CN208013068U - A kind of microscopic observation system with the controllable sample cell of temperature and pressure - Google Patents

Abstract

The utility model discloses a kind of microscopic observation system with the controllable sample cell of temperature, pressure, which can carry out ordinary optical microscope observation, can also carry out polarized light microscopy observation.System by visualization autoclave, temperature-controlling module, be quickly cooled down component, pressure control assembly, optical imaging system and constitute, heterogeneous microstructure evolution process of the high molecular material in particular atmosphere, quick changeable temperature transformation environment can be observed in the scale of 1 μm~1cm.For Study Polymer Melts, the condensed state development law research in hyperbaric environment provides a kind of novel characterization method to content disclosed by the utility model, also provides a kind of new approaches with phase separation for deep announcement polymer crystallization mechanism and regulation and control high molecular material crystallization.

Description

A kind of microscopic observation system with the controllable sample cell of temperature and pressure

Technical field

The present invention relates to a kind of microscopic observation systems, for observing high molecular material in particular atmosphere, quick changeable temperature transformation Heterogeneous microstructure evolution process in environment.

Background technology

High molecular material heterogeneous microstructure depends not only on the materials sheet such as the molecular composition of high molecular material, segmented structure The factor of body additionally depends on its environmental change history undergone in differentiation.People can be by changing the ring residing for material Border factor controlling microstructure, and then obtain the excellent mechanical property or specific function of high molecular material product. Newest research is found：In particular atmosphere, when environmental pressure or temperature quickly change, high molecular material is showed in routine The microstructure new construction and transformation behavior that can not be formed in evolution process.With the popularization of Macromolecular materials industry engineer application And development, in novel light porous polymer material and high-strength and high ductility Crystalline plastics material preparation and special copolymer Electrical property regulation and control etc. fields, be increasingly encountered high molecular material under different atmosphere, environmental pressure, ambient temperature conditions into Row prepares and regulation and control, and this pressure, temperature variation is relatively violent.To prepare these high-performance polymer materials and right Preparation process and technological parameter carry out Effective Regulation, it is necessary to the material from basic science angle research particular surroundings or drastic change operating mode Expect structural evolution and transformation behavior, but international research means and characterization instrument can not this materials of direct-on-line monitoring at present Behavior is compeled for the heterogeneous microstructure and transformation behavior for observing and studying in this environmental pressure or the quick change procedure of temperature The microscopic sdIBM-2+2q.p.approach means for the temperature and pressure quick response function to be had that is essential.

In terms of high molecular material heterogeneous microstructure develops under special environment and operating mode research means and observing system, Prader Research and Development Corporation disclosed in 2008 in China a kind of entitled " with adjustable fluid passage High-pressure cross-polar microscopy cells and application method " (publication number：CN 200810008638.4) patented technology.This is specially Device described in profit includes that pond body, fluid flowing passage and two windows keep component, and it includes two that the window, which keeps component, Or more light-transmissive window.Between the device can be adjusted in the case where not changing the crystal alignment of window between window Gap.It can be carried out while adjusting the thickness of fluid sample using the Researches on Fluids of the property of polarised light, this gap adjustment It can be carried out while will check that pond is pressurizeed.However, the device does not have temperature control function.

Southwest Petrol University disclosed a kind of entitled " microcosmic visualization stratum filtration mould of high temperature and pressure in 2014 in China Draft experiment device and method " (publication number：CN 2014102444772.X) patented technology.Device described in the patent includes to drive For system, stratum filtration simulation system, microcosmic visualization system and fluid analytical systems.The system can characterize complex reservoir The plane seepage flow characteristics and mechanism of oil displacement of displacement process in recovery process realize the continuous microcosmic visualization of dynamic to flow event Observation.But the system is suitable for observing flow process of the fluid in rock core intermediate plate, and it is not directed to sample cell cooling system, Temp-controled mode is more single.

Harbin Engineering University disclosed in China that a kind of entitled " high temperature is high in a kind of interbank narrow space in 2014 Press Gas- liquid two-phase flow visualization system " (publication number：CN 201410241897.7) patented technology.Dress described in the patent It sets middle electrical heating tube bank and forms interbank narrowed flow path with pressure cylinder inner circular chamber, form is provided on the barrel of pressure cylinder It is in cross to be divided into four groups, and form fastening frame is mounted on by bolt outside form, which includes four form windows, using 2 High-speed camera distinguishes the form window of 0 degree and 90 degree position of face.But the device is free of pressure control device, device inner cavity Pressure can not also measure in real time.

