CN104030634B - A kind of high-strength and high ductility RPC of carbon-doped nanometer tube and preparation method thereof - Google Patents
A kind of high-strength and high ductility RPC of carbon-doped nanometer tube and preparation method thereof Download PDFInfo
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Abstract
The invention provides the high-strength and high ductility RPC of a kind of carbon-doped nanometer tube, by cement, CNT, silicon ash, water reducer, silica sand, flyash, silica flour, steel fibre and water are that raw material is prepared from, in mixture, each constituent content is calculated as with mass fraction: cement 1,000 1200 parts, silicon ash 250 350 parts, slag powders 250 350 parts, water reducer 40 50 parts, silica sand 1,200 1400 parts, 180 230 parts of water, steel fibre 190 230 parts, 180 250 parts of flyash, silica flour 80 120 parts, Carbon nano-tube dispersant 0.1 5 parts, carbon nanotube powder 1 10 parts.A kind of method that present invention also offers RPC preparing described carbon-doped nanometer tube.The RPC comprcssive strength that the present invention obtains is up to 250 300MPa, and rupture strength reaches 45 60MPa, higher than tradition RPC200 level correlated performance.Simultaneously, the RPC material first crack strength utilizing CNT to prepare is greatly improved, material first crack strength under uniaxial direct tensile state reaches 10MPa, and peak stress correspondence elongation strain reaches more than 0.5%, drastically increases tradition RPC toughness of material and intensity.
Description
Technical field
The present invention relates to building material field, belong to a kind of cement based with superhigh intensity and high tenacity
Composite, is specifically related to RPC of a kind of carbon-doped nanometer tube and preparation method thereof.
Background technology
RPC (Reactive Powder Concrete) be continue high performance concrete it
After, at the tool that the nineties in last century is developed by France Pierre Richard et al. employing conventional material
There are superhigh intensity, high-durability, cement-based material.RPC material, according to closestpacking principle, is adopted
With high fine and close cement based homogeneous system model, using the quartz sand of 400-600 micron as aggregate, simultaneously
Mix micro-steel fibre and the active mineral of certain volume, and be equipped with the side such as molding pressure, heat treatment maintenance
Method, the cement composite substrate material of the superhigh intensity prepared.According to its composition with heat treatment mode not
With, the comprcssive strength of this concrete can reach 200MPa to 800MPa；Rupture strength is 20-
40MPa, is 4-6 times of high-strength concrete；Fracture toughness is up to 40000J/m2, it is normal concrete
250 times；Chloride ion permeability is the 1/25 of high-strength concrete, and impermeabilisation is very competent.RPC can
It is greatly reduced structure cross-section dimensions and goods deadweight, for requirements such as high-level structure, high ferro simple supported box beams
The structure that bearing capacity is high, increases structure and uses space；Utilize the high permeability resistant energy of RPC, use can be manufactured
Pipeline and the solid waste of making conveying corrosive liquid process container；The shock resistance of RPC, wearability are also
Can be applicable to position and the military defense engineering being prone to wear out in hydraulic engineering.
The steel-making slag powder prepared by " activity of steel slag powder concrete " of Publication No. CN 101050090A
RPC has saved cost, and can be applicable to make prefabricated components, highway and manometer tube
The fields such as road, but its intensity and toughness are the most relatively low.Publication No. CN 101560082A's
" ultrahigh-strength active powder concrete and manufacture method thereof " with the addition of more polymer, is unfavorable for mixing
The long-term mechanical property of solidifying soil, improves cost simultaneously.RPC large-scale application still suffers from present
Problem: on the one hand, the RPC comprcssive strength prepared under normal pressure heat curing condition is the lowest, through surveying
Try its comprcssive strength the highest also less than 150MPa, far below the technology of 200MPa level activity concrete
Index；On the other hand, either in scientific research or Practical Project, almost without to RPC material
Toughness and first crack strength claim, conventional RPC material elongation strain be less than 0.05%, and
And load drastically declines after the appearance of crack, toughness is poor.
