CN109856105A - A kind of Microscopic Identification method of clay mineral - Google Patents
A kind of Microscopic Identification method of clay mineral Download PDFInfo
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- CN109856105A CN109856105A CN201711236901.0A CN201711236901A CN109856105A CN 109856105 A CN109856105 A CN 109856105A CN 201711236901 A CN201711236901 A CN 201711236901A CN 109856105 A CN109856105 A CN 109856105A
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- clay mineral
- mineral
- clay
- sample
- laser
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- 239000002734 clay mineral Substances 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 26
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 23
- 239000011707 mineral Substances 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 239000004927 clay Substances 0.000 claims abstract description 10
- 238000004611 spectroscopical analysis Methods 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000004458 analytical method Methods 0.000 claims description 11
- 230000003595 spectral effect Effects 0.000 claims description 11
- 239000011435 rock Substances 0.000 claims description 7
- 238000001237 Raman spectrum Methods 0.000 claims description 5
- 238000001530 Raman microscopy Methods 0.000 claims description 4
- 238000011835 investigation Methods 0.000 claims description 3
- 230000004075 alteration Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000002050 diffraction method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004113 Sepiolite Substances 0.000 description 1
- 230000004523 agglutinating effect Effects 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000021321 essential mineral Nutrition 0.000 description 1
- 229910052900 illite Inorganic materials 0.000 description 1
- 210000000554 iris Anatomy 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 208000007578 phototoxic dermatitis Diseases 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
Abstract
The invention belongs to clay pit and Extract Mineralized Alteration technical fields, and in particular to a kind of Microscopic Identification method of clay mineral, method includes the following steps: step 1: acquisition ore sample；Step 2: the production of light thin slice and rock-mineral determination are carried out to acquisition sample ore；Step 3: Laser Roman spectroscopic analysis of composition is carried out to clay mineral in situ；Step 4: data processing compares Raman spectrogram and carries out precise Identification to clay mineral.The method of the present invention identifies clay mineral using laser Raman spectroscopy, test accuracy is high, it is easy to operate, used time is short, and test accuracy is high, easy to operate, used time is short, the pretreatment process of complex sample is not only avoided, while also disclosing the microcosmic feature of clay mineral and the relationship with other mineral, is laid the foundation to study structure, the origin cause of formation and the clay type of clay mineral.
Description
Technical field
The invention belongs to clay pit and Extract Mineralized Alteration technical fields, and in particular to a kind of Microscopic Identification side of clay mineral
Method.
Background technique
Clay mineral is the hydrous alumino silicates mineral of bedded structure, is the essential mineral component for constituting clay rock, soil,
Mostly in false six sides flake, flakey, mainly with Collections of microparticles body or fibrous output.According to crystal structure, composition characteristic and
Clay mineral can be divided into the mines such as kaolinite race, illite race, montmorillonite race, vermiculite race and sepiolite group by primary optical properties
Object.It is the works such as ceramics, refractory material, cement, papermaking, petrochemical industry, paint, weaving with plasticity, fire resistance and agglutinating property
The important natural material of industry.
Clay mineral grain is fine, generally less than 0.002mm, is partially in colloidal state, visually observes in blocky, earthy,
Also it is difficult accurately to distinguish them under general microscope, and clay mineral may also be similar to the optical property of other mineral,
This just more increases the difficulty for identifying clay mineral.For example, the photosensitiveness feature of pyrophillite and sericite, talcum is more similar, mine
Extract Mineralized Alteration occurs for Shi Ruo, and the two symbiosis together, is easily obscured, do not distinguished not come out substantially under microscope.So usually to borrow
The technological means such as X diffraction analysis and scanning electron microscope are helped to judge, these methods are also practical, effective, but process is more, take
With relatively expensive, pre-treatment carried out to sample and analyzed again, and X diffraction analysis can substantially judge the type of clay mineral,
But it cannot achieve coatings by situ.And now local laser Raman spectrum analysis technology is highly developed, is widely applied
It is studied in petroleum, Ore Deposits, petrology, inclusion enclave etc., but is not directed to judge clay mineral technical field, therefore, research
It is a kind of using local laser Raman spectrum to clay mineral carry out Microscopic Identification method be very significant and effective.
