CN1546976A - Clay or loose rock (sand) slice specimen preparation process - Google Patents
Clay or loose rock (sand) slice specimen preparation process Download PDFInfo
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- CN1546976A CN1546976A CNA2003101159464A CN200310115946A CN1546976A CN 1546976 A CN1546976 A CN 1546976A CN A2003101159464 A CNA2003101159464 A CN A2003101159464A CN 200310115946 A CN200310115946 A CN 200310115946A CN 1546976 A CN1546976 A CN 1546976A
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Abstract
The invention refers to a thin section sampling method for a kind of rock ore verification, especially refers to the quick sampling for clay and loose rock and sand sample. Takes the clay or loose rock (sand) samples fore preprocessing the thin section, uses surface activating agent to foam to preprocess, after beings filter and dried, adds in the bonding agent, firming agent and advancer, vibrates in the vibrator, then it can be grinded into pieces by the miller. It needn't special device, the process is simple, and the flow is short. And it generates no harm gas. The solidification time of original 'glue stewing method' is 1-4 hours, the method only need 20-25 minutes. The invention upgrades the efficiency for 4-10 times.
Description
Technical field:
The thin slice that the present invention relates to a kind of rock, mineral thin slice system of identification quadrat method, particularly clay or loose rock (sand) sample is identified quick sample preparation.
Background technology:
When the geology industry is identified rock forming mineral, at first rock forming mineral preparation of specimen flakiness or mating plate to be observed material composition, optical signature and the structure construction of rock forming mineral then under optical microscope, be described also " naming ".Make thin slice operation be: with microtome sample is downcut the thin slice of prescribed level, after polishing on the wafer lapping machine, is bonded on the microslide, through formalities such as corase grind, fine grinding and polishings, till thickness reaches requirement (0.03mm).For clay and loose rock (sand) sample, grind a definite plane and directly be bonded on the microslide because of can't directly cutting,, promptly sample particle is consolidated with cementing agent so must first make the sample base to sample, form a rigid body, and then operate by the abrasive disc formality.
The sample preparation technology of general clay or loose rock (sand) sample is: sample is not done any surface treatment, directly use rosin paraffin mixed liquor or epoxy resin-triethanolamine curing system as cementing agent, carry out " boiling glue " or perfusion.Through a few hours high temperature (80-130 ℃) digestion or insulation slaking, cooling back forms the sample base and carries out film-making again.
Write when for example introducing clay platelet preparation technology in " mineral rock chip technology made of stones and theoretical foundation " book: " because the loose frangible characteristics of this type of sample tool; therefore; blank can not cut with microtome; can only break a fritter off with one's hand; or lay with adz-eye hammer, or leave behind with hacksaw and to satisfy the soil block for preparing the ordinary sheet size and get final product.With pocket knife or sand paper reconditioning, obtain two planes and the more regular formalness of almost parallel again, just can boil glue then.Can sample gluing firmly be one of film-making key of success, soil block is crashed when preventing to boil the glue boiling, before the digestion earlier with soft tinsel or thin cotton thread with the soil block right-angled intersection tie up, and be a numbering, so that check after boiling glue tying line one end.Clay mineral is exquisiteness especially, and gummy glutinousness is big, is difficult for immersing the soil block deep, often only applies in surperficial skim, and a grinding glue-line comes off slightly, and sample is not as glued, and the meeting imbibition plays bulge, and then becomes plastic ooze.Therefore, select penetrating power strong, the jointing compound that has certain cohesive force again is crucial.Usually use paraffin and this type of sample of rosin epoxy glue digestion, can obtain promising result.In rosin and paraffin 4: 1-5: 1 ratio mixes, be put in the casserde or little aluminum pot of 700ml, place on the electric furnace that has fume extractor and heat, will tie good sample after the liquefaction and put into wherein, digestion 1-2h under fluidized state, deenergization puts pot to outdoor cooling, and glue is cooled to pasty state, when immersing the unlikely outflow of the glue of sample hole, take out sample, separate the bundle rope, put back in the Riker mount.Also available rosin and castor oil (20: 1) mixed liquor digestion, 130 ℃ of temperature, about 15min, temperature is too high, overlong time can cause that clay mineral is rotten.The frangible person's available epoxy glue method of loosing is put into epoxy resin, triethanolamine or other intermixture (liquid) with raw material, put in the vacuum drying chamber, temperature be 80 ℃ ±, about 1-2h, bonding agent can enter in the sample and go, original structure remains unchanged.”
