CN110333126A - The preparation method of test sample and the preparation system of test sample - Google Patents
The preparation method of test sample and the preparation system of test sample Download PDFInfo
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- HOOWDPSAHIOHCC-UHFFFAOYSA-N dialuminum tricalcium oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[Al+3].[Al+3].[Ca++].[Ca++].[Ca++] HOOWDPSAHIOHCC-UHFFFAOYSA-N 0.000 description 15
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Classifications
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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
- G01N1/36—Embedding or analogous mounting of samples
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
- G01N23/046—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material using tomography, e.g. computed tomography [CT]
-
- 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
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/366—Moulds; Demoulding
Landscapes
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Theoretical Computer Science (AREA)
- Engineering & Computer Science (AREA)
- Radiology & Medical Imaging (AREA)
- Pulmonology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The present invention relates to the preparation systems of a kind of preparation method of test sample and test sample.The preparation method of above-mentioned test sample includes the following steps: to prepare the different standard slurry of multiple initial water-cement ratios using the raw material for preparing test sample；The different standard slurry of multiple initial water-cement ratios is respectively placed in multiple sampling dies, the practical water-cement ratio of the standard slurry in each sampling die is then tested；According to multiple practical water-cement ratios and multiple initial water-cement ratios, the functional relation of practical water-cement ratio and initial water-cement ratio is established；According to the water-cement ratio of functional relation and test sample, the preparation water-cement ratio of test sample is calculated；According to water-cement ratio is prepared, raw material is configured to sample slurry；Sample slurry is placed in sampling die, test sample is obtained.The test sample that the preparation method of above-mentioned test sample enables to is micron-sized, and size is regular, be can be used in the test of X-ray nanometer CT scan.
Description
Technical field
The present invention relates to cementitious material fields, the system of preparation method and test sample more particularly to a kind of test sample
Standby system.
Background technique
X-ray 3 dimension imaging technology is widely used in the fields such as material, biology, medical treatment already.But in investigation of materials
Field, the sample preparation of high-resolution nanometer x-ray imaging technology, still without unified effective method.Especially in construction material
Research field, the preparation method of the cementitious material sample suitable for high-resolution nanometer x-ray imaging technology, rarer research.
It is main reason is that the more difficult basic demand for meeting high-resolution nanometer x-ray imaging technology of sample prepared.Root
According to the image-forming principle of X-ray, for micron x-ray imaging technology (use light source voltage 40kV~150kV), improve at
The resolution ratio of picture is intended to select the light source of relatively low energy intensity, and the general X-ray energy of nanometer resolution uses
5.4keV, Cr-K α or 8.0keV, Cu-K α reduces unit X-ray radiation quantum amount, and requires to increase the time for exposure, reduces
Sample and light source working distance, thus increase image contrast, raising resolution ratio, but the corresponding imaging that can reduce equipment
Range (FOV, Field of view) simultaneously reduces the thickness of sample that equipment can be imaged.If sample size is larger, beyond imaging
The part of range will not be then imaged by X-ray scanning, and three-dimensionalreconstruction result is caused to generate illusion.The X-ray of low energy intensity is then
Sample can not be penetrated, is detected and is imaged by detector.Therefore for having realized commercial X-ray nanometer CT scan equipment, root
Statement according to langbobier law to x-ray attenuation coefficient, in order to building cementing material realize Nano grade resolution ratio at
Picture reduces three-dimensionalreconstruction image error and improves signal-to-noise ratio, it is necessary to prepare micron-sized cementitious material sample.
The simplest sample preparation methods of tradition are to prepare micron level size by way of beaing, cutting by hand
Sample, and sample is placed on needle point to the preparation step for completing sample, but this method is easy to be artificial to introduce sample
Deformation even slight crack, and sample shape and size are random, irregular.In terms of cementitious material sample preparation, use is also researched and proposed
Goldleaf is obtained by the method cut again after clipping, but the sample shape of this method preparation is irregular, is unfavorable for being imaged；Separately
There is research also to propose the preparation method of the micron order sample sizes of another X-ray nanometer CT scan test, this method directly handle
Cement powders particle is placed on tungsten needle tip, and tungsten needle side is viscous to put the container for filling solution, and be integrally mounted on one compared with
In big polymer pipe, a constant humidity hydrated environment is constructed with this, but this method equally exists the sample shape of preparation
Irregular problem.
Summary of the invention
Based on this, it is necessary to which providing a kind of can make the regular shape of test sample and can be used in X-ray nanometer CT to sweep
Retouch the preparation method of the test sample of test.
In addition, also providing a kind of preparation system of test sample.
A kind of preparation method of test sample, includes the following steps:
The different standard slurry of multiple initial water-cement ratios is prepared using the raw material for preparing test sample, wherein the test
Sample is cementitious material, and the raw material includes solid material and solvent；
The different standard slurry of multiple initial water-cement ratios is respectively placed in multiple sampling dies, then test is each
The practical water-cement ratio of the standard slurry in the sampling die, the internal diameter of the sampling die are micron order；
According to multiple practical water-cement ratios and multiple initial water-cement ratios, establish the practical water-cement ratio and it is described just
The functional relation of beginning water-cement ratio；
According to the water-cement ratio of the functional relation and the test sample, the preparation water-cement ratio of the test sample is calculated；
According to the preparation water-cement ratio, the raw material is configured to sample slurry；And
The sample slurry is placed in the sampling die, the test sample is obtained.
The test sample is X-ray nanometer CT scan test sample in one of the embodiments,.
The internal diameter of the sampling die can less than X-ray nanometer CT scan test in one of the embodiments,
The maximum gauge of the test sample of test.
The standard slurry that multiple initial water-cement ratios are different is respectively placed in multiple in one of the embodiments,
It further include that the X-ray nanometer CT scan tests the test sample that can be tested most before step in sampling die
The determination step of big thickness, the determination step of the maximum gauge include:
The light tested according to the density of the solid material and effective atomic number and the X-ray nanometer CT scan
X-ray energy intensity used by source, according to formulaThe x-ray attenuation coefficient of the solid material is calculated,
Wherein, μ indicates that x-ray attenuation coefficient, ρ indicate density, and Z indicates that effective atomic number, E indicate X-ray energy intensity, and K is normal
Number；
According to equation φ=φ0Exp (- μ D) obtains the X-ray nanometer CT scan and tests the survey that can be tested
The maximum gauge of test agent, wherein φ indicates the photon intensity of outgoing, φ0Indicate incident photon intensity, φ and φ0Ratio
More than or equal to l/e, D is the thickness of the test sample.
