CN105044079A - Method and device for pyrolysis of organic matter - Google Patents

Method and device for pyrolysis of organic matter Download PDF

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Publication number
CN105044079A
CN105044079A CN201510436148.4A CN201510436148A CN105044079A CN 105044079 A CN105044079 A CN 105044079A CN 201510436148 A CN201510436148 A CN 201510436148A CN 105044079 A CN105044079 A CN 105044079A
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China
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laser
organic
focusing
electron microscope
scanning electron
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CN201510436148.4A
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Chinese (zh)
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CN105044079B (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 invention provides a method and device for pyrolysis of organic matter. The method comprises the steps that optical circuit calibration and intensity testing are conducted on a focusing laser to obtain a focusing laser beam with specified light intensity; pretreatment is conducted on an organic matter sample to obtain a scanning electron microscope sample; an organic matter area of the scanning electron microscope sample is selected; pyrolyzing is conducted on the organic matter area by utilizing the focusing laser beam, and real-time imaging is conducted on the organic matter area. According to the method and device for the pyrolysis of the organic matter, on the basis of a scanning electron microscope and the focusing laser, in-situ observation of the pyrolyzing process of the organic matter can be achieved. The method is an in-situ analysis method which really observes changes of the structure and the form of the organic matter along with the time in the pyrolyzing process, and the method can be used for research such as differentiation of different types of organic matter and evaluation of oil generating capacity of different types of the organic matter.

Description

A kind of method of organic cracking and device

Technical field

The application relates to organic quality Geochemistry studying technological domain, the method for particularly a kind of organic cracking and device.

Background technology

Organic geochemistry is a geochemical branch, composition, structure, Origin and evolution organic in main geologize body.Research contents can comprise: organic distribution and type, organic Origin and evolution.Since the sixties, kerogen degradation becomes the origin of oil viewpoint of oil to be widely accepted, people recognize the importance that research is organic, correspondingly in source rock evaluation and OIL SOURCE CORRELATION, carry out large quantity research, and successfully develop a large amount of new method, new technology, comprise the technology such as kerogen maceral lens-belowed identifying, high-resolution electron microscope imaging, kerogen maceration and pyrolysis, chromatography-mass spectroscopy are used in conjunction, nuclear magnetic resonance, can aspect research is organic from microcosmic imaging analysis to the macroscopical pyrolysis of organic matter etc. characteristic.

At present, in the process of carrying out organic cracking, often first organic matter is extracted from sample, carry out cracking experiment further, and then the result after utilizing electron microscope observation cracking to test.

In the process implementing the application, inventor finds prior art, and at least there are the following problems:

First, organicly due to heat, liquid effect and produce structural damage, also to introduce impurity simultaneously thus cause character to change in leaching process; Secondly, first to extract sample, cracking, recycling electron microscope observation, such step can cause sample to shift, and cannot realize in situ imaging, thus cannot ensure the accuracy of experiment.

Above it should be noted that, just conveniently to the technical scheme of the application, clear, complete explanation is carried out to the introduction of technical background, and facilitate the understanding of those skilled in the art to set forth.Only can not think that technique scheme is conventionally known to one of skill in the art because these schemes have carried out setting forth in the background technology part of the application.

Summary of the invention

The object of the embodiment of the present application is the method and the device that provide a kind of organic cracking.

The method of a kind of organic cracking that the embodiment of the present application provides and device are achieved in that

A method for organic cracking, described method comprises:

Light path calibration and strength test are carried out to confined laser, obtains the laser focusing bundle having and specify light intensity;

Pre-service is carried out to organic matter sample, obtains scanning electron microscope example;

Choose the organic region on described scanning electron microscope example;

Utilize described laser focusing bundle to carry out cracking to described organic region, and real time imagery is carried out to described organic region.

A device for organic cracking, described device comprises scanning electron microscope and is positioned at the laser generator of sample bin of described scanning electron microscope, focusing, light path reflecting mechanism, light intensity test mechanism, wherein:

Described laser generator, is used for producing laser beam;

Described focusing, is used for focusing on the laser beam that described laser generator produces;

Described light path reflecting mechanism, is used for adjusting the light path of laser beam after focusing on, and is centrally located at specified location with the laser beam after ensureing described focusing;

Described light intensity test mechanism, is used for testing the laser beam after described focusing and the process of light path reflecting mechanism, and regulates the power of described laser generator according to test result, obtain the laser focusing bundle having and specify light intensity.

