CN105044079B - A kind of method and device of organic matter cracking - Google Patents

A kind of method and device of organic matter cracking Download PDF

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Publication number
CN105044079B
CN105044079B CN201510436148.4A CN201510436148A CN105044079B CN 105044079 B CN105044079 B CN 105044079B CN 201510436148 A CN201510436148 A CN 201510436148A CN 105044079 B CN105044079 B CN 105044079B
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China
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organic matter
laser
focusing
sample
cracking
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CN201510436148.4A
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Chinese (zh)
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CN105044079A (en
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王晓琦
金旭
李建明
孙亮
刘晓丹
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中国石油天然气股份有限公司
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Abstract

The application provides a kind of method and device of organic matter cracking.Methods described includes:Light path calibration and strength test are carried out to confined laser, obtained with the focusing laser beam for specifying light intensity;Organic matter sample is pre-processed, obtains scanning electron microscope example;Choose the organic matter region on the scanning electron microscope example;The organic matter region is cracked using the focusing laser beam, and real time imagery is carried out to the organic matter region.A kind of method and device for organic matter cracking that the embodiment of the present application provides, based on ESEM and confined laser, is capable of the cracking process of home position observation organic matter.This method is the in-situ study method that organic matter structure changes over time with form in real observation cracking process, can be used for the differentiation of different type organic matter, and the research such as different organic matter oil generation merit ratings.

Description

A kind of method and device of organic matter cracking

Technical field

The application is related to organic quality Geochemistry studying technological domain, the more particularly to a kind of method and dress of organic matter cracking Put.

Background technology

Organic matter geochemistry is a geochemical branch, it is main study the composition of organic matter in geologic body, structure, Origin and evolution.Research contents can include:The distribution of organic matter and type, the origin of organic matter and evolution.Since the sixties, The origin of oil viewpoint of kerogen degradation into oil is widely accepted, it was recognized that the importance of research organic matter, correspondingly exists Carry out numerous studies in terms of source rock evaluation and OIL SOURCE CORRELATION, and successfully develop a large amount of new methods, new technology, including it is dry Junket root maceral lens-belowed identifying, high resolution electron microscope imaging, kerogen maceration and pyrolysis, chromatography-mass spectroscopy are used in conjunction, nuclear-magnetism Resonance etc. technology, can from microcosmic imaging analysis to organic matter macroscopic view pyrolysis etc. research organic matter characteristic.

At present, during organic matter cracking is carried out, often organic matter is extracted from sample first, further Ground carries out cracking experiment, then recycles the result after electron microscope observation cracking experiment.

During the application is implemented, inventor has found prior art, and at least there are the following problems:

First, organic matter can be acted on due to heat, liquid in extraction process and produce structural damage, while can also introduce impurity So as to cause property to change;Secondly, sample is first extracted, cracked, recycle electron microscope observation, such step meeting Cause sample to shift, in situ imaging can not be realized, so as to which the accuracy of experiment can not be ensured.

It should be noted that the introduction to technical background above be intended merely to the convenient technical scheme to the application carry out it is clear, Complete explanation, and facilitate the understanding of those skilled in the art and illustrate.Can not merely because these schemes the application's Background section is set forth and thinks that above-mentioned technical proposal is known to those skilled in the art.

The content of the invention

The purpose of the embodiment of the present application is to provide a kind of method and device of organic matter cracking.

What a kind of method and device for organic matter cracking that the embodiment of the present application provides was realized in:

A kind of method of organic matter cracking, methods described include:

Light path calibration and strength test are carried out to confined laser, obtained with the focusing laser beam for specifying light intensity;

Organic matter sample is pre-processed, obtains scanning electron microscope example;

Choose the organic matter region on the scanning electron microscope example;

The organic matter region is cracked using the focusing laser beam, and the organic matter region carried out real-time Imaging.