It is described according to multiple practical water-cement ratios and multiple initial water-cement ratios in one of the embodiments, it builds
The step of founding the functional relation of the practical water-cement ratio and the initial water-cement ratio include:
According to multiple practical water-cement ratios and multiple initial water-cement ratios, practical water-cement ratio and initial water-cement ratio are established
Relation curve；
The relation curve is subjected to linear fit, the function for obtaining the practical water-cement ratio and the initial water-cement ratio closes
System.
The practical glue of the standard slurry in each sampling die of test in one of the embodiments,
Than the step of in, the practical water-cement ratio of the standard slurry in each sampling die is tested using the method for thermal weight loss.
The standard slurry that the multiple initial water-cement ratio is different is respectively placed in multiple in one of the embodiments,
In step in sampling die, multiple sample preparations are respectively placed in by the standard slurry that vacuum drawn keeps multiple initial water-cement ratios different
Vacuum degree in mold, and during vacuum drawn is identical.
The material of the sampling die is polymer in one of the embodiments,.
A kind of preparation system of test sample, comprising:
Proportioner can install slurry；
Sampling die can install the slurry, and the internal diameter of the sampling die is micron order；
Material device is moved, the slurry in the proportioner can be transferred in the sampling die；And
Test device can test the water-cement ratio of the slurry in the sampling die.
The sampling die can be connected to the proportioner in one of the embodiments, and device packet is expected in the shifting
Connection unit and power unit are included, the connection unit can be connected to the sampling die, and the power unit can be with institute
Connection unit connection is stated, so that the slurry in the proportioner can be extracted in the sampling die.
The sampling die has feed inlet and bleeding point in one of the embodiments, and the feed inlet can be with institute
Proportioner connection is stated, the connection unit includes microsyringe and the connector that is detachably connected with the microsyringe,
The microsyringe can be connected to the power unit, and the connector can be connected to the bleeding point, and the connector
When being connected to the bleeding point, the connector and the sampling die are tightly connected, so that the slurry in the proportioner
Material can be extracted in the sampling die.
The power unit includes vacuum pump in one of the embodiments, and the vacuum pump can be single with the connection
Member connection, so that the slurry in the proportioner can be extracted in the sampling die.
Internal diameter in the preparation method of above-mentioned test sample due to the sampling die used for micron order, obtain
The size of test sample is micron-sized, and the regular shape of test sample, can be used in the test of X-ray nanometer CT scan.And
The preparation method of above-mentioned test sample by the initial water-cement ratio of multiple standard slurries and practical water-cement ratio, establishes practical water first
Glue is than the functional relation with initial water-cement ratio, so as to according to the water-cement ratio of functional relation and test sample to be prepared, meter
Calculation obtains the preparation water-cement ratio of sample slurry, is placed in sampling die to be configured to sample slurry, obtains above-mentioned water-cement ratio
Test sample.And the water-cement ratio of test sample is to being affected in the test of X-ray nanometer CT scan, only known test specimens
The water-cement ratio of product can be such that test sample tests for X-ray nanometer CT scan.Therefore, the preparation method of above-mentioned test sample
It can make that the size for the test sample being prepared is micron-sized, regular shape, and can be used in the survey of X-ray nanometer CT scan
In examination.
Detailed description of the invention
Fig. 1 is the process flow chart of the preparation method of the test sample of an embodiment；
Fig. 2 is the structural schematic diagram of the preparation system of the test sample of an embodiment；
Fig. 3 is respectively tricalcium silicate, dicalcium silicate, tricalcium aluminate for main ingredient in the cement standard product in embodiment 1
When, X-ray penetrates the attenuation length of sample and the graph of relation of X-ray energy；
Fig. 4 be embodiment 1 in cement standard product in main ingredient tricalcium silicate, dicalcium silicate, tricalcium aluminate thickness
When being 65 μm, X-ray penetrates the penetrance of sample and the graph of relation of X-ray energy；
Fig. 5 is the material of the sampling die in embodiment 1 when being PEEK, the attenuation length and X-ray energy of sampling die
Graph of relation；
Fig. 6 is that the material of the sampling die in embodiment 1 is PEEK, when overall diameter is 800 μm, the penetrance of sampling die
With the graph of relation of X-ray energy；
Fig. 7 is the graph of relation of the practical water-cement ratio and initial water-cement ratio in embodiment 1；
Fig. 8 (a) is the location drawing of the nano-indenter test of the A sample in embodiment 1, and Fig. 8 (b) is the nanometer pressure of A sample
The data profile of trace test, Fig. 8 (c) are big-sample data treated the Gauss curve fitting knot of the nano-indenter test of A sample
Fruit figure；
Fig. 9 (a) is the location drawing of the nano-indenter test of the B sample in embodiment 1, and Fig. 9 (b) is the nanometer pressure of B sample
The data profile of trace test, Fig. 9 (c) are big-sample data treated the Gauss curve fitting knot of the nano-indenter test of B sample
Fruit figure (contains sampling die)；
Figure 10 (a) is the image after the B sample three-dimensionalreconstruction in embodiment 1, and Figure 10 (b), Figure 10 (c) and Figure 10 (d) divide
Not Wei image in Figure 10 (a) after B sample three-dimensionalreconstruction three different directions 2 dimension sectioning images；
Figure 11 (a), Figure 11 (b) are respectively the 3 d image after the B sample three-dimensionalreconstruction in embodiment 1 is different degrees of.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with specific embodiment to invention is more fully described.Tool
Preferred embodiment of the invention is given in body embodiment.But the invention can be realized in many different forms,
It is not limited to the examples described herein.On the contrary, purpose of providing these embodiments is makes to the disclosure
Understanding it is more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
Body embodiment purpose, it is not intended that in limitation the present invention.
It should be noted that herein to sample slurry mixing when incorporation time there is no particular provisions, using this field
Hybrid mode known to technical staff.
There is no particular provisions to the X-ray nanometer CT scan equipment herein, using known to those skilled in the art
X-ray nanometer CT scan equipment.
