CN107354500A - A kind of glass fiber compound material of the grapheme modified claddings of nanoscale Fe3O4 and preparation method thereof - Google Patents
A kind of glass fiber compound material of the grapheme modified claddings of nanoscale Fe3O4 and preparation method thereof Download PDFInfo
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- CN107354500A CN107354500A CN201710569523.1A CN201710569523A CN107354500A CN 107354500 A CN107354500 A CN 107354500A CN 201710569523 A CN201710569523 A CN 201710569523A CN 107354500 A CN107354500 A CN 107354500A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
Abstract
The invention discloses a kind of nanoscale Fe3O4The glass fiber compound material of grapheme modified cladding, comprises the following steps：（1）Glass fibre is put into Muffle furnace and calcined, is sequentially placed into acetone, alkali lye and handles；（2）Glass fibre after processing is placed in the aqueous solution of silane coupler, infiltrated after taking out cleaning in bovine serum albumin solution, is placed in graphene oxide suspension after cleaning again, after drying, is put into sodium borohydride alkaline solution, is heated, is stirred, is dried；（3）Using redox graphene/glass fibre as anode, tiselius apparatus is built by negative electrode of carbon-point, with Fe3O4Suspension is plating solution, carries out electrophoretic deposition to graphene/glass fibre, composite is made.The invention discloses composite prepared by this method simultaneously.Composite prepared by the present invention has higher magnetic conductivity under the premise of conductive capability is ensured, can lift its performance in terms of electromagnetic shielding.
Description
Technical field
The present invention relates to a kind of composite, more particularly to a kind of nanoscale Fe3O4The glass fibre of grapheme modified cladding
Composite and preparation method thereof.
Background technology
With the development of science and technology and electronics industry, the application of various electronic equipments is increasing, forms electromagnetic pollution.
Electromagenetic wave radiation can not only damage health, disturb the normal work of electronic instrument, can also cause the leakage of confidential information, because
This, researches and develops High Performance Shielding material, reduces electromagnetic pollution to the social life for us and national defense construction all with important
Meaning.
Graphene be one kind by carbon atom with sp2The cellular flat film that hybrid form is formed, it is a kind of only one
The quasi- two-dimensional material of atomic layer level thickness, has good conduction, heat conductivility and mechanical property, and its electron mobility can reach 2
×105cm2/ VS, temperature stability is high, and for electrical conductivity up to 108 Ω/m, surface resistance is about 31 Ω/sq（310Ω/m2）, compare copper
It is conductive best material at room temperature or silver is lower.And specific surface area is big（2630m2/g）, thermal conductivity（It is at room temperature
5000W·m-1·K-1）It is 36 times of silicon, 20 times of GaAs, be copper（401WmK at room temperature）More than ten times.Individual layer stone
The thermal conductivity factor of black alkene is up to 5300W/mK, or even there are some researches show its thermal conductivity factor is up to 6600W/mK.Graphene is existing
Most hard and intensity highest material, its modulus of elasticity are 1.1Tpa, tensile strength 125Gpa in material.
Glass fibre as a kind of technical fiber material, be by frit under high temperature fused state wire drawing prepare and
Into with a series of premium properties energy such as high temperature resistant, resist chemical, intensity height, modulus height.Glass fibre turns into resin base
One of most important reinforcing material of composite, has obtained abundant application in fields such as Aeronautics and Astronautics, naval vessel, chemical industry metallurgicals.
Ferroso-ferric oxide is a kind of oxide of iron, and its chemical formula is Fe3O4.Ferroso-ferric oxide has ferromagnetism, such as fruit shape
Into particle radius in Nano grade, referred to as magnetic particles of ferroferric oxide.In contemporary electrified and informationized society, magnetic material
The application of material is very extensive.Fe 3 O 4 magnetic material as a kind of multifunction magnetic material, inhale by treatment, microwave in tumour
Receipts material, catalyst carrier, cell separation, magnetic recording material, magnetic fluid, medicine and other fields have been widely used.