For loose rock sample, " oil geology laboratory manual " is when discussing the making of dirty sandstone, mud stone, shale thin slice, regulation technology is as follows: " this rocks is because poor permeability; glue is difficult for entering, and the rock water absorptivity is strong again, often when heated baking; the rock expanded by heating; water evaporates in addition, is difficult for discharging, and volume increases to be made rock loose into fragment or blow voluntarily.So need infusion method to boil glue, be about to rock and bind with line, put into inherent 80-100 ℃ of glue pot, take out the rock cooling after boiling glue 40min, roughly grind into a plane, boil glue again, generally need boil 2-4 time, glue just can grind the plane.”
For the sand sample strand, introduced following method in " mineral rock chip technology made of stones and theoretical foundation ": " 1, the die cast method: this method has been utilized the good thermoplastic characteristics of jointing material.It is with Powdered plastics and sand sample, a kind of process of compression moulding under hot state.This method is used phenoplast and metal mold usually.Get an amount of sample according to the mold size.In sand sample and 1: 3 ratio of phenoplast, mix.Mold is heated to makes phenoplast when fusing (110-130 ℃), disconnect heating element then, with the sand sample and the plastic powders potpourri of mixing are poured in the mold rapidly in advance, it is spread out, be placed on the bottom equably, and use the module identical, again blank parts is filled it up with plastic powders its compacting with the mold shape, add a cover with forming press and exert pressure, be generally pressing time more than 10 minute.Temperature is very important when opening mold, if temperature is too low, plastics and mineral grain bonding are not firm, come off easily when grinding and polishing; If temperature is too high, plastics will expand (expansion coefficient of plastics is than about big ten times in glass), and mold is damaged.
This method has important disadvantages.Studies show that some mineral (as the sulfide of copper) are unsettled at 110-120 ℃, just bigger to some enhydrite influence; On the other hand, used high pressure can make some brittle mineral chipping, is easy to during grinding and polishing come off; The character of some mineral is morphed.Secondly, device therefor is complicated.
2, casting moulding: with mineral chip and an amount of consolidating material mixing (mineral chip and jointing compound volume 1: 3), pour in the mold, then mold is filled jointing compound,, slowly pour into downwards along glass bar for not disturbance mold bottom mineral chip.If what jointing compound used is liquid casting mold plastics or epoxide-resin glue, must add rigidizer and cold solid promoter before use in proportion, a soupspoon Caseolite liquid plastics adds 3 rigidizers and 3 cold solid promoter.The proportioning of epoxy resin and rigidizer will be decided on the kind of rigidizer.These two kinds of adhesive viscosities are bigger, and bubble is difficult for discharging voluntarily, must be placed in the vacuum several minutes, treat the bubble emptying after, put into the electric dry oven slaking again.Curing temperature is 50-80 ℃, and when the mineral that To Be Protected from Heat were arranged, the control temperature was low.To check amount of cure in the maturing process on time,, if can carve, also must further toast with finger nail portrayal surface, otherwise can viscous mill, treat that nail carves when motionless, i.e. slaking just can disconnect heating element, make its slowly cooling in stove, can't take out,, can cause and break because of cooling is too fast.”
The shortcoming of above-mentioned clay or loose rock (sand) sample sample making technology is: formality is loaded down with trivial details, and the time spent is tediously long, and some method also needs professional equipment.Process is used the naked light heating " to boil glue ", and is both dangerous, produces a large amount of harmful gases again, is unfavorable for environmental protection.For particle tiny clay and rock (sand) sample, the impulsive force when being not enough to tolerate section and grinding because of the consolidation strength with cementing agent usually has the phenomenon that comes off, in addition, with the slaking of need heating of epoxy resin-triethanolamine curing system strand, the time is long, and efficient is low.
Summary of the invention
The objective of the invention is shortcoming and deficiency at above-mentioned prior art, a kind of professional equipment that do not need is provided, technology is simple, operating process is short, and adhesion is strong, difficult drop-off when section and grinding, in operating process, do not need naked light, the sample preparation technology that no harmful gas produces.
