CN108314380A - A kind of graphene oxide-ferroso-ferric oxide magnetic liquid-cement-base composite material and preparation method thereof - Google Patents
A kind of graphene oxide-ferroso-ferric oxide magnetic liquid-cement-base composite material and preparation method thereof Download PDFInfo
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- CN108314380A CN108314380A CN201810099393.4A CN201810099393A CN108314380A CN 108314380 A CN108314380 A CN 108314380A CN 201810099393 A CN201810099393 A CN 201810099393A CN 108314380 A CN108314380 A CN 108314380A
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- graphene oxide
- cement
- magnetic liquid
- composite material
- base composite
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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
-
- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
-
- 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
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/00258—Electromagnetic wave absorbing or shielding materials
Abstract
The present invention discloses a kind of graphene oxide ferroso-ferric oxide magnetic liquid cement-base composite material and preparation method thereof.The graphene oxide Fe of the present invention3O4Because the incorporation of graphene oxide reduces the hole inside Behavior of Hardened Cement Paste inside magnetic liquid cement-base composite material, improve the pore structure of Behavior of Hardened Cement Paste so that the more uniform densification of gel in cement.Meanwhile the incorporation of graphene oxide can also reduce the generation of needle-shaped entringite so that the structure of Behavior of Hardened Cement Paste is more fine and close.Fe is additionally incorporated3O4This magnetic material of magnetic liquid increases the magnetic conductivity of composite material to improve the capability of electromagnetic shielding of this cement-base composite material.Meanwhile the proposition of present invention novelty replaces stirring by the way of ball milling, is difficult to be evenly distributed on the difficult point of cement-based material to overcome ferroso-ferric oxide magnetic liquid.Therefore, composite material of the invention, which is gathered around, has wide practical use.
Description
Technical field
The present invention relates to a kind of electromagnetic shielding composite materials, and in particular to a kind of graphene oxide-ferroso-ferric oxide
(Fe3O4) magnetic liquid-cement-base composite material and preparation method thereof.
Background technology
Existing cement-based electromagnetic shielding composite material generally use metal material or Carbon materials, but by being added
The characteristic of material is generally only capable of being electromagnetically shielded by the reflecting properties of metal material or the absorbing property of Carbon materials,
It is of high cost, it is difficult to stir evenly, be easy that there are leaky wave points.But it is the spy collectively constituted by electric field and magnetic field according to electromagnetic field
Point can largely improve cement base if can be added into cement base with high conductivity and high magnetic material
The dielectric constant and magnetic conductivity of material, to realize the shielding at two aspects of electric field and magnetic field.
The dynamic viscosity of commercially available ferroso-ferric oxide magnetic liquid can be up to 9.5mpa*s, be that (20 degrees Celsius are gone more than 9 times of water
The viscosity of ionized water is 1.006mpa*s).If magnetic liquid to be directly added into equally more sticky cement-based material, will be unable to
It is stirred uniformly using conventional method.In addition, common cement base agitating device usually contains ferro element, therefore in whipping process
In, it is easy so that ferroso-ferric oxide magnetic liquid is adsorbed on agitating device, to generate the separation with cement-based material.
In addition, the dry-mixed mode of generally use mixes graphene and cement powder at present, then carry out adding water
Stirring, also in fact is difficult to accomplish graphene being uniformly distributed in cement-based material in this way.
Invention content
In order to overcome the disadvantages and deficiencies of the prior art, the primary purpose of the present invention is that providing a kind of graphene oxide-
Fe3O4The preparation method of magnetic liquid-cement-base composite material.
Another object of the present invention is to provide the graphene oxide-Fe being prepared by above-mentioned preparation method3O4Magnetic
Liquid-cement-base composite material.The composite material has the characteristics that capability of electromagnetic shielding stabilization.