The content of the invention
The invention discloses a kind of nanoscale Fe3O4The preparation method of the glass fiber compound material of grapheme modified cladding,
Composite prepared by this method improves the technique that graphene is coated in fiberglass surfacing, and with electrophoretic deposition in stone
Nanoscale ferroso-ferric oxide is deposited on black alkene/glass fibre, high magnetic permeability graphene coated glass fibre is made, is had more preferable
Capability of electromagnetic shielding.
A kind of nanoscale Fe3O4The preparation method of the glass fiber compound material of grapheme modified cladding, including following step
Suddenly：
（1）The surface treatment of glass fibre：Glass fibre is put into Muffle furnace and calcined, is sequentially placed into acetone, alkali lye and handles；
（2）The preparation of graphene oxide/glass fibre：By step（1）Glass fibre after processing is placed in the water of silane coupler
Solution, infiltrated in bovine serum albumin solution after taking out cleaning, be placed in after cleaning again in graphene oxide suspension,
After drying, it is put into sodium borohydride alkaline solution, heats, stir, dries, graphene oxide/glass fibre is made；
（3）The modification of magnetic material：With step（2）In manufactured graphene oxide/glass fibre be anode, using carbon-point as negative electrode
Tiselius apparatus is built, with 1.0-1.5mg/ml Fe3O4Suspension is plating solution, and carrying out electrophoresis to graphene oxide/glass fibre sinks
Product, is made nanoscale Fe3O4The glass fiber compound material of grapheme modified cladding.
Preferably, the step（1）The middle temperature calcined in Muffle furnace that is put into glass fibre is 455-500 DEG C, calcining
Time is 1-2 hours；The step（1）The concentration of middle alkali lye is 1wt.%-30wt.%, and processing time is 0.5-6 hours.
It is highly preferred that the step（1）Alkali lye is sodium hydroxide solution, concentration 25wt.%.
Preferably, the step（2）In, the aqueous solution of silane coupler is the kh550 aqueous solution, concentration 1wt.%-
5wt.%, the time being placed in the silane coupler aqueous solution are 5min-10min.The handling process of silane coupler can substantially increase
BSA solidification effect.
Preferably, the step（2）The concentration of middle bovine serum albumin solution is 1-1.5wt.%, and cow's serum egg is arrived in infiltration
Time in white solution is 4h.
Preferably, the step（2）The concentration of middle graphene oxide suspension is 0.08-0.12wt.%, the temperature of drying
For 60 DEG C, drying time is 0.5 hour.
Preferably, the step（2）The concentration of middle boron hydracid sodium alkaline solution is 1.5g/L, pH value 10-13, hydroboration
The temperature of sodium alkaline solution is 80 DEG C, time 3h, dry temperature 60 C, time 1h.
Preferably, described step（3）In, Fe3O4Nano-scale particle, particle diameter 60-100nm are prepared for hydro-thermal method.
Preferably, described step（3）In, for the DC voltage of electrophoresis from 12v-21v, the electrophoretic deposition time is 60min.
The present invention discloses composite prepared by above-mentioned preparation method.
Beneficial effects of the present invention
The present invention provides a kind of nanoscale Fe3O4The preparation method of the glass fiber compound material of grapheme modified cladding, by stone
Black alkene is compound with glass fibre, is modified with ferroso-ferric oxide, selects suitable experimental condition, the composite of preparation, compares
Other binary composites, there is higher capability of electromagnetic shielding.
Brief description of the drawings
Fig. 1 is Fe prepared by embodiment 13O4The SEM figures of-graphene-glass fiber compound material；
Fig. 2 is Fe prepared by embodiment 13O4- graphene-glass fiber compound material EDS is tested；
Fig. 3 is that composite prepared by embodiment contrasts with unmodified composite electromagnet shield effect.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
（1）Glass fibre is calcined into 60min in 455 DEG C of Muffle furnaces, surface size is removed, then by glass fibre in acetone
Middle cleaning treatment, finally fiberglass surfacing is modified with 25wt.% sodium hydroxide solutions liquid.