The objective of the invention is to realize in the following manner, get clay or loose rock (sand) sample, surface modifier immersion carrying out pre-service with 0.5-5% concentration, after filtration after the oven dry, add cementing agent 5-10 milliliter successively, the hardening agent 0.1-0.3 milliliter of 50-100% concentration, the promoter 0.1-0.3 milliliter of 0.5-2% concentration, stir and shake on the earthquake device of back, take off just can on wafer lapping machine, cut after quiet and grind sheet.
Surface modifier is silane coupling agent or chromium complex coupling agent, and surface modifier and clay or loose rock (sand) sample ratio are 10: 1, and soak time 5-12 minute, concussion was 2-5 minute on the earthquake device, takes off static 15-30 minute; Cementing agent is a unsaturated polyester resin, comprises resins for universal use, casting resin, encapsulate resin, transparent resin and button resin, and hardening agent is methyl ethyl ketone peroxide or cycloethanone peroxide, and promoter is acid resistant cobalt or cobalt naphthenate.
Beneficial effect: with coupling agent the particulate sample surfaces is carried out modification and handle, make and form a contact bed between sample particle and organic adhesive, this coupling agent contact bed one end combines with the inorganic samples particle with chemical bond (or coordination bond, hydrogen bond are arranged simultaneously), other end solubilized is spread in the resin of boundary zone, tangle formation interpentrating polymer network with the big molecular link of resin, thereby improve the impact strength of cutting grain when section.Select the quick cured binders of normal temperature, " boiling glue " method, phenoplast and epoxy resin strand method that former clay or rock (sand) sample casting technology are adopted change in the lump with the quick curing system of unsaturated polyester resin-peroxidating first and second alkane-acid resistant cobalt carries out the strand sample preparation as cementing agent, technological process is simplified, equipment is simple, processing ease, former " boiling glue " method set time is 1-4 hour, only need 20-25 minute with this method, no harmful gas is overflowed, do not endanger environment, operating performance is easy, and the 4-10 that increases work efficiency doubly.
Embodiment:
Embodiment 1:
Getting clay sample 10 grams pours in the 150ml beaker, " KH560 " silicone couplet solution 100ml that adds concentration 2%, dispersed clay when stirring 2 minutes, place in the ultrasonic cleaning machine, it is identical with solution face in the beaker to add water in rinse bath, starts power supply, ultrasonic concussion 10 minutes, take out beaker and filter, the filtration back is standby after drying together with filter paper; The sample that takes by weighing after 2 grams are dried is poured in the 10ml small beaker, smash to pieces with splash bar, add " 196 " unsaturated polyester resin cementing agent 5ml successively, add concentration and be 0.2 milligram of 100% methyl ethyl ketone peroxide, concentration is 0.15 milliliter of 1% acid resistant cobalt, and concussion is 3 minutes on the back earthquake device that stirs, powered-down, place after 25 minutes, taking-up can be cut and be ground sheet.
Embodiment 2:
Take by weighing through clay sample 3 grams of surface modification treatment and oven dry and pour in the 20ml small beaker, smash to pieces with splash bar, add 10 milliliters of casting resins successively, concentration is 0.1 milliliter of 100% methyl ethyl ketone peroxide, concentration is 0.2 milliliter of 1% acid resistant cobalt, and concussion is 3 minutes on the back earthquake device that stirs, powered-down, place after 25 minutes, taking-up can be cut and be ground sheet.
Embodiment 3
Take by weighing loose rock (sand) sample 5 grams and pour in the 100ml beaker, add " KH560 " silicone couplet solution 50ml of 2%, soaked 5 minutes, standby behind the filtering drying.The sample that takes by weighing after 2 grams are dried is poured in the 10ml small beaker, add " S629 " unsaturated polyester resin 6ml successively, 0.15 milliliter of the methyl ethyl ketone peroxide that adds 100% concentration, the acid resistant cobalt that adds 1.5% concentration, 0.1 milliliter, concussion is 3 minutes on the back earthquake device that stirs, powered-down, place after 25 minutes, taking-up can be cut and be ground sheet.
Embodiment 4
Taking by weighing loose rock (sand) sample of 3 grams after surface modification treatment and oven dry pours in the 20ml small beaker, add button resin 8ml successively, 0.3 milliliter of the methyl ethyl ketone peroxide that adds 50% concentration, the acid resistant cobalt that adds 1.0% concentration, 0.25 milliliter, concussion is 3 minutes on the back earthquake device that stirs, powered-down, place after 25 minutes, taking-up can be cut and be ground sheet.
