rate on-line test method and device |
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- 2005-11-08 CN CN 200510061473 patent/CN100554936C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102426129A (en) * | 2011-12-21 | 2012-04-25 | 中国计量学院 | Sample heating device used in integrating-sphere reflectivity measurement |
| CN105928906A (en) * | 2016-06-20 | 2016-09-07 | 中国工程物理研究院流体物理研究所 | Dynamic measuring system for material reflectivity changing with temperature and measuring method |
| CN105928906B (en) * | 2016-06-20 | 2018-09-18 | 中国工程物理研究院流体物理研究所 | A kind of material reflectance dynamic measurement system varied with temperature and measurement method |
| CN109856071A (en) * | 2019-03-11 | 2019-06-07 | 西北核技术研究所 | A kind of spectrum on line diagnostic method and device |
| CN109781671B (en) * | 2019-03-11 | 2021-11-05 | 西北核技术研究所 | Transmission rate on-line test method and device |
| CN110118645A (en) * | 2019-04-19 | 2019-08-13 | 西北核技术研究所 | A kind of optical property integrated evaluating method of semielliptical reflecting surface |
| CN110044490A (en) * | 2019-05-21 | 2019-07-23 | 上海航天测控通信研究所 | A kind of fast switch type emissivity measurement device and measurement method |
| CN110044490B (en) * | 2019-05-21 | 2021-07-23 | 上海航天测控通信研究所 | Fast switching type emissivity measuring device and measuring method |
| CN111122451A (en) * | 2020-01-16 | 2020-05-08 | 青海省药品检验检测院 | Volatile oil separation and determination device |
| CN112285042A (en) * | 2020-10-13 | 2021-01-29 | 上海中科航谱光电技术有限公司 | Spectrum detector and method for measuring transmission spectrum characteristics of optical material |
| CN113533229A (en) * | 2021-06-25 | 2021-10-22 | 华东师范大学 | Portable temperature control device of spectrophotometer |
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