CN102033004A - Preparation method of pitch microsection - Google Patents
Preparation method of pitch microsection Download PDFInfo
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- CN102033004A CN102033004A CN2009101968540A CN200910196854A CN102033004A CN 102033004 A CN102033004 A CN 102033004A CN 2009101968540 A CN2009101968540 A CN 2009101968540A CN 200910196854 A CN200910196854 A CN 200910196854A CN 102033004 A CN102033004 A CN 102033004A
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Abstract
The invention relates to a preparation method of a pitch microsection, which is a technology for preparing thin sections for microscopic analysis, and is used for solving the problems that the traditional thin section preparation method is troublesome and high in cost. In the method, the characteristics that the heated molten coal pitch has certain cohesive property, thus the volatilization loss does not exist and an internal structure is not damaged when the coal pitch is cooled and then cured are utilized to prepare the thin sections. The preparation method comprises the following specific steps: crushing pitch into particles; putting the pitch particles on a glass slide; heating the pitch particles for dehydrating; after the dehydration, rising the heating temperature so that an analytic sample is softened and melted; putting a coverslip on the analytic sample, and placing a leveling weight above the coverslip to pressurize the analytic sample, so that the analytic sample is in a thin section shape; rising the heating temperature, and stopping after carrying out heat preservation for a time; and naturally cooling the bubble-free analytic sample to obtain the thin section. he preparation method of the thin section, complex steps such as rubber mixing, slicing, grinding, polishing and the like are omitted, and the prepared polished section has the advantages of good planeness, low cost and high efficiency.
Description
Technical field
The present invention relates to a kind of technology for preparing microscopic analysis with thin slice, specifically adopt the method for hot-press solidifying to obtain the microscopic analysis thin slice, to be used for the analysis of organic polymer materials such as pitch.
Background technology
Coal-tar pitch is that present raw material of wood-charcoal material is produced unique alternative cementing agent, and the quality of its quality plays crucial effects to exploitation and the production and the raw material of wood-charcoal material industrial expansion of high-performance carbon material.At present the user has proposed requirement to the index beyond the coal-tar pitch standard, as middle phase content etc.About 300～500 ℃, phase state in the middle of bitumen can occur in pyrolytic process, pre-orientation along with middle phase stage molecule, form tangible anisotropy, the cenotype that forms for the condensed-nuclei aromatics molecule that makes polymerization is stable, under surface tension effects, form ball, claim mesophasespherule (Mesophase beads).When it is grown up to 1～100 μ m, available polarized light microscope observing is to their form.
Mineral, coal petrography often will be made mating plate or thin slice, so that examine under a microscope its optical property.
S.Farooq (Indian Journal of Earth Science, 1989) has introduced a kind of quick and economic mating plate preparation method, and this article is pointed out if the material hole that is used for polishing is few, compact internal structure, and so, it just can directly grind; If the material that is used for polishing loose frangible, the crack is a lot, need that then it is carried out injecting glue and handle.Mineral light preparation of sections: the thin slice that is sawn into 5～6 millimeters thick behind the sample injecting glue. the side that is used for fixing polishes with 800 purpose abrasites, be contained in then on the petrofacies glass sheet, thick through being cut to 0.5mm, come wear down with abrasite again, the thickness that always is ground to sample has only till 60～70 microns.
In GB/T 16773-1997 coal petrography analytic sample preparation method, fine coal must process mix, be pressed into briquet with cementing agent, and then grinds, is polished to mating plate; Lump coal is boiled glue, section, grinding, polishing make the lump coal mating plate; Lump coal by reinforcing, section, grinding, bonding die, grind again, operation such as modification, cover plate laminates.Its step is complicated, and efficient is low, cost is high, operation requires high.