A kind of device of organic matter cracking, described device include ESEM and the sample bin positioned at the ESEM Interior laser generator, focusing, light path reflecting mechanism, light intensity test mechanism, wherein:

The laser generator, for producing laser beam;

The focusing, for being focused to laser beam caused by the laser generator;

The light path reflecting mechanism, for adjusting the light path of the laser beam after focusing on, to ensure the laser after the focusing Beam is centrally located at specified location;

The light intensity test mechanism, for testing the laser after the focusing and the processing of light path reflecting mechanism Beam, and according to the power of the test result regulation laser generator, obtain with the focusing laser beam for specifying light intensity.

A kind of method and device for organic matter cracking that the embodiment of the present application provides, based on ESEM and focus on laser Device, it is capable of the cracking process of home position observation organic matter.The side cracked in ESEM using laser that the application proposes It is owned by France first.This method is the in-situ study method that organic matter structure changes over time with form in real observation cracking process, It can be used for the differentiation of different type organic matter, and the research such as different organic matter oil generation merit ratings.

The present processes are first extracted relative to by organic matter, are then carried out cracking experiment and are seen again with electron microscope Examine with many advantages:First, organic matter will not produce structural damage because of the heat in extraction process, liquid effect, and not Impurity can be introduced or property changes;Secondly, can be accurately positioned using ESEM, real-time in-situ imaging, organic matter sample exists Do not shifted in whole process, ensure that the accuracy of experiment;Furthermore the energy of confined laser used herein is continuous It is adjustable, different organic matter setup parameters, strong applicability can be directed to.The foundation of this method and subsequent development, may further it promote The evaluation study of organic matter.

With reference to following explanation and accompanying drawing, the particular implementation of the application is disclose in detail, specifies the original of the application Reason can be in a manner of adopted.It should be understood that presently filed embodiment is not so limited in scope.In appended power In the range of the spirit and terms that profit requires, presently filed embodiment includes many changes, modifications and is equal.

The feature for describing and/or showing for a kind of embodiment can be in a manner of same or similar one or more Used in individual other embodiment, it is combined with the feature in other embodiment, or substitute the feature in other embodiment.

It should be emphasized that term "comprises/comprising" refers to the presence of feature, one integral piece, step or component when being used herein, but simultaneously It is not excluded for the presence or additional of one or more further features, one integral piece, step or component.

Brief description of the drawings

Included accompanying drawing is used for providing being further understood from the embodiment of the present application, which constitutes one of specification Point, for illustrating presently filed embodiment, and come together with word description to explain the principle of the application.Under it should be evident that Accompanying drawing in the description of face is only some embodiments of the present application, for those of ordinary skill in the art, is not paying wound On the premise of the property made is laborious, other accompanying drawings can also be obtained according to these accompanying drawings.In the accompanying drawings:

Fig. 1 is a kind of method flow diagram for organic matter cracking that the embodiment of the present application provides;

Fig. 2 is a kind of functional block diagram of the device for organic matter cracking that the embodiment of the present application provides.

Embodiment

In order that those skilled in the art more fully understand the technical scheme in the application, it is real below in conjunction with the application The accompanying drawing in example is applied, the technical scheme in the embodiment of the present application is clearly and completely described, it is clear that described implementation Example only some embodiments of the present application, rather than whole embodiments.It is common based on the embodiment in the application, this area All other embodiment that technical staff is obtained under the premise of creative work is not made, it should all belong to the application protection Scope.

Fig. 1 is a kind of method flow diagram for organic matter cracking that the embodiment of the present application provides.Although flow bag is described below The multiple operations occurred with particular order are included, but it should be clearly understood that these processes can include more or less operations, These operations sequentially can be performed or performed parallel (such as using parallel processor or multi-thread environment).The embodiment of the present application can By the way that confined laser is installed on ESEM, to be carried out in ESEM using confined laser to organic matter sample Cracking experiment, so as to realize the in-situ study to organic matter sample.As shown in figure 1, methods described includes:

S1:Light path calibration and strength test are carried out to confined laser, obtained with the focusing laser beam for specifying light intensity.