Referring to Fig. 1, the preparation method of the test sample of an embodiment, includes the following steps:
Step S110: the different standard slurry of multiple initial water-cement ratios is prepared using the raw material for preparing test sample, wherein
Test sample is cementitious material, and raw material includes solid material and solvent.
Wherein, test sample is X-ray nanometer CT scan test sample.Initial water-cement ratio refers to: in process for preparation, solvent
With the weight ratio of solid material.Specifically, in the present embodiment, solvent is water.Solid material can be tricalcium silicate, silicic acid
Dicalcium etc..
Step S120: the different standard slurry of multiple initial water-cement ratios is respectively placed in multiple sampling dies, is then surveyed
The practical water-cement ratio of the standard slurry in each sampling die is tried, the internal diameter of sampling die is micron order.
Specifically, the different standard slurry of multiple initial water-cement ratios is respectively placed in the step in multiple sampling dies,
It is respectively placed in multiple sampling dies by the standard slurry that vacuum drawn keeps multiple initial water-cement ratios different, and vacuum drawn mistake
Vacuum degree in journey is identical.In step S120, multiple standard slurries are entered into sampling die by vacuum drawn, are because making
The internal diameter of original mold tool is micron order, according to the mode directly extracted, it is more difficult to it extracts, and the time extracted is longer, and extract
The time longer solidification etc. that will cause standard slurry, and can not continue to be drawn into sampling die.Therefore, using vacuum drawn
Mode enters standard slurry in sampling die.Specifically, the time of vacuum drawn is 3min.
Further, the standard slurry for making multiple initial water-cement ratios different is by vacuum drawn into multiple sampling dies
Vacuum degree in step is identical.This is because vacuum degree is different, the reality of obtained standard sample under same initial water-cement ratio
Water-cement ratio is different.Therefore, when studying the relationship of practical water-cement ratio and initial water-cement ratio, set identical for vacuum degree, to make
Practical water-cement ratio is only related to initial water-cement ratio.
Wherein, practical water-cement ratio refers to: in sampling die, the weight ratio of water and solid material in standard slurry.
Specifically, in the step of testing the practical water-cement ratio of the standard slurry in each sampling die, using thermal weight loss
Method tests the practical water-cement ratio of the standard slurry in each sampling die.
Further, the step of testing the practical water-cement ratio of each standard slurry using the method for thermal weight loss include:
Solid material is tested, the benchmark weight-loss ratio curve of solid material is obtained；
Sampling die is tested, the benchmark weight-loss ratio curve of sampling die is obtained；
Standard sample is tested, the weight-loss ratio curve to get standard samples, and according to the benchmark of solid material weightlessness
The benchmark weight-loss ratio curve of rate curve and sampling die is corrected the weight-loss ratio curve of standard sample, and get standard samples school
Weight-loss ratio curve after just；
Weight-loss ratio curve after according to standard sample correction, the practical water-cement ratio to get standard samples.
Further, it is tested in above-mentioned test process using thermogravimetic analysis (TGA) equipment.
Specifically, the material of sampling die is polymer.Further, polymer is polyimide or polyether-ether-ketone.By
It can almost disregard in the x-ray attenuation coefficient of polymer, therefore, select the sampling die of polymer material as test sample
Installation container, test sample can be made for when testing, sampling die influences almost negligible to disregard on the result of test.
Sampling die is cylindrical shape.The internal diameter of sampling die be micron order, the test sample enabled to with a thickness of
It is micron-sized, and regular shape, and sampling die is cylindrical shape, when for the test of X-ray nanometer CT scan, to three-dimensional
It is scanned, to reconstruct the 3-D image of test sample.
Further, the internal diameter of sampling die is less than the maximum gauge of the test sample of X-ray nanometer CT scan test.Its
In, when maximum gauge refers to the test of X-ray nanometer CT scan, X-ray is incident from test sample and can be from test sample injection
Maximum distance.The maximum gauge of the test sample of X-ray nanometer CT scan test is micron order.Specifically, before step S120,
It further include the determination step of the maximum gauge for the test sample that the test of X-ray nanometer CT scan can be tested.Specifically, maximum thick
The determination step of degree includes:
The light source institute tested according to the density of solid material and effective atomic number and the X-ray nanometer CT scan
The X-ray energy intensity of use, according to formulaThe x-ray attenuation coefficient of solid material is calculated, wherein μ table
Show that x-ray attenuation coefficient, ρ indicate density, Z indicates that effective atomic number, E indicate X-ray energy intensity, and K is constant；
According to equation φ=φ0Exp (- μ D) obtains the test sample that the test of X-ray nanometer CT scan can be tested
Maximum gauge, wherein φ indicates the photon intensity of outgoing, φ0Indicate incident photon intensity, φ and φ0Ratio be greater than or wait
In 1/e, D is the thickness of test sample.
Wherein, when sample is by a variety of former molecular compounds, using effective atomic number, effective atomic number
The following formula of calculation basis:
In formula, fiThe power accounted in the entire total ectonuclear electron number of compound chemical formula for the ectonuclear electron number of i-th kind of atom
Compare again, ZiFor the atomic number of i-th kind of atom.
When the solid material of test sample is multiple compounds, the X-ray of each solid material compound is calculated separately
Attenuation coefficient, maximum x-ray attenuation coefficient is for being calculated most in the x-ray attenuation coefficient of multiple solid material compounds
Big thickness.
Herein, formulaIt is obtained by μ/ρ=a+b × (Z^3.8/E^3.2) simplification.For common solid
Raw material, K value are about 1.4 × 10-3。
Further, the internal diameter of sampling die is set smaller than X-ray nanometer CT scan and tests the sample that can be tested
Maximum gauge, test sample can be made to be placed in sampling die, be used for X-ray nanometer CT scan when, X-ray nanometer CT is swept
Retouch test X-ray can inter-hole testing sample, and test sample is fully fallen in the areas imaging of X-ray nanometer CT scan,
So as to pore structure, the material composition etc. for clearly studying test sample nanoscale.
Common X-ray nanometer CT scan equipment, X-ray monochromatic source energy have 5.4keV, 6.4keV and 8.0keV.When
It is the ordinary silicon of tricalcium silicate, dicalcium silicate and tricalcium aluminate etc. for main component when X-ray monochromatic source energy is 8keV
Acid salt cement, it is assumed that porosity zero, then the section ruler for the ordinary portland cement that X-ray nanometer CT scan equipment can test
Very little is 60 μm~150 μm.