Chinese patent application numbers 200810047917.1 discloses a kind of preparation method and device of soft coal petrography test sample, the steps include: that A. becomes the primary sample product with the coal petrography preparatory processing; B. the primary sample product are placed on the pallet fixing and centering; C. regulate the height of the blade of calibration; D. by bearing device and rotation sample pallet, blade is drawn circle at the test agent end face; E. cutter is scraped the cherry coal test agent along limbus by hand; F. repeat C, D, E step after whenever having scraped one section height; G unclamps sample centering clamping device when scraping to a half that surpasses specimen height, and the part that processes is put into groove, uses fixedly test agent of centering clamping device centering; Step C, D, E above repeating, half part in addition of processing sample finishes until whole test agent preparation.
The mating plate of above prior art or method for preparing slices all bother, and must the step through boiling complexity such as glue, section, grinding, polishing just can make the cost of manufacture height.
Summary of the invention
The objective of the invention is in order to overcome the problem that prior art exists, a kind of easy to make, cost is low, efficient is high pitch microsection preparation method is provided.
The objective of the invention is to be achieved through the following technical solutions:
A kind of pitch microsection preparation method may further comprise the steps:
S1 is broken into graininess with asphalt powder;
S2 places the pitch particulate on the microslide;
S3 carries out thermal dehydration 5～15min to the microslide that is equipped with the pitch particulate, and heating-up temperature is 90～100 ℃;
S4 has taken off and has improved heating-up temperature to 100～130 ℃ behind the water, makes as the softening melting of the pitch particulate of analytic sample;
S5 is put the lastblock cover glass on the analytic sample of melting, add a smooth weight to being in the analytic sample pressurization between microslide and the cover glass at aligning analytic sample place above the cover glass, makes described analytic sample be laminar;
S6 improves heating-up temperature to 120～150 ℃, makes the analytic sample insulation 10～20min of pressurized, stops heating afterwards, unloads smooth weight;
S7 analyzes described analytic sample and has or not bubble, and bubble-free analytic sample is carried out natural cooling, makes thin slice.
The granularity of each particulate is less than 3mm among the described step S1.
Pitch particulate among the described step S2 on the microslide is that 4～8mg is heavy.
The mode of described heating or employing baking oven for heating, or adopt infrared lamp irradiation heating.
Smooth weight among the described step S5 is 10～50g.
Sheet thickness among the described step S5 is 30～50 μ m.
Among the described step S7, alveolate analytic sample is taked following steps:
S71, the described cover glass that slides is to eliminate bubble;
S72 observes described analytic sample and also has or not bubble, and bubble-free analytic sample is carried out natural cooling, makes thin slice;
S73, in the time of can't eliminating bubble, then continue under the temperature of described step S6 heating and the described cover glass that slides to eliminate bubble;
S74 continues the observation analysis sample and also has or not bubble, and bubble-free analytic sample is carried out natural cooling, makes thin slice;
S75 is if also have bubble to need to make again.Beneficial effect of the present invention:
The present invention utilizes coal-tar pitch heating melting, has certain cohesiveness, solidifies during cooling again, does not have volatilization loss this moment, and its inner structure does not have ruined characteristics to make thin slice simultaneously.Make thin slice with this hot-press solidifying method, must be through not over-cooking complicated step such as glue, section, grinding, polishing, and the mating plate of making has the advantage that flatness is good, cost is low, efficient is high.
For further specifying above-mentioned purpose of the present invention, design feature and effect, the present invention is described in detail below with reference to accompanying drawing.
Description of drawings
Fig. 1 is a pitch microsection preparation method process flow diagram of the present invention.
Embodiment
Accompanying drawing below in conjunction with embodiment is elaborated to the specific embodiment of the present invention.
Referring to Fig. 1, Fig. 1 is a pitch microsection preparation method process flow diagram of the present invention, the present invention utilizes coal-tar pitch heating melting, has certain cohesiveness, solidify during cooling again, do not have volatilization loss this moment, its inner structure does not have ruined characteristics to make thin slice simultaneously, be that the present invention adopts the hot-press solidifying method to make thin slice, the concrete following explanation of making step.
S1 is broken into graininess with asphalt powder, and the granularity of each particulate is less than 3mm.
S2 takes by weighing the heavy pitch particulate of 4～8mg and places on the microslide.
