CN208818635U - The Peace Park detection device in situ for having laser heating - Google Patents
The Peace Park detection device in situ for having laser heating Download PDFInfo
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- CN208818635U CN208818635U CN201821595015.7U CN201821595015U CN208818635U CN 208818635 U CN208818635 U CN 208818635U CN 201821595015 U CN201821595015 U CN 201821595015U CN 208818635 U CN208818635 U CN 208818635U
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Abstract
The utility model belongs to Peace Park characterization technique in situ field, in particular to a kind of Peace Park detection device in situ for having laser heating.Including sample stage, laser heating and temperature-controlling system and air-channel system, wherein sample stage includes sequentially connected sample cell, adjustment mechanism and cabinet, optical element is equipped in cabinet, laser heating is with temperature-controlling system for emitting in laser to cabinet, laser is turned to and is focused on the sample in sample cell by optical element, laser heating and temperature control are carried out to sample, air-channel system is for vacuumizing sample cell and to provide the atmosphere of different pressures in sample cell.The utility model is small in size, changes conveniently, sample position can not only be adjusted in x-y plane, moreover it is possible to rotate 360 ° to sample；The utility model can in-situ characterization surface texture at different temperatures and pressures variation.
Description
Technical field
The utility model belongs to Peace Park characterization technique in situ field, in particular to a kind of to have what laser heated
Peace Park detection device in situ.
Background technique
Under the conditions of real reaction, the class for carrying out that in-situ characterization is a meaningful but great challenge is reacted catalysis
Topic, especially in situ detection is just more difficult for heterogeneous catalytic reaction, because reaction occurs in catalyst surface in heterogeneous catalysis,
In situ detection means to avoid the body phase signals interference of catalyst, reactants and products to identify surface signal.
Vibrational spectrum, such as infrared and Raman spectrum are commonly used in catalyticing research, to characterize intermolecular interaction, but it is red
Outer and Raman spectrum has response to body phase and surface molecular, requires consideration for how to extract adsorption point in situ in detection
The signal of son, this can undoubtedly be such that experiment becomes more sophisticated.
Peace Park has unique interface selective, this is that it has as a kind of second nonlinear optic means
Not in the sharpest edges of line spectrum (FT-IR & FT-RAMAN spectra).This characteristic is also substantially increased to interfacial molecular detection
Sensitivity.Foremost example is exactly the vibrational spectrum for the air/water interface that Shen Yuan earth et al. obtains, this spectrum is by several
The signal that water in molecular layers thick provides.At past more than 20 years, since it is with special interface sensibility, the side SFG
Method is by Successful utilization into each Interface Study, including gas-solid interface, gas-liquid interface and liquid-solid boundary, and shows to get over
To be more widely applied.
Application is mostly model catalyst system early stage Peace Park is in catalysis, will from Yeganeh in 2006 et al.
After total internal reflection method is used for Peace Park, just occurs the research to powder catalytic material successively.But due to total internal reflection
The device of Peace Park is relative complex, is extremely difficult to the high-temperature and high-pressure conditions of practical catalyst system, and surface species concentration
The problems such as low, dusty material is to the inhomogeneity of the scattering of signal, powder surface, the Peace Park signal-to-noise ratio made is very
Difference.This is also why Peace Park fails sufficiently to show its unique interface selective advantage in catalytic field, is being answered
With the paces that can could not also keep up with Industrial Catalysis and material science development.Therefore, practical Peace Park is designed and developed
Device improves experimental method, can let us preferably solved the problems, such as with Peace Park more, more especially urge
The problem of changing forward position and material science forward position.
Utility model content
In view of the above-mentioned problems, the purpose of this utility model is to provide a kind of original position for having laser heating and frequency vibration light
Spectrum detection device, it is relative complex to solve existing total internal reflection Peace Park device, it is extremely difficult to practical catalyst system
High-temperature and high-pressure conditions, and because surface species concentration is low, dusty material is to scattering, the inhomogeneity on powder surface of signal etc., make
The very poor problem of obtained Peace Park signal-to-noise ratio.