Step S130: according to multiple practical water-cement ratios and multiple initial water-cement ratios, practical water-cement ratio and initial glue are established
The functional relation of ratio.
Specifically, step S130 includes:
According to multiple practical water-cement ratios and multiple initial water-cement ratios, the relationship for establishing practical water-cement ratio and initial water-cement ratio is bent
Line；
Relation curve is subjected to linear fit, establishes the functional relation of practical water-cement ratio and initial water-cement ratio.
By establishing the functional relation of practical water-cement ratio and initial water-cement ratio, it is easy to implement the water to the test sample of preparation
Glue ratio it is controllable.For example, the test sample of a certain target water-cement ratio is prepared, it can be first according to practical water-cement ratio and initial water-cement ratio
Relation curve, obtain preparation water-cement ratio corresponding to the target water-cement ratio, be then configured to the raw material for preparing test sample
The preparation water-cement ratio, is subsequently placed in sampling die, obtains the test sample of target water-cement ratio, to realize the survey to preparation
The water-cement ratio of test agent it is controllable.
Step S140: according to the water-cement ratio of functional relation and test sample, the preparation water-cement ratio of test sample is calculated.
Wherein, water-cement ratio is prepared are as follows: in process for preparation, the weight ratio of solvent and solid material.It can by step S140
Obtain the preparation water-cement ratio of test sample.
Step S150: according to water-cement ratio is prepared, raw material is configured to sample slurry.
Specifically, raw material is configured to sample slurry according to above-mentioned preparation water-cement ratio by solid material and solvent.
Step S160: sample slurry is placed in sampling die, obtains test sample.
Wherein, sample slurry is placed in sampling die by vacuum drawn.Further, true during vacuum drawn
Reciprocal of duty cycle is identical as the vacuum degree during vacuum drawn in step S120.This is because vacuum degree is different, obtained practical water
Glue is more different than from the functional relation of initial water-cement ratio, could be according to above-mentioned functional relation and water only under identical vacuum degree
Glue ratio obtains the preparation water-cement ratio of test sample.
By the preparation method of above-mentioned test sample, the test sample enabled to is micron order size, and shape is advised
Then, water-cement ratio is controllable.
About the preparation of X-ray nanometer CT scan test sample, there is researcher to propose a kind of preparation method, the party
Method uses focused ion beam technology (Focus Ion Beam, FIB), can suitable for the excision forming of most of samples
Bombardment under nano-precision through ion beam accurately prepares sample, however this method equipment is expensive, and is only applicable to have in itself
The sample of some strength, and be not suitable for still being in the gelling sample at hydration reaction initial stage, be also not suitable for powder sample.Separately have
A kind of preparation method of micron order sample sizes for being useful in the test of X-ray nanometer CT scan is researched and proposed, this method is by swashing
Light polishes to the cylindrical sample of rotation, and size is only applicable to have some strength in itself up to 30 μm, but as FIB
Sample, and laser can leave the trace of deformation in the sample surfaces that preparation is completed, and influence result judgement.Research points out, lithium battery
The impacted range of cathode material is 10 μm.The preparation method for being traditionally used for the test sample of X-ray nanometer CT scan test obtains
The size of the test sample arrived is irregular, is easy to cause to deform to test sample surface, and the applicability of preparation method has centainly
Restriction.
And the preparation method of above-mentioned test sample has at least the following advantages:
(1) test sample that the preparation method of above-mentioned test sample enables to is having a size of micron order and regular shape.
(2) test sample that the preparation method of above-mentioned test sample is prepared can be used in the survey of X-ray nanometer CT scan
In examination, to analyze the structure of the nanoscale of test sample, material composition etc..
(3) preparation method of above-mentioned test sample is reproducible.
(4) preparation method of above-mentioned test sample will not leave the trace of deformation on the surface of test sample, and will not shadow
Ring result of the obtained test sample in being tested.
(5) preparation method of above-mentioned test sample can be used in the gelling sample at hydration reaction initial stage, and to the strong of sample
There is no limit for degree.
Referring to Fig. 2, the preparation system 10 of the test sample of an embodiment, including proportioner 100, sampling die
200, material device 300 and test device (not shown) are moved.
Wherein, proportioner 100 can install slurry.Specifically, slurry includes sample slurry and standard slurry.Sample slurry
Material and standard slurry are formulated by the raw material for preparing test sample.Standard slurry have it is multiple, multiple standard slurries it is initial
Water-cement ratio is different.
Specifically, proportioner 100 can be stirring pool.
Sampling die 200 can install above-mentioned slurry.Specifically, the internal diameter of sampling die 200 is micron order.Sampling die
200 be cylindrical shape.
Set cylindric for sampling die 200, and the internal diameter of sampling die 200 is micron order, the survey enabled to
The size of test agent is micron-sized, and regular shape, can be used in the test of X-ray nanometer CT scan, and receive for X-ray
When rice CT scan test, three-dimensional can be scanned, to reconstruct the 3-D image of test sample.
Further, the internal diameter of sampling die 200 is less than the test sample that the test of X-ray nanometer CT scan can be tested
Maximum gauge.Wherein, when maximum gauge refers to the test of X-ray nanometer CT scan, X-ray is incident from test sample and can be from test
The maximum distance that sample projects.
Sampling die 200 is polymeric molds.Specifically, sampling die 200 is polyimide mold or polyether-ether-ketone mould
Tool.The x-ray attenuation coefficient of the sampling die 200 of above-mentioned material almost can be ignored, to make the test being prepared
When for the test of X-ray nanometer CT scan, sampling die 200 will not impact test result sample.
Further, sampling die 200 can be connected to proportioner 100.Specifically, sampling die 200 has charging
Mouth and bleeding point, feed inlet can be connected to proportioner 100.
Moving material device 300 can be transferred to the slurry in proportioner 100 in sampling die 200.Specifically, material dress is moved
Setting 300 can be transferred to the slurry in proportioner 100 in sampling die 200 by way of extracting or drawing.Further
Ground, in the present embodiment, system can be transferred to for the slurry in proportioner 100 by way of extraction by moving material device 300
In original mold tool 200.It is appreciated that in other embodiments, ingredient can also be filled by way of absorption by moving material device 300
The slurry in 100 is set to be transferred in sampling die 200.