Chinese patent " high temperature and pressure carbon dioxide flooding super-viscous oil disclosed in the mandate that University of Science & Technology, Beijing applied in 2016 A kind of high temperature and pressure carbon dioxide flooding viscous crude is provided in visualization microcosmos experiment device and method " (CN201610831430.7) Microcosmos experiment device and method is visualized, the Precipitation Behavior of research asphalitine and its influence to coefficient of mining are applied to.The device Including being clamped with the model clamper of microcosmic visual model, displacement system, back pressure system, confining pressure system, pressure monitor system, temperature Control system and image capturing system are spent, the oil-gas reactivation variation of carbon dioxide displacement process can be clearly observed.But it should System is designed for observation fluid, is not suitable for observing the microcosmic evolutionary process of high molecular material static state.

There is only temperature control or the problems of pressure control function deficiency for the system and method for above-mentioned patent disclosure, and And it is not suitable for detecting the material evolution process under rapid pressure and temperature change yet.This is because the design of above system is not Consider how the critical oplescence phenomenon for preventing sample placement space from occurring.The phenomenon is when substance occurs acutely in Near The Critical Point Density fluctuation, light irradiates the substance and the strong scattering phenomenon that occurs.It is this when quickly variation occurs for pressure and temperature Phenomenon easilys lead to occur blank screen in imaging system, and then the parts of images of material evolution process is caused to be lost.It is even more serious , when the material system of tissues observed structural evolution speed, it is complete that this blank screen phenomenon also results in whole system Failure.

Invention content

In order to solve the above problem with realization monitored over time high molecular material in particular atmosphere, quick changeable temperature transformation environment Evolution process, the invention discloses a kind of microscopic observation systems with the controllable sample cell of temperature and pressure.The system can be used for Research supercritical fluid grows up behavior, macromolecule mixture in small molecule organic/inorganic solvent in the forming core of high molecular material Isothermal/alternating temperature crystallization process in high-pressure atmosphere of phase separation, high molecular material, high molecular material is in high-pressure atmosphere Melting process etc., be Study Polymer Melts condensed state development law research in different atmosphere, different temperatures, different pressures environment A kind of novel characterization method is provided, and then the formulation for regulation and control polymer crystallization and phase separation process scheme in actual production carries For theoretical direction.The microscopic observation system serves not only as ordinary optical microscopic observation system, it is also possible to make polarized light microscopy sight Examine system.

To achieve the goals above, the present invention adopts the following technical scheme that.

Microscopic observation system disclosed by the invention with the controllable sample cell of temperature and pressure, including visualization autoclave, temperature Degree control assembly is quickly cooled down component, pressure control assembly and optical imaging system；The visualization autoclave is for placing Sample to be observed；The visualization autoclave includes autoclave body and kettle cover, and the autoclave body is an open-topped tubular Upper glass window, ventilative gasket, lower glass window are pressed in autoclave body by structure, the kettle cover successively from top to bottom；It is described Upper glass window, ventilative gasket, form sample placement space between lower glass window；The autoclave body bottom and kettle cover Center opens up light hole of the own centre line on same straight line；Autoclave body go to the bottom light hole, lower glass window, ventilative gasket, Upper glass window and kettle cover center light hole composition visualization autoclave light path system；Light can be from the logical of autoclave body bottom center Unthreaded hole enters, and passes through lower glass window, ventilative gasket center, upper glass window successively, finally light hole is penetrated from kettle cover center Go out；The temperature-controlling module is used to control the temperature of visualization autoclave, and described is quickly cooled down component for fast quickly cooling But autoclave is visualized, the pressure control assembly is used to control the pressure of visualization autoclave；The optical imaging system Condensed state evolution process for observing, recording high molecular material.

Further, it is equipped with the first sealing ring on the section of the kettle cover and the cooperation of upper glass window, described first is close Seal is for preventing high-pressure fluid in autoclave body from being flowed out from kettle cover light hole.

Or/and the second sealing ring is equipped on the section that the kettle cover and autoclave body coordinate, second sealing ring is for preventing Only interface outflow of the high-pressure fluid between kettle cover and autoclave body in autoclave body.

Or/and it is equipped with third sealing ring on the section of autoclave body and the cooperation of lower glass window, the third sealing ring is used for Prevent the light hole that high-pressure fluid is gone to the bottom from autoclave body in autoclave body from flowing out.

First sealing ring, the second sealing ring, third sealing ring heatproof temperature be higher than 200 DEG C.

Further, the hardness of the ventilative gasket is more than the first sealing ring, the second sealing ring and third sealing ring Hardness, be less than upper glass window and lower glass window hardness, with ensure ventilative gasket can effectively transmit sealing jam-packed power. Ventilative gasket includes middle section and peripheral part, and intermediate portion is divided into hollow structure, as sample placement space, periphery Part is equipped with air channel or notch, realizes sample placement space and remaining space unicom in kettle.