To achieve the above object, the utility model adopts the following technical scheme:
A kind of Peace Park detection device in situ having laser heating, including the heating of sample stage, laser and temperature control
System and air-channel system, wherein sample stage includes sequentially connected sample cell, adjustment mechanism and cabinet, is equipped with light in the cabinet
Element is learned, with temperature-controlling system for emitting in laser to the cabinet, the optical element is used for will be described for the laser heating
The laser of laser heating and temperature-controlling system transmitting is turned to and is focused on the sample in sample cell, carries out laser heating to sample,
The temperature of the laser heating and temperature-controlling system control sample, the air-channel system is for vacuumizing sample cell and being sample cell
It is interior that the atmosphere of different pressures is provided.
The sample cell includes sample cell shell, preceding window and rear window, and wherein sample cell shell is connected to the adjustment
In mechanism, the front and back ends of the sample cell shell are respectively equipped with preceding window and rear window, and the laser heating is sent out with temperature-controlling system
The laser penetrated after window enter the sample cell in, be connected on the sample cell shell connect with the air-channel system into
Tracheae and escape pipe.
The sample cell shell includes the preceding outer wall and rear outer wall being tightly connected, and the preceding window is embedded at the preceding outer wall
It in the groove being equipped with, is sealed between the preceding window and the preceding outer wall equipped with O-ring seal, and solid by front pressuring plate
It is fixed, be equipped with front pad between the front pressuring plate and the preceding outer wall, it is described after window be embedded at it is described after outer wall be equipped with it is recessed
In slot, it is sealed between window and the rear outer wall equipped with O-ring seal after described, and fixed by rear fender, after described
Rear gasket is equipped between pressing plate and the rear outer wall.
Cooling-water duct is equipped with after described in outer wall, the both ends of the cooling-water duct are respectively and for inflow and outflow two
A cooling water pipe connection.
The adjustment mechanism includes adjustment frame, fixed platform, two-dimensional movement platform, L-type fixed station and turntable, wherein adjusting
Whole frame installation is on the stationary platform and installation site is adjustable, and the fixed platform is fixedly connected with two-dimensional movement platform, and described two
Dimension mobile platform is placed on L-type fixed station, and the L-type fixed station is connect with turntable, and the turntable is fixed on the cabinet
On, the sample cell is mounted on the adjustment frame.
The optical element includes lens and reflecting mirror, and wherein reflecting mirror is put with 45 ° of incidence angles and adds the laser
Heat is on the laser reflection to the lens of temperature-controlling system transmitting, and the lens are co-axially mounted with the sample, and being used for will be described
The laser of reflecting mirror transmitting focuses, and the laser facula at the sample back side is adjusted to suitable size.
Laser heating and temperature-controlling system include laser, TTL signal generator, computer and temperature measurer, wherein laser
Device is connect by TTL signal generator with computer, and the laser is for emitting laser to the optical element；The thermometric
Instrument is connect by cable with the computer, and the temperature measurer is used to detect the temperature of sample in the sample cell, and will be measured
Temperature is transmitted in computer, and the temperature signal that the computer is detected according to the temperature measurer passes through described in the control of PID adjusting method
The output power of laser.
The temperature measurer is the thermocouple contacted with the sample edge, the thermocouple by temperature acquisition card with it is described
Computer connection；Or the temperature measurer is the infrared radiation thermometer being set on the outside of the sample cell, the infrared radiation thermometer passes through
Cable is connect with the computer.
The air-channel system includes gas chamber and the gas source and molecular pump that connect with the gas chamber, and the gas chamber passes through air inlet pipe
Road and gas exhaust piping are connected to the sample cell.