（2）By step（1）Handled glass fibre is placed in 15min in the 2.5wt.% kh550 aqueous solution, takes out cleaning
4h in 1.5wt.% bovine serum albumin solutions is infiltrated afterwards, and the suspension of 0.12wt.% graphene oxides is placed in after cleaning again
60min in liquid, deionized water cleaning, drying, the temperature of drying is 60 DEG C, and drying time is 0.5 hour, then is dipped in
3h in 1.5g/L, pH value 10, the sodium borohydride alkaline solution that temperature is 80 DEG C, takes out dry temperature 60 C, time 1h.
（3）Using graphene-glass as anode, tiselius apparatus is built by negative electrode of carbon-point, is 80nm ferroso-ferric oxides by particle diameter
1.5mg/ml suspension is made in nano particle ultrasonic disperse in deionized water, as plating solution, under 15V voltages to graphene-
Glass carries out electrophoretic deposition 60min, nanoscale Fe3O4The glass fiber compound material of grapheme modified cladding.
Accompanying drawing 1 is Fe prepared by embodiment 13O4The SEM figures of-graphene-glass fiber compound material；Accompanying drawing 2 is embodiment
1 Fe prepared3O4- graphene-glass fiber compound material EDS is tested.
Embodiment 2
（1）Glass fibre is calcined into 60min in 460 DEG C of Muffle furnaces, surface size is removed, then by glass fibre in acetone
Middle cleaning treatment, finally fiberglass surfacing is modified with 15wt.% sodium hydroxide solutions liquid.
（2）By step（1）Handled glass fibre is placed in 15min in the 4wt.% kh550 aqueous solution, after taking out cleaning
4h in 1.5wt.% bovine serum albumin solutions is infiltrated, is placed in after cleaning again in 0.1wt.% graphene oxide suspensions
60min, deionized water cleaning, drying, the temperature of drying are 60 DEG C, and drying time is 0.5 hour, then be dipped in 1.5g/L,
3h in the sodium borohydride alkaline solution that pH value is 13, temperature is 80 DEG C, takes out dry temperature 60 C, time 1h.
（3）Using graphene-glass fibre as anode, tiselius apparatus is built by negative electrode of carbon-point, is that 60nm tetra- is aoxidized by particle diameter
1.0mg/ml suspension is made in three iron nano-particle ultrasonic disperses in deionized water, as plating solution, to graphite under 18V voltages
Alkene/glass carries out electrophoretic deposition 60min, nanoscale Fe3O4The glass fiber compound material of grapheme modified cladding.
Embodiment 3
（1）Glass fibre is calcined into 60min in 500 DEG C of Muffle furnaces, surface size is removed, then by glass fibre in acetone
Middle cleaning treatment, finally fiberglass surfacing is modified with 20wt.% sodium hydroxide solutions liquid.
（2）By step（1）Handled glass fibre is placed in 15min in the aqueous solution of 2.5wt.% silane couplers, takes out clear
4h in 1.0wt.% bovine serum albumin solutions is infiltrated after washing, being placed in 0.08wt.% graphene oxides after cleaning again hangs
60min in supernatant liquid, deionized water cleaning, drying, the temperature of drying is 60 DEG C, and drying time is 0.5 hour, then is dipped in
3h in 1.5g/L, pH value 12, the sodium borohydride alkaline solution that temperature is 80 DEG C, takes out dry temperature 60 C, time 1h.
（3）Using graphene-glass as anode, tiselius apparatus is built by negative electrode of carbon-point, is 100nm ferroso-ferric oxides by particle diameter
1.5mg/ml suspension is made in nano particle ultrasonic disperse in deionized water, as plating solution, under 21V voltages to graphene-
Glass carries out electrophoretic deposition 60min, the glass fiber compound material of the grapheme modified claddings of nanoscale Fe3O4.
