CN107651920A - A kind of modified graphene cement-base composite material and its preparation and application - Google Patents
A kind of modified graphene cement-base composite material and its preparation and application Download PDFInfo
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- CN107651920A CN107651920A CN201710918624.5A CN201710918624A CN107651920A CN 107651920 A CN107651920 A CN 107651920A CN 201710918624 A CN201710918624 A CN 201710918624A CN 107651920 A CN107651920 A CN 107651920A
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- Prior art keywords
- cement
- composite material
- graphene
- base composite
- modified graphene
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/90—Electrical properties
- C04B2111/94—Electrically conducting materials
Abstract
The present invention relates to a kind of modified graphene cement-base composite material and its preparation and application, the modified graphene cement-base composite material includes following components according to mass parts：30~50 parts of water, 100 parts of cement, 0.35~2 part of naphthalene water reducer, 0.5~4 part of graphene, 100~300 parts of normal sand；Preparation flow is as follows：1) naphthalene water reducer solution is prepared；2) modified graphene suspension is prepared；3) prepared by modified graphene cement-base composite material.Compared with prior art, the graphene cement-base composite material of the present invention has the advantages that preparation technology is simple, high mechanical strength, good endurance, compact structure, and its voltage sensitive sensor prepared has the advantages such as stress and strain monitoring signal are sensitive, signal to noise ratio is low, militarys service is stable and concrete compatibility is good.The voltage sensitive sensor has broad application prospects in fields such as concrete structure monitoring, traffic flow statistics and road surface deicings.
Description
Technical field
The present invention relates to a kind of modified graphene cement-base composite material and its preparation and application, belong to cement base composite wood
Material field.
Background technology
The health monitoring of great concrete structure engineering and infrastructure have the function that to the mankind it is more and more important,
As an inexorable trend of civil engineering industry development, this is mainly due to harsh natural environment and material itself aging
Catastrophic failure can be produced to structure, so as to cause very serious threat to the security of the lives and property of people.Based on existing skill
Art, can be applicable to the voltage sensitive sensor of concrete structure health monitoring mainly includes carbon nano-tube enhanced cement-base material, emulsion
Modified graphene cement-base composite material etc., still, these sensors have high cost, preparation technology complexity, stress and answered
The shortcomings of becoming low monitoring sensitivity, poor durability.With the development of nanometer technology, increasing researcher should by nano material
For in cement-based material, not only increasing the mechanical performance of cement-based material, and impart cement-based material electricity, thermal and magnetic etc.
Specific function.Graphene causes the research interest of numerous scholars, passes through special process as a kind of New Two Dimensional nano material
Finely dispersed graphene is spiked into acquisition cement-base composite material voltage sensitive sensor in cement material, it has good lead
Electrically, stronger pressure-sensitive and the features such as excellent durability, at the same it is good with concrete compatibility.Graphene cement base composite wood
Material voltage sensitive sensor has boundless research and application prospect, such as in traffic detection, distress in concrete and damage monitoring
Deng field.
Since A.Geim and K.Novoselov in 2004 obtains single-layer graphene using micromechanics stripping method, graphene
Just favor is enjoyed with its unique texture and excellent properties.However, the hydrophily of graphene is poor, and the model moral between particle
Magnificent power effect makes it easily reunite, if graphene powder is directly incorporated into cement matrix, the group of graphene itself
Poly- property makes it can not improve the performance of cement-based material.Therefore, prepare dispersed graphene suspension, change graphene
Ways added, optimization preparation technology, for graphene cement-base composite material it is successful prepare it is particularly important.
Graphene is to be currently known the most strong material of electric conductivity, is a kind of good material for preparing cement base voltage sensitive sensor
Material.The present invention mainly optimizes improvement from graphene dispersing solution, sensor preparation technology and voltage signal acquisition etc.,
Propose a kind of modified graphene cement-base composite material and its preparation and application.
The content of the invention
Technical problem：It is an object of the invention to provide a kind of modified graphene cement-base composite material and its prepare and answer
With the modified graphene cement-base composite material excellent in mechanical performance, sensitivity coefficient are high, excellent durability, and prepare simple.
Technical scheme：The invention provides a kind of modified graphene cement-base composite material, the modified graphene cement base
Composite includes following components according to mass parts：
Wherein：
Described cement is Portland cement, and its 28d intensity is not less than 52.5MPa.
The water-reducing rate of described naphthalene water reducer is 15%~25%.