The embodiment of the present application can carry out home position observation based on cracking of the ESEM to organic matter.Carried out to organic matter Before cracking experiment, the embodiment of the present application can first carry out the operation of light path calibration and strength test to confined laser, obtain Take focusing laser beam.Specifically, the confined laser of the embodiment of the present application can include:Laser generator, focusing, light path Reflecting mechanism and light intensity test mechanism, correspondingly, the behaviour that light path calibration and strength test are carried out to confined laser Make, following four steps can specifically be included by obtaining the focusing laser beam with specified light intensity:

S101:Laser beam is produced using the laser generator.

The laser generator that the application uses can be power continuously adjustabe and the optional laser generator of wavelength, its In, the power bracket of institute's book laser generator can be 0.5 to 1.2W, and wavelength can be 1064nm, 532nm or 266nm. In the preferred embodiment of the application one, the power of the laser generator could be arranged to 1W, and wavelength could be arranged to 532nm, this The power and wavelength of sample set the results contrast that cracking can be caused to test preferable.

S102:The laser beam is focused using the focusing.

Laser beam caused by laser generator described in step S101 needs just meet cracking experiment by subsequent treatment Requirement.Specifically, the embodiment of the present application can be focused using the focusing to the laser beam.So, can be with The laser beam for enabling to dissipate originally is focused on a bit, and the focus level of laser beam can be embodied by focusing on beam spot.Specifically Ground, in the preferred embodiment of the application one, the focusing can be lens group, each in the lens group by reconciling Interval between mirror, the focusing beam spot of the laser beam can be adjusted to default size.In the embodiment of the present application, it is described poly- The size of burnt beam spot could be arranged to 1 μm.

S103:Light path calibration is carried out to the laser beam after focusing using light path reflecting mechanism, after ensureing the focusing Laser beam is centrally located at specified location.

In some embodiments, the laser beam can utilize light path reflecting mechanism to the laser after focusing after over-focusing Shu Jinhang light path calibrations, it thereby may be ensured that the laser beam after the focusing is centrally located at specified location.The light path school Light path reflecting mechanism will definitely be passed through to refer to, change the transmission path of the laser beam after the focusing, so as to so that the focusing Laser beam afterwards is centrally located at specified location.In the embodiment of the present application, the specified location can be cracked with fingering row The opening position that the organic matter sample of experiment is put.In the preferred embodiment of the application one, the light path reflecting mechanism can be anti- Mirror is penetrated, by the reflection of minute surface, so as to change the transmission path of the laser beam after the focusing.

S104:Utilize laser of the light intensity test mechanism test after the focusing and the processing of light path reflecting mechanism Beam, and according to the power of the test result regulation laser generator, obtain with the focusing laser beam for specifying light intensity.

During due to being focused mechanism and the processing of light path reflecting mechanism, power loss can be brought to the laser beam, from And the power of laser beam of the power of the laser beam after focusing and light path calibration with being set in step S101 is caused not to be inconsistent.Therefore, The embodiment of the present application is passed through before the laser beam after using the focusing and light path calibration, it is necessary to be tested using light intensity test mechanism The laser beam crossed after the focusing and the processing of light path reflecting mechanism, and the laser generator is adjusted according to test result Power, obtain with the focusing laser beam for specifying light intensity.Specifically, the laser beam that can be detected in real time according to light intensity test mechanism Light intensity, and the light intensity of the detection and specified light intensity are contrasted, but the light intensity of the detection is different from the specified light intensity When, the power output of the laser generator can be adjusted, until the light intensity of the detection is all mutually with the light intensity specified Only.

, can be to obtain the focusing laser beam described in step S1 by the processing of above three step.Focused on After laser beam, it can treat that subsequent step is disposed, it is necessary to using described poly- with the diaphragm of confined laser described in temporary close The diaphragm of the confined laser is opened during burnt laser beam again.

S2:Organic matter sample is pre-processed, obtains scanning electron microscope example.