The thickness of ventilative gasket is less than 2cm, i.e., upper the distance between glass window and lower glass window opposite face are less than 2cm.The heatproof temperature of ventilative gasket is higher than the heatproof temperature of all sealing rings.

Further, the temperature-controlling module includes temperature controller, heating element, thermocouple, signal cable；Its Temperature inside middle temperature controller input terminal connection thermocouple acquisition autoclave body, output end are connected by signal cable and heating element It connects；Temperature controller can be exported observed temperature value to computer by data collecting card, and computer completes the prison to temperature data It surveys and records.

Further, the component that is quickly cooled down includes autoclave refrigerating seat, the first shut-off valve, liquid pump, liquid constant Incubator and coolant liquid pipeline；The autoclave refrigerating seat is a tubular structure, and the visualization autoclave is mounted on described Autoclave refrigerating seat in, the light hole that is passed through for light source is equipped on the pedestal of the autoclave refrigerating seat；The light hole It is coaxial with autoclave body bottom light hole, the coolant liquid pipeline is placed in the autoclave refrigerating seat；The cooling Liquid pipeline forms a circulation loop with liquid pump, liquid thermostat, and the first shut-off valve is equipped on the circulation loop；Liquid Ranging from -100 DEG C~100 DEG C of the temperature control of body insulating box.

Further, the pressure control assembly includes fluid source, plunger pump, the second shut-off valve, third shut-off valve, row Put valve, pressure sensor and pipeline；Wherein fluid source port connects plunger pump intake, and outlet of plunger pump is sequentially connected the second cut-off Valve, pressure sensor, visualization autoclave inlet and outlet, the line branching between pressure sensor and the second shut-off valve are sequentially connected Third shut-off valve and drain valve.The fluid of fluid source output can be water, carbon dioxide, nitrogen, organic solvent etc..At second section In the state that only valve is opened, third shut-off valve is closed, plunger pump can be high with constant pressure or the control visualization of constant current both of which Press pressure in kettle.Plunger pump pressure control ranging from 0.1Mpa~65Mpa.Drain valve can adjust fluid rate of discharge.Pressure sensing The collected pressure signal of device is transferred to by data collecting card in computer, and computer completes the monitoring to pressure data and record.

Further, the optical imaging system is arranged in order by light source, amplification focusing component and image collecting device It constitutes；The light source is arranged on the outside of the light hole of autoclave refrigerating seat, and amplification focusing component is placed in kettle cover On the outside of heart light hole, amplification focusing component is connected with image collecting device, the image collecting device and computer phase Even.

Preferably, the optical imaging system further includes being polarized eyeglass and analyzing eyeglass, is polarized eyeglass and analyzing eyeglass To choose to install component；To realize ordinary optical observation, then the two eyeglasses need not be installed；To realize polarized light microscopy observation, Installation is then needed to be polarized eyeglass and analyzing eyeglass.

Further, light source can be, but not limited to, LED light source.Image collecting device type can be, but not limited to, CMOS or CCD.The optical magnification adjustable extent of amplification focusing component is 0.1-100 times.

Further, sample light transmittance is not less than 60%, is in chip shape, sheet thickness ranging from 0.005 μm~500 μ m。

The application method of the present invention is as follows：

(1) in normal pressure, normal temperature environment microscopic observation sample method：

Step (1), by sample to be tested produced as sheets；

Step (2), lower glass window is placed on inside autoclave body, sample is placed on the upper surface of lower glass window；

Step (3), pressure control assembly, temperature-controlling module and the power supply being quickly cooled down in component in closing system, and It remains off；

Step (4), the amplification factor of adjustment amplification focusing component, focuses on chip sample central core, adjusts the intensity of light source, Image collecting device is set and shoots total duration, time for exposure etc., prepares shooting；

Step (5) starts image collecting device, starts to take pictures or record a video, and store image；

Step (6), shooting terminates, and closes system various components power supply.

(2) in normal pressure, varying temperature environment microscopic observation sample method：

Step (1), by sample to be tested produced as sheets；

Step (2), lower glass window, ventilative gasket are placed sequentially in inside autoclave body, and sample is put into ventilative pad In the space at piece center, then upper glass window and kettle cover are sequentially placed in ventilative gasket upper surface；

Step (3) is closed whole valves and power supply in pressure control assembly, and is remained off；

Liquid thermostat temperature is arranged in step (4), keeps liquid pump standby mode；

Step (5), as needed, set temperature control program, including the target temperature of heating process, target heating speed Rate, the target temperature of cooling procedure, target rate of temperature fall etc.；

Step (6), the amplification factor of adjustment amplification focusing component, focuses on chip sample central core, adjusts the intensity of light source, Image collecting device is set and shoots total duration, time for exposure etc., prepares shooting；

Step (7), running temperature control program, sample cell are controlled by temperature controller and the interoperation of liquid pump Temperature；

Step (8) starts image collecting device, is taken pictures or recorded a video when selecting, and store image；

Step (9), shooting terminates, and closes system various components power supply.