The purpose of the invention is achieved by the following technical solution：
A kind of graphene oxide-Fe3O4The preparation method of magnetic liquid-cement-base composite material, includes the following steps：
Step A：Prepare test material：Main material has：Graphene oxide powder, portland cement, tetrasiloxane quaternary ammonium
Villaumite, 25% tetramethyl ammonium hydroxide solution (technical grade), dimethicone, distilled water analyze pure FeCl2, analyze pure FeCl3,
98%HCl, 1% ammonium hydroxide；
Step B：Prepare Fe3O4Magnetic liquid：According to molal weight than 1:2 mixing FeCl3And FeCl2, will obtain mixture according to
1:5 mass ratio is dissolved in distilled water, stirring to formation brown solution；Fe is added in brown solution2+With Fe3+Mole matter
The HCl solution of summation 1% is measured, is stored at room temperature 6~8 hours after stirring 2~2.5min；It is slowly dropped into 1% in obtained solution
Ammonium hydroxide, observation form brown black precipitate；Continue to be slowly dropped into ammonium hydroxide, until the pH value of solution is between 9.2~9.8；Precipitation point
Fe is obtained from after3O4Particle；By Fe3O4Particle is according to mass ratio 1：It lives on 10 surfaces that 25% tetramethyl ammonium hydroxide solution is added
Property agent so that particle is suspended in liquid medium using ultrasonic oscillation 20~25 minutes；After standing is cooled to room temperature, nothing is taken out
The particle of method dissolving；Ultrasonic oscillation process is repeated, until obtaining stable Fe there is no precipitation particle in solution3O4Magnetic liquid；
Step C：Configure graphene oxide dispersant：Fit quality ratio is：Tetrasiloxane quaternary ammonium villaumite：Dimethicone：
Deionized water=5:1:15；Tetrasiloxane quaternary ammonium villaumite and dimethicone are put into glass beaker, 2~2.5min is stirred,
Make tetrasiloxane quaternary ammonium villaumite and dimethicone at homogeneous phase；It is then slowly added into water, continues 15~18min of stirring；It will mix
It closes object and is placed on mulser the 15~18min of emulsification of the rotating speed with 3000~3500r/min, obtain graphene oxide dispersant；
Step D：Graphene oxide disperses：Graphene oxide and graphene oxide dispersant are with 1:1.5 volume ratios mix, and stir
15~18min is mixed, graphene oxide suspension is prepared into；
Step E：Prepare cement-base composite material：Raw material quality ratio is：Portland cement：Graphene oxide suspension：
Fe3O4Magnetic liquid：Water=10：1：1：4；By portland cement and Fe3O4Magnetic liquid is added to according to aforementioned proportion in planetary ball mill
300~320min of ball milling so that Fe3O4Magnetic liquid and the full and uniform mixing of cement；In net slurry blender, water, stirring 3 are added
~3.5min；Graphene oxide suspension is added, 1~1.5min is stirred；By in the slurry injection mold after stirring, use
300~350MPa pressure suppresses 10~15min, will be unloaded after test specimen compression moulding；Mold is impregnated to take out afterwards for 24 hours in water and is taken off
Mould continues under normal temperature condition, the graphene oxide-Fe that the maintenance that is soaked in water obtains3O4Magnetic liquid-cement-base composite material 28d,
Test material preparation is completed.
In step B,
Preferably, it is stored at room temperature 6 hours after stirring 2min；
Preferably, described to use the time of ultrasonic oscillation for 20min；
In step C,
Preferably, the time of the stirring is 2min；
Preferably, the time for continuing stirring is 15min；
Preferably, the condition of the emulsification is to emulsify 15min with the rotating speed of 3000r/min；
In step D,
Preferably, the time of the stirring is 15min；
In step E,
Preferably, the time of the ball milling is 300min；
Preferably, the time stirred after the addition water is 3min；
Preferably, the time stirred after graphene oxide suspension that adds is 1min；
Preferably, the condition of the compacting is to suppress 10min with 300MPa pressure.
A kind of graphene oxide-Fe3O4Magnetic liquid-cement-base composite material, is prepared by above-mentioned preparation method.
The present invention mechanism be：The present invention is based on the correlative studys of graphene oxide cement-base composite material, propose multiple
Fe is added in condensation material3O4Graphene oxide-Fe is made in magnetic liquid3O4Magnetic liquid-cement-base composite material.It is currently used for being electromagnetically shielded
Cement-base composite material be also limited to high conductivity, low magnetic permeability.The present invention is based on the thinkings for improving magnetic conductivity, propose in oxygen
In graphite alkene cement-base composite material, it is added into Fe3O4Magnetic liquid improves the magnetic conductivity of composite material.But Fe3O4Magnetic liquid moves
Power viscosity can be up to 9.5mpa*s, be more than 9 times of water (viscosity of 20 degrees Celsius of deionized waters is 1.006mpa*s).Therefore such as
What is by the very big Fe of viscosity3O4Magnetic liquid is uniformly mixed into cement matrix, and the difficult point for being this research is also the main mesh of the present invention
's.The present invention is by planetary ball mill by cement, graphene oxide solution and Fe3O4Magnetic liquid three mixes so that graphite oxide
Alkene solution and Fe3O4Magnetic liquid is dispersed in cement, then by way of compaction moulding, is prepared with good electromagnetic shielding
The cement-base composite material component of performance.
