CN106442107A - Rock-like material for stress test and its preparation method and application - Google Patents
Rock-like material for stress test and its preparation method and application Download PDFInfo
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- CN106442107A CN106442107A CN201610860689.4A CN201610860689A CN106442107A CN 106442107 A CN106442107 A CN 106442107A CN 201610860689 A CN201610860689 A CN 201610860689A CN 106442107 A CN106442107 A CN 106442107A
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- rock
- carbon nanotube
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- gypsum
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
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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
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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
- G01N2001/2893—Preparing calibration standards
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0298—Manufacturing or preparing specimens
Abstract
The invention relates to a rock-like material for stress test and its preparation method and application. The rock-like material comprises gypsum layers and carbon nanotube layers, the carbon nanotube layers are interposed among the gypsum layers, and the gypsum layers and the carbon nanotube layers are alternated. The preparation method comprises the following steps: distributing carbon nanotubes in water and polyvinylpyrrolidone to prepare carbon nanotube suspension, adding a gypsum retarder in the carbon nanotube suspension and stirring, and then adding the high strength gypsum to stir to obtain carbon nanotube slurry mixture; adding a gypsum retarder into water and then adding high strength gypsum to produce gypsum slurry; sequentially pouring the gypsum slurry and the carbon nanotube slurry mixture into a mold, and detaching to obtain the material after consolidation. Compared with the prior art, the rock-like material contains the carbon nanotube layers, original nonconductive specimen is changed into locally conductive specimen, and metal spraying do not need to be used because of an electron microscope such that shortcomings of the uneven distribution of the metal layers during gold spraying, influence on sectional microscopic morphology and others shortcomings are avoided.
Description
Technical field
The present invention relates to a kind of rock-like materials, especially relate to a kind of rock-like materials for stress test and its system
Preparation Method and application.
Background technology
In building field, the destructive characteristics of material are most important for engineering with collapse state, with theoretical research
The progress of deep and engineering technology, the research to material stress destruction characteristic also develops towards the direction that becomes more meticulous.If can be
Thin sight obtains material in the stress distribution for destroying section, it is possible to judge the stress of structure or the soil body in corresponding site,
Reference is provided so as to the improvement for material or structure.
In order to obtain the distribution mode of contact stresses of material, many observation methods arise at the historic moment, and electron-microscope scanning technology is exactly a kind of
The observation method that shape characteristic carefully seen by material can intuitively be obtained.Conventional sample is mostly non-conductive at present, using electron-microscope scanning
When method observes nonconducting sample, in order to the electric conductivity, the mitigation sample that increase sample surfaces are charged, need to lead sample
Electric treatment.Conventional method is metal spraying, i.e., spray one layer of W or Au to specimen surface using ion sputtering instrument, then by conduction
Adhesive tape is connected to the surface layer of sample on sample stage, derives excess electron.There are a lot of drawbacks in this method, for material
For destroying section, the concavo-convex relief intensity of the shape of sightingpiston is larger, and metal spraying is difficult a sightingpiston when process and is all sprayed onto,
Want spraying uniformly even more impossible；Additionally, metal spraying process is also possible to impact the shape characteristic of material surface, cover very
To the details of morphology for changing section crystal, the accuracy of observing effect and test is affected.
Content of the invention
The purpose of the present invention is exactly to provide one kind to exempt from metal spraying process, analyze to test and accurately use to solve the above problems
Rock-like materials in stress test and its preparation method and application.
The purpose of the present invention is achieved through the following technical solutions：
A kind of rock-like materials for stress test, described rock-like materials include gypsic horizon and carbon nanotube layer,
Described carbon nanotube layer is mixed in the middle of gypsic horizon, and gypsic horizon is distributed alternately with carbon nanotube layer.
Described gypsic horizon and carbon nanotube layer are parallel to each other.
Described gypsic horizon is 4-6 with the thickness ratio of carbon nanotube layer：1.
Described carbon nanotube layer includes multi-walled carbon nano-tubes.
The preparation method of the described rock-like materials for stress test, specifically includes following steps：
(1) CNT is dispersed in the mixed liquor of clear water and polyvinylpyrrolidone, prepares carbon nano tube suspension；
(2) calcium sulphate retarder stirring being added in carbon nano tube suspension, adds high strength gypsum stirring, present to Gypsum Fibrosum
Flow regime, prepared carbon nano tube paste mixture；
(3) calcium sulphate retarder stirring being added in clear water, adds high strength gypsum, stir to Gypsum Fibrosum and assume flow regime,
Prepared calcium plaster；
(4) pour alternate successively to calcium plaster obtained in step (3) and carbon nano tube paste mixture obtained in step (2)
Build in a mold, after maintenance solidification, form removal is obtained the material.
Step (1) using magnetic agitation and supersound process, the weight of described clear water, polyvinylpyrrolidone and CNT
Amount ratio is 1500-2500：8-12：1.