The method of a kind of organic cracking that the embodiment of the present application provides and device, based on scanning electron microscope and confined laser, can the cracking process of home position observation organic matter.What the application proposed utilizes laser to carry out the method genus of cracking first in scanning electron microscope.The method really observes the time dependent in-situ study method of organic Structure and morphology in cracking process, may be used for the differentiation of dissimilar organic matter, and the research such as different organic oil generation merit ratings.

The method of the application is first extracted relative to by organic matter, then carry out cracking experiment to carry out observation with electron microscope again there is many-sided advantage: first, organic can not because of the heat in leaching process, liquid effect and produce structural damage, and impurity can not be introduced or character changes; Secondly, utilize scanning electron microscope accurately to locate, real-time in-situ imaging, organic matter sample does not shift in whole process, ensure that the accuracy of experiment; Moreover the energy continuously adjustabe of the confined laser that the application is used, can for the organic setup parameter of difference, and applicability is strong.The foundation of the method and subsequent development, may promote organic evaluation study further.

With reference to explanation hereinafter and accompanying drawing, disclose in detail the particular implementation of the application, the principle specifying the application can adopted mode.Should be appreciated that, thus the embodiment of the application is not restricted in scope.In the spirit of claims and the scope of clause, the embodiment of the application comprises many changes, amendment and is equal to.

The feature described for a kind of embodiment and/or illustrate can use in one or more other embodiment in same or similar mode, combined with the feature in other embodiment, or substitutes the feature in other embodiment.

Should emphasize, term " comprises/comprises " existence referring to feature, one integral piece, step or assembly when using herein, but does not get rid of the existence or additional of one or more further feature, one integral piece, step or assembly.

Accompanying drawing explanation

Included accompanying drawing is used to provide the further understanding to the embodiment of the present application, which constitutes a part for instructions, for illustrating the embodiment of the application, and comes together to explain the principle of the application with text description.Apparently, the accompanying drawing in the following describes is only some embodiments of the application, for those of ordinary skill in the art, under the prerequisite not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.In the accompanying drawings:

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

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

Embodiment

Technical scheme in the application is understood better in order to make those skilled in the art person, below in conjunction with the accompanying drawing in the embodiment of the present application, technical scheme in the embodiment of the present application is clearly and completely described, obviously, described embodiment is only some embodiments of the present application, instead of whole embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not making other embodiments all obtained under creative work prerequisite, all should belong to the scope of the application's protection.

The method flow diagram of a kind of organic cracking that Fig. 1 provides for the embodiment of the present application.Although hereafter describe flow process to comprise the multiple operations occurred with particular order, but should have a clear understanding of, these processes can comprise more or less operation, and these operations can sequentially perform or executed in parallel (such as using parallel processor or multi-thread environment).The embodiment of the present application by being installed in scanning electron microscope by confined laser, can utilizing confined laser to carry out cracking experiment to organic matter sample, thus can realize the in-situ study to organic matter sample in scanning electron microscope.As shown in Figure 1, described method comprises:

S1: carry out light path calibration and strength test to confined laser, obtains the laser focusing bundle having and specify light intensity.

The embodiment of the present application can carry out home position observation based on scanning electron microscope to the cracking of organic matter.Before carrying out cracking experiment to organic matter, the embodiment of the present application first can carry out the operation of light path calibration and strength test to confined laser, obtains laser focusing bundle.Particularly, the confined laser of the embodiment of the present application can comprise: laser generator, focusing, light path reflecting mechanism and light intensity test mechanism, correspondingly, described operation confined laser being carried out to light path calibration and strength test, obtains to have and specifies the laser focusing harness body of light intensity can comprise following four steps:

S101: utilize described laser generator to produce laser beam.

The laser generator that the application adopts can be the laser generator of power continuously adjustabe and wavelength selectable, and wherein, 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 application one preferred embodiment, the power of described laser generator can be set to 1W, and wavelength can be set to 532nm, and it is desirable that such power and wavelength arrange the results contrast that cracking can be made to test.

S102: utilize described focusing to focus on described laser beam.

The laser beam that laser generator described in step S101 produces needs the requirement that just can meet cracking experiment through subsequent treatment.Particularly, the embodiment of the present application can utilize described focusing to focus on described laser beam.Like this, the laser beam of originally dispersing can be enable to focus on a bit, and the focus level of laser beam can be embodied by focused beam acts spot.Particularly, in the application one preferred embodiment, described focusing can be lens combination, through reconciling the interval in described lens combination between each lens, the focused beam acts spot of described laser beam can be adjusted to default size.In the embodiment of the present application, the size of described focused beam acts spot can be set to 1 μm.

S103: utilize light path reflecting mechanism to carry out light path calibration to the laser beam after focusing on, is centrally located at specified location with the laser beam after ensureing described focusing.