Specifically, moving material device 300 includes connection unit 310 and power unit 320, and connection unit 310 can be with sample preparation
Mold 200 is connected to, and connection unit 310 can be connected to power unit 320, so that the slurry in proportioner 100 can be by
It extracts into sampling die 200.
Wherein, connection unit 310 includes microsyringe 312 and the connector being detachably connected with microsyringe 312
314.Microsyringe 312 can be connected to power unit 320.Connector 314 can be connected to bleeding point, and connector 314 and pumping
When port is connected to, connector 314 and sampling die 200 are tightly connected, so that the slurry in proportioner 100 can be extracted to system
In original mold tool 200.Due to sampling die 200 internal diameter be it is micron-sized, cannot directly be connected to power unit 320, therefore, elder generation
Sampling die 200 is connected to microsyringe 312, is then connected to again with power unit 320.
Specifically, connector 314 includes female Luer 3142 and seperated connector 3144.Female Luer 3142 can with it is micro into
Sample device 312 is detachably connected.Seperated connector 3144 can be detachably connected with female Luer 3142, and seperated connector 3144 can
It is connected to the bleeding point of sampling die 200.Further, connector 314 further includes sword ring, and sword ring can with female Luer 3142
Dismantling connection, and sword ring can be detachably connected with seperated connector 3144, so that female Luer 3142 can be with microsyringe
312 are detachably connected.Sampling die 200 is connected to microsyringe 312 by above-mentioned connector 314, sampling die can be made
200 are tightly connected with microsyringe 312.It is appreciated that connector 314 is not limited to above-mentioned connector, it is any can be by sampling die
200 connectors 314 being tightly connected with microsyringe 312 can be used as the connector 314 of present embodiment.
Further, connection unit 320 further includes pipeline 316.Microsyringe 312 passes through pipeline 316 and power unit
320 connections.In the present embodiment, pipeline 316 is hard gel pipe.It is appreciated that in other embodiments, pipeline 316
It can also be other pipelines 316, it is any the pipeline 316 that microsyringe 312 is connected to power unit 320 can be made
For the pipeline 316 of present embodiment.
Power unit 320 includes vacuum pump 322, and vacuum pump 322 can be connected to connection unit 310, and 322 energy of vacuum pump
It is enough to extract the slurry in proportioner 100 into sampling die 200.Further, vacuum pump 322 can be with connection unit
310 microsyringe 312 is connected to.
Further, power unit 320 further includes power supply 324.Power supply 324 can be electrically connected with vacuum pump 322
It connects.Specifically, power supply 324 is electrically connected by conducting wire with vacuum pump 322.Power supply 324 can by adjust electric current and
Voltage, to adjust the vacuum degree of vacuum pump 322.In the present embodiment, power supply 324 is DC power supply.It is appreciated that
Power supply 324 is not limited to DC power supply, and the power supply 324 of any vacuum degree that can adjust vacuum pump 322 can be made
For the power supply 324 of present embodiment.
In some embodiments, power unit 320 further includes drying bottle 326.Drying bottle 326 can connect with vacuum pump 322
It is logical, and drying bottle 326 can be connected to connection unit 310, so that vacuum pump 322 can be connected to connection unit 310.Specifically
Ground, drying bottle 326 can be connected to the microsyringe 312 of connection unit 310.Setting drying bottle 326 can install decimated
Impurity etc. in journey prevents from polluting power unit 320.
Further, power unit 320 further includes pressure vacuum gauge 328.Pressure vacuum gauge 328 can be with drying bottle 326
Connection, to show the vacuum degree in drying bottle 326.Be arranged pressure vacuum gauge 328 can clearly display it is true in drying bottle 326
Reciprocal of duty cycle.
Further, vacuum pump 322, drying bottle 326, microsyringe 312, female Luer 3142, seperated connector 3144
And the connection between sampling die 200 is required to be sealed connection by high vacuum silicone grease.
Test device can test the water-cement ratio of the slurry in sampling die.Specifically, test device is thermogravimetic analysis (TGA)
Equipment.
When the preparation system 10 of above-mentioned test sample is used to prepare test sample, application method is as follows:
(1) power supply 324 and vacuum pump 322 are connected by conducting wire, vacuum pump 322 is connected to drying bottle 326, and will
Pressure vacuum gauge 328 is connected to drying bottle 326, and drying bottle 326 is connected to one end of microsyringe 312 by pipeline 316,
The other end of microsyringe 312 passes sequentially through the pumping of female Luer 3142, sword ring and seperated connector 3144 and sampling die 200
Port connection.
(2) switch for opening power supply 324 and vacuum pump 322, adjusts electric current and voltage, passes through pressure vacuum gauge 328
Obtain specific vacuum degree.
(3) sampling die 200 is inserted into the proportioner 100 for being filled with the standard slurry of known initial water-cement ratio, is led to
Vacuum pump 322 is crossed to extract standard slurry into sampling die 200.
(4) thermogravimetic analysis (TGA) equipment is opened, and the standard slurry in sampling die 200 is tested, obtains standing paste
The practical water-cement ratio of material.
(5) step (3) and step (4) are repeated, the practical water-cement ratio of multiple standard slurries is obtained, according to multiple practical glues
Than with multiple initial water-cement ratios, establish the functional relation of practical water-cement ratio and initial water-cement ratio.
(6) according to the glue of test sample to be prepared when above-mentioned functional relation, the preparation glue of sample slurry is obtained
Than.
(7) sampling die 200 is inserted into the proportioner 100 for installing sample slurry, is starched sample by vacuum pump 322
Material is extracted into sampling die 200, obtains test sample.
The preparation system of above-mentioned test sample has at least the following advantages:
(1) preparation system of above-mentioned test sample is simple, and micron order, test specimens of uniform size can be prepared
Product.
(2) water-cement ratio for the test sample that the preparation system of above-mentioned test sample enables to is controllable, and can be used in X
In the test of ray nanometer CT scan.
