CN108680471A - A method of alkali-activated carbonatite reaction process is observed and characterized with digital holographic microscope - Google Patents
A method of alkali-activated carbonatite reaction process is observed and characterized with digital holographic microscope Download PDFInfo
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- CN108680471A CN108680471A CN201810322946.8A CN201810322946A CN108680471A CN 108680471 A CN108680471 A CN 108680471A CN 201810322946 A CN201810322946 A CN 201810322946A CN 108680471 A CN108680471 A CN 108680471A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000003513 alkali Substances 0.000 title claims abstract description 26
- 239000010430 carbonatite Substances 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000012190 activator Substances 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000012544 monitoring process Methods 0.000 claims abstract description 4
- 239000000376 reactant Substances 0.000 claims abstract description 3
- 239000012188 paraffin wax Substances 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 230000001427 coherent effect Effects 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 abstract description 17
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000012512 characterization method Methods 0.000 abstract description 2
- 235000019353 potassium silicate Nutrition 0.000 description 17
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 17
- 239000000243 solution Substances 0.000 description 14
- 239000002893 slag Substances 0.000 description 13
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 11
- 239000002994 raw material Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000013005 condensation curing Methods 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000001093 holography Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 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
- 239000010410 layer Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000008844 regulatory mechanism Effects 0.000 description 1
- 238000009666 routine test Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
- G01N15/0227—Investigating particle size or size distribution by optical means using imaging; using holography
- G01N2015/0233—Investigating particle size or size distribution by optical means using imaging; using holography using holography
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Holo Graphy (AREA)
Abstract
The method that the invention discloses a kind of to be observed with digital holographic microscope and characterize alkali-activated carbonatite reaction process.This method includes：（1）Prepare sealing slide：After mixing by reactant and alkali-activator, glass slide is dropped to rubber head dropper, then covered, then seal；（2）Real-time monitoring reaction course in situ, obtains hologram：Sealing slide is placed on the objective table of digital holographic microscope, selectes region to be seen, adjustment focuses to that picture is clear, shoots the hologram in region to be seen；（3）The volume that the hologram of acquisition is obtained to particle different moments by three-dimensional reconstruction and integral and calculating, to calculate rate of dissolution.The present invention provides the holographic microscope technologies for the hologram for generating one or more particulate samples, the three-D profile of scattering and principle of interference reduction particle based on light, the particle of distinguishable nano-grade size；Can in in-situ characterization alkali-activated carbonatite cementitious material system one or more particulate samples rate of dissolution and reaction process.
Description
Technical field
The present invention relates to a kind of testing fields of alkali-activated carbonatite cementitious material reaction process, and in particular to one kind is by digital hologram
Rate of dissolution of the raw materials particles in alkali-activator and anti-is observed and is characterized in the quantitative analysis of the hologram of microscope record
The method for answering process.
Background technology
Alkali-activated carbonatite cementitious material be by with pozzolanic activity or latent hydraulicity raw material and alkali-activator it is anti-
Answer, slurry have gelling, and by after a certain period of time can condensation cure material.Wherein, slag, flyash, metakaolin
It all can serve as the raw material of alkali-activated carbonatite cementitious material system with substances such as carbonate mines.In recent decades, alkali-activated carbonatite gelling material
Material obtains the extensive concern of global construction material researchers, compared with traditional portland cementitious material, alkali-activated carbonatite
Cementitious material is not only using industrial residue or low-grade natural resources as raw material, and its preparation process only needs " mill ", coal
And the comsumption of natural resources such as high-grade lime stone are few, energy consumption consumption is few, and greenhouse gas emissions are low, are more energy-saving and environmentally friendly.Alkali swashs
Hair jelly gel material also shows excellent other than the advantage for having low-carbon environment-friendly in the performances such as intensity, acid-alkali-corrosive-resisting.So
And the reaction mechanism of alkali-activated carbonatite cementitious material is still unintelligible, causes the performance regulatory mechanism of the system unsound.Applied to cement
The conventional test technique of sill, such as XRD, TG and SEM can only characterize the object phase in some stage of reaction system, and cannot be former
The position reaction process of a certain system of real-time characterization and the dissolving precipitation reaction process of quantitatively characterizing reaction rate, especially early stage.