Summary of the invention
It is an object of the invention to solve to judge to cannot achieve original position when clay mineral kind in existing X diffraction analysis technology
The defect of micro-zone analysis provides a kind of Microscopic Identification method of clay mineral.
The technical scheme adopted by the invention is that:
A kind of Microscopic Identification method of clay mineral, method includes the following steps:
Step 1: acquisition ore sample；
Step 2: the production of light thin slice and rock-mineral determination are carried out to acquisition sample ore；
Step 3: Laser Roman spectroscopic analysis of composition is carried out to clay mineral in situ；
Step 4: data processing compares Raman spectrogram and carries out precise Identification to clay mineral.
Step 1 as described above: acquisition ore sample, comprising: field on-the-spot investigation acquires the rock of argillaceous mineral
Sample, sample specification are 3 × 6 × 9cm, and sample is 5 pieces.
Step 2 as described above: the production of light thin slice and rock-mineral determination are carried out to acquisition sample ore, comprising: to the sample ore of acquisition into
Row slice, is fabricated to the light thin slice of 0.3mm, the composition of rock CLAY MINERALS AND THEIR SIGNIFICANCE is observed on microscope, and by clay mineral
The circle of position comes out, and is used for next step Laser Roman spectroscopic analysis of composition.
Step 3 as described above: Laser Roman spectroscopic analysis of composition is carried out to clay mineral in situ, comprising: setting LR laser raman
Analyze Laser-Raman microspectroscopy used, wavelength 532nm, 50~4200cm of scanning range-1, the temperature of test is 25 DEG C,
Humidity is 50%；Smooth thin slice to be measured is placed on microobject platform, transillumination light-seeking is used to clay mineral, by laser
It focuses on the more uniform position of clay mineral, is quickly scanned with dynamically taking spectral model to carry out a wide scope, according to spectral peak
The strong and weak, demand of spectral resolution and clay mineral select the susceptibility of the susceptibility laser power of laser power corresponding
Slit/pinhole width, grating line and laser power；According to test request and clay mineral situation setting respective scanned range,
CCD time for exposure and scanning times are automatically controlled by a computer system and complete scanning.
Step 4 as described above: data processing compares Raman spectrogram and carries out precise Identification to clay mineral, comprising: is right
The data that clay combining measures are handled, and the Raman spectrogram of clay mineral is made, with existing clay mineral in the world
Standard Raman spectroscopy figure compare and analyze, and then the accurate judgement mineral are which kind of clay mineral belonged to.
The beneficial effects of the present invention are:
(1) the Microscopic Identification method for a kind of clay mineral that the present invention designs, gives full play to the advanced of laser Raman spectroscopy
Effect of the technological means on analysis clay mineral, decomposited from complicated paragenetic association of minerals accurate clay mineral and its
Component, the not complicated sample preparation procedure of this method, avoids the generation of error in preparation process, at the same have it is easy to operate,
Minute is short and sensitivity advanced analysis advantage.
(2) the present invention is based on the analyses and processing, ore to Kirghizstan's tower Lars state ore sample experimental data
It the research achievement of CLAY MINERALS AND THEIR SIGNIFICANCE and finds out on the basis of being compared with the clay mineral in other 5 mineral deposits (point)
, cover that wide, validity is good, strong applicability, accuracy are good.
(3) the method for the present invention identifies clay mineral using laser Raman spectroscopy, and test accuracy is high, easy to operate, uses
When it is short, test accuracy is high, and easy to operate, the used time is short, not only avoids the pretreatment process of complex sample, while also disclosing viscous
The microcosmic feature of native mineral and the relationship with other mineral are established to study structure, the origin cause of formation and the clay type of clay mineral
Basis, while also giving a clue to illustrate its substance source and forming environment, and the origin cause of formation and clay for inquiring into clay mineral
Change type all to have very important significance.