CNT is the material that the elastic modelling quantity being currently known is the highest, the Young mould of SWCN
Amount reaches more than 1TPa, about 5 times of steel.The density of CNT is generally 1.3-
1.4g/cm3, it is 1/6th of steel；Its elastic strain reaches 5%-12%, is more than the 60 of steel
Times.The indexs such as the intensity of CNT, toughness, specific surface area are far superior to traditional fibre, in theory
It is provided that the interfacial area transmission stress bigger than traditional fibre composite, cement can be strengthened simultaneously
The intensity of based composites and toughness.Multi-walled carbon nano-tubes (MWCNTs) is joined reactive powder
In concrete material, utilize multi-walled carbon nano-tubes to fill the small spaces within RPC, effectively reduce
The initial imperfection of RPC material internal.Multi-walled carbon nano-tubes is carried out by the present invention by chemical treatment means
Chemical modification so that with official's energy such as carboxylic acid group, hydroxyl on the surface of modified multi-walled carbon nano-tubes
Group.Owing to RPC hydrated product existing a large amount of unhydrated cement granules and unnecessary calcium hydroxide
Deng hydrated product, the functional group of multi-wall carbon nano-tube tube-surface can be with the hydrated calcium silicate in hydrated product
Or Ca (OH) (C-S-H)2Reacting, strengthen on the interface between CNT and matrix is strong
Covalent force, the microstructure of RPC material is improved, thus improve composite cracking strength and
Overall mechanical property.The addition of appropriate CNT and micro-steel fibre makes RPC compare high performance concrete
Having higher toughness, limit tensile strain reaches 0.5%, and has obvious elongation strain hardening
Characteristic.
Document CN101274831 discloses a kind of composite side manufacturing carbon nano-tube enhanced cement
Method, this material is by dispersing agent for fibre, organic solvent, carbon fiber, CNT, deionized water, super
Plasticiser, polymer emulsion, mineral admixture and cement production systD；Described in document CN101239800
Cement-based material is mainly by CNT, dispersant, thickening stabilizing agent, cement admixture, surpasses and mould
Agent, defoamer and cement production systD.Dispersion material therefor and preparation method that above-mentioned document is applied are equal
More complicated, it is unfavorable for that construction material produces popularization on a large scale.Centrifuge is applied to carbon by the present invention
In the dispersion of nanotube, achieve good dispersion effect, the most enterprising at RPC material preparation method
Go improvement, be more suitable for the large-scale application of RPC material.
Summary of the invention
The technical problem to be solved is to provide the high-strength and high ductility activity powder of a kind of carbon-doped nanometer tube
End concrete, this concrete is relatively costly for RPC in prior art, and in reality
In engineer applied, the problem that the comprcssive strength of RPC is relatively low relative to external product, pass through
Admixture CNT improve the cracking strength of RPC and elongation strain performance, simultaneously can also
Improve the comprcssive strength under its room temperature and heat curing condition.
The high-strength and high ductility RPC of the carbon-doped nanometer tube that the present invention provides, is received by cement, carbon
Mitron, silicon ash, water reducer, silica sand, flyash, silica flour, steel fibre and water be raw material preparation and
Becoming, in mixture, each constituent content is calculated as with mass fraction:
Cement 1000-1200 part, silicon ash 250-350 part,
Slag powders 250-350 part, water reducer 40-50 part,
Silica sand 1200-1400 part, water 180-230 part,
Steel fibre 190-230 part, flyash 180-250 part,
Silica flour 80-120 part, Carbon nano-tube dispersant 0.1-5 part,
Carbon nanotube powder 1-10 part.
Further, described mixture calculates optimum match ratio content with mass fraction in each component
For:
Cement 1000 parts, silicon ash 300 parts,
Slag powders 300 parts, water reducer 40 parts,
Silica sand 1400 parts, 200 parts of water,
Steel fibre 200 parts, 200 parts of flyash,
Silica flour 100 parts, Carbon nano-tube dispersant 1 part,
Carbon nanotube powder 5 parts.