(3) in transformation, normal temperature environment microscopic observation sample method：

Step (1), by sample to be tested produced as sheets；

Third sealing ring, lower glass window, ventilative gasket are placed sequentially in inside autoclave body, sample are put by step (2) In the space for entering ventilative gasket center, upper glass window then is placed in ventilative gasket upper surface, in kettle cover groove and kettle Body upper surface groove installs the first sealing ring and the second sealing ring respectively, is connected kettle cover simultaneously each above-mentioned with autoclave body with bolt Each component jam-packed；

Step (3) opens the second shut-off valve, opens third shut-off valve, and opening plunger pump is adjusted to constant current mode, with 1~ The flow of 20mL/min injects particular fluid to sample cell, and air in kettle is discharged；

Step (4), closing temperature control assembly and cooling control assembly power supply, and remain off；

Step (5) sets the pressure control program of particular fluid, including the goal pressure of pressure process, mesh as needed Mark compression rate, the goal pressure of pressure reduction, target rate of pressure reduction etc.；

Step (6), the amplification factor of adjustment amplification focusing component, focuses on chip sample central core, adjusts the intensity of light source, Image collecting device is set and shoots total duration, time for exposure etc., prepares shooting；

Step (7), operating pressure control program, pass through plunger pump, the interoperation of the second shut-off valve and third shut-off valve To control the pressure of particular fluid in sample cell；

Step (8) starts image collecting device, is taken pictures or recorded a video when selecting, and store image；

Step (9), shooting terminates, and closes system various components power supply.

(4) in transformation, varying temperature environment microscopic observation sample method：

Step (1), by sample to be tested produced as sheets；

Third sealing ring, lower glass window, ventilative gasket are placed sequentially in inside autoclave body, sample are put by step (2) In the space for entering ventilative gasket center, upper glass window then is placed in ventilative gasket upper surface, in kettle cover groove and kettle Body upper surface groove installs the first sealing ring and the second sealing ring respectively, is connected kettle cover simultaneously each above-mentioned with autoclave body with bolt Each component jam-packed；

Step (3) opens the second shut-off valve, opens third shut-off valve, and opening plunger pump is adjusted to constant current mode, with 1~ The flow of 20mL/min injects particular fluid to sample cell, and air in kettle is discharged；

Liquid thermostat temperature is arranged in step (4), keeps liquid pump standby mode；

Step (5), as needed, set temperature control program, including the target temperature of heating process, target heating speed Rate, the target temperature of cooling procedure, target rate of temperature fall etc.；

Step (6) sets the pressure control program of particular fluid, including the goal pressure of pressure process, mesh as needed Mark compression rate, the goal pressure of pressure reduction, target rate of pressure reduction etc.；

Step (7), the amplification factor of adjustment amplification focusing component, focuses on chip sample central core, adjusts the intensity of light source, Image collecting device is set and shoots total duration, time for exposure etc., prepares shooting；

Step (8), while running temperature control program and pressure control program pass through matching for temperature controller and liquid pump Conjunction acts to control sample cell temperature, and sample is controlled by the interoperation of plunger pump, the second shut-off valve and third shut-off valve The pressure of particular fluid in pond；

Step (9) starts image collecting device, is taken pictures or recorded a video when selecting, and store image；

Step (10), shooting terminates, and closes system various components power supply.

Beneficial effects of the present invention：

Compared to the common light microscope with thermal station and with the petrographic microscope of thermal station, system provided by the invention can be with Observe Microstructure Development process of the high molecular material in particular atmosphere, quick changeable temperature transformation environment；It is provided by the invention can Depending on changing system, for Study Polymer Melts, the research of condensed state development law provides a kind of novel characterization hand in high-pressure atmosphere environment Section can provide process program for regulation and control polymer crystallization, phase separation, and realize cohesive energy and segment in polymer crystallization theory The decoupling of locomitivity is studied, and new approaches are provided further deeply to disclose polymer crystallization mechanism.

Description of the drawings

The accompanying drawings which form a part of this application are used for providing further understanding of the present application, and the application's shows Meaning property embodiment and its explanation do not constitute the improper restriction to the application for explaining the application.

Fig. 1 is the microscopic observation system schematic diagram provided by the invention with the controllable sample cell of temperature, pressure.