Detailed description of the invention
A kind of Fig. 1: flow chart for identifying clay mineral method of the present invention；
Fig. 2: in other of the invention specific embodiments in certain beryllium pyrophillite laser Raman spectroscopy figure.
Specific embodiment
Invention is further described in detail with reference to the accompanying drawings and examples.
As shown in Figure 1, a kind of Microscopic Identification method of clay mineral, method includes the following steps:
Step 1: acquisition ore sample；Field on-the-spot investigation acquires the rock sample of argillaceous mineral, sample specification 3
× 6 × 9cm, sample are 5 pieces.
Step 2: the production of light thin slice and rock-mineral determination are carried out to acquisition sample ore；The sample ore of acquisition is sliced, is fabricated to
The light thin slice of 0.3mm, observes the composition of rock CLAY MINERALS AND THEIR SIGNIFICANCE on microscope, and the circle of position of clay mineral is come out, and uses
In next step Laser Roman spectroscopic analysis of composition.
Step 3: Laser Roman spectroscopic analysis of composition is carried out to clay mineral in situ；It is used micro- sharp that LR laser raman analysis is set
Light Raman spectrometer, it is LABHR-VIS LabRAM HR800 type laser micro-raman spectrometry that LR laser raman, which analyzes instrument,
Instrument, wavelength 532nm, 50~4200cm-1 of scanning range, the temperature of test are 25 DEG C, humidity 50%；By smooth thin slice to be measured
It is placed on microobject platform, transillumination light-seeking is used to clay mineral, it is more uniform that laser is focused on into clay mineral
On position, quickly scanned with dynamically taking spectral model to carry out a wide scope, according to the power of spectral peak, the demand of spectral resolution with
And clay mineral selects corresponding slit/pinhole width, grating line to the susceptibility of the susceptibility laser power of laser power
And laser power；Respective scanned range, CCD time for exposure and scanning times are set according to test request and clay mineral situation,
It is automatically controlled by a computer system and completes scanning.
Step 4: data processing compares Raman spectrogram and carries out precise Identification to clay mineral: surveying to clay combining
The data obtained are handled, and the Raman spectrogram of clay mineral is made, with the standard Raman spectroscopy for having clay mineral in the world
Figure compares and analyzes, and then the accurate judgement mineral are which kind of clay mineral belonged to.
Other specific embodiments are as follows, and invention is further described in detail by taking the ore of certain argillaceous mineral as an example.
Step 1: carrying out field study in the ore area of certain argillaceous mineral, and acquire the ore sample of argillaceous mineral
Product, sample requirement is fresh, generally 3 × 6 × 9cm, and sample size is at least 5 pieces.
Step 2: the production of light thin slice and rock-mineral determination are carried out to the ore of acquisition.Firstly, the ore to acquisition is sliced,
The light thin slice of 0.3mm or so is made, then observes the clay mineral composition of ore on microscope, and by the position of clay mineral
It irises out and, be used for next step Laser Roman spectroscopic analysis of composition.
Step 3: analysis test being carried out to petrographic thin section CLAY MINERALS AND THEIR SIGNIFICANCE using laser Raman spectroscopy.LR laser raman analyzes institute
It is LABHR-VIS LabRAM HR800 type Laser-Raman microspectroscopy with instrument, wavelength 532nm, scanning range 50~
4200cm-1, the temperature of test is 25 DEG C, humidity 50%.According to JY/T002-1996, " laser Raman spectrum analysis method is logical
Then ", the light thin slice by be measured containing clay mineral is placed on microobject platform, and using transillumination light-seeking, laser is gathered
Coke is on the relatively uniform position of clay mineral.First spectral model is taken to carry out the quick scanning an of wide scope with dynamic, according to spectrum
The power at peak, the demand of spectral resolution and clay mineral to the susceptibility of laser power, setting pinhole aperture is 300 μm,
Slit width is 100 μm, grating line is 1200T and laser power≤25% or 10%.According to test request and clay mineral
Situation sets scanning range as 100-4000cm-1, the CCD time for exposure is 10-20s and scanning times are 5-10 times, and by calculating
Machine automatic control system completes scanning.