The present invention has the following advantages and effects with respect to the prior art：
Graphene oxide-the Fe of the present invention3O4Magnetic liquid-cement-base composite material is a kind of novel electromagnetic shielding material, tool
Have the characteristics that capability of electromagnetic shielding is good, is a kind of emerging cement-base composite material.The composite inner is because of graphene oxide
Incorporation reduce the hole inside Behavior of Hardened Cement Paste, improve the pore structure of Behavior of Hardened Cement Paste so that the more uniform cause of gel in cement
It is close.Meanwhile the incorporation of graphene oxide can also reduce the generation of needle-shaped entringite so that the structure of Behavior of Hardened Cement Paste is more fine and close.
Fe is additionally incorporated3O4This magnetic material of magnetic liquid increases the magnetic conductivity of composite material to improve this cement base composite wood
The capability of electromagnetic shielding of material.Meanwhile the proposition of present invention novelty replaces stirring by the way of ball milling, to overcome four
Fe 3 O magnetic liquid is difficult to be evenly distributed on the difficult point of cement-based material.Therefore graphene oxide-Fe3O4Magnetic liquid-cement base is compound
Material, which is gathered around, to have wide practical use.
Description of the drawings
Fig. 1 is full frequency band shield effectiveness curve graph within the scope of 300MHz-3GHz.
Specific implementation mode
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
Step A：Prepare ordinary cement based composites, number C0.Using common 325 portland cement, the ratio of mud is
0.5,500g cement is weighed, cement powder is poured into net slurry blender, after stirring 10s, pours into water by 250g water, continues to stir 2min.
The cement mortar that finishes of stirring is poured into mold, surface smoothes out, form removal after standing for 24 hours, be put into standard curing box (20 DEG C, 98%
Humidity) maintenance 28d, takes out for use.
Step B：Prepare graphene oxide-cement-base composite material, number C1.Using common 325 portland cement, water ash
Than being 0.4,500g cement, 200g water, 50g graphene oxide suspensions are weighed.Cement powder is poured into net slurry blender, is stirred
After 10s, water is poured into, continues to stir 2min, pours into graphene oxide suspension, stir 1min.The cement mortar that stirring finishes is fallen
Enter in mold, surface smoothes out, form removal after standing for 24 hours, is put into (20 DEG C, 98% humidity) maintenance 28d of standard curing box, and taking-up waits for
With.
Wherein, the preparation of the graphene oxide suspension：Graphene oxide and graphene oxide dispersant are with 1:1.5
Volume ratio mixes, and stirs 15min, is prepared into graphene oxide suspension；
The preparation of the graphene oxide dispersant：Fit quality ratio is：Tetrasiloxane quaternary ammonium villaumite：Dimethyl-silicon
Oil：Deionized water=5:1:15；Tetrasiloxane quaternary ammonium villaumite and dimethicone are put into glass beaker, 2min is stirred, makes
Tetrasiloxane quaternary ammonium villaumite and dimethicone are at homogeneous phase；It is then slowly added into water, continues to stir 15min；Mixture is put
The rotating speed emulsification 15min with 3000r/min on mulser is set, graphene oxide dispersant is obtained.
Step C：Prepare Fe3O4Magnetic liquid-cement-base composite material, number C2.Using common 325 portland cement, the ratio of mud
0.5, weigh 500g cement, 250g water, 50g Fe3O4Magnetic liquid.By cement, Fe3O4Magnetic liquid is added to ball milling in planetary ball mill
300min.The mixed-powder of acquisition is poured into net slurry blender, water is added, persistently stirs 3min.By the slurry after stirring
Body injects in mold, suppresses 10min with 300MPa pressure, will be unloaded after test specimen compression moulding.By mold impregnate in water for 24 hours after
Demoulding is taken out, is continued under normal temperature condition, be soaked in water maintenance 28d, takes out for use.