In the embodiment of the present application, the organic matter sample can select Sichuan Basin Lower Paleozoic strata Bamboo Temple group shale sample Product, before cracking experiment is carried out to the organic matter sample, it can be pre-processed, obtain scanning electron microscope example.Tool Body, the embodiment of the present application can carry out cutting to organic matter sample and drill through, and be carried out to cutting the organic matter sample after drilling through Mechanical polishing and ion beam cross section polishing, and the organic matter sample after processing is defined as scanning electron microscope example.Specific In implementation process, the organic matter sample after the embodiment of the present application drills through to cutting mechanically polishes, organic so as to obtain The smooth flat of quality sample.Further, after carrying out ion beam polishing to the organic matter sample after mechanically polishing, can obtain To the flat surface of organic matter sample.It should be noted that the embodiment of the present application is to organic matter sample when pre-processing, no Need to carry out the surface of organic matter sample the processing for plating conductive layer.Because if conductive layer is plated to the surface of organic matter sample Words, can cause to block to the region subsequently cracked, so as to influence the process of post laser cracking.In the embodiment of the present application, The organic matter sample of conductive layer is not plated when Electronic Speculum is imaged, and electron beam can be utilized to realize, subsequently be had detailed elaboration.

S3:Choose the organic matter region on the scanning electron microscope example.

After scanning electron microscope example is obtained, the embodiment of the present application can choose the organic matter area on the scanning electron microscope example Domain, to be ready for cracking experiment.Specifically, the preferred embodiment of the application one can be by sweeping described in the selection of following three steps Retouch the organic matter region on electron microscopic sample:

S301:The scanning electron microscope example is placed on the sample platform of scanning electronic microscope in ESEM storehouse;

S302:The ESEM storehouse is evacuated storehouse;

S303:The scanning electron microscope example in the vacuum storehouse is imaged using backscattered electron probe, and base Colourity difference in the result of imaging, choose the organic matter region on the scanning electron microscope example.

The scanning electron microscope example can be placed on the sample platform of scanning electronic microscope in ESEM storehouse by the embodiment of the present application, And vacuum imaging pattern is used, choose the organic matter region in the scanning electron microscope example.Specifically, by the ESEM sample After product are placed on the sample platform of scanning electronic microscope in ESEM storehouse, height gas differential pressure can be utilized, the ESEM storehouse is taken out Come true hole capital after selling all securities., can be from the scanning electron microscope example in the backscattered electron probe acquisition vacuum storehouse in the vacuum storehouse Backscatter images.In the backscatter images, there is colourity difference in organic matter with mineral grain, wherein, organic matter is in back scattering Black is shown as in image, mineral grain then shows as grey, can more collect to select black by image recognition mechanism In region.Specifically, an area threshold can be pre-set, when what is identified in the area threshold is black region When, can be so that the area be defined as into organic matter region.For example, it is 5 μ that the embodiment of the present application, which can pre-set area threshold, m2, described image identification mechanism can carry out image recognition on the scanning electron microscope example, when 5 μm2Region in be black During region, follow-up cracking experiment can be remained so that the block area is defined as into organic matter region.

S4:The organic matter region is cracked using the focusing laser beam, and the organic matter region is carried out Real time imagery.

Behind organic matter region on the scanning electron microscope example is selected, the embodiment of the present application can be with the utilization focusing Laser beam cracks to the organic matter region, and carries out real time imagery to the organic matter region, so as in real time The process of observation cracking experiment.Specifically, the preferred embodiment of the application one can be realized by following three steps:

S401:The mobile sample platform of scanning electronic microscope, visited with ensuring that the organic matter region is located at the backscattered electron The underface for the electron beam that hair is penetrated;

S402:The organic matter region is imaged using backscattered electron probe.