The following are specific embodiment parts:
Embodiment 1
The X-ray nanometer CT scan test equipment of the present embodiment is the Sigray Faast of U.S. Sigray company exploitation
Nano XRM, the selection of energy of light source intensity: high-velocity electrons hit the monochromatic 8keV characteristic spectrum linear light (Cu-K α) that copper target generates.This
In the preparation system of the test sample of embodiment, thermogravimetic analysis (TGA) equipment is the resistance to 4495F that speeds of Germany, and power supply is direct current
Source.
The raw material that test sample is prepared in the present embodiment includes: that GSB14-1510 ruggedness test cement standard sample is (main
Want composition are as follows: tricalcium silicate, dicalcium silicate, tricalcium aluminate；Production unit: China Building Material Scientific Research General Institute, it is simple below
Claim cement standard product) and deionized water.The initial glue of standard slurry is such as shown in the following table 1:
The initial water-cement ratio of 1 various criterion slurry of table
| Standard slurry number | S1 | S2 | S3 | S4 | S5 | S6 |
| Initial water-cement ratio | 0.4 | 0.6 | 0.7 | 0.8 | 1.0 | 1.3 |
The preparation process of the test sample of the present embodiment is as follows:
(1) according to formulaWhen X-ray energy intensity is 8keV, respectively obtain main in cement standard product
The x-ray attenuation coefficient of composition tricalcium silicate is 0.0160, the x-ray attenuation coefficient of dicalcium silicate is 0.0148, tricalcium aluminate
X-ray attenuation coefficient be 0.0141.Wherein, K value is about 1.4 × 10-3.Then according to langbobier law equation φ=
φ0Exp (- μ D), due to φ and φ0Ratio be greater than or be equal to 1/e, so work as φ and φ0Ratio be 1/e when, respectively
Obtain test cement standard product in main ingredient tricalcium silicate, dicalcium silicate, tricalcium aluminate maximum gauge be respectively 62.50 μ
m、67.68μm、70.84μm。
Fig. 3 is the attenuation length and X-ray of main ingredient tricalcium silicate, dicalcium silicate, tricalcium aluminate in cement standard product
The graph of relation of energy.Attenuation length is the maximum gauge of test sample, i.e., as φ and φ0Ratio be 1/e when, test specimens
The thickness of product.The drafting of the graph of relation of attenuation length and X-ray energy, first according to formulaEach X is obtained to penetrate
X-ray attenuation coefficient corresponding to heat input, then according to φ=φ0Exp (- μ D) is obtained as φ and φ0Ratio be 1/e
When, the thickness (i.e. attenuation length) of test sample, to obtain the relation curve of attenuation length and X-ray energy.From upper in Fig. 3
The attenuation length of tricalcium aluminate, dicalcium silicate and tricalcium silicate and the relation curve of X-ray energy are respectively corresponded to lower curve.
Sample is not considered under the X-ray energy intensity of 8keV according to the relation curve of attenuation length and X-ray energy
When porosity profiles, the maximum gauge that main ingredient tricalcium silicate, dicalcium silicate, tricalcium aluminate allow in cement standard product is distinguished
It is 62.50 μm, 67.68 μm, 70.84 μm.It should be noted that the permission thickness is to consider that sample is assumed in as the main component
It is calculated respectively when one of.
Be respectively 62.50 μm according to the maximum gauge that tricalcium silicate obtained above, dicalcium silicate, tricalcium aluminate allow,
67.68 μm, 70.84 μm, therefore, the thickness of sample should be less than 62.50 μm, but since the maximum allowable thickness of above three is
It is obtained under the independent extreme case for calculating and not considering porosity, therefore, 62.50 μm can be slightly larger than in practical selection.Separately
Outside, it is contemplated that the size of commercially available sampling die is generally 125 μm, 65 μm and 25 μm.Therefore, comprehensively consider above-mentioned factor, select
The internal diameter for selecting sampling die is 65 μm.
Fig. 4 be cement standard product in main ingredient tricalcium silicate, dicalcium silicate, tricalcium aluminate with a thickness of 65 μm when, silicon
Sour tricalcium, dicalcium silicate, the penetrance of tricalcium aluminate and X-ray energy graph of relation, wherein penetrance be φ and φ0's
Ratio.In Fig. 4, curve respectively corresponds the penetrance and X-ray energy of tricalcium silicate, dicalcium silicate and tricalcium aluminate from top to bottom
Relation curve.Sample is not considered under the X-ray energy intensity of 8keV according to the relation curve of penetrance and X-ray energy
When porosity profiles, X-ray wearing when penetrating tricalcium silicate, the dicalcium silicate, tricalcium aluminate that sectional dimension is 65 μm respectively
Saturating rate is 35.5%, 38.4%, 40.1%.Due in langbobier law formula, φ and φ0Ratio be greater than or be equal to 1/
E (i.e. 36.7%), and when with a thickness of 65 μm, penetrance the wearing except tricalcium silicate of tricalcium silicate, dicalcium silicate, tricalcium aluminate
Saturating rate is slightly smaller outer, other are all larger than 1/e.But it should be noted that the penetrance is to consider that sample is assumed in as the main component
It is calculated respectively when one of, and based on the extreme case for not considering hole in above-mentioned calculating, and is to have in actual conditions
Certain hole, therefore, the penetrance of one of them is slightly smaller than 1/e can also be with.Therefore, above-mentioned penetrance statistics indicate that, X-ray
Nano scanning CT can penetrate sectional dimension and be 65 μm of sample, and be able to detect imaging.
In the present embodiment, according to Fig. 3 and Fig. 4's as a result, select inside diameter for 65 μm polyether-ether-ketone (PEEK) pipe make
For sampling die.
Fig. 5 is the material of sampling die when being PEEK, the attenuation length of sampling die and the relation curve of X-ray energy
Figure.According to Fig. 5, selected 65 μm of sampling die PEEK pipes of interior diameter, the permission maximum under the X-ray energy intensity of 8keV
Overall diameter is 1180 μm.Therefore, in actual selection PEEK pipe, overall diameter is less than 1180 μm.And the overall diameter of PEEK pipe is got over
It is small, it is smaller to the Imaging of sample to be tested.In addition, therefore, selecting overall diameter for 800 μ according to the model of commercially available PEEK pipe
The PEEK of m is managed.