S3 carries out thermal dehydration 5～15min to the microslide that is equipped with the pitch particulate, and heating-up temperature is advisable for 90～100 ℃.Heating means can adopt baking oven for heating, and will be equipped with the microslide of pitch particulate and put into baking oven this moment; Also can shine the microslide that is equipped with the pitch particulate with infrared lamp heats.
S4 has taken off and has improved heating-up temperature to 100～130 ℃ behind the water, makes as the softening melting of the pitch particulate of analytic sample, and temperature should not be carried De Taigao, and too high meeting makes the trickling of pitch particulate, the volatilization of melting, can make pitch composition, structural change like this.
S5, on the analytic sample of melting, put the lastblock cover glass, aiming at the smooth weight that the analytic sample place adds a 10～50g above cover glass pressurizes (as adopting counterweight), make analytic sample pressurized between microslide and cover glass of melting, analytic sample is evenly and is as thin as transparent laminarly, the thickness of thin slice is 30～50 μ m.
S6, improve heating-up temperature to 120～150 ℃, generally be higher than 20～40 ℃ of asphalt softening points, make the analytic sample insulation 10～20min of pressurized, stop heating afterwards, unload smooth weight (heat if put into baking oven, take out microslide and cover glass this moment and be in analytic sample between them, and unload smooth weight).
S7 analyzes described analytic sample and has or not bubble.
S71, if bubble arranged, slide lid slide a little is to eliminate bubble.
S72 observes described analytic sample and also has or not bubble.
S73 in the time of can't eliminating bubble, then continues under the temperature of above-mentioned steps S6 heating and slide lid slide to eliminate bubble.
S74 continues the observation analysis sample and also has or not bubble.
S75 is if also have bubble to need to make again.
S8, analytic sample does not have and carries out natural cooling behind the bubble and promptly make thin slice among above-mentioned S7, S72, the S74.
Can be directly after laminating microslide and cover glass and the analytic sample that is between them thereof be together examined under a microscope, conveniently also can be opened cover glass for observing.
Embodiment one
Mid-temperature pitch is crushed to below the granularity 3mm.The pitch particulate that takes by weighing 4mg places on the microslide.Putting into temperature is set is 90 ℃ baking oven thermal dehydration 5min.Taken off and improved heating-up temperature to 105 ℃ behind the water, made analytic sample soften melting.Put cover glass on the melting sample, the top adds a 50g counterweight.Improve temperature to 120 ℃, take out microslide and cover glass behind the insulation 15min and be in analytic sample between them.The slide lid slide is eliminated bubble a little.Print to be analyzed is cooled to thin slice.
Embodiment two
Mid-temperature pitch is crushed to below the granularity 3mm.The pitch particulate that takes by weighing 6mg places on the microslide.Putting into temperature is set is 95 ℃ baking oven thermal dehydration 8min.Taken off and improved heating-up temperature to 110 ℃ behind the water, made analytic sample soften melting.Put cover glass on the melting sample, the top adds a 20g counterweight.Improve temperature to 130 ℃, take out microslide and cover glass behind the insulation 10min and be in analytic sample between them.The slide lid slide is eliminated bubble a little.Print to be analyzed is cooled to thin slice.
Embodiment three
Modified pitch is crushed to below the granularity 3mm.The pitch particulate that takes by weighing 8mg places on the microslide.Putting into temperature is set is 100 ℃ baking oven thermal dehydration 10min.Taken off and improved heating-up temperature to 120 ℃ behind the water, made analytic sample soften melting.Put cover glass on the melting sample, the top adds a 20g counterweight.Improve temperature to 140 ℃, take out microslide and cover glass behind the insulation 20min and be in analytic sample between them.The slide lid slide is eliminated bubble a little.Print to be analyzed is cooled to thin slice.