The cracking experiment that the embodiment of the present application can select backscattered electron to pop one's head in the organic matter region carries out real-time Imaging, therefore, before cracking experiment is carried out, can move the sample platform of scanning electronic microscope, to ensure the organic matter region Positioned at the underface of the electron beam of backscattered electron probe transmitting, so, the electron beam of backscattered electron probe transmitting can To be projected directly on the organic matter region, so as to be imaged exactly to it.

S403:The focusing laser beam is irradiated on the organic matter region, the organic matter region is cracked.

When carrying out cracking experiment, the embodiment of the present application can open the diaphragm of confined laser, will be adjusted in step S1 Good focusing laser beam is irradiated on the organic matter region, so as to carry out laser pyrolysis to the organic matter region.

It can be utilized for the ease of being more accurately observed to cracking process, in the preferred embodiment of the application one secondary Electronic probe, the organic matter region is imaged, so as to preferably observe the process of cracking experiment.

It should be noted that although selected shale samples in the embodiment of the present application as organic matter sample, but the application Carry out crack experiment in-situ study method be equally applicable in other source rock samples containing organic matter, the application to this not Limit.

The embodiment of the present application also provides a kind of device of organic matter cracking.Fig. 2 is that one kind that the embodiment of the present application provides has The functional block diagram of the device of machine matter cracking.As shown in Fig. 2 described device includes ESEM 100 and positioned at the scanning Laser generator 200, focusing 300 in the sample bin of Electronic Speculum 100, light path reflecting mechanism 400, light intensity test mechanism 500, Wherein:

The laser generator 200, for producing laser beam;

The focusing 300, for being focused to laser beam caused by the laser generator;

The light path reflecting mechanism 400, for adjusting the light path of the laser beam after focusing on, to ensure swashing after the focusing Light beam is centrally located at specified location;

The light intensity test mechanism 500, for testing swashing after the focusing and the processing of light path reflecting mechanism Light beam, and according to the power of the test result regulation laser generator, obtain with the focusing laser beam for specifying light intensity.

Specifically, in the preferred embodiment of the application one, the light path reflecting mechanism 400 can be speculum.

Specifically, in the preferred embodiment of the application one, described device also includes the sample positioned at the ESEM 100 Backscattered electron probe 600 in storehouse, the backscattered electron probe 600 is positioned at sample stage in the scanning electron microscope example storehouse Top and sample stage described in face, for being imaged to the scanning electron microscope example on the sample stage.

The embodiment of the present application is based on ESEM and confined laser, is capable of the cracking process of home position observation organic matter.This The method cracked in ESEM using laser that application proposes is belonged to first.This method is in real observation cracking process The in-situ study method that organic matter structure changes over time with form, can be used for the differentiation of different type organic matter, and not Studied with organic matter oil generation merit rating etc..

The present processes are first extracted relative to by organic matter, are then carried out cracking experiment and are seen again with electron microscope Examine with many advantages:First, organic matter will not produce structural damage because of the heat in extraction process, liquid effect, and not Impurity can be introduced or property changes;Secondly, can be accurately positioned using ESEM, real-time in-situ imaging, organic matter sample exists Do not shifted in whole process, ensure that the accuracy of experiment;Furthermore the energy of confined laser used herein is continuous It is adjustable, different organic matter setup parameters, strong applicability can be directed to.The foundation of this method and subsequent development, may further it promote The evaluation study of organic matter.

As seen through the above description of the embodiments, those skilled in the art can be understood that the application can Realized by the mode of software plus required general hardware platform.Based on such understanding, the technical scheme essence of the application On the part that is contributed in other words to prior art can be embodied in the form of software product.The computer software product It can be stored in storage medium, such as ROM/RAM, magnetic disc, CD, including some instructions are causing a computer equipment (can be personal computer, server, either network equipment etc.) performs some of each embodiment of the application or embodiment Method described in part.