The particle diameter of the graphene is 7~8 μm, and thickness is less than 10nm, and specific surface area is not less than 120m2/g。
The SiO of described normal sand2Content is not less than 98wt%, and its particle size range is 0.08~2mm, wherein 0.08~
0.5mm, 0.5~1.0mm and 1.0~2.0mm respectively account for 1/3.
Described modified graphene cement-base composite material 28d compression strength is not less than 60MPa, and rupture strength is not less than
9MPa。
Present invention also offers a kind of preparation method of modified graphene cement-base composite material, comprise the following steps：
1) naphthalene water reducer solution is prepared：By naphthalene water reducer add needed for mixing water total amount 50%~80% water
In, stir, obtain naphthalene water reducer solution；
2) modified graphene suspension is prepared：Graphene powder is added in naphthalene water reducer solution in batches, ultrasound point
Finely dispersed modified graphene suspension is obtained after dissipating；
3) prepared by modified graphene cement-base composite material：Graphene suspension is added in cement powder, adds sand
With remaining water, after stirring, grinding tool is injected, is gently shaken to closely knit, it is compound to can obtain modified graphene cement base after maintenance
Material.
Wherein：
Adding graphene powder in naphthalene water reducer solution in batches described in step 2), is disperseed after ultrasonic disperse
Uniform graphene suspension comprises the following steps that：Added every time into naphthalene water reducer solution cement gross mass 0.05%~
0.5% graphene powder, afterwards using 100~500W of power 30~90min of ultrasonic cleaner ultrasound or 300~
1000W 10~30min of ultrasonic cell disruptor ultrasound；After graphene powder all adds, using the super of 1000~1500W
Sound wave cell disruptor 10~60min of ultrasound, obtains finely dispersed modified graphene suspension.
Maintenance described in step 3) refers to conserve 28d under conditions of temperature is 20 ± 2 DEG C, relative humidity is more than 95%
More than.
Present invention also offers a kind of application of modified graphene cement-base composite material, the modified graphene cement base is answered
Condensation material is applied to voltage sensitive sensor.
Wherein：
The stress sensitivity of described voltage sensitive sensor is 0.5%/MPa~5%/MPa, and strain sensitivity is 50~500.
Described voltage sensitive sensor by modified graphene cement-base composite material test block and be embedded in its four internal electricity
Pole is formed, and four electrodes are sequentially distributed in the same surface of test block from left to right, and symmetrical with the axis of test block surface
Distribution, form two interior electrodes and two external electrodes, conductive phase of the graphene as the test block in test block.
The size (length) of the test block of described graphene cement-base composite material is 80~160 × 20~40 × 20
~40mm3, the distance between described two interior electrodes are the distance between 20~40mm, described two external electrodes for 60~
120mm。
When described voltage sensitive sensor carries out signal detection, apply 5~10V DC voltage for two external electrodes, adopt
To sensor circulate the loading and unloading of compression with electronic universal tester, using electrochemical workstation to electric in two
Pole carries out the collection of voltage signal, the collection strained using digital collection instrument, the loading and unloading of the circulation compression
Speed be 50~400N/s, maximum crushing stress is 5~20MPa, minimum compression 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Every 0.1s~
2s gathers a data, and voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 1s~5s.
Beneficial effect：Compared with prior art, the invention has the advantages that：
Graphene has fabulous electric conductivity and excellent mechanical property, and the present invention is using graphene as conductive filler, using naphthalene
Based water reducer is modified to graphene, is reduced its surface energy, is made it have good dispersion；
Ultrasonic disperse is carried out using ultrasonic cleaner and ultrasonic cell disruptor, is derived from dispersiveness and stability
Preferable graphene suspension, and solve graphene dispersion unequal caused cement-base composite material mechanics, electricity and pressure
The problems such as quick performance uniformity and poor repeatability；
Prepared modified graphene cement base voltage sensitive sensor perceptual sensitivity is high, before having boundless application
Scape.
Brief description of the drawings
Fig. 1 is the illustraton of model of graphene cement base voltage sensitive sensor；
Fig. 2 is the pass between the voltage change ratio and stress that modified graphene cement-base composite material is corresponded in embodiment 2
System's figure.
Embodiment
With reference to specific embodiment, the present invention is expanded on further, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention, after the present invention has been read, various equivalences of the those skilled in the art to the present invention
The modification of form falls within the application appended claims limited range.