And the reaction of alkali-activated carbonatite cementitious material is concentrated mainly on early stage, late phase reaction rate is slow, therefore the morning of alkali-activated carbonatite cementitious material
Phase reaction process is the key that influence its performance, to its early reaction study extremely important.
For the problem present on, digital holographic microscope can be very good to solve the problems, such as this." holography " refers to object
The all information for the light wave that body is sent out：Both included wavelength (color), amplitude or intensity (light and shade), also including phase (with position phase
It closes).Digital holographic microscope be it is a kind of using interference and diffraction principle, by the characteristic parameter amplitude of Object light wave and phase to interfere
The form of striped is recorded, and makes its reproduction, to form the technology with original stereo-picture true to nature.This skill at present
Art is widely used in the research of three-dimensional position tracking of cell, but does not have been reported that also the technology being applied to cementitious material field
The three-D profile of particle is tracked to characterize alkali-activated carbonatite cementitious material system reaction process.
Invention content
In order to overcome the disadvantages mentioned above and deficiency of the prior art, the purpose of the present invention is to provide one kind can in situ in real time
The test method of alkali-activated carbonatite cementitious material system reaction process is monitored, this method can be with quantitatively characterizing raw materials particles in alkali-activated carbonatite
Rate of dissolution in agent provides effective information for research alkali-activated carbonatite cementitious material system reaction process and kinetics.
The purpose of the present invention can be realized by following technical solution：
A method of alkali-activated carbonatite reaction process is observed and characterized with digital holographic microscope, is included the following steps：(1) it makes
Standby sealing slide：After mixing by reactant and alkali-activator, it draws 3-5 with rubber head dropper and drops to glass slide, then cover
Coverslip, then seal；(2) real-time monitoring reaction course in situ, obtains hologram：Sealing slide is placed on digital hologram to show
On the objective table of micro mirror, region to be seen is selected, adjustment focuses to that picture is clear, shoots the hologram in region to be seen；(3)
The volume that the hologram of acquisition is obtained to particle different moments by three-dimensional reconstruction and integral and calculating, to calculate rate of dissolution,
Analyze reaction process.
Further, step (1) sealing uses paraffin or vacuum resin.
Further, in step (2), the digital holographic microscope includes laser light source and science camera.
Further, the equal and generation at a distance from is dry with coherent source for the object light of the laser light source inclusion phase
It relates to.
Further, the science camera is used for recording the hologram of alkali-activated carbonatite cementitious material system particle reaction process.
Further, in step (3), the three-dimensional reconstruction is analyzed entirely by Rayleigh-Sommerfeld equations
Breath figure；Integral and calculating is obtained by rebuilding the software of particle volume.
Further, method of the invention can also be combined with other routine test means (such as XRD, SEM), characterize object
Phase change and product morphology development, analysis product chemistry ingredient.
Further, when observing and characterize alkali-activated carbonatite process with digital holographic microscope, slide locations, laser light source strength
Degree, focal plane etc. remain unchanged, it is ensured that digital holographic microscope can monitor the anti-of alkali-activated carbonatite cementitious material system in real time in situ
It should dynamic.
Compared with prior art, the invention has the advantages that and technique effect：With existing cementitious material reaction process
Research means are compared, and the advantageous effect of technical scheme of the present invention is that one or more raw material can be monitored in real time in situ
Alkali-activated carbonatite reaction process, morpholoy development and the object phase change of grain are ground for alkali-activated carbonatite cementitious material system reaction mechanism and dynamics
Offer valid data are provided.
Description of the drawings
Fig. 1 is the operating diagram of digital holographic microscope.
Fig. 2 is hologram record and particle outline three-dimensional reconstruction schematic diagram.
Fig. 3 is reaction process hologram of the carbonate mine particle in water glass solution.