In some embodiment, described laser beam, after focusing on, can utilize light path reflecting mechanism to carry out light path calibration to the laser beam after focusing on, thus can ensure the laser beam after described focusing be centrally located at specified location.Described light path calibration can refer to, by light path reflecting mechanism, change the transmission path of the laser beam after described focusing, thus can make the laser beam after described focusing be centrally located at specified location.In the embodiment of the present application, described specified location can the organic matter sample position of putting of fingering row cracking experiment.In the application one preferred embodiment, described light path reflecting mechanism can be catoptron, by the reflection of minute surface, thus can change the transmission path of the laser beam after described focusing.

S104: utilize light intensity test mechanism to test the laser beam after described focusing and the process of light path reflecting mechanism, and regulate the power of described laser generator according to test result, obtain the laser focusing bundle having and specify light intensity.

During owing to carrying out focusing and the process of light path reflecting mechanism, bring power loss can to described laser beam, thus cause the power of the laser beam arranged in the power of the laser beam after focusing and light path calibration and step S101 not to be inconsistent.Therefore, before the laser beam of the embodiment of the present application after using described focusing and light path calibration, need to utilize light intensity test mechanism to test the laser beam after described focusing and the process of light path reflecting mechanism, and the power of described laser generator is regulated according to test result, obtain the laser focusing bundle having and specify light intensity.Particularly, the light intensity of the laser beam that can detect in real time according to light intensity test mechanism, and the light intensity of this detection is contrasted with specifying light intensity, but when the light intensity of described detection is different from described appointment light intensity, the output power of described laser generator can be regulated, till the light intensity of described detection is identical with described light intensity of specifying.

Through the process of above-mentioned three steps, the laser focusing bundle described in step S1 just can be obtained.After obtaining laser focusing bundle, can the diaphragm of confined laser described in temporary close, treat that subsequent step is disposed, need to use described laser focusing Shu Shizai to open the diaphragm of described confined laser.

S2: pre-service is carried out to organic matter sample, obtains scanning electron microscope example.

In the embodiment of the present application, described organic matter sample can select Sichuan Basin Lower Paleozoic strata Bamboo Temple group shale samples, before carrying out cracking experiment to described organic matter sample, can carry out pre-service, obtain scanning electron microscope example to it.Particularly, the embodiment of the present application can be carried out cutting to organic matter sample and be drilled through, and carries out mechanical buffing and ion beam cross section polishing to the organic matter sample after cutting drills through, and the organic matter sample after process is defined as scanning electron microscope example.In specific implementation process, the embodiment of the present application carries out mechanical buffing to cutting the organic matter sample after drilling through, thus can obtain the smooth flat of organic matter sample.Further, after ion beam polishing is carried out to the organic matter sample carried out after mechanical buffing, the flat surface of organic matter sample can be obtained.It should be noted that, the embodiment of the present application, when carrying out pre-service to organic matter sample, does not need the process of carrying out plating conductive layer to the surface of organic matter sample.Because if to the plated surface conductive layer of organic matter sample, can cause follow-up region of carrying out cracking and block, thus affect the process of post laser cracking.In the embodiment of the present application, the organic matter sample not plating conductive layer, when Electronic Speculum imaging, can utilize electron beam to realize, and follow-uply has detailed elaboration.

S3: choose the organic region on described scanning electron microscope example.

After obtaining scanning electron microscope example, the embodiment of the present application can choose the organic region on described scanning electron microscope example, to prepare to carry out cracking experiment.Particularly, the application one preferred embodiment can choose the organic region on described scanning electron microscope example by following three steps:

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

S302: be evacuated described scanning electron microscope storehouse storehouse;

S303: utilize backscattered electron to pop one's head in and imaging is carried out to the described scanning electron microscope example in described vacuum storehouse, and based on the colourity difference in the result of imaging, choose the organic region on described scanning electron microscope example.

Described scanning electron microscope example can be placed on the sample platform of scanning electronic microscope in scanning electron microscope storehouse by the embodiment of the present application, and adopts vacuum imaging pattern, chooses the organic region in described scanning electron microscope example.Particularly, be placed in by described scanning electron microscope example after on the sample platform of scanning electronic microscope in scanning electron microscope storehouse, can utilize height gas differential pressure, be evacuated described scanning electron microscope storehouse storehouse.In this vacuum storehouse, backscattered electron probe can be selected to obtain the backscatter images of the scanning electron microscope example in described vacuum storehouse.In this backscatter images, organic exist colourity difference with mineral grain, and wherein, organicly in backscatter images, show as black, mineral grain then shows as grey, just can select by image recognition mechanism the region that black comparatively concentrates.Particularly, an area threshold can be pre-set, when identify in this area threshold be black region time, just this area can be defined as organic region.Such as, the embodiment of the present application can pre-set area threshold is 5 μm 2, described image recognition mechanism can carry out image recognition on described scanning electron microscope example, when 5 μm 2region in when being black region, just this block area can be defined as organic region, wait until follow-up cracking experiment.