Further, described cement is composite Portland cement or Portland cement, within 28 days, resists
Compressive Strength >=52.5MPa, rupture strength >=7.0MPa, the ratio table of cement is long-pending not less than 360m2/kg。
Specific surface area 20-28m of described silicon ash2/ g, its SiO2Content >=90%, described water reducer is
Non-retardation setting type poly-shuttle acid series high-performance powder water reducer, its water-reducing rate >=30%.
Described silica sand particle size range 0.1-0.6mm, described silica flour particle diameter is 5-50 μm, silica flour
SiO2Content >=99%.
Described steel fibre is shaped as long and straight type and end hook type, diameter about 0.2mm, a length of 3-
12mm, draw ratio >=30, tensile strength >=2000MPa.
Described slag powders is S95 grade slag powder or S105 grade slag powder, and flyash is one-level fine coal
Ash, density is 2.6g/cm3。
Described CNT can be obtained by large-scale industrial production, and purity is more than 95%, average caliber
Being about 20-60nm, length is about 5-15 micron.
Described Carbon nano-tube dispersant is a kind of aromatic compound, and its activity substance content is 90%,
Moisture is 10%, and cloud point is 68 DEG C.
A kind of method that present invention also offers RPC preparing described carbon-doped nanometer tube,
Comprise the steps:
(1) weigh in the water of carbon nanotube powder 200 parts of weight of addition of 5 parts of weight；
(2) Carbon nano-tube dispersant weighing 1 part of weight adds the CNT described in step (1)
With in the mixed liquor of water and stir evenly；
(3) mixed solution of step (2) gained is inserted ultrasonic washing unit carries out ultrasonic point
Dissipating, ultrasonic time is about 20-30 minute, until mixed solution presents uniform black, bottom is without heavy
Form sediment, prepare the most scattered carbon nano tube dispersion liquid；
(4) it is centrifuged the most scattered carbon nano tube dispersion liquid centrifuge processing, centrifugal
The rotating speed of machine is 15000 revs/min, and centrifugation time is about 30-60 minute, by the upper strata after centrifugal treating
Dispersion liquid takes out, and bottom precipitation carries out ultrasonic disperse again according to step (3), until CNT
The most stable is distributed in aqueous solution, obtains carbon nano tube dispersion liquid.
(5) by cement, silicon ash, slag powders, flyash, silica sand, silica flour, water reducer, steel
Fiber mix homogeneously, adds dry mixing 2-3 minute in blender, and each component ratio is as follows:
Cement 1000 parts, silicon ash 300 parts,
Slag powders 300 parts, water reducer 40 parts,
Silica sand 1400 parts, silica flour 100 parts,
Steel fibre 200 parts, 200 parts of flyash.
(6) carbon nano tube dispersion liquid prepared according to step (4), first by three/
The CNT dispersion soln of two adds in the mixture in step (5), stirs 3-5 minute；
(7) remaining 1/3rd CNT dispersion solns are added to described step (6)
In mixture, after stirring 3-5 minute, obtain the RPC mixture stirred；
(8) the above-mentioned RPC mixture obtaining stirring is poured in prefabricated mould, carries out
The suitable 60-120s aftershaping that vibrates carries out the maintenance of test specimen, the maintenance of test specimen be divided into standard curing and
High Temperature Curing two ways: the first is standard curing, standard curing condition is temperature 20 ± 2 DEG C, phase
To humidity more than 95%, test specimen pours after molding the demoulding after standard curing 2 days, and the test specimen after the demoulding is again
26 days available products of standard curing；The second is High Temperature Curing, and test specimen pours standard curing after molding
The demoulding after 2 days, moves into the RPC material after the demoulding in concrete High Temperature Curing equipment, in 6h
Slowly it is warming up to 300 DEG C and thermostatic curing 24h evenly, after it is slowly cooled to room temperature, then enters
Column criterion maintenance 25 days, obtains product.