Embodiment 1：The cement-based material of modified graphene is not filled
202.5g water is added in 450g cement, stirred slowly to uniform using glue sand agitator, 1350g normal sands is slow
Add and continue to stir, inject mould, gently shake to after closely knit, standard curing 28d.
The modified graphene cement-base composite material compression strength is 55MPa, rupture strength 8.2MPa.
It is 80 × 40 × 40mm in size3Graphene cement-base composite material test block in embedment 4 electrodes obtain it is pressure-sensitive
Sensor, and four electrodes are sequentially distributed in the same surface of test block from left to right, and it is symmetrical with the axis of test block surface
Distribution, forms two interior electrodes and two external electrodes, it is described from the distance between two interior electrodes be 40mm, described two dispatches from foreign news agency
The distance between pole is 60mm.
Apply 10V DC voltage for two external electrodes, circulation pressure is carried out to sensor using electronic universal tester
The loading and unloading of stress, using electrochemical workstation two interior electrodes are carried out with the collection of voltage signal, using digital collection
The collection that instrument is strained, the speed of the loading and unloading of the circulation compression is 50N/s, maximum crushing stress 5MPa,
Minimum compression is 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Adopted every 0.1s
Collect a data, voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 1s.
The blank cement-based material, without pressure-sensitive.
Embodiment 2：Graphene volume is 0.5% graphene cement based sensor of cement quality
A kind of modified graphene cement-base composite material is by water, cement, graphene, naphthalene water reducer (Nanjing Su Botexin
Materials Co., Ltd provides), normal sand composition, wherein, the particle diameter of graphene is 7~8 μm, and thickness is less than 10nm, specific surface area
For not less than 120m2/g.1.575g naphthalene water reducer powder is first weighed, is well mixed with 162g water, by 0.225g (cement qualities
0.05%) graphene powder is added in naphthalene water reducer solution, uses the ultrasonic cell disruptor ultrasound that power is 360W
10min；Repeat the above steps 4 times；0.225g graphene powders are added in above-mentioned graphene dispersing solution again, are using power
720W ultrasonic cell disruptor ultrasound 10min；Repeat the above steps 4 times, until graphene volume is 2.25g.Finally, adopt
The ultrasonic cell disruptor ultrasound 10min for being 1200W with power, obtains finely dispersed modified graphene suspension.Will be upper
State modified graphene suspension to be added in 450g cement powders, while add 40.5g water, stirred slowly to equal using glue sand agitator
It is even, 1350g normal sands are slowly added thereto, continue to stir, inject mould, are gently shaken to after closely knit, temperature be 20 DEG C,
Relative humidity obtains modified graphene cement-base composite material after conserving 28d under conditions of being more than 95%.
Modified graphene cement-base composite material 28d compression strength is 65.5MPa, rupture strength 9MPa.
It is 80 × 40 × 40mm in size3Black alkene cement-base composite material test block in embedment 4 electrodes obtain pressure-sensitive biography
Sensor, and four electrodes are sequentially distributed in the same surface of test block from left to right, and symmetrically divided with the axis of test block surface
Cloth, forms two interior electrodes and two external electrodes, it is described from the distance between two interior electrodes be 40mm, described two external electrodes
The distance between be 60mm.
Apply 10V DC voltage for two external electrodes, circulation pressure is carried out to sensor using electronic universal tester
The loading and unloading of stress, using electrochemical workstation two interior electrodes are carried out with the collection of voltage signal, using digital collection
The collection that instrument is strained, the speed of the loading and unloading of the circulation compression is 50N/s, maximum crushing stress 5MPa,
Minimum compression is 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Adopted every 0.1s
Collect a data, voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 1s.
The voltage sensitive sensor has a stronger pressure-sensitive, and strain sensitivity and stress sensitivity be respectively 95,0.75%/
MPa。
Embodiment 3：Graphene volume is 1% graphene cement based sensor of cement quality
A kind of modified graphene cement-base composite material is by water, cement, graphene, naphthalene water reducer (Nanjing Su Botexin
Materials Co., Ltd provides), normal sand composition, wherein, the particle diameter of graphene is 7~8 μm, and thickness is less than 10nm, specific surface area
For not less than 120m2/g.2.25g naphthalene water reducer powder is first weighed, is well mixed with 162g water, by 0.45g (cement qualities
0.1%) graphene powder is added in naphthalene water reducer solution, uses the ultrasonic cell disruptor ultrasound that power is 360W
15min；Repeat the above steps 4 times；0.45g graphene powders are added in above-mentioned graphene dispersing solution again, are using power
720W ultrasonic cell disruptor ultrasound 30min；Repeat the above steps 4 times, until graphene volume is 4.5g.Finally, adopt
The ultrasonic cell disruptor ultrasound 30min for being 1200W with power, obtains finely dispersed modified graphene suspension.Will be upper
State modified graphene suspension to be added in 450g cement powders, while add 40.5g water, stirred slowly to equal using glue sand agitator
It is even, 1350g normal sands are slowly added thereto, continue to stir, inject mould, are gently shaken to after closely knit, temperature be 20 DEG C,
Relative humidity obtains modified graphene cement-base composite material after conserving 28d under conditions of being more than 95%.
