CN110274806A - A kind of flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant - Google Patents
A kind of flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant Download PDFInfo
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- CN110274806A CN110274806A CN201910557574.1A CN201910557574A CN110274806A CN 110274806 A CN110274806 A CN 110274806A CN 201910557574 A CN201910557574 A CN 201910557574A CN 110274806 A CN110274806 A CN 110274806A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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Abstract
The invention discloses a kind of flaking methods of the ultra-thin inclusion enclave thin slice of high-low temperature resistant: rock sample is dried in baking oven；Configure binder；It is solid that glue is carried out to obtained rock sample with the binder of configuration；Obtained rock sample is subjected to flat surface grinding and plane polishing；Obtained rock sample burnishing surface is pasted on glass slide with binder；Obtained rock sample is sliced, is ground and is polished；Obtained inclusion enclave chip sample is cleaned, is saved.The present invention can make ultra-thin, high-low temperature resistant inclusion enclave thin slice, can, individual small, homogenization temperature high this feature lithology fluid inclusion analysis few to inclusion enclave quantity better inclusion enclave chip sample is provided, further promote the reliability and accuracy of such rock inclusion detection data, for oil-gas migration, accumulation stages research service, it is suitable for inclusion enclave microexamination, thermometric and Fluid Inclusion Compositions LR laser raman constituent analysis.
Description
Technical field
The invention belongs to rock sample preparation fields in oil-gas exploration, and it is super that more specifically, it relates to a kind of high-low temperature resistants
The flaking method of thin inclusion enclave thin slice.
Background technique
Fluid inclusions homogenization temperature, freezing point temperature test and LR laser raman constituent analysis are able to reflect research area oil
Gas accumulation stages, paleocurrent volume property, paleogeotherm paleopressure capture fluid properties, have to Hydrocarbon Formation Reservoirs and oil-gas migration research
Significance.
It is thin to can satisfy conventional inclusion enclave using unloading piece method for 0.08mm-0.1mm for traditional inclusion enclave sheet thickness
Piece qualification requirement, but when clast sandstone partial size is small (thin-hone), inclusion enclave quantity is few, individual smaller (less than 3.5 μm)
When, extreme difficulties are brought to searching second inclusion and inclusion temperature using traditional flaking method.Compare identical lithologic character
Inclusions under rock casting body flake (thickness about 0.03mm) mirror, inclusion enclave abundance and clarity increase bright under casting body flake
Aobvious, therefore, in face of the rock of the above lithologic character, in a certain range, petrographic thin section is thinner, and effect is better.By inclusion enclave piece
It is ideal to be milled to 0.04mm, inclusion enclave is unlikely to abrasion rupture under the thickness, and the inclusion enclave of 2-3um size is high-visible.
Traditional unloading piece method will be difficult to unloading piece for the sample of 0.04mm, unloading piece, take and save during inclusion enclave piece
It is easy to break and wreck.Therefore it needs using not unloading piece method, inclusion enclave is not during the film-making of unloading piece method, usually using 502
Glue carries out consolidation and bonding die, general 502 glue high temperature resistant can only be low temperature resistant to arrive -20 DEG C to 165 DEG C or so, works as survey
When trying temperature higher than 165 DEG C or when being lower than -20 DEG C, 502 glue can melt or solidify failure, cause inclusion enclave thin slice dirty, difficult
To observe inclusion enclave phase-state change and homogenization temperature, freezing point temperature measurement, in addition, 502 glue at high temperature can combustion decomposition life
At hydrogen cyanide, the substance is toxic.It (is generally required when in face of higher homogenization temperature (being greater than 165 DEG C or so) test or freezing point temperature
Be chilled to -100 DEG C, then heating observation) testing requirement when, it is clear that 502 glue are not applied for as consolidating agent and bonding die agent
Inclusion temperature demand in special circumstances above, needs to seek new binder.
Summary of the invention
The present invention few, individual small, this high feature of homogenization temperature for inclusion enclave quantity, proposes that a kind of high-low temperature resistant is ultra-thin
The flaking method of inclusion enclave thin slice, to overcome in the prior art to defect present in the type rock sample inclusion enclave film-making,
Ultra-thin, high-low temperature resistant inclusion enclave thin slice can be made, it being capable of few to inclusion enclave quantity, individual small, this high spy of homogenization temperature
The fluid inclusion analysis for levying lithology provides better inclusion enclave chip sample, further promotes such rock inclusion detection data
Reliability and accuracy are oil-gas migration, accumulation stages research service.