Pressure detector and residual gas analyzer are connected on the gas chamber
Compared with prior art, the utility model have the following advantages that and the utility model has the advantages that
1. non-contact laser heats.The utility model guarantees that only sample is in maximum temperature in sample cell when heating, keeps away
Exempt from the interference of side reaction, and heating efficiency is high；
2. Non-contact Infrared Temperature Measurement.The utility model can directly measure sample table by window using infrared radiation thermometer
Face temperature, is not contacted with sample, and will not influence the light path of Peace Park；
3. program intelligent temperature control.The utility model controls the output of temperature and laser using multistage programming and pid parameter
Power may be implemented the mild thermostatic process of lifting/lowering, and can control lifting/lowering temperature rate during lifting/lowering temperature；
4. features simple structure.The utility model is small in size, changes conveniently, sample position can not only be adjusted in x-y plane,
Sample can also be rotated 360 °；
5. Peace Park detection in situ.The utility model can in-situ characterization surface texture at different temperatures and pressures
Variation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model；
Fig. 2 is the structural schematic diagram of sample stage in the utility model；
Fig. 3 is the exploded view of sample stage in the utility model；
Fig. 4 is the SFG spectrum of lauryl sodium sulfate on z-cut alpha-quartz crystal in the utility model embodiment one；
Fig. 5 is that different temperatures is annealed to lauryl sodium sulfate on z-cut alpha-quartz crystal in the utility model embodiment one
The influence of SFG spectrum, (a) SSP (letter successively represents with frequency light as S-polarization, visible light be S-polarization, infrared light as P polarization),
(b) PPP (letter successively represents with frequency light as P polarization, visible light be P polarization, infrared light as P polarization)；
Fig. 6 is that Pt nano particle is added dropwise in the utility model embodiment two on z-cut alpha-quartz crystal, in 1.17atm CO
SFG spectrum in atmosphere；
Fig. 7 is that Pt nano particle is added dropwise in the utility model embodiment two on z-cut alpha-quartz crystal, when different CO pressure
SFG spectrum, SSP spectrum when 6 ° of (a), (b) 36 ° when SSP spectrum.
In figure: 1 is preceding window, and 2 be sample, and 3 be rear window, and 4 be front pad, and 5 be front pressuring plate, and 6 be preceding outer wall, and 7 be O-shaped
Sealing ring, 8 be escape pipe, and 9 be air inlet pipe, and 10 be cooling water pipe, and 11 be adjustment frame, and 12 be fixed platform, and 13 be two-dimensional movement
Platform, 14 be turntable, and 15 be pedestal, and 16 be lens, and 17 be reflecting mirror, and 18 be rear outer wall, and 19 be rear gasket, 20 be after press
Plate, 21 be L-type fixed station, and 22 be rear cover, and 23 be unthreaded hole, and 24 be sample cell, and 25 be adjustment mechanism, and 26 be optical element, and 27 are
Cabinet, 28 be pressure detector, and 29 be gas source, and 30 be molecular pump, and 31 be residual gas analyzer, and 32 be laser, and 33 be TTL
Signal generator, 34 be thermocouple, and 35 be temperature acquisition card, and 36 be computer, and 37 be infrared radiation thermometer, and 38 be gas chamber, and M is infrared
Light, N are visible light, and D is and frequency light.
Specific embodiment
In order to keep the purpose of this utility model, technical solution and advantage clearer, with reference to the accompanying drawing and it is embodied
The utility model is described in detail in example.
As shown in Figure 1, a kind of Peace Park detection device in situ for having laser heating provided by the utility model,
Including sample stage, laser heating and temperature-controlling system and air-channel system, wherein sample stage includes sequentially connected sample cell 24, adjustment
Mechanism 25 and cabinet 27, cabinet 27 is interior to be equipped with optical element 26, and laser heating is with temperature-controlling system for emitting laser to cabinet 27
Interior, optical element 26 is used to turn to and focus to the sample 2 in sample cell 24 for laser, carries out laser heating to sample 2, swashs
The temperature of light heating and temperature-controlling system control sample 2, air-channel system are used to vacuumize sample cell 24 and to mention in sample cell 24
For the atmosphere of different pressures.