Fig. 4 is the three-dimensional reconstruction process schematic of carbonate mine particle.
Fig. 5 is rate of dissolution figure of the carbonate mine particle in water glass solution.
Fig. 6 is reaction process hologram of the granulated blast-furnace slag particle in water glass solution.
Fig. 7 is the three-dimensional reconstruction process schematic of granulated blast-furnace slag particle.
Fig. 8 is rate of dissolution figure of the granulated blast-furnace slag particle in water glass solution.
Specific implementation mode
The method that the present invention relates to a kind of to be observed with digital holographic microscope and characterize alkali-activated carbonatite reaction process.Specifically
Be by alkali-activator and composition granule to be excited in a manner of big water-solid ratio after mixing, mixture is prepared into slide,
It is used in combination paraffin or vacuum grease to seal.Then, slide is placed on the objective table of digital holographic microscope, monitoring in real time in situ is anti-
Process is answered, hologram is shot.The schematic diagram of the digital holographic microscope in this method as shown in Figure 1, as seen from the figure, use
Wavelength is the blue light laser source of 473nm, is divided into two through beam splitter, wherein the laser beam for being pointed into sample is known as object light, another beam
Referred to as reference light.Including the object light of sample three-dimensional information is interfered with reference light, the hologram of formation is got off by cameras record.
Hologram records particle outline three-dimensional reconstruction schematic diagram, as shown in Fig. 2, the hologram for having recorded sample message is soft by computer
Part carries out three-dimensional reconstruction, and three-dimensional reconstruction mode refers to by solving Rayleigh-Sommerfeld equations, and specific equation is as follows
Wherein, Es(r, 0) is the scattered amplitude of focal plane；R=(x, y) is the position on horizontal plane；h-z(r) it is
Rayleigh-Sommerfeld propagation factors；The position that z is vertically oriented.
The result of reconstruction includes plurality of pictures, these pictures are superimposed, the Three-dimensional Gravity composition of sample is constituted,
At this point, the volume of sample particle can be calculated by formula (2)：
Wherein, VtWhen being moment t, the volume of sample particle；SkIt is the area of kth layer；Δ h is the distance of adjacent interlayer；n
For the maximum number of plies, k is the number of plies.
The rate of dissolution of sample particle certain time period can be indicated by formula (3)
Wherein v is rate of dissolution, Vt1And Vt2It is moment t respectively1And t2When, the volume of sample particle；t1And t2It is record sample
Two moment of product hologram.
Embodiment
With reference to embodiment, the present invention will be further described, it should be noted that embodiment is not constituted to this
Invent the limitation of desired protection.
Embodiment 1
Carbonate mine particle is uniformly mixed with alkali-activator water glass solution, 3-5 drop carbonic acid is added dropwise using rubber head dropper
The mixed solution of salt mine and waterglass is to glass slide, and then covered, is sealed using vacuum resin or paraffin, will be prepared
The slide of completion is placed on holographic microscope objective table.Particle to be seen is moved into sighting center and adjusts focal length to suitable shape
State.Laser is two by beam splitter portion, wherein it is object light to be pointed into sample to be tested, another beam is reference light, and two-beam source exists
Microscope focal plane interferes, and is recorded by science camera, and Fig. 3 is carbonate mine particle in water glass solution
Reaction process hologram.Fig. 4 is the three-dimensional reconstruction process schematic of carbonate mine particle, acquired by shown in Fig. 4 (a-c)
Hologram first use Image J to deduct back end, then the process of three-dimensional reconstruction is completed by Matlab, which is based on
Rayleigh-Sommerfeld equations, shown in carbonate mine particle outline result such as Fig. 4 (d-f) of reconstruction, which corresponds to public
Formula (1).It is based on Matlab three-dimensional reconstructions as a result, carry out integral and calculating using Image J, obtain particle different moments body
Product, the process correspond to formula (2).Fig. 5 is rate of dissolution figure of the carbonate mine particle in water glass solution, as shown, logical
The volume change for crossing same particle in calculating certain time can be obtained the rate of dissolution of particle, which corresponds to formula (3).It should
Average dissolution rate of the carbonate mine particle in 12 hours in water glass solution is 75.33 μm3·h-1.In waterglass,
Carbonate mine particle size is gradually reduced as time went on, is in course of dissolution.