Modified graphene cement-base composite material 28d compression strength is 68MPa, rupture strength 10MPa.
It is 80 × 40 × 40mm in size3Black alkene cement-base composite material test block in embedment 4 electrodes obtain pressure-sensitive biography
Sensor, and four electrodes are sequentially distributed in the same surface of test block from left to right, and symmetrically divided with the axis of test block surface
Cloth, forms two interior electrodes and two external electrodes, it is described from the distance between two interior electrodes be 40mm, described two external electrodes
The distance between be 60mm.
Apply 10V DC voltage for two external electrodes, circulation pressure is carried out to sensor using electronic universal tester
The loading and unloading of stress, using electrochemical workstation two interior electrodes are carried out with the collection of voltage signal, using digital collection
The collection that instrument is strained, the speed of the loading and unloading of the circulation compression is 50N/s, maximum crushing stress 5MPa,
Minimum compression is 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Adopted every 0.1s
Collect a data, voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 1s.
The voltage sensitive sensor has a stronger pressure-sensitive, and strain sensitivity and stress sensitivity be respectively 300,2.9%/
MPa。
Embodiment 4：Graphene volume is the graphene cement base voltage sensitive sensor of cement quality 2%
A kind of modified graphene cement-base composite material is by water, cement, graphene, naphthalene water reducer (Nanjing Su Botexin
Materials Co., Ltd provides), normal sand composition, wherein, the particle diameter of graphene is 7~8 μm, and thickness is less than 10nm, specific surface area
Not less than 120m2/g.First weigh 4.5g naphthalene water reducer powder, be well mixed with 162g water, by 1.125g (cement quality
0.25%) graphene powder is added in naphthalene water reducer solution, uses the ultrasonic cell disruptor ultrasound that power is 360W
15min；Repeat the above steps 3 times；1.125g graphene powders are added in above-mentioned graphene dispersing solution, are using power
720W ultrasonic cell disruptor ultrasound 30min；Repeat the above steps 3 times, until graphene volume is 9g.Finally, use
Power is 1200W ultrasonic cell disruptor ultrasound 45min, can obtain finely dispersed solution.By above-mentioned graphene solution
It is added in 450g cement powders, while adds 40.5g water, is stirred slowly to uniform using glue sand agitator, 1350g normal sands are delayed
Slowly add and continue to stir, inject mould, gently shake to the bar that after closely knit, temperature is 22 DEG C, relative humidity is more than 95%
Modified graphene cement-base composite material is obtained after conserving 28d under part.
Modified graphene cement-base composite material 28d compression strength is 72MPa, rupture strength 11MPa.
It is 80 × 40 × 40mm in size3Black alkene cement-base composite material test block in embedment 4 electrodes obtain pressure-sensitive biography
Sensor, and four electrodes are sequentially distributed in the same surface of test block from left to right, and symmetrically divided with the axis of test block surface
Cloth, forms two interior electrodes and two external electrodes, it is described from the distance between two interior electrodes be 40mm, described two external electrodes
The distance between be 60mm.
Apply 10V DC voltage for two external electrodes, circulation pressure is carried out to sensor using electronic universal tester
The loading and unloading of stress, using electrochemical workstation two interior electrodes are carried out with the collection of voltage signal, using digital collection
The collection that instrument is strained, the speed of the loading and unloading of the circulation compression is 50N/s, maximum crushing stress 5MPa,
Minimum compression is 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Adopted every 0.1s
Collect a data, voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 1s.
The voltage sensitive sensor has stronger pressure-sensitive, and strain sensitivity and stress sensitivity are respectively 500,5%/MPa.