As Figure 2-3, sample cell 24 includes sample cell shell, preceding window 1 and rear window 3, and sample cell shell is connected to
On adjustment mechanism 25, the front and back ends of sample cell shell are respectively equipped with preceding window 1 and rear window 3, and laser heating is sent out with temperature-controlling system
The laser penetrated window 3 after enters in sample cell 24, and the air inlet pipe 9 connecting with air-channel system is connected on sample cell shell and is gone out
Tracheae 8.
Further, sample cell shell includes the preceding outer wall 6 and rear outer wall 18 being tightly connected, and preceding window 1 is outer before being embedded at
It is in groove that wall 6 is equipped with and fixed by front pressuring plate 5, be equipped with front pad 4 between front pressuring plate 5 and preceding window 1, preceding window 1 with
O-ring seal 7 is equipped between preceding outer wall 6.Window 3 is embedded in the groove that rear outer wall 18 is equipped with and by rear fender 20 afterwards
It is fixed, it is equipped with O-ring seal 7 between rear window 3 and rear outer wall 18, rear gasket 19 is equipped between rear fender 20 and rear window 3.Afterwards
Cooling-water duct is equipped in outer wall 18, the both ends of cooling-water duct connect with two cooling water pipes 10 for inflow and outflow respectively
It connects.Forward and backward outer wall and forward and backward pressing plate are all made of stainless steel material, and front pad 4 and rear gasket 19 use Teflon material.
Adjustment mechanism 25 includes adjustment frame 11, fixed platform 12, two-dimensional movement platform 13, L-type fixed station 21 and turntable
14, wherein adjustment frame 11 is mounted in fixed platform 12 and installation site is adjustable, and fixed platform 12 and two-dimensional movement platform 13 are solid
Fixed connection, two-dimensional movement platform 13 are placed on L-type fixed station 21, and L-type fixed station 21 is connect with turntable 14, and turntable 14 is fixed
On cabinet 27, sample cell 24 is mounted on adjustment frame 11.Two-dimensional movement platform 13 is for driving sample cell 24 in X-Y plane
Mobile, turntable 14 is for driving sample cell 24 to rotate around 360 ° of Y-axis.
Optical element 26 includes lens 16 and reflecting mirror 17, and wherein reflecting mirror 17 is put with 45 ° of incidence angles and adds laser
Heat is on the laser reflection to lens 16 of temperature-controlling system transmitting, and lens 16 are co-axially mounted with sample 2, for emitting reflecting mirror 17
Laser focus, the laser facula at 2 back side of sample is adjusted to suitable size.
As shown in Figure 1, laser heating and temperature-controlling system include laser 32, TTL signal generator 33, computer 36 and thermometric
Instrument, wherein laser 32 is connect by TTL signal generator 33 with computer 36, and laser 32 is for emitting laser to optical element
On 26；Temperature measurer is connect by cable with computer 36, temperature of the temperature measurer for sample 2 in test sample pond 24, and will be surveyed
It obtains temperature to be transmitted in computer 36, the temperature signal that computer 36 is detected according to temperature measurer controls described sharp by PID adjusting method
The output power of light device 32.
The thermocouple 34 with 2 EDGE CONTACT of sample can be used in temperature measurer, and thermocouple 34 passes through temperature acquisition card 35 and computer
36 connections；Or the infrared radiation thermometer 37 for being set to 24 outside of sample cell can be used in temperature measurer, infrared radiation thermometer 37 passes through cable
It is connect with computer 36.
Air-channel system includes gas chamber 38 and the gas source connecting with gas chamber 38 29 and molecular pump 30, and gas chamber 38 passes through air inlet pipeline
It connect with the air inlet pipe 9 of sample cell 24, is connect by gas exhaust piping with the escape pipe 8 of sample cell 24.It is also connected on gas chamber 38
Pressure detector 28 and residual gas analyzer 31.