Claims (5)
1. one kind relates to clay or loose rock (sand) thin slice sample preparation technology, it is characterized in that: get clay or loose rock (sand) sample, surface modifier immersion carrying out pre-service with 0.5-5% concentration, after filtration after the oven dry, add cementing agent 5-10 milliliter successively, the hardening agent 0.1-0.3 milliliter of 50-100% concentration, the promoter 0.1-0.3 milliliter of 0.5-2% concentration, shake on oscillator the back that stirs, and takes off just can cut on wafer lapping machine after static to grind sheet.
2. according to described clay of claim 1 or loose rock (sand) thin slice sample preparation technology, it is characterized in that: surface modifier is silane coupling agent or chromium complex coupling agent, surface modifier and clay or loose rock (sand) sample ratio are 10: 1, and soak time is 5-12 minute.
3. according to described clay of claim 1 or loose rock (sand) thin slice sample preparation technology, it is characterized in that: concussion is 2-5 minute on the earthquake device, takes off static 15-30 minute.
4. according to described clay of claim 1 or loose rock (sand) thin slice sample preparation technology, it is characterized in that: cementing agent is a unsaturated polyester resin, and hardening agent is methyl ethyl ketone peroxide or cycloethanone peroxide, and promoter is acid resistant cobalt or cobalt naphthenate
5. according to claim 1,4 described clays or loose rock (sand) thin slice sample preparation technology, it is characterized in that: unsaturated polyester resin comprises resins for universal use, casting resin, encapsulate resin, transparent resin and button resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310115946 CN1253704C (en) | 2003-12-17 | 2003-12-17 | Clay or loose rock (sand) slice specimen preparation process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310115946 CN1253704C (en) | 2003-12-17 | 2003-12-17 | Clay or loose rock (sand) slice specimen preparation process |
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| CN1546976A true CN1546976A (en) | 2004-11-17 |
| CN1253704C CN1253704C (en) | 2006-04-26 |
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| CN 200310115946 Expired - Fee Related CN1253704C (en) | 2003-12-17 | 2003-12-17 | Clay or loose rock (sand) slice specimen preparation process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101158624B (en) * | 2007-11-15 | 2010-09-29 | 中国科学院南京地质古生物研究所 | Preparation method of large area stalactite loaded thin sheet |
| CN101964156A (en) * | 2010-10-31 | 2011-02-02 | 大庆油田有限责任公司 | Long-term preservation method for well 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 |
| CN104515698A (en) * | 2014-12-31 | 2015-04-15 | 包钢集团矿山研究院（有限责任公司） | Method for rapidly polishing polished section |
| CN104973884A (en) * | 2015-06-09 | 2015-10-14 | 云南磷化集团有限公司 | Impregnation treatment method of loose ore |
| CN108847112A (en) * | 2018-09-03 | 2018-11-20 | 中国地质调查局南京地质调查中心 | A kind of science popularization rock core contracting sample column and preparation method thereof |
-
2003
- 2003-12-17 CN CN 200310115946 patent/CN1253704C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101158624B (en) * | 2007-11-15 | 2010-09-29 | 中国科学院南京地质古生物研究所 | Preparation method of large area stalactite loaded thin sheet |
| CN101964156A (en) * | 2010-10-31 | 2011-02-02 | 大庆油田有限责任公司 | Long-term preservation method for well core |
| CN101964156B (en) * | 2010-10-31 | 2012-01-18 | 大庆油田有限责任公司 | Long-term preservation method for well 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 |
| 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 |
| CN104515698A (en) * | 2014-12-31 | 2015-04-15 | 包钢集团矿山研究院（有限责任公司） | Method for rapidly polishing polished section |
| CN104515698B (en) * | 2014-12-31 | 2017-10-17 | 包钢集团矿山研究院（有限责任公司） | A kind of quick method for grinding mating plate |
| CN104973884A (en) * | 2015-06-09 | 2015-10-14 | 云南磷化集团有限公司 | Impregnation treatment method of loose ore |
| CN108847112A (en) * | 2018-09-03 | 2018-11-20 | 中国地质调查局南京地质调查中心 | A kind of science popularization rock core contracting sample column and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1253704C (en) | 2006-04-26 |
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