Embodiment 5：Graphene volume is the graphene cement base voltage sensitive sensor of cement quality 4%
A kind of modified graphene cement-base composite material is by water, cement, graphene, naphthalene water reducer (Nanjing Su Botexin
Materials Co., Ltd provides), normal sand composition, wherein, the particle diameter of graphene is 7~8 μm, and thickness is less than 10nm, specific surface area
For not less than 120m2/g.First weigh 9g naphthalene water reducer powder, be well mixed with 162g water, by 2.25g (cement quality
0.5%) graphene powder is added in naphthalene water reducer solution, uses the ultrasonic cell disruptor ultrasound that power is 360W
30min；Repeat the above steps 3 times；2.25g graphene powders are added in above-mentioned graphene dispersing solution, are using power
720W ultrasonic cell disruptor ultrasound 30min；Repeat the above steps 3 times, be 18g to graphene volume.Finally, using work(
Rate is 1200W ultrasonic cell disruptor ultrasound 60min, can obtain finely dispersed solution.Above-mentioned graphene solution is added
Enter into 450g cement powders, while add 40.5g water, stirred slowly to uniform using glue sand agitator, 1350g normal sands is slow
Add and continue to stir, inject mould, gently shake to after closely knit, in the bar that temperature is 18 DEG C, relative humidity is more than 95%
Modified graphene cement-base composite material is obtained after conserving 28d under part.
The modified graphene cement-base composite material compression strength is 60MPa, rupture strength 9.5MPa.
It is 80 × 40 × 40mm in size3Black alkene cement-base composite material test block in embedment 4 electrodes obtain pressure-sensitive biography
Sensor, and four electrodes are sequentially distributed in the same surface of test block from left to right, and symmetrically divided with the axis of test block surface
Cloth, forms two interior electrodes and two external electrodes, it is described from the distance between two interior electrodes be 40mm, described two external electrodes
The distance between be 60mm.
Apply 10V DC voltage for two external electrodes, circulation pressure is carried out to sensor using electronic universal tester
The loading and unloading of stress, using electrochemical workstation two interior electrodes are carried out with the collection of voltage signal, using digital collection
The collection that instrument is strained, the speed of the loading and unloading of the circulation compression is 50N/s, maximum crushing stress 5MPa,
Minimum compression is 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Adopted every 0.1s
Collect a data, voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 1s.
The voltage sensitive sensor has a stronger pressure-sensitive, and strain sensitivity and stress sensitivity be respectively 260,2.5%/
MPa。
Embodiment 6：Graphene volume is 1% graphene cement based sensor of cement quality
A kind of modified graphene cement-base composite material is by water, cement, graphene, naphthalene water reducer (Nanjing Su Botexin
Materials Co., Ltd provides), normal sand composition, wherein, the particle diameter of graphene is 7~8 μm, and thickness is less than 10nm, specific surface area
For not less than 120m2/g.2.25g naphthalene water reducer powder is first weighed, is well mixed with 67.5g water, by 0.45g (cement qualities
0.1%) graphene powder is added in naphthalene water reducer solution, uses the ultrasonic cleaner ultrasound 90min that power is 100W；
Repeat the above steps 4 times；0.45g graphene powders are added in above-mentioned graphene dispersing solution again, the use of power are 1200W's
Ultrasonic cell disruptor ultrasound 20min；Repeat the above steps 4 times, until graphene volume is 4.5g；It is using power finally
1500W ultrasonic cell disruptor ultrasound 30min, obtains finely dispersed modified graphene suspension.By above-mentioned modified stone
Black alkene suspension is added in 450g cement powders, while adds 67.5g water, is stirred slowly to uniform, general using glue sand agitator
450g normal sands are slowly added thereto, and continue to stir, and inject mould, are gently shaken to after closely knit, temperature be 20 DEG C, it is relatively wet
Spend to obtain modified graphene cement-base composite material after conserving 28d under conditions of more than 95%.
It is 80 × 20 × 20mm in size3Black alkene cement-base composite material test block in embedment 4 electrodes obtain pressure-sensitive biography
Sensor, and four electrodes are sequentially distributed in the same surface of test block from left to right, and symmetrically divided with the axis of test block surface
Cloth, forms two interior electrodes and two external electrodes, it is described from the distance between two interior electrodes be 20mm, described two external electrodes
The distance between be 60mm.
Apply 5V DC voltage for two external electrodes, circulation pressure is carried out to sensor using electronic universal tester should
The loading and unloading of power, using electrochemical workstation two interior electrodes are carried out with the collection of voltage signal, using digital collection instrument
The collection strained, the speed of the loading and unloading of the circulation compression is 100N/s, maximum crushing stress 5MPa, most
Small compression is 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Adopted every 0.1s
Collect a data, voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 1s.