The working principle of the utility model is:
When detection, a branch of adjustable broadband infrared light of central wavelength and a branch of narrowband visible light pass through preceding window 1 in sample 2
Front surface is overlapped a branch of generation and frequency light (SFG) and frequency light (SFG) and enters monochromator by collecting optical path；Laser 32 emits
The unthreaded hole 23 that is equipped with by cabinet 27 of beam of laser penetrate on reflecting mirror 17, laser is vertically reflexed to lens by reflecting mirror 17
On 16, laser is focused the window 3 after and beats the rear surface in sample 2 by lens 16, is heated to sample 2, is utilized thermocouple
34 enter in sample cell 24 temperature for measuring sample 2 from escape pipe 8, or are measured using infrared radiation thermometer 37 by preceding window 1
Sample temperature writes the power output of program intelligent control temperature and laser 32, realizes the temperature control to sample；Laser heating and
Infrared radiation thermometer thermometric be it is contactless, can effectively avoid the interference to sample 2 surface and frequency spectrum, though thermocouple temperature measurement is
Contact temperature-measuring, but it is sensitiveer to the response of temperature, and accuracy is high.
Embodiment one
Lauryl sodium sulfate (SDS) Peace Park and annealing temperature on z-cut alpha-quartz crystal are surveyed according to the following conditions
Spend the influence to spectrum:
In the present embodiment, preceding 1 material of window is calcirm-fluoride, and the material of sample 2 is z-cut alpha-quartz crystal, rear 3 He of window
The material of lens 16 is zinc selenide.Laser 32 is CO2Laser, thermometric mode are using 34 thermometric of thermocouple, by thermocouple
34 are sticked to the edge of quartz crystal rear surface, guarantee that heating laser will not directly strike on thermocouple 34.
In the present embodiment, the size of quartz crystal is 16 × 2mm of Φ, takes the 15 μ L drop of SDS ethanol solution of 0.27mmol/L
In strand DNA on Surface of Quartz crystal, area is about 40mm2.Then stainless steel outer wall is dismantled, vacuumizes, adjusts after pressing upper quartz crystal with tantalum piece
Infrared light M and visible light N is saved, two-beam is overlapped on sample 2 after the preceding window 1 of calcirm-fluoride material, carbon dioxide laser
Window 3 is beaten at the quartz crystal back side after zinc selenide material, is heated to quartz crystal.
The Peace Park of SDS on quartz crystal is measured under room temperature in vacuo, as shown in figure 4, SSP and PPP can see
Apparent C-H vibration peak, vibration frequency with can be mapped substantially in document.When azimuth differs 60 °, z-cut α quartz
The non resonant signal size of crystal is constant, but opposite in phase, and the resonance signal of its surface molecular is with orientation angular transformation, therefore
When going to -24 ° from 36 °, spectrum is flipped, symmetrical above and below.
It about 206 DEG C of the fusing point of lauryl sodium sulfate, is heated in vacuum, 150 DEG C of annealing 10min and frequency light (SFG) spectrum
Signal magnitude is basically unchanged, as shown in Fig. 5 (a), (b).And close to fusing point, 200 DEG C of vacuum annealing 10min, due to quartz surfaces
The volatilization of part SDS molecule, SFG spectral signal are obviously reduced.250 DEG C of higher temperature annealing, are substantially not visible the vibration knot of SDS
Structure.
Embodiment two
According to the following conditions survey z-cut alpha-quartz crystal on be added dropwise Pt nano particle under different CO air pressures and frequency vibration
Spectrum:
In the present embodiment, the material of preceding window 1 is calcirm-fluoride, and the material of sample 2 is z-cut alpha-quartz crystal, rear window 3
Material with lens 16 is zinc selenide.Laser 32 is CO2Laser, thermometric mode are using 34 thermometric of thermocouple, by thermoelectricity
Even 34 are sticked to the edge of quartz crystal rear surface, guarantee that heating laser will not directly strike on thermocouple.