Fig. 6 is that the material of sampling die is PEEK, and internal diameter is 65 μm, with a thickness of 735 μm, i.e., when overall diameter is 800 μm, and system
The penetrance of original mold tool and the graph of relation of X-ray energy.According to Fig. 6, selected 65 μm of sampling die PEEK of interior diameter
Pipe, under the X-ray energy intensity of 8keV, the penetrance when penetrating 800 μm of hollow PEEK pipe is 53.5%, meets lambert
Requirement in Beer law formula.
Therefore, according to above-mentioned experimental result, selecting inside diameter for 65 μm, overall diameter 0.8mm, length is the poly- of 50mm
The sampling die of ether ether ketone (PEEK) Guan Zuowei the present embodiment.
(2) DC power supply and vacuum pump are connected by conducting wire, vacuum pump is connected to drying bottle by pipeline, and by vacuum
Pressure gauge is connected to drying bottle, drying bottle is connected to one end of microsyringe by pipeline, the other end of microsyringe
Female Luer, sword ring and seperated connector is passed sequentially through to be connected to sampling die.
(3) switch for opening DC power supply and vacuum pump, under the premise of blocking sampling die sample introduction end, reference vacuum pressure
Power table, adjustment Current Voltage value allows the vacuum values of pressure vacuum gauge to reach target value 2kPa, in this, as the pumping of microsyringe
Sample driving force.
(4) successively the standard slurry of S1~S6 enters in sampling die in extraction table 1, and extracting the time is 3 minutes.
(5) the weight-loss ratio curve that cement standard product are measured by thermogravimetric analyzer, the benchmark for establishing cement standard product are weightless
Rate curve；The weight-loss ratio curve that sampling die is measured by thermogravimetric analyzer, establishes the benchmark weight-loss ratio curve of sampling die.So
The weight-loss ratio curve of sample S1~S6 with sampling die is measured by thermogravimetric analyzer afterwards, and deducts tricalcium silicate and sample preparation mould
The benchmark weight-loss ratio curve of tool, the weight-loss ratio curve of sample S1~S6 after being corrected obtain the practical water of sample S1~S6
Glue ratio.The relation curve of practical water-cement ratio and initial water-cement ratio is established, as shown in Figure 7.Fig. 7 is practical water-cement ratio and initial glue
The graph of relation of ratio.
(6) the target water-cement ratio of test sample to be prepared is set as 50%, at this time target water-cement ratio=practical water-cement ratio,
It can be seen that the vacuum pressure when setting pressure vacuum gauge from the relation curve of practical water-cement ratio and initial water-cement ratio in Fig. 7
When value is 2kPa, preparing water-cement ratio is 0.68.
(7) it is 0.68 mixing to prepare water-cement ratio by cement standard product and water, obtains sample slurry.
(8) vacuum degree be 2kPa when, sample slurry is entered in sampling die by vacuum drawn, extraction the time be
3min obtains the test sample that practical water-cement ratio is 0.5.
In order to verify the present embodiment test sample preparation method applicability, the present embodiment pass through respectively to conventional system
The sample (preparing on common-use size mold) of Preparation Method and the sample of this preparation method preparation carry out nano indentation test, comparison two
The component of person's hydrated product, secondary proof quantitatively controls the micron order test sample that water-cement ratio obtains to be had with customary preparation methods
Comparativity.You need to add is that existing research is pointed out, nano-indentation experiment can characterize cement-like by the Indentation Modulus obtained
Three object phases of product, (high density hydrated calcium silicate is solidifying by respectively LS C-S-H (low-density hydrated calcium silicate gel), HD C-S-H
Glue) and HD/CH complex, the component of the cement sample prepared under different water-binder ratios, three object phases may also change accordingly.Root
According to the load Protonation constant of the present embodiment, object here mutually refers to the solid phase of sample and the complex response of hole phase, that is, represents power
Learn the sample data of property.
The test sample that two practical water-cement ratios of A, B are 50% is prepared using cement standard product as raw material respectively, when maintenance
Between be 3 days.Wherein B sample is 0.68 using the initial water-cement ratio that the above-mentioned preparation method of the present embodiment is prepared, practical
The test sample that water-cement ratio is 0.5.A sample use from diameter in the molding test block of the cylindrical die of 2cm, height 1cm break
The sample that shape obtains prepares initial water-cement ratio using 50%.Nano indentation test, impression number are carried out respectively to two samples of A, B
Amount is 30 × 10, the loading method controlled using load, and surge pressure is 2000 μ N, and the load time is 5 seconds, for 2 seconds, is unloaded
It carries the time 5 seconds.Shown in the result of acquired nano-indenter test such as table 2, Fig. 8 (a)~Fig. 8 (c) and Fig. 9 (a)~Fig. 9 (c).
Table 2 is to pass through big-sample data processing mode according to test result after A, B sample carry out nano-indenter test respectively
And the volume fraction of each object phase obtained after Gauss curve fitting.Fig. 8 (a) is the location drawing of the nano-indenter test of A sample, Fig. 8 (b)
For the data profile of the nano-indenter test of A sample, Fig. 8 (c) is the big-sample data processing of the nano-indenter test of A sample
Gaussian fitting result figure afterwards.Fig. 9 (a) is the location drawing of the nano-indenter test of B sample, and Fig. 9 (b) is the nanometer pressure of B sample
The data profile of trace test, Fig. 9 (c) are sample data treated the Gaussian fitting result of the nano-indenter test of B sample
Figure (contains sampling die).Wherein, test equipment is that sea thinks to create TI950 nano-hardness tester, and Indentation Modulus result is by equipment to adding
It is automatically derived to carry unloading curve analysis.
Table 2A sample, B sample nano-indenter test under the volume fraction of each object phase that divides
Using the sample of the preparation method preparation of the test sample of the present embodiment it can be seen from table 2, Fig. 8 (c) and Fig. 9 (c)
Its each object phase volume fraction of product is more almost the same than with the sample using conventional method for making sample preparation, do not consider it is some statistically
Error when, LD C-S-H and HD C-S-H ratio is about 3: 1, there is no because test sample preparation method and device and sample
The size of product and the representativeness for affecting sample itself.