The purpose of the present invention is what is be achieved through the following technical solutions.
The flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant of the present invention, comprising the following steps:
1) rock sample is dried in an oven；
2) binder is configured；
3) it is solid to carry out glue to the rock sample that step 1) obtains for the binder configured with step 2)；
4) rock sample for obtaining step 3) carries out flat surface grinding and plane polishing；
5) the rock sample burnishing surface that step 4) obtains is pasted on glass slide with the binder that step 2) obtains；
6) rock sample for obtaining step 5) is sliced, is ground and is polished；
7) the inclusion enclave chip sample that step 6) obtains cleaned, saved.
The drying temperature of rock sample is 80 DEG C in step 1).
Binder is configured using epoxy resin and curing agent according to the ratio of regulation in step 2), in specific temperature
Lower carry out heating, viscosity reducing.
The epoxy resin and curing agent volume ratio are 100:16, are stirred in mixed process using glass bar single direction
It mixes, 2h in 80 DEG C of baking oven is placed in binder after mixing evenly and carries out heating, viscosity reducing.
Step 3) detailed process: the configured binder of step 2) is poured into the rock sample that step 1) obtains, will
Rock sample after casting is placed in 4h in 80 DEG C of baking oven, is then shut off baking oven Temperature fall.
Step 4) detailed process: the rock sample that step 3) is obtained roughly ground, middle mill, fine grinding, fine grinding, after fine grinding
Rock sample polished on polishing machine with 1 μm of < of polishing fluid, until plane is as bright as a sixpence.
Step 5) detailed process: in the 1 drop configured binder of step 2) of glass slide center drop in paste process, by step
4) the rock sample burnishing surface obtained is affixed on glass slide, gentle pressure, makes that stick glue-line is uniform and thin, bubble-free, then will
Sample is placed under 0.2kg counterweight, and natural cooling cements.
Step 6) detailed process: the rock sample that step 5) obtains is roughly ground, middle mill, fine grinding, the package after fine grinding
Then sample is successively refined and is polished on glass plate and polishing machine, after polishing with a thickness of 0.04-0.05mm by body chip sample
Inclusion enclave chip sample with a thickness of 0.04mm, burnishing surface is as bright as a sixpence.
Inclusion enclave thin slice twin polishing to making, with a thickness of 0.04mm, i.e., quartzy interference colours are that level-one is yellow, show light
It is clean such as mirror, without scratch under microscope.
Step 7) detailed process: will dip in the spirituous writing brush inclusion enclave chip sample that gently outwash step 6) obtains, will
The inclusion enclave chip sample cleaned up is dried up with hair dryer, is fitted into clean plastic sample bag, is posted label.
Compared with prior art, the beneficial effects brought by the technical solution of the present invention are as follows:
Present invention reagent used in entire film-making process is less, only epoxy resin, curing agent and three kinds of alcohol, this hair
250 DEG C bright of binder high temperature resistant >, low temperature resistant < -120 DEG C, can be avoided traditional 502 glue solid glues and bonding die bring without
Method high-low temperature resistant drawback, using not unloading piece method, inclusion enclave sample mill it is thinner, inclusion enclave observe when, the depth of field obviously becomes smaller, 2-3 μ
The small packet body of m is also high-visible, and inclusion enclave translucency and clarity significantly increase, and can be used for multiple times, and avoids unloading piece method
Unloading piece, take and save during the fragmentation of inclusion enclave piece, phenomena such as being badly deformed.
Therefore, the present invention can satisfy that inclusion enclave quantity is few, high this feature rock sample package of the small, homogenization temperature of individual
The preparation demand of sample needed for body sample homogenization temperature, freezing point temperature and LR laser raman constituent analysis.
Specific embodiment
The invention will be further described below.
The flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant of the present invention, comprising the following steps:
(1) it dries sample: rock sample is dried in baking oven.
Rock sample is sequentially placed into the grilled pallet of picture, the position of good each sample is recorded, sample will be housed
Pallet is put into baking oven, and oven temperature is set as 80 DEG C, and constant temperature time 4h, temperature is excessively high, the inclusion enclave in rock sample by
It destroys.It should be noted that when taking out sample after sample drying and wear anti-scald gloves.
(2) binder is configured
Binder uses epoxy resin and curing agent to be configured according to regulation volume ratio for 100:16, needs in mixed process
It is stirred with glass bar single direction, 2h in 80 DEG C of baking oven is placed in binder after mixing evenly and carries out heating drop
It is viscous, the reason is that the mixing stick viscosity is minimum at 80 DEG C, is conducive to glue and consolidate in link stick infiltration hole.