In the present embodiment, the size of quartz crystal is 16 × 2mm of Φ, the partial size about 50nm of Pt nano particle used.Take Pt
Powder 1mg adds 7mL ethyl alcohol, and ultrasound obtains the alcohol dispersion liquid of Pt nano particle, takes 35 μ L of the dispersion liquid, drips in quartz-crystal body surface
Face, area about 100mm2.Then stainless steel outer wall is dismantled, is vacuumized after pressing upper quartz crystal with tantalum piece, adjusts infrared light M and can
Light-exposed N, two-beam are overlapped on sample 2 after the preceding window 1 of calcirm-fluoride material, and carbon dioxide laser passes through zinc selenide material
Rear window 2 beat at the quartz crystal back side, quartz crystal is heated.
Before measure spectrum, sample is first in 250 DEG C of vacuum annealing 20min.Then pass to 1.17atm CO gas and frequency vibration
Dynamic spectrum can see apparent CO vibration peak, as shown in fig. 6, z-cut alpha-quartz crystal does not have SSP and PPP off-resonance letter at 6 °
Number, 2075cm-1Nearby the vibration peak on Pt is adsorbed on for CO.Infrared light used is broadband infrared, and part infrared light can be by gas
Phase CO absorbs.As shown in Fig. 7 (a), (b), z-cut alpha-quartz crystal has SSP non resonant signal, 2125cm at 36 °-1And 2170cm-1It is nearby the absorption of gas phase CO, with the reduction of CO air pressure, absorption can obviously weaken, and the signal of Pt-CO also can decrease, very
It can't detect the signal of Pt-CO under sky.From experimental result, although nano particle can scatter part light, but still energy
SFG signal is enough measured, main cause has two o'clock, first is that only having response, therefore the amount of Pt powder used to interface signals with frequency spectrum
Can be considerably less, scattering is not very serious；Second is that the signal of Pt-CO is very big, even if there is no quartz crystal non resonant signal,
It can see very strong Pt-CO signal, and there is quartz crystal non resonant signal to be conducive to improve signal-to-noise ratio.Therefore, load can not had to
Under high-temperature and high-pressure conditions and frequency vibration may be implemented to the problem of the scattering of light and spectral signal-noise ratio difference in heart powder nanometer material
Dynamic spectral measurement.
Heating laser 32 including but not limited to carbon dioxide laser, He-Ne laser, semiconductor laser, can root
Different types of laser is selected according to actual demand.The material of preceding window 1, rear window 3 and lens 16 includes but is not limited to be fluorinated
Calcium, barium fluoride, magnesium fluoride, sapphire, vitreous silica, zinc selenide.According to actually used visible wavelength, infrared light wavelength and red
The preceding window 1 of outer temperature measurer response wave length selection unlike material, after selecting unlike material according to actually used laser wavelength
Window 3 and lens 16.
The material of sample 2 includes but is not limited to vitreous silica, quartz crystal, titanium dioxide, and size includes but is not limited to Φ
16×2mm,10×5×0.5mm,8×8×0.5mm.It designs fluted on stainless steel outer wall, the side of sample 2 is pushed down using tantalum piece
Edge, can effectively prevent the sliding of sample 2, and reduce the contact area of sample 2 Yu stainless steel outer wall, reduce heat transfer.
Thermometric mode includes but is not limited to thermocouple temperature measurement, infrared measurement of temperature, semiconductor thermometric, thermal resistance survey in temperature control part
Temperature.Wherein 34 measured temperature value of thermocouple passes on computer 36 by temperature acquisition card 35, or is passed through by infrared radiation thermometer 37
Cable passes to temperature value on computer 36, reads temperature using Labview program, using multistage programming and pid parameter to laser
The output power of device 32 carries out feedback control, to realize the mild thermostatic process of lifting/lowering, and can control during lifting/lowering temperature
Lifting/lowering temperature rate processed.37 temp measuring method of infrared radiation thermometer is contactless temperature-measuring, with 2 surface of sample without directly contacting.
In the embodiments of the present invention, two-dimensional movement platform 13 and turntable 14 are commercial products, and two-dimensional movement is flat
Platform 13 is purchased in SIGMAKOKI company, model TSDH-602S；Turntable 14 is purchased in THORLABS company, model
NR360S/M。
The utility model uses laser heating method, and heat source and sample 2 only heat sample 2 without directly contacting,
Guarantee that only sample 2 is in maximum temperature in sample cell 24 when heating, in addition to heating efficiency is high, more can effectively avoid other positions,
Such as heat source of stainless steel outer wall, contact heating, the excessively high measurement that side reaction interference and frequency spectrum occurs of temperature.