Comparative example 1
（1）Glass fibre is placed in 400 DEG C of Muffle furnace thermal cleaning handles 50min, then in turn through acetone, 6mol/L
Hydrochloric acid solution, deionized water cleaning, are subsequently placed in standby after being dried in 60 DEG C of baking oven；
（2）Glass fibre by pretreatment is put in the bovine serum albumin(BSA) 50ml solution that mass fraction is 1.0% and soaked
60min is handled, during which, every 5min liftings once；
（3）At room temperature, the ultrapure aqueous dispersions 50ml of graphite oxide that mass fraction is 0.1% is prepared, by bovine serum albumin contour painting
The glass fibre of energyization impregnation 30min in graphite oxide dispersion, take out, and use deionized water rinsing；It is subsequently placed in
It is dried for standby in 55 DEG C of baking ovens；
（4）By hydroiodic acid, acetic acid with volume ratio 1:2 ratio prepares solution 10ml and is placed in sealing container, while will obtain
The glass fibre of graphite oxide cladding is fixed on the upper strata of closed container, the reduction-oxidation graphite 20min at 40 DEG C, obtained stone
The glass fiber compound material of black alkene cladding.
Comparative example 2
（1）Graphene oxide water solution is prepared, and 0.1mg/ml graphene oxide dispersion solns are obtained after ultrasonic disperse processing；Again
Compound concentration is 0.2mol/L ferrous sulfate aqueous solution；
（2）By step（1）Graphene oxide dispersion soln be heated to 50 DEG C and continual ultrasonic 30min, ferrous sulfate is water-soluble
Liquid is slowly dropped to graphene oxide dispersion soln, rate of addition 5ml/min, obtains precursor mixed solution；
（3）By step（2）Precursor mixed solution be heated to 90 DEG C and continual ultrasonic 30min, add 30ml 0.1mol/L
Sodium hydrate aqueous solution, regulation system pH value be 10；
（4）After reaction system is maintained at 90 DEG C and continual ultrasonic reaction 120min, reaction product is obtained, after rear Magneto separate is multiple
8h is dried in vacuo at 60 DEG C, obtained black powder is ferroso-ferric oxide/graphene oxide composite material.
Comparative example 3
（1）Glass fibre is calcined into 50min in 400 DEG C of Muffle furnaces, surface size is removed, successively by acetone, 6mol/L
Hydrochloric acid solution, deionized water cleaning, be subsequently placed in 60 DEG C of baking oven dry after it is standby.
（2）Glass fibre by pretreatment is put in the bovine serum albumin(BSA) 50ml solution that mass fraction is 1.0%
Immersion treatment 60min, during which, every 5min liftings once.At room temperature, it is ultrapure to prepare the graphite oxide that mass fraction is 0.1%
Aqueous dispersions 50ml, by the glass fibre of bovine serum albumin(BSA) functionalization in graphite oxide dispersion impregnation 30min, take
Go out, and use deionized water rinsing；It is subsequently placed in 55 DEG C of baking ovens and is dried for standby.
（3）Using graphene-glass as anode, tiselius apparatus is built by negative electrode of carbon-point, is 80nm ferroso-ferric oxides by particle diameter
1.5mg/ml suspension is made in nano particle ultrasonic disperse in deionized water, as plating solution, under 15V voltages to graphene-
Glass carries out electrophoretic deposition 60min, the glass fiber compound material of the grapheme modified claddings of nanoscale Fe3O4.Fig. 3 is embodiment
The composite of preparation contrasts with unmodified composite electromagnet shield effect.
Claims (10)
- A kind of 1. nanoscale Fe3O4The preparation method of the glass fiber compound material of grapheme modified cladding, it is characterised in that bag Include following steps：（1）The surface treatment of glass fibre：Glass fibre is put into Muffle furnace and calcined, is sequentially placed into acetone, alkali lye and handles；（2）It is prepared by graphene oxide/glass fibre：By step（1）Glass fibre after processing is placed in the water-soluble of silane coupler Liquid, infiltrated in bovine serum albumin solution after taking out cleaning, be placed in after cleaning again in graphene oxide suspension, dried After dry, it is put into sodium borohydride alkaline solution, heats, stir, dries, graphene oxide/glass fibre is made；（3）The modification of magnetic material：With step（2）Middle graphene oxide/glass fibre is anode, and electricity is built by negative electrode of carbon-point Swimming pool, with 1.0-1.5mg/ml Fe3O4Suspension is plating solution, carries out electrophoretic deposition to graphene oxide/glass fibre, is made Nanoscale Fe3O4The glass fiber compound material of grapheme modified cladding.