Step 4: the data that clay combining measures being handled, the Raman spectrogram of clay mineral, such as Fig. 2 is made
It is shown, in order to verify the accuracy of spectrogram, selects 5 clay minerals respectively in 5 petrographic thin sections and carry out Raman spectrum point
Analysis, finally compares and analyzes the Raman spectrogram of measurement and original standard Raman spectroscopy figure in the world, and then accurately sentence
The clay mineral that breaks is pyrophillite.
The present invention is explained in detail above in conjunction with drawings and examples, but the present invention is not limited to above-mentioned implementations
Example, within the knowledge of a person skilled in the art, can also make without departing from the purpose of the present invention
Various change out.The content being not described in detail in the present invention can use the prior art.
Claims (5)
1. a kind of Microscopic Identification method of clay mineral, it is characterised in that: method includes the following steps:
Step 1: acquisition ore sample；
Step 2: the production of light thin slice and rock-mineral determination are carried out to acquisition sample ore；
Step 3: Laser Roman spectroscopic analysis of composition is carried out to clay mineral in situ；
Step 4: data processing compares Raman spectrogram and carries out precise Identification to clay mineral.
2. a kind of Microscopic Identification method of clay mineral according to claim 1, it is characterised in that: the step one:
Acquiring ore sample, comprising: field on-the-spot investigation acquires the rock sample of argillaceous mineral, and sample specification is 3 × 6 × 9cm,
Sample is 5 pieces.
3. a kind of Microscopic Identification method of clay mineral according to claim 1, it is characterised in that: the step 2: right
It acquires sample ore and carries out the production of light thin slice and rock-mineral determination, comprising: the sample ore of acquisition is sliced, the light for being fabricated to 0.3mm is thin
Piece, observes the composition of rock CLAY MINERALS AND THEIR SIGNIFICANCE on microscope, and the circle of position of clay mineral is come out, and is used for next step laser
Raman spectrum analysis.
4. a kind of Microscopic Identification method of clay mineral according to claim 1, it is characterised in that: the step three:
Laser Roman spectroscopic analysis of composition is carried out to clay mineral in situ, comprising: setting LR laser raman analyzes laser micro-raman spectrometry used
Instrument, wavelength 532nm, 50~4200cm of scanning range-1, the temperature of test is 25 DEG C, humidity 50%；Smooth thin slice to be measured is pacified
It is placed on microobject platform, transillumination light-seeking is used to clay mineral, laser is focused on into the more uniform position of clay mineral
Set, quickly scanned with dynamically taking spectral model to carry out a wide scope, according to the power of spectral peak, the demand of spectral resolution and
Clay mineral to the susceptibility of the susceptibility laser power of laser power select corresponding slit/pinhole width, grating line and
Laser power；Respective scanned range, CCD time for exposure and scanning times are set according to test request and clay mineral situation, by
Computer automatic control system completes scanning.
5. a kind of Microscopic Identification method of clay mineral according to claim 1, it is characterised in that: the step 4: number
It according to processing, compares Raman spectrogram and precise Identification is carried out to clay mineral, comprising: the data that clay combining measures are carried out
Processing, is made the Raman spectrogram of clay mineral, compares point with the standard Raman spectroscopy figure for having clay mineral in the world
Analysis, and then the accurate judgement mineral are which kind of clay mineral belonged to.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362636A (en) * | 2020-11-04 | 2021-02-12 | 西安建筑科技大学 | Chlorite mineral species identification method based on Raman spectrum |
| CN112683880A (en) * | 2020-12-28 | 2021-04-20 | 山东大学 | Device and method for rapidly determining mineral content based on Raman spectrum analysis |
| CN115561269A (en) * | 2022-10-21 | 2023-01-03 | 核工业北京地质研究院 | Method for analysing minerals in rock |
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