The utility model is suitable for different temperatures and original position and frequency spectral detection under pressure, and wherein temperature range is 25-
600 DEG C, pressure limit 10-5Pa-150Pa。
The utility model can be used for measuring to be carried on a shoulder pole in the including but not limited to orientation and structure, sample of sample surfaces binding molecule
Carry the orientation and structure of film and its surface adsorbed molecules, support on sample nano particle and its surface adsorbed molecules orientation and
Structure.
The laser heating method and sample temperature control method can be used for the design of other spectral measurement devices, including but unlimited
Infrared spectroscopy, Raman spectrum or fluorescence spectral measuring are used in detection device.
The foregoing is merely the embodiments of the present invention, are not intended to limit the protection scope of the utility model.It is all
Any modification, equivalent substitution and improvement made within spirit of the present utility model and principle, extension etc., are all contained in this reality
With in novel protection scope.
Claims (10)
1. a kind of Peace Park detection device in situ for having laser heating, which is characterized in that add including sample stage, laser
Heat and temperature-controlling system and air-channel system, wherein sample stage includes sequentially connected sample cell (24), adjustment mechanism (25) and cabinet
(27), optical element (26) are equipped in the cabinet (27), the laser heating and temperature-controlling system are used to emit laser to described
In cabinet (27), the optical element (26) is used to that laser heating and the laser that temperature-controlling system emits to be turned to and be focused to
On sample (2) in sample cell (24), laser heating is carried out to sample (2), the laser heating controls sample with temperature-controlling system
(2) temperature, the air-channel system are used to vacuumize sample cell (24) and to provide the gas of different pressures in sample cell (24)
Atmosphere.
2. the Peace Park detection device in situ according to claim 1 for having laser heating, which is characterized in that institute
Stating sample cell (24) includes sample cell shell, preceding window (1) and rear window (3), and wherein sample cell shell is connected to the adjustment
In mechanism (25), the front and back ends of the sample cell shell are respectively equipped with preceding window (1) and rear window (3), the laser heating with
The laser of temperature-controlling system transmitting window (3) after through enter the sample cell (24) it is interior, be connected on the sample cell shell and institute
State the air inlet pipe (9) and escape pipe (8) of air-channel system connection.
3. the Peace Park detection device in situ according to claim 2 for having laser heating, which is characterized in that institute
Stating sample cell shell includes the preceding outer wall (6) and rear outer wall (18) being tightly connected, and the preceding window (1) is embedded at the preceding outer wall
(6) O-ring seal (7) are equipped in the groove being equipped with, between the preceding window (1) and the preceding outer wall (6) to be sealed, and
It is fixed by front pressuring plate (5), front pad (4) are equipped between the front pressuring plate (5) and the preceding outer wall (6), the rear window (3)
It is embedded in the groove that the rear outer wall (18) is equipped with, is equipped between window (3) and the rear outer wall (18) after described O-shaped close
Seal (7) is sealed, and fixed by rear fender (20), after being equipped between the rear fender (20) and the rear outer wall (18)
Gasket (19).
4. the Peace Park detection device in situ according to claim 3 for having laser heating, which is characterized in that institute
It states and is equipped with cooling-water duct in rear outer wall (18), the both ends of the cooling-water duct are respectively and for two coolings of inflow and outflow
Water pipe (10) connection.
5. the Peace Park detection device in situ according to claim 1 for having laser heating, which is characterized in that institute
Adjustment mechanism (25) is stated to include adjustment frame (11), fixed platform (12), two-dimensional movement platform (13), L-type fixed station (21) and turn
Dynamic platform (14), wherein adjustment frame (11) is mounted on fixed platform (12) and installation site is adjustable, the fixed platform (12) with
Two-dimensional movement platform (13) is fixedly connected, and the two-dimensional movement platform (13) is placed on L-type fixed station (21), and the L-type is fixed
Platform (21) is connect with turntable (14), and the turntable (14) is fixed on the cabinet (27), sample cell (24) installation
On the adjustment frame (11).