S4: utilize described laser focusing bundle to carry out cracking to described organic region, and real time imagery is carried out to described organic region.

Behind organic region on selected described scanning electron microscope example, the embodiment of the present application just can utilize described laser focusing bundle to carry out cracking to described organic region, and real time imagery is carried out to described organic region, thus the process of cracking experiment can be observed in real time.Particularly, the application one preferred embodiment can be realized by following three steps:

S401: mobile described sample platform of scanning electronic microscope, to guarantee that described organic region is positioned at immediately below described backscattered electron probe ejected electron bundle;

S402: utilize described backscattered electron to pop one's head in and imaging is carried out to described organic region.

The embodiment of the present application can select the cracking experiment of backscattered electron probe to described organic region to carry out real time imagery, therefore, before carrying out cracking experiment, described sample platform of scanning electronic microscope can be moved, to guarantee that described organic region is positioned at immediately below described backscattered electron probe ejected electron bundle, like this, backscattered electron probe ejected electron bundle can directly project on described organic region, thus can exactly to its imaging.

S403: described laser focusing bundle is irradiated on described organic region, cracking is carried out to described organic region.

When carrying out cracking experiment, the embodiment of the present application can open the diaphragm of confined laser, the laser focusing bundle regulated is irradiated on described organic region in step S1, thus can carry out laser pyrolysis to described organic region.

For the ease of observing cracking process more exactly, in the application one preferred embodiment, secondary electron can be utilized to pop one's head in, imaging is carried out to described organic region, thus the process that can cracking observed better to test.

It should be noted that, although selected shale samples as organic matter sample in the embodiment of the present application, the in-situ study method that the application carries out cracking experiment has been equally applicable to other containing in organic source rock sample, and the application does not limit this.

The embodiment of the present application also provides a kind of device of organic cracking.The functional block diagram of the device of a kind of organic cracking that Fig. 2 provides for the embodiment of the present application.As shown in Figure 2, described device comprises scanning electron microscope 100 and is positioned at the laser generator 200 of sample bin of described scanning electron microscope 100, focusing 300, light path reflecting mechanism 400, light intensity test mechanism 500, wherein:

Described laser generator 200, is used for producing laser beam;

Described focusing 300, is used for focusing on the laser beam that described laser generator produces;

Described light path reflecting mechanism 400, is used for adjusting the light path of laser beam after focusing on, and is centrally located at specified location with the laser beam after ensureing described focusing;

Described light intensity test mechanism 500, is used for testing the laser beam after described focusing and the process of light path reflecting mechanism, and regulates the power of described laser generator according to test result, obtain the laser focusing bundle having and specify light intensity.

Particularly, in the application one preferred embodiment, described light path reflecting mechanism 400 can be catoptron.

Particularly, in the application one preferred embodiment, described device also comprises the backscattered electron probe 600 of the sample bin being positioned at described scanning electron microscope 100, described backscattered electron probe 600 is positioned at the top of described scanning electron microscope example storehouse sample stage and just to described sample stage, is used for carrying out imaging to the scanning electron microscope example on described sample stage.

The embodiment of the present application, can the cracking process of home position observation organic matter based on scanning electron microscope and confined laser.What the application proposed utilizes laser to carry out the method genus of cracking first in scanning electron microscope.The method really observes the time dependent in-situ study method of organic Structure and morphology in cracking process, may be used for the differentiation of dissimilar organic matter, and the research such as different organic oil generation merit ratings.

The method of the application is first extracted relative to by organic matter, then carry out cracking experiment to carry out observation with electron microscope again there is many-sided advantage: first, organic can not because of the heat in leaching process, liquid effect and produce structural damage, and impurity can not be introduced or character changes; Secondly, utilize scanning electron microscope accurately to locate, real-time in-situ imaging, organic matter sample does not shift in whole process, ensure that the accuracy of experiment; Moreover the energy continuously adjustabe of the confined laser that the application is used, can for the organic setup parameter of difference, and applicability is strong.The foundation of the method and subsequent development, may promote organic evaluation study further.