The voltage sensitive sensor has a stronger pressure-sensitive, and strain sensitivity and stress sensitivity be respectively 321,2.70%/
MPa。
Embodiment 7：Graphene volume is 1% graphene cement based sensor of cement quality
A kind of modified graphene cement-base composite material is by water, cement, graphene, naphthalene water reducer (Nanjing Su Botexin
Materials Co., Ltd provides), normal sand composition, wherein, the particle diameter of graphene is 7~8 μm, and thickness is less than 10nm, specific surface area
For not less than 120m2/g.2.25g naphthalene water reducer powder is first weighed, is well mixed with 94.5g water, by 0.45g (cement qualities
0.1%) graphene powder is added in naphthalene water reducer solution, uses the ultrasonic cleaner ultrasound 75min that power is 200W；
Repeat the above steps 4 times；0.45g graphene powders are added in above-mentioned graphene dispersing solution again, the use of power are 1200W's
Ultrasonic cell disruptor ultrasound 20min；Repeat the above steps 4 times, until graphene volume is 4.5g；It is using power finally
1400W ultrasonic cell disruptor ultrasound 45min, obtains finely dispersed modified graphene suspension.By above-mentioned modified stone
Black alkene suspension is added in 450g cement powders, while adds 63g water, is stirred slowly to uniform using glue sand agitator, by 900g
Normal sand is slowly added thereto, and continues to stir, and injects mould, is gently shaken to after closely knit, temperature be 20 DEG C, relative humidity be
Modified graphene cement-base composite material is obtained after conserving 28d under conditions of more than 95%.
It is 100 × 20 × 40mm in size3Graphene cement-base composite material test block in embedment 4 electrodes obtain it is pressure-sensitive
Sensor, and four electrodes are sequentially distributed in the same surface of test block from left to right, and it is symmetrical with the axis of test block surface
Distribution, forms two interior electrodes and two external electrodes, it is described from the distance between two interior electrodes be 40mm, described two dispatches from foreign news agency
The distance between pole is 80mm.
Apply 6V DC voltage for two external electrodes, circulation pressure is carried out to sensor using electronic universal tester should
The loading and unloading of power, using electrochemical workstation two interior electrodes are carried out with the collection of voltage signal, using digital collection instrument
The collection strained, the speed of the loading and unloading of the circulation compression is 200N/s, maximum crushing stress 10MPa,
Minimum compression is 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Adopted every 0.5s
Collect a data, voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 2s.
The voltage sensitive sensor has a stronger pressure-sensitive, and strain sensitivity and stress sensitivity be respectively 293,2.0%/
MPa。
Embodiment 8：Graphene volume is 1% graphene cement based sensor of cement quality
A kind of modified graphene cement-base composite material is by water, cement, graphene, naphthalene water reducer (Nanjing Su Botexin
Materials Co., Ltd provides), normal sand composition, wherein, the particle diameter of graphene is 7~8 μm, and thickness is less than 10nm, specific surface area
For not less than 120m2/g.2.25g naphthalene water reducer powder is first weighed, is well mixed with 141.75g water, by 0.45g (cementaceous
0.1%) graphene powder is added in naphthalene water reducer solution amount, uses the ultrasonic cleaner ultrasound that power is 360W
60min；Repeat the above steps 4 times；0.45g graphene powders are added in above-mentioned graphene dispersing solution again, are using power
1200W ultrasonic cell disruptor ultrasound 20min；Repeat the above steps 4 times, until graphene volume is 4.5g；Last profit
The ultrasonic cell disruptor ultrasound 45min for being 1200W with power, obtains finely dispersed modified graphene suspension.Will be upper
State modified graphene suspension to be added in 450g cement powders, while add 60.75g water, using glue sand agitator stir slowly to
Uniformly, 1125g normal sands are slowly added thereto, continue to stir, inject mould, gently shaken to after closely knit, be 20 in temperature
DEG C, relative humidity be more than 95% under conditions of conserve 28d after obtain modified graphene cement-base composite material.
It is 120 × 40 × 40mm in size3Black alkene cement-base composite material test block in embedment 4 electrodes obtain pressure-sensitive biography
Sensor, and four electrodes are sequentially distributed in the same surface of test block from left to right, and symmetrically divided with the axis of test block surface
Cloth, forms two interior electrodes and two external electrodes, it is described from the distance between two interior electrodes be 30mm, described two external electrodes
The distance between be 90mm.