Prepare one, 200mL beaker, according to rock sample situation, measures appropriate epoxy resin and curing agent, epoxy resin
(618 type) and curing agent (triethanolamine) volume ratio are 100:16, need to be stirred with glass bar single direction in mixed process
It mixes, in order to avoid large quantity of air is mixed into mixing stick.Binder after mixing evenly is placed in 80 DEG C of baking oven and is heated
Viscosity reduction.
(3) glue is solid: it is solid to carry out glue with the rock sample that the binder that step (2) configure obtains step (1).
Step (2) configured binder is poured into the rock sample that step (1) obtains, rock core and wall heart sample can
It is directly poured, landwaste can be placed in aluminium lid and be poured by chip sample, and the rock sample after casting is placed in 80 DEG C of baking oven
Middle 4h, is then shut off baking oven Temperature fall, and Temperature fall is conducive to mix stick solidification.
(4) flat surface grinding and polishing: the rock sample that step (3) is obtained carries out flat surface grinding and plane polishing.
The rock sample that step (3) obtains is roughly ground, middle mill, fine grinding, fine grinding, the rock sample after fine grinding is being thrown
It is polished on ray machine with 1 μm of < of polishing fluid, until plane is as bright as a sixpence.
Corase grinding plane: the good rock sample of solid glue is added into water preliminary grinding with No. 100 diamond dust on wafer lapping machine；
Middle flat surface grinding: by the rock sample after preliminary grinding grinding and it is upper mix with No. 400 diamond dust with water in grind, be milled to planar light
It is sliding；
Fine grinding plane: the rock sample behind middle flat surface grinding is milled to planar light with the good diamond dust of W7 and water mixing fine grinding
It is sliding；
Finished plane: it by the rock sample of the good plane of fine grinding, is mixed with W7 diamond dust with water and is refined on a glass, be milled to flat
Until face is bright.
Polishing: the rock sample after fine grinding is polished with the polishing liquid of 1 μ in polishing machine row, it is desirable that the rock sample after polishing is thrown
Smooth surface is bright and clean such as mirror.
The corase grinding, middle mill, fine grinding, fine grinding and polishing link, each link will wash with water clean sample after the completion
Surface can only use the diamond dust of corresponding grade every time, different diamond dust cannot mix.
(5) the rock sample burnishing surface that step (4) obtains bonding die: is pasted onto load glass with the binder that step (2) obtains
On piece.
In 1 drop step (2) configured binder of glass slide center drop, the rock that step (4) is obtained in paste process
Sample burnishing surface is affixed on glass slide, gentle pressure, makes that stick glue-line is uniform and thin, bubble-free, is then placed in sample
Under 0.2kg counterweight, cemented to natural cooling.
The glass slide is single side frosted glass plate, selects ground glass surface to drip gluing sample when bonding die.
(6) it is sliced, is ground and polishes: the rock sample that step (5) obtains is sliced, is ground and is polished.
The rock sample obtained to step (5) roughly ground, middle mill, fine grinding, the inclusion enclave chip sample thickness after fine grinding
For 0.04-0.05mm, then sample is successively refined and polished on glass plate and polishing machine, the inclusion enclave sheet-like after polishing
For product with a thickness of 0.04mm, burnishing surface is as bright as a sixpence.
Slice: the glass slide for gluing rock sample being placed in cutting machine, makes sure to keep in mind to suck sliver surely, gently presses incision
Piece machine, it is careful to cut, ensure to take down sliver after cutting machine stops operating after cutting.
Grinding: grinding is consistent with polishing step and step (4), and the inclusion enclave thin slice twin polishing to making needs
It is to be noted that the print thickness about 0.04mm after polishing, i.e. quartzy interference colours are that level-one is yellow, the bright and clean such as mirror of sample, single polarisation is shown
Under micro mirror mineral grain cleaning it is transparent, without blade scratch, if not up to standard, need to polish again, until satisfied.
Under fluorescent light, burnishing surface is reflective relatively strong, is smooth to the touch for the as bright as a sixpence finger of burnishing surface.
(7) it cleans, save: the inclusion enclave chip sample that step (6) obtains being cleaned, is saved.
The spirituous writing brush inclusion enclave chip sample that gently outwash step (6) obtains, the package that will be cleaned up will be dipped in
Body chip sample is dried up with hair dryer, is fitted into clean plastic sample bag, is posted label.