As seen through the above description of the embodiments, those skilled in the art can be well understood to the mode that the application can add required general hardware platform by software and realizes.Based on such understanding, the technical scheme of the application can embody with the form of software product the part that prior art contributes in essence in other words.This computer software product can be stored in storage medium, as ROM/RAM, magnetic disc, CD etc., comprising some instructions in order to make a computer equipment (can be personal computer, server, or the network equipment etc.) perform the method described in some part of each embodiment of the application or embodiment.

Claims (10)

1. a method for organic cracking, is characterized in that, described method comprises:
Light path calibration and strength test are carried out to confined laser, obtains the laser focusing bundle having and specify light intensity;
Pre-service is carried out to organic matter sample, obtains scanning electron microscope example;
Choose the organic region on described scanning electron microscope example;
Utilize described laser focusing bundle to carry out cracking to described organic region, and real time imagery is carried out to described organic region.
2. the method for organic cracking as claimed in claim 1, is characterized in that, described confined laser comprises: laser generator, focusing, light path reflecting mechanism and light intensity test mechanism;
Correspondingly, described light path calibration and strength test are carried out to confined laser, obtain to have and specify the laser focusing bundle of light intensity to comprise:
Described laser generator is utilized to produce laser beam;
Described focusing is utilized to focus on described laser beam;
Utilize light path reflecting mechanism to focus on after laser beam carry out light path calibration, with ensure focus on after laser beam be centrally located at specified location;
Utilize light intensity test mechanism to test the laser beam after described focusing and the process of described light path reflecting mechanism, and regulate the power of described laser generator according to test result, obtain the laser focusing bundle having and specify light intensity.
3. the method for organic cracking as claimed in claim 2, is characterized in that, described focusing is lens combination, and described light path reflecting mechanism is catoptron.
4. the method for organic cracking as claimed in claim 1, is characterized in that, describedly carries out pre-service to organic matter sample, obtains scanning electron microscope example and comprises:
Carry out cutting to organic matter sample to drill through, and mechanical buffing and ion beam cross section polishing are carried out to the organic matter sample after cutting drills through, and the organic matter sample after process is defined as scanning electron microscope example.
5. the method for organic cracking as claimed in claim 1, is characterized in that, described in the organic region chosen on described scanning electron microscope example comprise:
Described scanning electron microscope example is placed on the sample platform of scanning electronic microscope in scanning electron microscope storehouse;
Be evacuated described scanning electron microscope storehouse storehouse;
Utilize backscattered electron to pop one's head in and imaging is carried out to the described scanning electron microscope example in described vacuum storehouse, and based on the colourity difference in the result of imaging, choose the organic region on described scanning electron microscope example.
6. the method for organic cracking as claimed in claim 5, is characterized in that, describedly utilizes described laser focusing bundle to carry out cracking to described organic region, and carries out real time imagery to described organic region and comprise:
Mobile described sample platform of scanning electronic microscope, to guarantee that described organic region is positioned at immediately below described backscattered electron probe ejected electron bundle;
Utilize described backscattered electron to pop one's head in and imaging is carried out to described organic region;
Described laser focusing bundle is irradiated on described organic region, cracking is carried out to described organic region.
7. the method for organic cracking as claimed in claim 6, is characterized in that, pop one's head in utilizing described backscattered electron after carrying out the step of imaging to described organic region, described method also comprises:
Utilize secondary electron to pop one's head in and imaging is carried out to described organic region.
8. a device for organic cracking, is characterized in that, described device comprises scanning electron microscope and is positioned at the laser generator of sample bin of described scanning electron microscope, focusing, light path reflecting mechanism, light intensity test mechanism, wherein:
Described laser generator, is used for producing laser beam;
Described focusing, is used for focusing on the laser beam that described laser generator produces;
Described light path reflecting mechanism, is used for adjusting the light path of laser beam after focusing on, and is centrally located at specified location with the laser beam after ensureing described focusing;
Described light intensity test mechanism, is used for testing the laser beam after described focusing and the process of light path reflecting mechanism, and regulates the power of described laser generator according to test result, obtain the laser focusing bundle having and specify light intensity.
9. the device of organic cracking as claimed in claim 8, is characterized in that, described light path reflecting mechanism is catoptron.
10. the device of organic cracking as claimed in claim 8, it is characterized in that, described device also comprises the backscattered electron probe being positioned at described scanning electron microscope example storehouse, described backscattered electron probe is positioned at the top of the sample bin sample stage of described scanning electron microscope and just to described sample stage, is used for carrying out imaging to the scanning electron microscope example on described sample stage.
CN201510436148.4A 2015-07-23 2015-07-23 A kind of method and device of organic matter cracking CN105044079B (en)

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