- 2. preparation method as claimed in claim 1, its feature is in the step（1）It is middle that glass fibre is put into Muffle furnace The temperature of calcining is 455-500 DEG C, and calcination time is 1-2 hours；The step（1）The concentration of middle alkali lye is 1wt.%-30wt.%, and processing time is 0.5-6 hours.
- 3. preparation method as claimed in claim 1, its feature is in the step（1）Alkali lye is sodium hydroxide solution, and concentration is 25wt.%。
- 4. preparation method as claimed in claim 1, its feature is in the step（2）In, the aqueous solution of silane coupler is The kh550 aqueous solution, concentration 1wt.%-5wt.%, the time being placed in the silane coupler aqueous solution are 5min-15min.
- 5. preparation method as claimed in claim 1, its feature is in the step（2）The concentration of middle bovine serum albumin solution For 1-1.5wt.%, it is 4h to infiltrate the time in bovine serum albumen solution.
- 6. preparation method as claimed in claim 1, its feature is in the step（2）The concentration of middle graphene oxide suspension For 0.08-0.12wt.%, the temperature of drying is 60 DEG C, and drying time is 0.5 hour.
- 7. preparation method as claimed in claim 1, its feature is in the step（2）The concentration of middle boron hydracid sodium alkaline solution For 1.5g/L, pH value 10-13, the temperature of sodium borohydride alkaline solution is 80 DEG C, time 3h, dry temperature 60 C, when Between be 1h.
- 8. preparation method as claimed in claim 1, its feature is in described step（3）In, Fe3O4Nanometer is prepared for hydro-thermal method Grade particles, particle diameter 60-100nm.
- 9. preparation method as claimed in claim 1, its feature is in described step（3）In, the DC voltage of electrophoresis is from 12v- 21v, electrophoretic deposition time are 60min.
- 10. nanoscale Fe prepared by the preparation method described in a kind of one of claim 1-93O4The glass of grapheme modified cladding Fibrous composite.
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Cited By (4)
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| CN109706737A (en) * | 2019-01-22 | 2019-05-03 | 重庆纤维研究设计院股份有限公司 | Based on the modified glass fibre guard glass fibre cotton and preparation method thereof with thermal insulation performance of bovine serum albumin(BSA) and graphene oxide |
| CN109867455A (en) * | 2019-03-06 | 2019-06-11 | 史玉成 | A kind of environmental-friendly glass fiber and its processing technology of high-modulus |
| CN112047646A (en) * | 2020-08-27 | 2020-12-08 | 泰山玻璃纤维有限公司 | Preparation method of graphene-coated glass fiber |
| CN112055528A (en) * | 2020-09-15 | 2020-12-08 | 福州大学 | Preparation method of graphene-coated glass fiber reinforced plastic |
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| CN109706737A (en) * | 2019-01-22 | 2019-05-03 | 重庆纤维研究设计院股份有限公司 | Based on the modified glass fibre guard glass fibre cotton and preparation method thereof with thermal insulation performance of bovine serum albumin(BSA) and graphene oxide |
| CN109867455A (en) * | 2019-03-06 | 2019-06-11 | 史玉成 | A kind of environmental-friendly glass fiber and its processing technology of high-modulus |
| CN111285625A (en) * | 2019-03-06 | 2020-06-16 | 史玉成 | Processing technology of high-modulus environment-friendly glass fiber |
| CN112047646A (en) * | 2020-08-27 | 2020-12-08 | 泰山玻璃纤维有限公司 | Preparation method of graphene-coated glass fiber |
| CN112055528A (en) * | 2020-09-15 | 2020-12-08 | 福州大学 | Preparation method of graphene-coated glass fiber reinforced plastic |
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