The present invention compared with prior art has the advantage that
(1) RPC of carbon-doped nanometer tube of the present invention, by reactive powder
Adding CNT, described CNT is can be with a length of 5-20 of large-scale industrial production
Micron, the nanometer stage material of diameter 20-60 nanometer.Discovery is studied, due to RPC through inventor
Material is heterogeneous, multi-level composite, has nano level C-S-H gel, micron-sized silicon ash
And slag, the most millimetre-sized quartz sand.If simply mixing single steel fibre, only improve
Performance after RPC MATRIX CRACKING, in order to improve the performance of RPC on the whole, the present invention utilizes many walls
Small spaces within carbon nano-tube filled RPC, the effectively initial imperfection within reduction, improve material
Cracking strength and globality.Multi-walled carbon nano-tubes can effectively delay the generation of initial crack and send out
Exhibition, thus on a microscopic scale RPC material is carried out toughness reinforcing.When fracture propagation is macrocrack,
Multi-walled carbon nano-tubes is the most ineffective, then by the steel fibre being across between crack to undertake lotus
Load effect, it can be seen that both fibers can play respective in the different stress stages of material damage
Effect, the resistance playing mutual supplement with each other's advantages splits effect, solves that RPC tensile strength is low, the asking of poor toughness
Topic.Steel fibre and CNT intensity that the present invention selects are higher good with the adhesive property of base material.
This material macroscopic view Ultimate Tensile strains up to 1%, and tension first crack strength reaches 10MPa, peak load
Strain reaches 0.5%.Its mechanism is for form a plurality of micro-crack (single crack width during material tension
Degree is 50-100 microns, crack spacing about l0-15mm).Macroscopical tension stress of this material-
Strain stress relation shows as not reducing with the increase tension stress of stretching strain, and the strain hardening the most generally said is existing
As.After arriving peak load, load slowly reduces, the formation of a plurality of microcrack in drawing process
The macroscopical stretching strain making material increases several ten times larger.In the case of having high tenacity concurrently, the present invention is at normal pressure
Comprcssive strength under heat curing condition can be up to 200-300MPa, rupture strength 40-60MPa.Root
Consulting a large amount of prior art literature according to inventor, RPC typically uses high pressure in engineering
Steam curing, every related performance indicators is far below the technical parameter of the present invention, and maintenance is set by it
Standby and construction condition requires higher, is unfavorable for the popularization of RPC material.
(2) the RPC preparation method of carbon-doped nanometer tube of the present invention, first by water
Mud, silica sand, silica flour, water reducer, silicon ash, steel fibre, slag, flyash mix homogeneously, make
It is evenly distributed in matrix, thus improves the reactivity between them；The carbon of specified quantitative is received
Mitron is distributed in aqueous solution, is then poured in Binder Materials and is stirred, and can make RPC material
Each component mix homogeneously in material.The RPC material flowability finally given is fine, it is simple to molding and executing
Work.The RPC prepared by the method for the invention, the comprcssive strength under normal pressure and temperature maintenance
Being reached for 200MPa, rupture strength reaches 40MPa；Under normal pressure heat curing condition, comprcssive strength reaches
For 300MPa, rupture strength reaches 60MPa.Have that production technology is simple, intensity is high, toughness
The advantages such as good, low cost, easy construction.
Accompanying drawing explanation
Fig. 1 is can stably to preserve the carbon nano tube dispersion liquid of more than three months；
Fig. 2 is the CNT microcosmic scanned picture after dispersion；
Fig. 3 microcosmic picture that is CNT present in the RPC material.
Detailed description of the invention
Below in conjunction with embodiment and with reference to accompanying drawing, the present invention is further described in detail, but is not limited to
This.