Although function and the course of work of the invention are described above, the invention is not limited to above-mentioned tools
Body function and the course of work, the above mentioned embodiment is only schematical, rather than restrictive, this field it is common
Technical staff under the inspiration of the present invention, without breaking away from the scope protected by the purposes and claims of the present invention, may be used also
By make it is many in the form of, all of these belong to the protection of the present invention.
Claims (10)
1. a kind of flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant, which comprises the following steps:
1) rock sample is dried in an oven；
2) binder is configured；
3) it is solid to carry out glue to the rock sample that step 1) obtains for the binder configured with step 2)；
4) rock sample for obtaining step 3) carries out flat surface grinding and plane polishing；
5) the rock sample burnishing surface that step 4) obtains is pasted on glass slide with the binder that step 2) obtains；
6) rock sample for obtaining step 5) is sliced, is ground and is polished；
7) the inclusion enclave chip sample that step 6) obtains cleaned, saved.
2. the flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant according to claim 1, which is characterized in that in step 1)
The drying temperature of rock sample is 80 DEG C.
3. the flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant according to claim 1, which is characterized in that in step 2)
Binder is configured using epoxy resin and curing agent according to the ratio of regulation, carries out heating, viscosity reducing within specified temperatures.
4. the flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant according to claim 3, which is characterized in that the epoxy
Resin and curing agent volume ratio are 100:16, are stirred in mixed process using glass bar single direction, to after mixing evenly
Binder be placed in 80 DEG C of baking oven 2h and carry out heating, viscosity reducing.
5. the flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant according to claim 1, which is characterized in that step 3) tool
Body process: the configured binder of step 2) is poured into the rock sample that step 1) obtains, by the rock sample after casting
It is placed in 4h in 80 DEG C of baking oven, is then shut off baking oven Temperature fall.
6. the flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant according to claim 1, which is characterized in that step 4) tool
Body process: the rock sample that step 3) is obtained roughly ground, middle mill, fine grinding, fine grinding, and the rock sample after fine grinding is being polished
It is polished on machine with 1 μm of < of polishing fluid, until plane is as bright as a sixpence.
7. the flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant according to claim 1, which is characterized in that step 5) tool
Body process: in the 1 drop configured binder of step 2) of glass slide center drop, the rock sample that step 4) is obtained in paste process
Burnishing surface is affixed on glass slide, gentle pressure, makes that stick glue-line is uniform and thin, bubble-free, and sample is then placed in 0.2kg weight
Under code, natural cooling is cemented.
8. the flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant according to claim 1, which is characterized in that step 6) tool
Body process: roughly grinding the rock sample that step 5) obtains, middle mill, fine grinding, the inclusion enclave chip sample after fine grinding with a thickness of
Then sample is successively refined and is polished on glass plate and polishing machine by 0.04-0.05mm, the inclusion enclave chip sample after polishing
With a thickness of 0.04mm, burnishing surface is as bright as a sixpence.
9. the flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant according to claim 8, which is characterized in that making
Inclusion enclave thin slice twin polishing, with a thickness of 0.04mm, i.e., quartzy interference colours are that level-one is yellow, show it is bright and clean such as mirror, under microscope
Without scratch.
10. the flaking method of the ultra-thin inclusion enclave thin slice of high-low temperature resistant according to claim 1, which is characterized in that step 7)
Detailed process: the spirituous writing brush inclusion enclave chip sample that gently outwash step 6) obtains, the package that will be cleaned up will be dipped in
Body chip sample is dried up with hair dryer, is fitted into clean plastic sample bag, is posted label.
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| CN113432908A (en) * | 2021-07-05 | 2021-09-24 | 中国石油化工股份有限公司 | Glue scraping method for rock slice production |
| CN113533003A (en) * | 2021-09-16 | 2021-10-22 | 常州欣盛半导体技术股份有限公司 | Slicing manufacturing method for checking cross section of COF (chip on film) carrier tape |
| CN113916621A (en) * | 2020-07-07 | 2022-01-11 | 中国石油化工股份有限公司 | Method for preparing inclusion slice sample and application thereof |
| CN114112563A (en) * | 2020-08-26 | 2022-03-01 | 中国石油天然气股份有限公司 | Loose sandy sediment slice and manufacturing method and application thereof |
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| CN113533003A (en) * | 2021-09-16 | 2021-10-22 | 常州欣盛半导体技术股份有限公司 | Slicing manufacturing method for checking cross section of COF (chip on film) carrier tape |
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