Embodiment four
Modified pitch is crushed to below the granularity 3mm.The pitch particulate that takes by weighing 8mg places on the microslide.With infrared lamp irradiation thermal dehydration 15min.Taken off and improved heating-up temperature to 130 ℃ behind the water, made analytic sample soften melting.Put cover glass on the melting sample, the top adds a 10g counterweight.Improve temperature to 150 ℃, stop heating behind the insulation 10min, remove counterweight.The slide lid slide is eliminated bubble a little.Print to be analyzed is cooled to thin slice.
Those of ordinary skill in the art will be appreciated that, above embodiment is used for illustrating purpose of the present invention, and be not as limitation of the invention, as long as in essential scope of the present invention, all will drop in the scope of claim of the present invention variation, the modification of the above embodiment.
Claims (7)
1. pitch microsection preparation method is characterized in that may further comprise the steps:
S1 is broken into graininess with asphalt powder;
S2 places the pitch particulate on the microslide;
S3 carries out thermal dehydration 5～15min to the microslide that is equipped with the pitch particulate, and heating-up temperature is 90～100 ℃;
S4 has taken off and has improved heating-up temperature to 100～130 ℃ behind the water, makes as the softening melting of the pitch particulate of analytic sample;
S5 is put the lastblock cover glass on the analytic sample of melting, add a smooth weight to being in the analytic sample pressurization between microslide and the cover glass at aligning analytic sample place above the cover glass, makes described analytic sample be laminar;
S6 improves heating-up temperature to 120～150 ℃, makes the analytic sample insulation 10～20min of pressurized, stops heating afterwards, unloads smooth weight;
S7 analyzes described analytic sample and has or not bubble, and bubble-free analytic sample is carried out natural cooling, makes thin slice.
2. pitch microsection preparation method as claimed in claim 1 is characterized in that:
The granularity of each particulate is less than 3mm among the described step S1.
3. pitch microsection preparation method as claimed in claim 1 is characterized in that:
Pitch particulate among the described step S2 on the microslide is that 4～8mg is heavy.
4. pitch microsection preparation method as claimed in claim 1 is characterized in that:
The mode of described heating or employing baking oven for heating, or adopt infrared lamp irradiation heating.
5. pitch microsection preparation method as claimed in claim 1 is characterized in that:
Smooth weight among the described step S5 is 10～50g.
6. pitch microsection preparation method as claimed in claim 1 is characterized in that:
Sheet thickness among the described step S5 is 30～50 μ m.
7. pitch microsection preparation method as claimed in claim 1 is characterized in that:
Among the described step S7, alveolate analytic sample is taked following steps:
S71, the described cover glass that slides is to eliminate bubble;
S72 observes described analytic sample and also has or not bubble, and bubble-free analytic sample is carried out natural cooling, makes thin slice;
S73, in the time of can't eliminating bubble, then continue under the temperature of described step S6 heating and the described cover glass that slides to eliminate bubble;
S74 continues the observation analysis sample and also has or not bubble, and bubble-free analytic sample is carried out natural cooling, makes thin slice;
S75 is if also have bubble to need to make again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101968540A CN102033004B (en) | 2009-09-30 | 2009-09-30 | Preparation method of pitch microsection |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101968540A CN102033004B (en) | 2009-09-30 | 2009-09-30 | Preparation method of pitch microsection |
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| Publication Number | Publication Date |
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| CN102033004A true CN102033004A (en) | 2011-04-27 |