Obtained B sample is scanned using above-mentioned X-ray nanometer CT scan test equipment.Parameter in scanning process
Are as follows: time for exposure 130s, it is bining2 that detector, which merges display pixel point, and scanning range is -90 °~90 °, and step-length is
0.1 °, total duration 234000s, the mode used is big visual field mode (Large Field of View), LFOV=80 at this time
μm, 1 individual pixel is up to 0.04 μm of size at bining2.Wherein, Figure 10 (a) is the image after B sample three-dimensionalreconstruction,
Figure 10 (b), Figure 10 (c) and Figure 10 (d) are respectively 2 dimensions of three different directions of image (Figure 10 (a)) after B sample three-dimensionalreconstruction
Sectioning image.Figure 11 (a), Figure 11 (b) are respectively the 3 d image after B sample three-dimensionalreconstruction is different degrees of.
It can be seen that 1, sample topography is rule from Figure 10 (b), Figure 10 (c) and Figure 10 (d) and Figure 11 (a), Figure 11 (b)
Then cylindric, as long as and sampling die do not change, which can repeat to realize；2, the mold selected is due to material
X-ray attenuation coefficient it is minimum and uniform in material, stay in grade, thus to the X-ray of the cementitious material prepared inside it at
Picture process influence is minimum, has little influence on the judgement to result；3, since " wall is imitated between internal cementitious material and sampling die
Answer " effect, produce interfacial transition zone, the transition region using this preparation method not because generate, but any glue
The phenomenon that solidifying sample can generate when being prepared by any mold, therefore this preparation method can reflect practical routine to a certain degree
Sample transition region in the case of preparation provides multiple research objects by the screening to test result.
Above-mentioned experimental result shows that the preparation method of the test sample of the present embodiment and preparation system can be prepared
Micron-sized test sample, and the regular shape of test sample, water-cement ratio are controllable, can be used in the test of X-ray nanometer CT scan
In.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (12)
1. a kind of preparation method of test sample, which comprises the steps of:
The different standard slurry of multiple initial water-cement ratios is prepared using the raw material for preparing test sample, wherein the test sample
For cementitious material, the raw material includes solid material and solvent；
The different standard slurry of multiple initial water-cement ratios is respectively placed in multiple sampling dies, then test is each described
The practical water-cement ratio of the standard slurry in sampling die, the internal diameter of the sampling die are micron order；
According to multiple practical water-cement ratios and multiple initial water-cement ratios, the practical water-cement ratio and the initial water are established
The functional relation of glue ratio；
According to the water-cement ratio of the functional relation and the test sample, the preparation water-cement ratio of the test sample is calculated；
According to the preparation water-cement ratio, the raw material is configured to sample slurry；And
The sample slurry is placed in the sampling die, the test sample is obtained.
2. the preparation method of test sample according to claim 1, which is characterized in that the test sample is received for X-ray
Rice CT scan test sample.
3. the preparation method of test sample according to claim 2, which is characterized in that the internal diameter of the sampling die is less than
The maximum gauge for the test sample that the X-ray nanometer CT scan test can be tested.
4. the preparation method of test sample according to claim 3, which is characterized in that described by multiple initial glues
It further include that the X-ray nanometer CT scan is surveyed before the step being respectively placed in multiple sampling dies than different standard slurries
The determination step of the maximum gauge for the test sample that can be tested is tried, the determination step of the maximum gauge includes:
The light source institute tested according to the density of the solid material and effective atomic number and the X-ray nanometer CT scan
The X-ray energy intensity of use, according to formulaThe x-ray attenuation coefficient of the solid material is calculated,
In, μ indicates that x-ray attenuation coefficient, ρ indicate density, and Z indicates that effective atomic number, E indicate X-ray energy intensity, and K is constant；
According to equation φ=φ0Exp (- μ D) obtains the X-ray nanometer CT scan and tests the test specimens that can be tested
The maximum gauge of product, wherein φ indicates the photon intensity of outgoing, φ0Indicate incident photon intensity, φ and φ0Ratio be greater than
Or it is equal to 1/e, D is the thickness of the test sample.
5. the preparation method of test sample according to claim 1, which is characterized in that described according to multiple practical water
Glue ratio and multiple initial water-cement ratios, the step of establishing the functional relation of the practical water-cement ratio and the initial water-cement ratio packet
It includes:
According to multiple practical water-cement ratios and multiple initial water-cement ratios, the pass of practical water-cement ratio and initial water-cement ratio is established
It is curve；
The relation curve is subjected to linear fit, obtains the functional relation of the practical water-cement ratio Yu the initial water-cement ratio.
6. the preparation method of test sample according to claim 1, which is characterized in that each sample preparation mould of test
In the step of practical water-cement ratio of the standard slurry in tool, tested in each sampling die using the method for thermal weight loss
The standard slurry practical water-cement ratio.
7. the preparation method of test sample according to claim 1, which is characterized in that described by the multiple initial glue
It is respectively placed in the step in multiple sampling dies than different standard slurries, multiple initial water-cement ratios is made not by vacuum drawn
Same standard slurry is respectively placed in multiple sampling dies, and the vacuum degree during vacuum drawn is identical.
8. the preparation method of test sample according to claim 1, which is characterized in that the material of the sampling die is poly-
Close object.
9. a kind of preparation system of test sample characterized by comprising
Proportioner can install slurry；
Sampling die can install the slurry, and the internal diameter of the sampling die is micron order；
Material device is moved, the slurry in the proportioner can be transferred in the sampling die；And
Test device can test the water-cement ratio of the slurry in the sampling die.
10. the preparation system of test sample according to claim 9, which is characterized in that the sampling die can be with institute
Proportioner connection is stated, the shifting material device includes connection unit and power unit, and the connection unit can be with the sample preparation
Mold connection, the power unit can be connected to the connection unit, so that the slurry in the proportioner can
It is extracted in the sampling die.
11. the preparation system of test sample according to claim 10, which is characterized in that the sampling die has charging
Mouthful and bleeding point, the feed inlet can be connected to the proportioner, the connection unit include microsyringe and with institute
The connector that microsyringe is detachably connected is stated, the microsyringe can be connected to the power unit, the connector energy
It is enough be connected to the bleeding point, and when the connector is connected to the bleeding point, the connector seals company with the sampling die
It connects, so that the slurry in the proportioner can be extracted in the sampling die.
12. the preparation system of test sample according to claim 10, which is characterized in that the power unit includes vacuum
Pump, the vacuum pump can be connected to the connection unit, so that the slurry in the proportioner can be extracted to
In the sampling die.
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