Reaction process and rate of dissolution of the 2 granulated blast-furnace slag particle of embodiment in water glass solution
Granulated blast-furnace slag particle is uniformly mixed with alkali-activator water glass solution, 3-5 drops are added dropwise using rubber head dropper
The mixed solution of granulated blast-furnace slag and waterglass is to glass slide, and then covered, close using vacuum resin or paraffin
Envelope will prepare the slide completed and be placed on holographic microscope objective table.Particle to be seen is moved into sighting center and adjusts focal length
To proper states.Laser is two by beam splitter portion, wherein it is object light to be pointed into sample to be tested, another beam is reference light, two
Light source beam is interfered in microscope focal plane, and is recorded by science camera, as Fig. 6 granulated blast-furnace slag particles exist
Shown in reaction process hologram in water glass solution.Fig. 7 is the three-dimensional reconstruction process schematic of granulated blast-furnace slag particle, such as
Shown in Fig. 7 (a-c), obtained hologram first uses Image J to deduct back end, then the mistake of three-dimensional reconstruction is completed by Matlab
Journey, the reconstruction process are based on Rayleigh-Sommerfeld equations, granulated blast-furnace slag particle outline result such as Fig. 7 of reconstruction
(d-f) shown in, which corresponds to formula (1).It is based on Matlab three-dimensional reconstructions as a result, carry out integral and calculating using Image J,
Volume of the particle in different moments is obtained, which corresponds to formula (2).Fig. 8 is granulated blast-furnace slag particle in water glass solution
In rate of dissolution figure, as shown, can be obtained the molten of particle by calculating the volume change of same particle in certain time
Rate is solved, which corresponds to formula (3).Average dissolution of the granulated blast-furnace slag particle in 12 hours in water glass solution
Rate is 1.5 × 105μm3·h-1.In waterglass, granulated blast-furnace slag particle size is gradually reduced as time went on,
In course of dissolution.
Claims (7)
1. a kind of method observed with digital holographic microscope and characterize alkali-activated carbonatite reaction process, which is characterized in that including following
Step：（1）Prepare sealing slide：After mixing by reactant and alkali-activator, glass slide is dropped to rubber head dropper, is then covered
Upper coverslip, then seal；（2）Real-time monitoring reaction course in situ, obtains hologram：Sealing slide is placed on digital hologram
On microscopical objective table, region to be seen is selected, adjustment focuses to that picture is clear, shoots the hologram in region to be seen；
（3）The volume that the hologram of acquisition is obtained to particle different moments by three-dimensional reconstruction and integral and calculating, to calculate dissolving speed
Rate analyzes reaction process.
2. the method as described in claim 1, it is characterised in that step（1）In, the sealing uses paraffin or vacuum resin.
3. the method as described in claim 1, it is characterised in that step（2）In, the digital holographic microscope includes laser light
Source and science camera.
4. method as claimed in claim 3, which is characterized in that the object light of the laser light source inclusion phase is logical with coherent source
The distance crossed is equal and interferes.
5. method as claimed in claim 3, which is characterized in that the science camera is used for recording alkali-activated carbonatite cementitious material system
The hologram of particle reaction process.
6. the method as described in claim 1, it is characterised in that step（3）In, the three-dimensional reconstruction is to pass through Rayleigh-
Sommerfeld equations analyze hologram；Three-dimensional reconstruction result is obtained by Matlab；Integral and calculating is obtained by Image J
It arrives.
7. the method as described in claim 1, it is characterised in that step（1）It is described to drop to glass slide specifically use with rubber head dropper
Rubber head dropper draws 3-5 and drops to glass slide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110108201A (en) * | 2019-04-26 | 2019-08-09 | 华南理工大学 | The high-precision off-axis digital holography microscope equipment and imaging method of transflector double mode |
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