| CN102033004B CN102033004B (en) | 2012-03-21 |
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| CN2009101968540A Expired - Fee Related CN102033004B (en) | 2009-09-30 | 2009-09-30 | Preparation method of pitch microsection |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033005A (en) * | 2009-09-30 | 2011-04-27 | 上海宝钢化工有限公司 | Preparation method of asphalt sample for microscopic analysis of reflected light |
| CN102495020A (en) * | 2011-11-30 | 2012-06-13 | 长安大学 | Method for determining coal pitch by utilizing infrared spectrogram of coal pitch |
| CN102680294A (en) * | 2012-05-17 | 2012-09-19 | 扬州大学 | Preparation method of modified asphalt fluorescent micro-morphological structure image source sample |
| CN102768812A (en) * | 2011-05-06 | 2012-11-07 | 中国科学院理化技术研究所 | Visualized microscopic model of real core and manufacturing method of visualized microscopic model of real core |
| CN104101525A (en) * | 2014-07-16 | 2014-10-15 | 云南磷化集团有限公司 | Method for rapidly preparing sheet by powdered phosphorite |
| CN104297432A (en) * | 2014-10-22 | 2015-01-21 | 中国石油天然气股份有限公司 | Method for determining resource quantity of deep crude oil cracking gas |
| CN104502168A (en) * | 2014-12-22 | 2015-04-08 | 内蒙古工业大学 | Method for preparing asphalt micro-meso analysis sample by adopting silicone mold |
| CN104568545A (en) * | 2015-01-20 | 2015-04-29 | 中国石油大学(华东) | Manufacturing method of shale rock lamina |
| CN107037239A (en) * | 2016-11-28 | 2017-08-11 | 内蒙古工业大学 | The essence control thermoforming preparation method of bitumen samples is observed suitable for AFM |
| CN108181344A (en) * | 2016-12-08 | 2018-06-19 | 上海宝钢化工有限公司 | The method for measuring solid asphalt softening point |
| CN112798591A (en) * | 2020-12-25 | 2021-05-14 | 国家能源集团宁夏煤业有限责任公司 | Method for analyzing morphology and size of polymer crystal ball |
-
2009
- 2009-09-30 CN CN2009101968540A patent/CN102033004B/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033005B (en) * | 2009-09-30 | 2012-12-26 | 上海宝钢化工有限公司 | Preparation method of asphalt sample for microscopic analysis of reflected light |
| CN102033005A (en) * | 2009-09-30 | 2011-04-27 | 上海宝钢化工有限公司 | Preparation method of asphalt sample for microscopic analysis of reflected light |
| CN102768812B (en) * | 2011-05-06 | 2015-02-11 | 中国科学院理化技术研究所 | Visualized microscopic model of real core and manufacturing method of visualized microscopic model of real core |
| CN102768812A (en) * | 2011-05-06 | 2012-11-07 | 中国科学院理化技术研究所 | Visualized microscopic model of real core and manufacturing method of visualized microscopic model of real core |
| CN102495020A (en) * | 2011-11-30 | 2012-06-13 | 长安大学 | Method for determining coal pitch by utilizing infrared spectrogram of coal pitch |
| CN102680294A (en) * | 2012-05-17 | 2012-09-19 | 扬州大学 | Preparation method of modified asphalt fluorescent micro-morphological structure image source sample |
| CN104101525A (en) * | 2014-07-16 | 2014-10-15 | 云南磷化集团有限公司 | Method for rapidly preparing sheet by powdered phosphorite |
| CN104297432A (en) * | 2014-10-22 | 2015-01-21 | 中国石油天然气股份有限公司 | Method for determining resource quantity of deep crude oil cracking gas |
| CN104502168A (en) * | 2014-12-22 | 2015-04-08 | 内蒙古工业大学 | Method for preparing asphalt micro-meso analysis sample by adopting silicone mold |
| CN104502168B (en) * | 2014-12-22 | 2017-12-05 | 内蒙古工业大学 | The fine method for seeing analysis sample of pitch is prepared using silica gel mould |
| CN104568545A (en) * | 2015-01-20 | 2015-04-29 | 中国石油大学(华东) | Manufacturing method of shale rock lamina |
| CN107037239A (en) * | 2016-11-28 | 2017-08-11 | 内蒙古工业大学 | The essence control thermoforming preparation method of bitumen samples is observed suitable for AFM |
| CN108181344A (en) * | 2016-12-08 | 2018-06-19 | 上海宝钢化工有限公司 | The method for measuring solid asphalt softening point |
| CN112798591A (en) * | 2020-12-25 | 2021-05-14 | 国家能源集团宁夏煤业有限责任公司 | Method for analyzing morphology and size of polymer crystal ball |
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|---|---|
| CN102033004B (en) | 2012-03-21 |
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