Apply 8V DC voltage for two external electrodes, circulation pressure is carried out to sensor using electronic universal tester should
The loading and unloading of power, using electrochemical workstation two interior electrodes are carried out with the collection of voltage signal, using digital collection instrument
The collection strained, the speed of the loading and unloading of the circulation compression is 300N/s, maximum crushing stress 15MPa,
Minimum compression is 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Gathered every 1s
Data, voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 4s.
The voltage sensitive sensor has a stronger pressure-sensitive, and strain sensitivity and stress sensitivity be respectively 200,1.5%/
MPa。
Embodiment 9：Graphene volume is 1% graphene cement based sensor of cement quality
A kind of modified graphene cement-base composite material is by water, cement, graphene, naphthalene water reducer (Nanjing Su Botexin
Materials Co., Ltd provides), normal sand composition, wherein, the particle diameter of graphene is 7~8 μm, and thickness is less than 10nm, specific surface area
For not less than 120m2/g.2.25g naphthalene water reducer powder is first weighed, is well mixed with 180g water, by 0.45g (cement qualities
0.1%) graphene powder is added in naphthalene water reducer solution, uses the ultrasonic cleaner ultrasound 30min that power is 500W；
Repeat the above steps 4 times；0.45g graphene powders are added in above-mentioned graphene dispersing solution again, the use of power are 1200W's
Ultrasonic cell disruptor ultrasound 20min；Repeat the above steps 4 times, until graphene volume is 4.5g；It is using power finally
1000W ultrasonic cell disruptor ultrasound 60min, obtains finely dispersed modified graphene suspension.By above-mentioned modified stone
Black alkene suspension is added in 450g cement powders, while adds 45g water, is stirred slowly to uniform using glue sand agitator, by 1350g
Normal sand is slowly added thereto, and continues to stir, and injects mould, is gently shaken to after closely knit, temperature be 20 DEG C, relative humidity be
Modified graphene cement-base composite material is obtained after conserving 28d under conditions of more than 95%.
It is 160 × 40 × 40mm in size3Black alkene cement-base composite material test block in embedment 4 electrodes obtain pressure-sensitive biography
Sensor, and four electrodes are sequentially distributed in the same surface of test block from left to right, and symmetrically divided with the axis of test block surface
Cloth, forms two interior electrodes and two external electrodes, it is described from the distance between two interior electrodes be 40mm, described two external electrodes
The distance between be 120mm.
Apply 10V DC voltage for two external electrodes, circulation pressure is carried out to sensor using electronic universal tester
The loading and unloading of stress, using electrochemical workstation two interior electrodes are carried out with the collection of voltage signal, using digital collection
The collection that instrument is strained, the speed of the loading and unloading of the circulation compression is 400N/s, and maximum crushing stress is
20MPa, minimum compression 0MPa.
The method of the collection for using electrochemical workstation that two interior electrodes are carried out with voltage signal for：Gathered every 2s
Data, voltage regulation limits are from -10V~10V, and total time is 4000s.
It is described use the acquisition method that digital collection instrument is strained for：1 data is acquired every 5s.
The voltage sensitive sensor has stronger pressure-sensitive, and strain sensitivity and stress sensitivity are respectively 123,1%/MPa.
Comparative example 1,2,3,4,5 is understood, under identical preparation technology, mixes the cement-base composite material tool of modified graphene
There is pressure-sensitive；The volume of graphene is properly increased, the pressure-sensitive of modified graphene cement-base composite material can be increased；But work as graphite
When alkene volume is too high, the reason such as scattered uneven, reunion of graphene can cause the monitoring signals of sensor are relative to weaken.
Fig. 2 is in case study on implementation 2, mixes the cement-base composite material of graphene under fixed loading amplitude CYCLIC LOADING, electricity
Pressure and the graph of a relation of loading and unloading；It is shown in figure under small stress, because elastic deformation is repeatable, in each CYCLIC LOADING
During, voltage increases and reduced with load during loading；Voltage increases when unloaded, has between voltage and loading and unloading obvious
Corresponding relation.
Table 1 is strain sensitivity and stress sensitivity in embodiment 2,3,4 and 5, and contrast finds the modification stone compared with high additive
Black alkene cement-base composite material sensor has stronger stress and strain monitoring signal.But when graphene volume is too high, stone
The reasons such as the scattered uneven, reunion of black alkene can cause the monitoring signals of sensor are relative to weaken.