The weight ratio of the carbon nano tube suspension, calcium sulphate retarder and high strength gypsum described in step (2) is 15-25：1：90-
110, described calcium sulphate retarder adopts alkaline phosphatase salt retarder.
The weight ratio of the clear water, calcium sulphate retarder and high strength gypsum described in step (3) is 1：0.04-0.06：4-6.
Mould described in step (4) is 100mm × 40mm × 10mm, and casting process vibrated simultaneously, and by each layer
Surface is floating, and the time of the maintenance is 24h.
CNT as a kind of good marking materials, after disperseing to which, can be uniformly distributed in the sample, due to
Carbon nanotube sizes are nanoscale, and the several orders of magnitude less than conventional material size add using disclosed in CNT of the present invention
Amount, does not affect the macromechanical property of material, while the electric conductivity of CNT is good, after addition material in scan test
Can avoid the pollution to specimen surface as conductive material so as to metalling film process be carried out without to sample.
As the standard specimen of stress distribution test, sample can be destroyed using rock-like materials obtained in this method
Experiment, the sample after destruction is made comprising section and the observing samples of CNT interlayer are destroyed, is directly entered with scanning electron microscope
Row observation, according to the thin sight form of gypsum crystal and CNT, by the destruction profile scanning figure of complicated applied force sample with simple
The electron-microscope scanning figure of stress destruction is compared, so as to obtain the stress distribution that sample is destroyed on section.
After the present invention is improved to traditional electron-microscope scanning observation procedure, CNT interlayer can be originally nonconducting
Sample is changed into local conduction, therefore using without the need in specimen surface spray metal before electron-microscope scanning, so as to avoid metal spraying process
The shortcomings of middle metal level skewness, impact section carefully see form.Additionally, the multi-walled carbon nano-tubes in interlayer is also used as mark
Know the stress state in region residing for thing auxiliary judgment, so as to obtain the stress distribution situation of section is destroyed under complicated applied force state.
Meanwhile, CNT interlayer is relatively thin, and when carrying out breaking test to sample, Impact direction is vertical with interbed length direction, does not affect
The mechanical property of material entirety.
Description of the drawings
Fig. 1 is the structural representation of rock-like materials of the present invention；
Fig. 2 is rock-like materials sectional schematic diagram of the present invention；
Fig. 3 is the schematic diagram of electron-microscope scanning sample of the present invention；
In figure：1- carbon nanotube layer；The pure gypsic horizon of 2-；3- sample section；4- sample stage；5- conductive tape.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of rock-like materials for stress test, including carbon nanotube layer 1 and pure gypsic horizon 2, institute as shown in Figure 1, Figure 2
Show, specifically adopt and be prepared by the following steps：
Step 1：Prepare multi-walled carbon nano-tubes suspension.In order to reduce the shadow of the incorporation to the strength of materials of multi-walled carbon nano-tubes
Ring, during managing at which, the carbon nanotube particulate of coherent condition is disperseed.By water, multi-walled carbon nano-tubes, polyvinyl pyrrole
Alkanone is 20 according to quality:0.01:0.1 ratio is weighed each sample respectively, then the polyvinylpyrrolidone of 0.1g is added to
In beaker equipped with 20ml water, magnetic agitation is completely dissolved to polyvinylpyrrolidone, finally by the multi-walled carbon nano-tubes of 0.01g
It is added in solution, after magnetic agitation 2-3min, to mixed solution supersound process 5min.It can be found that mixed solution is muddy,
Under high light, observation can see that beaker bottom is precipitated without black nano pipe substantially, illustrate that dispersion effect is relatively good.
Step 2：Gypsum Fibrosum is prepared with CNT mixed solution.Multi-walled carbon nano-tubes top suspension 20ml is taken, is added
1g calcium sulphate retarder, magnetic agitation is completely dissolved to retarder, without bulky grain accumulation.Then gross weight 100g is added by several times
High strength gypsum, is stirred well to Gypsum Fibrosum and assumes flow regime.
Step 3：Prepare calcium plaster.Clear water 5ml is taken, 0.25g calcium sulphate retarder is added, calcium sulphate retarder adopts alkaline phosphatase
Salt retarder, magnetic agitation is completely dissolved to retarder, without bulky grain accumulation.Then the height of gross weight 25g is added by several times
Strong Gypsum Fibrosum, is stirred well to Gypsum Fibrosum and assumes flow regime.
Step 4：Prepare experimental sample.First by the Gypsum Fibrosum for stirring pour into 100mm × 40mm × 10mm from molding jig
In, when bottom surface is 40mm × 10mm, to pour height into about 4mm, it is changed to pour one layer of Gypsum Fibrosum and CNT mixed solution, thickness into
About 1mm, is further continued for pouring gypsum slurries into.Fully vibrate in casting process, to discharge the bubble in model.Simultaneously by surface
Floating, 24h is conserved, form removal after plaster model solidification, that is, obtain rock-like materials.