In figure, 1, light source；2, it is polarized eyeglass；3, analyzing eyeglass；4, amplification focusing component；5, high-speed image sampling device； 6, autoclave body；7, kettle cover；8, upper glass window；9, lower glass window；10, bolt；11, the first sealing ring；12, the second sealing ring； 13, third sealing ring；14, ventilative gasket；15, temperature controller；16, heating element；17, thermocouple；18, signal cable； 19, sample placement space；20, data collecting card；21, computer；22, autoclave refrigerating seat；23, the first shut-off valve；24, liquid Pump；25, liquid thermostat；26, coolant liquid pipeline；27, fluid source；28, plunger pump；29, the second shut-off valve；30, third is ended Valve；31, drain valve；32, pressure sensor；33, pipeline.

Fig. 2 is ventilative gasket construction schematic diagram provided by the invention.In figure, 34, laminar sample.

Carbon dioxide during quick pressure releasing that Fig. 3 observes for ordinary optical microscopic system provided by the invention/ The phase separation of polymethyl methacrylate (PMMA) system.

Fig. 4 be polarized light microscopy systematic observation provided by the invention to crystallizations of the PLLA in 6.9MPa carbon dioxide Journey.

Specific implementation mode

It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field The identical meanings of understanding.

It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.

Being quickly cooled down for heretofore described " being quickly cooled down component " refers to the cooling speed of sample cell in cooling procedure Rate maximum is up to 6 DEG C/s.

The high pressure of " autoclave " in the present invention refers to that the internal gas pressure value born of autoclave body after sealing is reachable 30MPa.In pressure leak process, the pressure of autoclave can pressure release to atmospheric pressure, pressure release rate is up to 20MPa/s.

The invention will be further described with embodiment below in conjunction with the accompanying drawings.

As shown in Figure 1, the microscopic observation system disclosed by the invention with the controllable sample cell of temperature and pressure includes visualization Autoclave, temperature-controlling module are quickly cooled down component, pressure control assembly and optical imaging system.The visualization high pressure Kettle is used to control the temperature of visualization autoclave for placing sample to be observed, temperature-controlling module, and described is quickly cooled down Component is used to control the pressure of visualization autoclave for being quickly cooled down visualization autoclave, the pressure control assembly；Institute State condensed state evolution process of the optical imaging system for observing, recording high molecular material.

Wherein, visualization autoclave includes autoclave body 6, kettle cover 7, upper glass window 8, lower glass window 9, bolt 10, first Sealing ring 11, the second sealing ring 12, third sealing ring 13, ventilative gasket 14.Lower glass window 9, ventilative gasket 14, upper glass Glass window 8 is sequentially arranged in autoclave body 6, with bolt 10 by kettle cover 6 and the connection of autoclave body 7 and each above-mentioned each component jam-packed；And It is equipped with the first sealing ring 11 on the section of the kettle cover and the cooperation of upper glass window, the first sealing ring 11 is for preventing in autoclave body High-pressure fluid is flowed out from kettle cover light hole.It is equipped with the second sealing ring 12 on the section that the kettle cover and autoclave body coordinate, second is close Seal 12 is used to prevent interface outflow of the high-pressure fluid between kettle cover and autoclave body in autoclave body.Coordinate in autoclave body and lower glass window Section be equipped with third sealing ring 13, what the third sealing ring 13 was used to prevent high-pressure fluid in autoclave body from go to the bottom from autoclave body leads to Unthreaded hole flows out；First sealing ring 11, the second sealing ring 12, third sealing ring 13 heatproof temperature be higher than 200 DEG C of realities Now visualize the sealing of autoclave；Autoclave body 6 is gone to the bottom and 7 center of kettle cover opens up light hole, and light can be from the bottom of autoclave body 6 center Light hole enters, and passes through lower glass window 9,14 center of ventilative gasket, upper glass window 8 successively, finally from 7 center of kettle cover Light hole projects.The space that lower glass window 9, ventilative gasket 14 and upper glass window 8 surround is for placing observed sample Product.

Further, ventilative gasket 14 includes middle section and peripheral part, and intermediate portion is divided into hollow structure, as Sample placement space, peripheral part are equipped with air channel or notch, realize that sample placement space joins with remaining space in kettle It is logical.Fig. 2 gives the appearance schematic diagram of ventilative gasket, and the arrangement of ventilating groove can select mode as shown in Figure 2, Radially it is arranged in peripheral part multiple, number is unrestricted, may be used and is uniformly distributed, and can also select non-homogeneous point Cloth；The thickness of ventilative gasket 14 is 1cm, i.e., upper the distance between glass window 8 and lower 9 opposite face of glass window are 1cm.

Further, visualization autoclave autoclave body 6 and 7 material of kettle cover can be but not limited to stainless steel.First is close The material of seal 11, the second sealing ring 12 and third sealing ring 13 can be but not limited to fluorubber.The material of ventilative gasket 14 Matter can be but not limited to polytetrafluoroethylene (PTFE).The material of upper glass window 8 and lower glass window 9 can be but not limited to sapphire And high purity quartz.The material of autoclave refrigerating seat 22 can be but not limited to aluminium alloy.