The embodiment 2 of table 1, embodiment 3, embodiment 4 and the strain in embodiment 5 and stress sensitivity
In summary, the modified graphene cement-base composite material in case study on implementation of the present invention, it is using cement as gelling material
Material, naphthalene water reducer are dispersant, and graphene is conductive filler, and normal sand is the cement base composite wood that fine aggregate is combined
Material.Graphene uniform with satisfactory electrical conductivity is distributed in cement-base composite material by the invention, and experiment shows that graphene is assigned
Cement-base composite material pressure-sensitive is given；The volume of graphene is properly increased, answering for graphene cement-base composite material can be increased
Power and ga(u)ge factor, be advantageous to cement base pressure sensitive and be applied to engineering in practice.
Claims (10)
- A kind of 1. modified graphene cement-base composite material, it is characterised in that：The modified graphene cement-base composite material according to Mass parts include following components：
- A kind of 2. modified graphene cement-base composite material as claimed in claim 1, it is characterised in that：Described cement is general Logical portland cement, its 28d intensity are not less than 52.5MPa.
- A kind of 3. modified graphene cement-base composite material as claimed in claim 1, it is characterised in that：Described naphthalene system diminishing The water-reducing rate of agent is 15%~25%.
- A kind of 4. modified graphene cement-base composite material as claimed in claim 1, it is characterised in that：The grain of the graphene Footpath is 7~8 μm, and thickness is less than 10nm, and specific surface area is not less than 120m2/g。
- A kind of 5. modified graphene cement-base composite material as claimed in claim 1, it is characterised in that：Described normal sand SiO2Content is not less than 98wt%, and its particle size range is 0.08~2mm, wherein 0.08~0.5mm, 0.5~1.0mm and 1.0~ 2.0mm respectively accounts for 1/3.
- A kind of 6. modified graphene cement-base composite material as claimed in claim 1, it is characterised in that：Described modified graphite Alkene cement-base composite material 28d compression strength is not less than 60MPa, and rupture strength is not less than 9MPa.
- A kind of 7. preparation method of modified graphene cement-base composite material as claimed in claim 1, it is characterised in that：The party Method comprises the following steps：1) naphthalene water reducer solution is prepared：By naphthalene water reducer add needed for mixing water total amount 50%~80% water in, stir Mix uniformly, obtain naphthalene water reducer solution；2) modified graphene suspension is prepared：Graphene powder is added in naphthalene water reducer solution in batches, after ultrasonic disperse Obtain finely dispersed modified graphene suspension；3) prepared by modified graphene cement-base composite material：Graphene suspension is added in cement powder, sand is added and remains Remaining water, after stirring, grinding tool is injected, is gently shaken to closely knit, modified graphene cement-base composite material is can obtain after maintenance.
- A kind of 8. preparation method of modified graphene cement-base composite material as claimed in claim 7, it is characterised in that：Step 2) adding graphene powder in naphthalene water reducer solution in batches described in, obtains finely dispersed graphene after ultrasonic disperse Suspension comprises the following steps that：The graphite of cement gross mass 0.05%~0.5% is added into naphthalene water reducer solution every time Alkene powder, afterwards using 100~500W of power ultrasonic cleaner ultrasound 30~90min or 300~1000W ultrasonic wave 10~30min of cell disruptor ultrasound；After graphene powder all adds, crushed using 1000~1500W supersonic cell Machine 10~60min of ultrasound, obtains finely dispersed modified graphene suspension.
- A kind of 9. preparation method of modified graphene cement-base composite material as claimed in claim 7, it is characterised in that：Step 3) maintenance described in refers to conserve more than 28d under conditions of temperature is 20 ± 2 DEG C, relative humidity is more than 95%.
- A kind of 10. application of modified graphene cement-base composite material as claimed in claim 1, it is characterised in that：The modification Graphene cement-base composite material is applied to voltage sensitive sensor, and the stress sensitivity of described voltage sensitive sensor be 0.5%/ MPa~5%/MPa, strain sensitivity are 50~500.
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| CN112430035A (en) * | 2020-11-25 | 2021-03-02 | 江南大学 | Graphene oxide-pervious concrete composite material and preparation method thereof |
| CN112500067A (en) * | 2020-11-25 | 2021-03-16 | 长安大学 | Piezoresistive self-sensing cement concrete material, pavement structure and paving method |
| CN113799252A (en) * | 2021-10-09 | 2021-12-17 | 于胜斌 | Production process of cement-based conductive composite material based on graphene particles |
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