Wherein, the Fe3O4The preparation of magnetic liquid：According to molal weight than 1:2 mixing FeCl3And FeCl2, will be mixed
Object is closed according to 1:5 mass ratio is dissolved in distilled water, stirring to formation brown solution；Fe is added in brown solution2+With Fe3 +The HCl solution of molal weight summation 1% is stored at room temperature 6 hours after stirring 2min；1% ammonia is slowly dropped into obtained solution
Water, observation form brown black precipitate；Continue to be slowly dropped into ammonium hydroxide, until the pH value of solution is between 9.2~9.8；Precipitation separation
After obtain Fe3O4Particle；By Fe3O4Particle is according to mass ratio 1：10 are added the surface-active of 25% tetramethyl ammonium hydroxide solution
Agent made particle suspend in liquid medium using ultrasonic oscillation 20 minutes；After standing is cooled to room temperature, taking-up can not dissolve
Particle；Ultrasonic oscillation process is repeated, until obtaining stable Fe there is no precipitation particle in solution3O4Magnetic liquid.
Step D：Prepare graphene oxide-Fe3O4Magnetic liquid-cement-base composite material, number C3.Using common 325 silicate
Cement, the ratio of mud 0.4 weigh 500g cement, 200g water, 50g Fe3O4Magnetic liquid, 50g graphene oxide suspensions.By cement and
Fe3O4Magnetic liquid is added to ball milling 300min in planetary ball mill according to aforementioned proportion.The mixed-powder of acquisition is poured into net slurry to stir
Machine is mixed, water is added, persistently stirs 3min, adds graphene oxide suspension, stirs 1min.By the slurry after stirring
It injects in mold, suppresses 10min with 300MPa pressure, will be unloaded after test specimen compression moulding.Mold immersion is taken afterwards for 24 hours in water
Go out demoulding, continues under normal temperature condition, the graphene oxide-Fe that the maintenance that is soaked in water obtains3O4Magnetic liquid-cement-base composite material
28d, test material preparation are completed, and are taken out for use.
The 28d intensity of C0-C3 samples, dielectric constant, electrical loss angle tangent within the scope of 300MHz-3GHz are tested respectively
Value, magnetic conductivity.Strength test standard is national standard GB/T 17671-1999, and dielectric constant, electrical loss angle tangent value, magnetic conductivity are surveyed
Test-object standard is national standard GJB2038A-2011.Sample number into spectrum and test result are as shown in table 1.
1 C0-C3 sampling test data of table
Can be seen that incorporation graphene oxide suspension from 1 data result of table can be substantially improved the dielectric constant of material,
Namely increase polarization of the material under electric field action, while the tangent value of electrical loss angle is there has also been significantly increasing,
Also from another side illustration under electric field action, graphene oxide suspension can increase the dielectric loss performance of material.
On the other hand, Fe3O4The admixture of magnetic liquid then increases the magnetic conductivity of material, also means that, the magnetization of material under magnetic fields
Degree greatly improves.Show that graphene oxide suspension and Fe is added in mixing by experimental data3O4Magnetic liquid can be prepared
The good concrete material of capability of electromagnetic shielding.Fig. 1 is always to shield in 0-3GHz (300MHz-3GHz is effectively to shield wave band) range
Efficiency is covered, also illustrates foregoing invention effect.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of graphene oxide-Fe3O4The preparation method of magnetic liquid-cement-base composite material, it is characterised in that including following step
Suddenly：
Step A：Prepare test material：Main material has：Graphene oxide powder, portland cement, tetrasiloxane quaternary ammonium villaumite,
25% tetramethyl ammonium hydroxide solution, dimethicone, distilled water analyze pure FeCl2, analyze pure FeCl3, 98%HCl, 1% ammonia
Water；
Step B：Prepare Fe3O4Magnetic liquid：According to molal weight than 1:2 mixing FeCl3And FeCl2, mixture will be obtained according to 1:5
Mass ratio is dissolved in distilled water, stirring to formation brown solution；Fe is added in brown solution2+With Fe3+Molal weight summation
1% HCl solution is stored at room temperature 6~8 hours after stirring 2~2.5min；It is slowly dropped into 1% ammonium hydroxide in obtained solution, sees
It examines to form brown black precipitate；Continue to be slowly dropped into ammonium hydroxide, until the pH value of solution is between 9.2~9.8；It is obtained after precipitation separation
Fe3O4Particle；By Fe3O4Particle is according to mass ratio 1：10 are added the surfactant of 25% tetramethyl ammonium hydroxide solution, use