Wherein, temperature-controlling module includes temperature controller 15, heating element 16, thermocouple 17, signal cable 18.Wherein 15 input terminal of temperature controller connects the temperature that thermocouple 17 acquires autoclave body 6 inner space, output end by signal cable 18 with Heating element 16 connects.Temperature controller 15 can be exported observed temperature value to computer 21, computer by data collecting card 20 21 complete the monitoring to temperature data and record.

Wherein, it includes autoclave refrigerating seat 22, the first shut-off valve 23, liquid pump 24, liquid thermostat to be quickly cooled down component 25 and coolant liquid pipeline 26；It visualizes autoclave to be mounted in autoclave refrigerating seat 22, cooling is placed in autoclave refrigerating seat Pipeline, the outlet of liquid thermostat 25 connection 24 entrance of liquid pump, the first shut-off valve 23 of the outlet of liquid pump 24 connection, autoclave cooling 22 entrances, the outlet of autoclave refrigerating seat 22 connection 25 entrance of liquid thermostat.Ranging from -100 DEG C of the temperature control of liquid thermostat 25 ~100 DEG C；

Specifically, autoclave refrigerating seat 22 is a tubular structure, the visualization autoclave is mounted on the height It presses in kettle refrigerating seat 22, the light hole passed through for light source is equipped on the pedestal of the autoclave refrigerating seat 22；The light hole It is coaxial with the bottom of autoclave body 6 light hole.

Wherein, pressure control assembly includes fluid source 27, plunger pump 28, the second shut-off valve 29, third shut-off valve 30, discharge Valve 31, pressure sensor 32 and pipeline 33.Wherein the outlet of fluid source 27 connection 28 entrance of plunger pump, the outlet of plunger pump 28 connect successively Connect the second shut-off valve 29, pressure sensor 32, visualization autoclave inlet and outlet, pressure sensor 32 and the second shut-off valve 29 it Between line branching be sequentially connected third shut-off valve 30 and drain valve 31.Fluid source 27 can be water, carbon dioxide, nitrogen, have Solvent etc..In the state that the second shut-off valve 29 is opened, third shut-off valve 30 is closed, plunger pump 28 can be with constant pressure or perseverance Flow pressure in both of which control visualization autoclave.28 pressure control of plunger pump ranging from 0.1Mpa~65Mpa.Pressure sensor 32 Collected pressure signal is transferred to by data collecting card 20 in computer 21, the monitoring of 21 complete paired data of computer and record.

Wherein, optical imaging system by light source 1, be polarized eyeglass 2, analyzing eyeglass 3, amplification focusing component 4 and high speed image Harvester 5 is arranged in order composition；The light source 1 is arranged on the outside of the light hole of autoclave refrigerating seat 22, the amplification Focusing component 4 is placed on the outside of 7 center light hole of kettle cover, and amplification focusing component 4 is connected with image collecting device 5, institute The image collecting device 5 stated is connected with computer 21；

Light source 1 enters from the light hole of autoclave refrigerating seat 22, passes through from the light hole at the bottom of autoclave body 6 center, passes through successively Glass window 9,14 center of ventilative gasket, upper glass window 8 are crossed down, is finally projected from 7 center light hole of kettle cover, amplification focusing Component 4 receives the light transmitted.

It is to choose to install component to be polarized eyeglass 2 and analyzing eyeglass 3.To realize ordinary optical observation, then need not install this two A eyeglass；To realize polarized light microscopy observation, then installation is needed to be polarized eyeglass 2 and analyzing eyeglass 3.

Further, light source 1 can be, but not limited to, LED white light sources.5 type of high-speed image sampling device can be But it is not limited to CMOS.The optical magnification adjustable extent of amplification focusing component 4 is 0.1-100 times.

Further, sample light transmittance is not less than 60%, is in chip shape 34, sheet thickness ranging from 0.005 μm~500 μm。

It is described in detail below with several embodiments：

Embodiment 1

Carbon dioxide/polymethyl methacrylate during quick pressure releasing is observed using ordinary optical microscopic function (PMMA) phase separation of system：

Step (1), by PMMA produced as sheets, thickness is 200 μm；

Third sealing ring 13, lower glass window 9, ventilative gasket 14 are placed sequentially in inside autoclave body 6 by step (2), Sample 34 is put into the space 19 at 14 center of ventilative gasket, then places upper glass window in 14 upper surface of ventilative gasket 8, the first sealing ring 11 and the second sealing ring 12 are installed respectively in 7 groove of kettle cover and 6 upper surface groove of autoclave body, it will with bolt 10 Kettle cover 7 and the connection of autoclave body 6 are simultaneously each above-mentioned each component jam-packed；