Claims (7)

  1. A kind of 1. method of organic matter cracking, it is characterised in that methods described includes:
    Light path calibration and strength test are carried out to confined laser, obtained with the focusing laser beam for specifying light intensity;
    Organic matter sample is pre-processed, obtains scanning electron microscope example;
    Choose the organic matter region on the scanning electron microscope example;
    Using it is described focusing laser beam the organic matter region is cracked, and to the organic matter region carry out in real time into Picture;
    Wherein, the organic matter region chosen on the scanning electron microscope example includes:
    The scanning electron microscope example is placed on the sample platform of scanning electronic microscope in ESEM storehouse;
    The ESEM storehouse is evacuated storehouse;
    The scanning electron microscope example in the vacuum storehouse is imaged using backscattered electron probe, and the knot based on imaging Colourity difference in fruit, choose the organic matter region on the scanning electron microscope example;
    It is described that the organic matter region is cracked using the focusing laser beam, and the organic matter region is carried out real-time Imaging includes:
    The mobile sample platform of scanning electronic microscope, to ensure that the organic matter region is located at the electricity of backscattered electron probe transmitting The underface of beamlet;
    The organic matter region is imaged using backscattered electron probe;
    The focusing laser beam is irradiated on the organic matter region, the organic matter region is cracked.
  2. 2. the method for organic matter cracking as claimed in claim 1, it is characterised in that the confined laser includes:Laser is sent out Raw device, focusing, light path reflecting mechanism and light intensity test mechanism;
    Correspondingly, it is described that light path calibration and strength test are carried out to confined laser, obtain the focusing with specified light intensity and swash Light beam includes:
    Laser beam is produced using the laser generator;
    The laser beam is focused using the focusing;
    Light path calibration is carried out to the laser beam after focusing using light path reflecting mechanism, to ensure the centre bit of the laser beam after focusing on In specified location;
    The laser beam tested using light intensity test mechanism after the focusing and light path reflecting mechanism processing, and root The power of the laser generator is adjusted according to test result, is obtained with the focusing laser beam for specifying light intensity.
  3. 3. the method for organic matter cracking as claimed in claim 2, it is characterised in that the focusing is lens group, described Light path reflecting mechanism is speculum.
  4. 4. the method for organic matter cracking as claimed in claim 1, it is characterised in that described to be located in advance to organic matter sample Reason, obtaining scanning electron microscope example includes:
    Cutting is carried out to organic matter sample to drill through, and the organic matter sample after drilling through is mechanically polished and ion beam is cut to cutting Mirror polish processing, and the organic matter sample after processing is defined as scanning electron microscope example.
  5. 5. the method for organic matter cracking as claimed in claim 1, it is characterised in that utilizing backscattered electron probe pair After the step of organic matter region is imaged, methods described also includes:
    The organic matter region is imaged using secondary electron probe.
  6. 6. a kind of device of organic matter cracking, it is characterised in that described device includes ESEM and positioned at the scanning electricity Laser generator, focusing, light path reflecting mechanism in the sample bin of mirror, light intensity test mechanism, wherein:
    The laser generator, for producing laser beam;
    The focusing, for being focused to laser beam caused by the laser generator;
    The light path reflecting mechanism, for adjusting the light path of the laser beam after focusing on, to ensure the laser beam after the focusing It is centrally located at specified location;
    The light intensity test mechanism, for testing the laser beam after the focusing and the processing of light path reflecting mechanism, and The power of the laser generator is adjusted according to test result, is obtained with the focusing laser beam for specifying light intensity;
    Wherein, described device also includes the backscattered electron probe in the scanning electron microscope example storehouse, the back scattering electricity Son the probe top of sample stage and sample stage described in face in the sample bin of the ESEM, for the sample stage On scanning electron microscope example be imaged.
  7. 7. the device of organic matter cracking as claimed in claim 6, it is characterised in that the light path reflecting mechanism is speculum.
CN201510436148.4A 2015-07-23 2015-07-23 A kind of method and device of organic matter cracking CN105044079B (en)

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CN107247039A (en) * 2017-07-06 2017-10-13 温州职业技术学院 The Electronic Speculum detection method and device of laser localization irradiation sample Surface Dynamic Processes

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