Ultrasonic oscillation 20~25 minutes makes particle suspend in liquid medium；After standing is cooled to room temperature, that can not be dissolved is taken out
Grain；Ultrasonic oscillation process is repeated, until obtaining stable Fe there is no precipitation particle in solution3O4Magnetic liquid；
Step C：Configure graphene oxide dispersant：Fit quality ratio is：Tetrasiloxane quaternary ammonium villaumite：Dimethicone：Go from
Sub- water=5:1:15；Tetrasiloxane quaternary ammonium villaumite and dimethicone are put into glass beaker, 2~2.5min is stirred, makes four
Silicone quat villaumite and dimethicone are at homogeneous phase；It is then slowly added into water, continues 15~18min of stirring；By mixture
It is placed on mulser the rotating speed with 3000~3500r/min and emulsifies 15~18min, obtain graphene oxide dispersant；
Step D：Graphene oxide disperses：Graphene oxide and graphene oxide dispersant are with 1:1.5 volume ratios mix, stirring 15
~18min is prepared into graphene oxide suspension；
Step E：Prepare cement-base composite material：Raw material quality ratio is：Portland cement：Graphene oxide suspension：Fe3O4
Magnetic liquid：Water=10：1：1：4；By portland cement and Fe3O4Magnetic liquid is added to ball milling in planetary ball mill according to aforementioned proportion
300~320min so that Fe3O4Magnetic liquid and the full and uniform mixing of cement；In net slurry blender, water is added, stirring 3~
3.5min；Graphene oxide suspension is added, 1~1.5min is stirred；By in the slurry injection mold after stirring, use
300~350MPa pressure suppresses 10~15min, will be unloaded after test specimen compression moulding；Mold is impregnated to take out afterwards for 24 hours in water and is taken off
Mould continues under normal temperature condition, the graphene oxide-Fe that the maintenance that is soaked in water obtains3O4Magnetic liquid-cement-base composite material 28d,
Test material preparation is completed.
2. according to the graphene oxide-Fe described in claim 13O4The preparation method of magnetic liquid-cement-base composite material, it is special
Sign is：
In step B, it is stored at room temperature 6 hours after stirring 2min；
It is described to use the time of ultrasonic oscillation for 20min in step B.
3. according to the graphene oxide-Fe described in claim 13O4The preparation method of magnetic liquid-cement-base composite material, it is special
Sign is：
In step C, the time of the stirring is 2min；
In step C, the time for continuing stirring is 15min.
4. according to the graphene oxide-Fe described in claim 13O4The preparation method of magnetic liquid-cement-base composite material, it is special
Sign is：
In step C, the condition of the emulsification is to emulsify 15min with the rotating speed of 3000r/min.
5. according to the graphene oxide-Fe described in claim 13O4The preparation method of magnetic liquid-cement-base composite material, it is special
Sign is：
In step D, the time of the stirring is 15min.
6. according to the graphene oxide-Fe described in claim 13O4The preparation method of magnetic liquid-cement-base composite material, it is special
Sign is：
In step E, the time of the ball milling is 300min.
7. according to the graphene oxide-Fe described in claim 13O4The preparation method of magnetic liquid-cement-base composite material, it is special
Sign is：
In step E, the time stirred after the addition water is 3min.
8. according to the graphene oxide-Fe described in claim 13O4The preparation method of magnetic liquid-cement-base composite material, it is special
Sign is：
In step E, the time stirred after graphene oxide suspension that adds is 1min.
9. according to the graphene oxide-Fe described in claim 13O4The preparation method of magnetic liquid-cement-base composite material, it is special
Sign is：
In step E, the condition of the compacting is to suppress 10min with 300MPa pressure.
10. a kind of graphene oxide-Fe3O4Magnetic liquid-cement-base composite material, it is characterised in that any by claim 1~9
Preparation method described in is prepared.
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| CN110451893B (en) * | 2019-08-28 | 2022-04-15 | 成都理工大学 | Cement-based electromagnetic development composite material, preparation method and application thereof |
| CN110818374A (en) * | 2019-11-19 | 2020-02-21 | 湖北工业大学 | Graphene gypsum-based electromagnetic shielding composite material doped with wet-milled steel slag and preparation method thereof |
| CN114573284A (en) * | 2022-05-09 | 2022-06-03 | 太原理工大学 | Graphene oxide magnetic oriented dispersion reinforced cement-based composite material and preparation method thereof |
| CN114573284B (en) * | 2022-05-09 | 2022-07-26 | 太原理工大学 | Graphene oxide magnetic directional dispersion reinforced cement-based composite material and preparation method thereof |
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