6. the Peace Park detection device in situ according to claim 1 for having laser heating, which is characterized in that institute
Stating optical element (26) includes lens (16) and reflecting mirror (17), and wherein reflecting mirror (17) is put with 45 ° of incidence angles and will be described
With on the laser reflection to the lens (16) of temperature-controlling system transmitting, the lens (16) and the sample (2) are same for laser heating
Axis installation, the laser for emitting the reflecting mirror (17) focus, the laser facula at the sample (2) back side are adjusted to close
Suitable size.
7. the Peace Park detection device in situ according to claim 1 for having laser heating, which is characterized in that institute
It states laser heating and temperature-controlling system includes laser (32), TTL signal generator (33), computer (36) and temperature measurer, wherein swashing
Light device (32) is connect by TTL signal generator (33) with computer (36), and the laser (32) is used to emit laser to described
On optical element (26)；The temperature measurer is connect by cable with the computer (36), and the temperature measurer is for detecting the sample
The temperature of product pond (24) interior sample (2), and measured temperature is transmitted in computer (36), the computer (36) is according to the survey
The temperature signal of warm instrument detection controls the output power of the laser (32) by PID adjusting method.
8. the Peace Park detection device in situ according to claim 7 for having laser heating, which is characterized in that institute
Stating temperature measurer is the thermocouple (34) with the sample (2) EDGE CONTACT, and the thermocouple (34) passes through temperature acquisition card (35)
It is connect with the computer (36)；Or the temperature measurer is the infrared radiation thermometer (37) being set on the outside of the sample cell (24),
The infrared radiation thermometer (37) is connect by cable with the computer (36).
9. the Peace Park detection device in situ according to claim 1 for having laser heating, which is characterized in that institute
Stating air-channel system includes gas chamber (38) and the gas source (29) and molecular pump (30) that connect with the gas chamber (38), the gas chamber (38)
It is connected to by air inlet pipeline and gas exhaust piping with the sample cell (24).
10. the Peace Park detection device in situ according to claim 9 for having laser heating, which is characterized in that
Pressure detector (28) and residual gas analyzer (31) are connected on the gas chamber (38).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821595015.7U CN208818635U (en) | 2018-09-29 | 2018-09-29 | The Peace Park detection device in situ for having laser heating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821595015.7U CN208818635U (en) | 2018-09-29 | 2018-09-29 | The Peace Park detection device in situ for having laser heating |
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| CN208818635U true CN208818635U (en) | 2019-05-03 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110967301A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院大连化学物理研究所 | In-situ sum frequency vibration spectrum detection device with laser heating function |
| CN112748073A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Material in-situ characterization sample cell and use method thereof |
| CN112946001A (en) * | 2019-11-26 | 2021-06-11 | 中国科学院大连化学物理研究所 | Component identification method for solid particle pollutants in solid-liquid laser cooling liquid |
| CN112748073B (en) * | 2019-10-31 | 2024-05-31 | 中国石油化工股份有限公司 | Material in-situ characterization sample cell and use method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110967301A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院大连化学物理研究所 | In-situ sum frequency vibration spectrum detection device with laser heating function |
| CN110967301B (en) * | 2018-09-29 | 2023-10-03 | 中国科学院大连化学物理研究所 | In-situ sum frequency vibration spectrum detection device with laser heating function |
| CN112748073A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Material in-situ characterization sample cell and use method thereof |
| CN112748073B (en) * | 2019-10-31 | 2024-05-31 | 中国石油化工股份有限公司 | Material in-situ characterization sample cell and use method thereof |
| CN112946001A (en) * | 2019-11-26 | 2021-06-11 | 中国科学院大连化学物理研究所 | Component identification method for solid particle pollutants in solid-liquid laser cooling liquid |
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