If not the raw material used in embodiment refers in particular to, it is industrial chemicals known, commercially available, specifically
For:
Portland cement: P.O 52.5, commercially available；
S95 grade slag powder specific surface area >=400m2/ kg, 7d activity index >=75%, 28d activity index
>=95%, commercially available；S105 slag powders specific surface area >=500m2/ kg, 7d activity index >=95%, 28d
Activity index >=105%, commercially available；
Silica sand, particle diameter is 100-600 μm, and mean diameter is 200 μm, and modulus of fineness is 2.2, city
Sell；
Silicon ash, apparent density is 150-250kg/m3, specific surface area 20-28m2/ g, mean diameter is
0.1-0.3 μm, amorphous Si O in described silicon ash2Content is >=90%, commercially available；
Described water is water for industrial use；
Silica flour, particle size range is 5-50 μm, SiO in described silica flour2Content >=99%, commercially available；
Poly-shuttle acid water reducer, solid powder, water-reducing rate is 20%-30%, commercially available；
Steel fibre, is shaped as long and straight type or end hook type, steel fibre diameter 0.20mm, length 3-
12mm, tensile strength >=2000MPa, commercially available；
Multi-walled carbon nano-tubes, character is black powder, its a length of 5-15 μm, diameter 20-60nm,
Commercially available；
Carbon nano-tube dispersant, commercially available；
Above-described embodiment is only for clearly demonstrating example, and not limit to embodiment
Fixed.For those of ordinary skill in the field, can also make on the basis of the above description
The change of other multi-form or variation.Here without also all of embodiment being given thoroughly
Lift, and the obvious change thus extended out or variation are still in the invention claim
Protection domain among.
Claims (10)
1. the high-strength and high ductility RPC of a carbon-doped nanometer tube, it is characterized in that it is that raw material is prepared from by cement, CNT, Carbon nano-tube dispersant, slag powders, silicon ash, water reducer, silica sand, flyash, silica flour, steel fibre and water, in mixture, each constituent content is calculated as with mass fraction:
Cement 1000-1200 part, silicon ash 250-350 part,
Slag powders 250-350 part, water reducer 40-50 part,
Silica sand 1200-1400 part, water 180-230 part,
Steel fibre 190-230 part, flyash 180-250 part,
Silica flour 80-120 part, Carbon nano-tube dispersant 0.1-5 part,
Carbon nanotube powder 1-10 part.
The high-strength and high ductility RPC of a kind of carbon-doped nanometer tube the most according to claim 1, it is characterised in that match ratio content optimum in each component in described mixture is:
Cement 1000 parts, silicon ash 300 parts,
Slag powders 300 parts, water reducer 40 parts,
Silica sand 1400 parts, 200 parts of water,
Steel fibre 200 parts, 200 parts of flyash,
Silica flour 100 parts, Carbon nano-tube dispersant 1 part,
Carbon nanotube powder 5 parts.
The high-strength and high ductility RPC of a kind of carbon-doped nanometer tube the most according to claim 1, it is characterized in that described cement is composite Portland cement or Portland cement, 28 days comprcssive strength >=52.5MPa, rupture strength >=7.0MPa, the specific surface area of cement is not less than 360m2/kg。
The high-strength and high ductility RPC of a kind of carbon-doped nanometer tube the most according to claim 1, it is characterised in that specific surface area 20-28m of described silicon ash2/ g, its SiO2Content >=90%, described water reducer is non-retardation setting type polycarboxylic acid series high-performance powder water reducer, its water-reducing rate >=30%.
The high-strength and high ductility RPC of a kind of carbon-doped nanometer tube the most according to claim 1, it is characterised in that described silica sand particle size range 0.1-0.6mm, described silica flour particle diameter is 5-50 m, the SiO of silica flour2Content >=99%.
The high-strength and high ductility RPC of a kind of carbon-doped nanometer tube the most according to claim 1, it is characterised in that described steel fibre is shaped as long and straight type and end hook type, diameter 0.2mm, a length of 3-12mm, draw ratio >=30, tensile strength >=2000MPa.