Step (3) opens the second shut-off valve 29, opens third shut-off valve 30, and opening plunger pump 28 is adjusted to constant current mode, Carbon dioxide is injected to sample cell with the flow of 1~20mL/min, air in kettle is discharged；

Step (4), opens temperature controller 15, heating sample cell to a certain temperature, which is higher than the glass of PMMA Change transition temperature；

Step (5) closes third shut-off valve 30, plunger pump 28 is adjusted to constant voltage mode, continues to inject dioxy to sample cell Change carbon, until setup pressure value (being 14MPa for the embodiment)；

Step (6) waits for that sample cell temperature and pressure is stablized in setting value, starts timing 1 hour；

Step (7), in timing course, the amplification factor of adjustment amplification focusing component 4 focuses on chip sample central core, 1 intensity of light source is adjusted, setting image collecting device 5 shoots total duration, time for exposure, shooting number, prepares shooting；

Step (8) at the end of timing, closes the second shut-off valve 29, starts image while opening third shut-off valve 30 Harvester 5 starts to be continuously shot or record a video；In the process, the pressure change of sample cell is violent, and rate of change is about 1000MPa/min。

Step (9), shooting terminates, storage shooting image, as shown in Figure 3.Closing temperature controller 15 closes plunger pump 28；

Step (10) opens the first shut-off valve 23, liquid pump 24 is opened, with room temperature water cooling sample cell.

Embodiment 2

Using crystallization process of the polarized light microscopy function observation l-lactic acid (PLLA) in high-pressure carbon dioxide：

Step (1), by PLLA produced as sheets, thickness is 15 μm；

Third sealing ring 13, lower glass window 9, ventilative gasket 14 are placed sequentially in inside autoclave body by step (2), Sample 34 is put into the space 19 at 14 center of ventilative gasket, then places upper glass window 8 in 14 upper surface of ventilative gasket, The first sealing ring 11 and the second sealing ring 12 are installed respectively in 7 groove of kettle cover and 6 upper surface groove of autoclave body, with bolt 10 by kettle cover 7 and autoclave body 6 connection and each above-mentioned each component jam-packed；

Step (3) opens the second shut-off valve 29, opens third shut-off valve 30, and opening plunger pump 28 is adjusted to constant current mode, Carbon dioxide is injected to sample cell with the flow of 1~20mL/min, air in kettle is discharged；

Step (4), opens temperature controller 15, and heating sample cell makes PLLA be in molten condition to PLLA fusing points；

Step (5) closes third shut-off valve 30, plunger pump 28 is adjusted to constant voltage mode, continues to inject dioxy to sample cell Change carbon, until setup pressure value；

Step (6) waits for that sample cell temperature and pressure is stablized in setting value, starts timing 30min.

Step (7), in timing course, the amplification factor of adjustment amplification focus pack 4 focuses on chip sample central core, 1 intensity of light source is adjusted, is installed additional between light source 1 and sample cell bottom light hole and is polarized eyeglass 2, in image collecting device 5 and sample Install analyzing eyeglass 3 between the upper cover light hole of product pond additional.Analyzing eyeglass 3 is rotated, until 5 visual field complete extinction of image collecting device, 5 time for exposure of image collecting device is set, shooting is prepared；

Step (8), at the end of timing, 15 setting value of adjustment temperature controller temperature is opened simultaneously to PLLA crystallization temperatures First shut-off valve 23 and liquid pump 24 will visualize autoclave fast cooling to PLLA crystallization temperatures with cryogenic liquid；Herein In the process, temperature change is violent, and rate of temperature fall is about 6 DEG C/s.

Step (9) when reaching crystallization temperature, starts timing, is shot and store image.It is as shown in Figure 4 to shoot image；

Step (10), end to be crystallized, closing temperature controller 15 close plunger pump 28, close image collecting device 5；

Step (11) opens the first shut-off valve 23, opens fluid pump 24, cooling sample cell to room temperature.

Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not protects model to the present invention The limitation enclosed, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not Need to make the creative labor the various modifications or changes that can be made still within protection scope of the present invention.

Claims (8)

1. a kind of microscopic observation system with the controllable sample cell of temperature and pressure, which is characterized in that including visualization autoclave, temperature Degree control assembly is quickly cooled down component, pressure control assembly and optical imaging system；The visualization autoclave is for placing Sample to be observed；The visualization autoclave includes autoclave body and kettle cover, and the autoclave body is an open-topped tubular Upper glass window, ventilative gasket, lower glass window are pressed in autoclave body by structure, the kettle cover successively from top to bottom；It is described Upper glass window, ventilative gasket, form sample placement space between lower glass window；The autoclave body bottom and kettle cover Center opens up light hole of the own centre line on same straight line；Autoclave body go to the bottom light hole, lower glass window, ventilative gasket, Upper glass window and kettle cover center light hole composition visualization autoclave light path system；Light can be from the logical of autoclave body bottom center Unthreaded hole enters, and passes through lower glass window, ventilative gasket center, upper glass window successively, finally light hole is penetrated from kettle cover center Go out；The temperature-controlling module is used to control the temperature of visualization autoclave, and described is quickly cooled down component for fast quickly cooling But autoclave is visualized, the pressure control assembly is used to control the pressure of visualization autoclave；The optical imaging system Condensed state evolution process for observing, recording high molecular material.