Embodiment 2
The rock-like materials that embodiment 1 is obtained are tested for section stress analysis, using obtained rock-like materials as
Standard specimen carries out breaking test, as shown in figure 3, test sample is placed on sample stage 4,5 band of conducting resinl is placed on survey
Have a try between sample and sample stage 4, sample section 3 can be detected, in the case of destruction section is not disturbed, cut portion subpackage
Electron-microscope scanning sample is made containing sample of the section with CNT interlayer is destroyed, observation destroys the thin sight form of section.In Electronic Speculum
In scanning figure, it can be observed that gypsum crystal assumes different form spies from multi-walled carbon nano-tubes in different destroying on section
Levy.The gypsum crystal for being destroyed on section with pure drawing, pure shear and the thin sight form of CNT are contrasted, it can be determined that residing position
The stress state that puts, finally gives the stress envelope for destroying on section.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, and difference is the consumption of material, in the present embodiment, CNT
In suspension, the weight ratio of clear water, polyvinylpyrrolidone and CNT is 2500：12：1, CNT in carbon nanotube layer
The weight ratio of suspension, calcium sulphate retarder and high strength gypsum is 25：1：110, clear water in pure gypsic horizon, calcium sulphate retarder with high-strength
The weight ratio of Gypsum Fibrosum is 1：0.06：6, the thickness of obtained sample gypsic horizon is 6mm, and the thickness of carbon nanotube layer is 1mm.
Embodiment 4
The present embodiment is substantially the same manner as Example 1, and difference is the consumption of material, in the present embodiment, CNT
In suspension, the weight ratio of clear water, polyvinylpyrrolidone and CNT is 1500：8：1, CNT in carbon nanotube layer
The weight ratio of suspension, calcium sulphate retarder and high strength gypsum is 15：1：90, clear water in pure gypsic horizon, calcium sulphate retarder with high-strength
The weight ratio of Gypsum Fibrosum is 1：0.04：4, the thickness of obtained sample gypsic horizon is 5mm, and the thickness of carbon nanotube layer is 1mm.
Claims (10)
1. a kind of rock-like materials for stress test, it is characterised in that described rock-like materials include gypsic horizon and carbon
Nanotube layer, described carbon nanotube layer is mixed in the middle of gypsic horizon, and gypsic horizon is distributed alternately with carbon nanotube layer.
2. a kind of rock-like materials for stress test according to claim 1, it is characterised in that described gypsic horizon
It is parallel to each other with carbon nanotube layer.
3. a kind of rock-like materials for stress test according to claim 1, it is characterised in that described gypsic horizon
Thickness ratio with carbon nanotube layer is 4-6：1.
4. a kind of rock-like materials for stress test according to claim 1, it is characterised in that described carbon nanometer
Tube layer includes multi-walled carbon nano-tubes.
5. a kind of preparation method of the as claimed in claim 1 rock-like materials for being used for stress test, it is characterised in that concrete
Comprise the following steps：
(1) CNT is dispersed in the mixed liquor of clear water and polyvinylpyrrolidone, prepares carbon nano tube suspension；
(2) calcium sulphate retarder stirring being added in carbon nano tube suspension, adds high strength gypsum stirring, assume flowing to Gypsum Fibrosum
State, prepared carbon nano tube paste mixture；
(3) calcium sulphate retarder stirring being added in clear water, add high strength gypsum, stir to Gypsum Fibrosum and assume flow regime, is obtained
Calcium plaster；
(4) it is cast in alternate successively to calcium plaster obtained in step (3) and carbon nano tube paste mixture obtained in step (2)
In mould, after maintenance solidification, form removal is obtained the material.
6. the preparation method of the rock-like materials for stress test according to claim 5, it is characterised in that step
(1) using magnetic agitation and supersound process, the weight ratio of described clear water, polyvinylpyrrolidone and CNT is 1500-
2500：8-12：1.
7. the preparation method of the rock-like materials for stress test according to claim 5, it is characterised in that step
(2) the weight ratio of carbon nano tube suspension, calcium sulphate retarder and high strength gypsum described in is 15-25：1：90-110.
8. the preparation method of the rock-like materials for stress test according to claim 5, it is characterised in that step
(3) the weight ratio of clear water, calcium sulphate retarder and high strength gypsum described in is 1：0.04-0.06：4-6.
9. the preparation method of the rock-like materials for stress test according to claim 5, it is characterised in that step
(4) casting process is vibrated, and will be floating per layer of surface, and the time of the maintenance is 24h.
10. a kind of application of the rock-like materials for being used for stress test as claimed in claim 1, it is characterised in that described
Rock-like materials are used for the stress distribution of material damage section to be tested.
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| CN201610860689.4A CN106442107B (en) | 2016-09-28 | 2016-09-28 | Rock-like materials and its preparation method and application for stress test |
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Cited By (1)
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| CN111855752A (en) * | 2020-03-20 | 2020-10-30 | 同济大学 | Wall surface structure capable of representing humidity change of bonding mortar and testing method thereof |
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