The high-strength and high ductility RPC of a kind of carbon-doped nanometer tube the most according to claim 1, it is characterised in that described slag powders is S95 grade slag powder or S105 grade slag powder, flyash is first level flour coal ash, and the density of flyash is 2.6g/cm3。
The high-strength and high ductility RPC of a kind of carbon-doped nanometer tube the most according to claim 1, it is characterised in that described CNT can be obtained by large-scale industrial production, purity is more than 95%, and average caliber is 20-60nm, a length of 5-15 micron.
The high-strength and high ductility RPC of a kind of carbon-doped nanometer tube the most according to claim 1, it is characterised in that described Carbon nano-tube dispersant is a kind of aromatic compound, and its activity substance content is 90%, and moisture is 10%, and cloud point is 68 DEG C.
10. the method preparing the high-strength and high ductility RPC of the arbitrary described carbon-doped nanometer tube of claim 1-9, comprises the steps:
(1) weigh in the water of carbon nanotube powder 200 parts of weight of addition of 5 parts of weight；
(2) weigh in the CNT described in Carbon nano-tube dispersant addition step (1) of 1 part of weight and the mixed liquor of water and stir evenly；
(3) being inserted by the mixed solution of step (2) gained and carry out ultrasonic disperse in ultrasonic washing unit, ultrasonic time is 20-30 minute, until mixed solution presents uniform black, bottom, without precipitation, prepares the most scattered carbon nano tube dispersion liquid；
(4) it is centrifuged the most scattered carbon nano tube dispersion liquid centrifuge processing, the rotating speed of centrifuge is 15000 revs/min, centrifugation time is 30-60 minute, upper strata dispersion liquid after centrifugal treating is taken out, bottom precipitation carries out ultrasonic disperse again according to step (3), until the most stable being distributed in aqueous solution of CNT, obtain carbon nano tube dispersion liquid；
(5) by cement, silicon ash, slag powders, flyash, silica sand, silica flour, water reducer, steel fibre mix homogeneously, adding dry mixing 2-3 minute in blender, each component ratio is as follows:
Cement 1000 parts, silicon ash 300 parts,
Slag powders 300 parts, water reducer 40 parts,
Silica sand 1400 parts, silica flour 100 parts,
Steel fibre 200 parts, 200 parts of flyash；
(6) carbon nano tube dispersion liquid prepared according to step (4), first adds the CNT dispersion soln of 2/3rds in the mixture in step (5), stirs 3-5 minute；
(7) remaining 1/3rd CNT dispersion solns are added in the mixture to described step (6), after stirring 3-5 minute, obtain the RPC mixture stirred；
(8) the above-mentioned RPC mixture obtaining stirring is poured in prefabricated mould, carry out the suitable 60-120s aftershaping that vibrates and carry out the maintenance of test specimen, the maintenance of test specimen is divided into standard curing and High Temperature Curing two ways: the first is standard curing, standard curing condition is 20 ± 2 ° of C of temperature, relative humidity more than 95%, test specimen pours the demoulding after molding standard curing 2 days, and the test specimen after the demoulding carries out 26 days available products of standard curing again；The second is High Temperature Curing, test specimen pours after molding the demoulding after standard curing 2 days, RPC material after the demoulding is moved in concrete High Temperature Curing equipment, 300 DEG C and thermostatic curing 24h slowly it are warming up to evenly in 6h, after it is slowly cooled to room temperature, carry out standard curing 25 days again, obtain product.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001240440A (en) * | 2000-02-25 | 2001-09-04 | Taiheiyo Cement Corp | Steel fiber for reinforcing concrete and fiber reinforced concrete |
| CN101239800B (en) * | 2008-03-07 | 2011-03-23 | 哈尔滨工业大学 | Carbon nano-tube enhanced cement-base composite material and preparation method thereof |
| CN101560082B (en) * | 2008-04-16 | 2012-11-21 | 柳州欧维姆机械股份有限公司 | Ultrahigh-strength active powder concrete and preparation method thereof |
| CN101274831B (en) * | 2008-05-16 | 2012-06-27 | 哈尔滨工业大学 | Carbon nano-tube fiber cement-based material and preparation thereof |
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