2. a kind of microscopic observation system with the controllable sample cell of temperature and pressure as described in claim 1, which is characterized in that The section of the kettle cover and the cooperation of upper glass window is equipped with the first sealing ring, and the first sealing ring is for preventing high-pressure spray in autoclave body Body is flowed out from kettle cover light hole；

Or/and it is equipped with the second sealing ring, the second sealing ring, for preventing in autoclave body on the section that the kettle cover and autoclave body coordinate Interface outflow of the high-pressure fluid between kettle cover and autoclave body；

Or/and it is equipped with third sealing ring on the section of autoclave body and the cooperation of lower glass window, the third sealing ring is for preventing The light hole outflow that high-pressure fluid is gone to the bottom from autoclave body in autoclave body；

First sealing ring, the second sealing ring, third sealing ring heatproof temperature be higher than 200 DEG C.

3. a kind of microscopic observation system with the controllable sample cell of temperature and pressure as described in claim 1, which is characterized in that institute The hardness for the ventilative gasket stated is more than the hardness of the first sealing ring, the second sealing ring and third sealing ring, is less than upper windowpane The hardness of mouth and lower glass window；Ventilative gasket includes middle section and peripheral part, and intermediate portion is divided into hollow structure, is made For sample placement space, peripheral part is equipped with air channel or notch, realizes sample placement space and remaining space in kettle Unicom；The thickness of ventilative gasket is less than 2cm, i.e., upper the distance between glass window and lower glass window opposite face are less than 2cm, The heatproof temperature of ventilative gasket is higher than the heatproof temperature of all sealing rings.

4. a kind of microscopic observation system with the controllable sample cell of temperature and pressure as described in claim 1, which is characterized in that institute The temperature-controlling module stated includes temperature controller, heating element, thermocouple, signal cable；Wherein temperature controller input terminal The temperature inside thermocouple acquisition autoclave body is connected, output end is connect by signal cable with heating element；Temperature controller can be with Observed temperature value is exported to computer by data collecting card, computer completes the monitoring to temperature data and record.

5. a kind of microscopic observation system with the controllable sample cell of temperature and pressure as described in claim 1, which is characterized in that institute The component that is quickly cooled down stated includes autoclave refrigerating seat, the first shut-off valve, liquid pump, liquid thermostat and coolant liquid pipeline；Institute It is a tubular structure to state autoclave refrigerating seat, and the visualization autoclave is mounted in the autoclave refrigerating seat, The pedestal of the autoclave refrigerating seat is equipped with the light hole passed through for light source；The light hole and autoclave body bottom light hole are same Axis is placed with the coolant liquid pipeline in the autoclave refrigerating seat；The coolant liquid pipeline and liquid pump, liquid Insulating box forms a circulation loop, and the first shut-off valve is equipped on the circulation loop.

6. a kind of microscopic observation system with the controllable sample cell of temperature and pressure as described in claim 1, which is characterized in that institute The pressure control assembly stated includes fluid source, plunger pump, the second shut-off valve, third shut-off valve, drain valve, pressure sensor and pipe Road；Wherein fluid source port connects plunger pump intake, and outlet of plunger pump is sequentially connected the second shut-off valve, pressure sensor, visual Change autoclave inlet and outlet, the line branching between pressure sensor and the second shut-off valve is sequentially connected third shut-off valve and discharge Valve.

7. a kind of microscopic observation system with the controllable sample cell of temperature and pressure as described in claim 1, which is characterized in that institute The optical imaging system stated is arranged in order and is constituted by light source, amplification focusing component and image collecting device；The light source setting On the outside of the light hole of autoclave refrigerating seat, amplification focusing component is placed on the outside of the light hole of kettle cover center, described Amplification focusing component is connected with image collecting device, and the image collecting device is connected with computer.

8. a kind of microscopic observation system with the controllable sample cell of temperature and pressure as claimed in claim 7, which is characterized in that institute The optical imaging system stated further includes being polarized eyeglass and analyzing eyeglass, and it is to choose to install component to be polarized eyeglass and analyzing eyeglass；To reality Existing ordinary optical observation, then need not install the two eyeglasses；To realize polarized light microscopy observation, then installation is needed to be polarized eyeglass With analyzing eyeglass.