CN115340688A - Preparation method of shell-like composite material with sandwich structure - Google Patents
Preparation method of shell-like composite material with sandwich structure Download PDFInfo
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- CN115340688A CN115340688A CN202211082066.0A CN202211082066A CN115340688A CN 115340688 A CN115340688 A CN 115340688A CN 202211082066 A CN202211082066 A CN 202211082066A CN 115340688 A CN115340688 A CN 115340688A
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- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002070 nanowire Substances 0.000 claims abstract description 94
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 20
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 20
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 15
- 238000000967 suction filtration Methods 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 26
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 229940063656 aluminum chloride Drugs 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims description 5
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 230000033228 biological regulation Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 230000007774 longterm Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims 3
- 230000008025 crystallization Effects 0.000 claims 3
- 239000002002 slurry Substances 0.000 claims 3
- 239000011259 mixed solution Substances 0.000 claims 2
- 239000012716 precipitator Substances 0.000 claims 2
- 239000003570 air Substances 0.000 claims 1
- 239000012670 alkaline solution Substances 0.000 claims 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims 1
- 239000001768 carboxy methyl cellulose Substances 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims 1
- 230000009977 dual effect Effects 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- 239000011261 inert gas Substances 0.000 claims 1
- 229910052901 montmorillonite Inorganic materials 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 4
- 239000003960 organic solvent Substances 0.000 abstract description 4
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 12
- 229910021529 ammonia Inorganic materials 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000000872 buffer Substances 0.000 description 6
- 239000007853 buffer solution Substances 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000004809 Teflon Substances 0.000 description 4
- 229920006362 Teflon® Polymers 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000013557 residual solvent Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000011449 brick Substances 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 229920002101 Chitin Polymers 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- NIWMEUWZZDPUEQ-UHFFFAOYSA-M sodium;azane;hydroxide Chemical compound N.[OH-].[Na+] NIWMEUWZZDPUEQ-UHFFFAOYSA-M 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- -1 alkalis Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000002977 biomimetic material Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229920003123 carboxymethyl cellulose sodium Polymers 0.000 description 1
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 125000004356 hydroxy functional group Chemical group O* 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
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Abstract
The invention relates to the field of materials, and mainly relates to a preparation method of a shell-like composite material with a sandwich structure. The composite material consists of graphene oxide, alumina nanowires, polyvinyl alcohol and a small amount of glutaraldehyde, and is assembled by a vacuum-assisted suction filtration method, and the thickness, the diameter and even the shape of the composite material can be adjusted by a vacuum suction filtration device. The preparation process is simple, common workers can master the learning, the prepared composite material has the characteristics of high strength and high toughness, the composite material can maintain good appearance and mechanical property even being soaked in acid, alkali and organic solvents or subjected to ultrasound, the composite material can always keep good self-supporting property and structural stability in a humid environment, the composite material can be used as a structural material in an extreme environment, and the composite material has a great application prospect in the fields of aerospace and engineering.
Description
Technical Field
The invention belongs to the field of materials, and relates to preparation of gamma-hydroxy aluminum oxide nanowires, amorphous aluminum oxide nanowires, crystalline-amorphous coexistent (dual-phase) aluminum oxide nanowires and completely crystallized gamma-aluminum oxide nanowires, in particular to preparation of a shell-like composite material which is reinforced by the nanowires and has a sandwich structure.
Background
The strength and toughness are the most basic properties of the structural material, and provide a main reference for evaluating the mechanical properties of the structural material. In general, strength and toughness are contradictory, with high strength materials always exhibiting brittleness and high toughness materials generally exhibiting low strength. Therefore, the development of structural materials with high strength and high toughness is one of the major challenges in engineering.
Over millions of years of excellence and decline, the organisms in the nature are transformed into almost perfect structures and functions. Therefore, in the past decades, a large number of researchers have prepared biomimetic materials with different functions by studying towards nature and imitating their intrinsic structures. In terms of structural materials, shells are the objects in which the model is typically simulated. The nacreous layer in the shell consists of about 95% of typical brittle material Wen Danpian (calcium carbonate micron flakes) and about 5% organic matter (protein and chitin fibers), which is comparable in strength to aragonite but with a more than 3000 times greater toughness. Based on this, the structure and composition of the pearl layer are studied in detail by researchers, and the ultrahigh toughness is found to be derived from a unique 'brick-mud structure' constructed by Wen Danpian (brick) and organic matter (mud). Inspired by the above, researchers have prepared a series of layered composite materials with high strength and high toughness superior to the shells by changing the components of the bricks and the mud. Among them, graphene Oxide (GO) is the most popular inorganic nanosheet (serving as a brick) due to its platelet morphology, excellent mechanical properties, and abundant oxygen-containing functional groups on the surface. Since the first GO-based layered composites were successfully prepared by vacuum filtration methods, a number of strategies such as interfacial crosslinking, nanosheet reinforcement, bridging, etc. were developed to improve their mechanical properties. However, most of the strategies or concerns have focused on the layered "brick-and-mud" structure present in the nacre layer and the interfacial modification therein, and lack novel structural design. Therefore, in order to pursue higher mechanical properties, researchers can only improve the mechanical properties of the structural material by searching for stronger sheets or organic substances on the basis of the 'brick-mud' structure of the laminated structure, which greatly limits the application.
Detailed characterization of the natural nacreous layer is known, in which there are also nanofibres (chitin) and ceramic bridges, rigid in one dimension, immersed in a laminar structure stacked by aragonite and organic matter, which can hinder the sliding of the laminar structure and the creation, propagation, etc. of cracks when the nacreous layer is subjected to damage. Inspired by the above, introducing rigid nanowires into the traditional shell-like composite material to construct a novel sandwich structure with one-dimensional nanowire support is an effective way to further improve the strength and toughness of the structural material.
Disclosure of Invention
Aiming at the problem that the strength and toughness of the existing structural material cannot be obtained simultaneously, the invention adopts cheap metal salt, buffer solution and the like as raw materials, obtains the one-dimensional alumina nanowire by a hydrothermal method and high-temperature calcination, then uniformly mixes the one-dimensional alumina nanowire with graphene oxide nanosheets and organic polymers, and realizes the preparation of the one-dimensional ceramic nanowire reinforced shell-like composite material with a sandwich structure and high strength and toughness by using a vacuum-assisted suction filtration mode. Which comprises the following steps:
firstly, preparing 17.5mL of sodium hydroxide-ammonia water buffer solution (the concentration of sodium hydroxide and the concentration of ammonia water are both 2.5mol/L and the two solutions are mixed in equal volumes), and dropwise adding 17.5mL of prepared colorless transparent AlCl 3 The solution is maintained in a state of vigorous stirring in the dripping process, and the color of the solutionAnd gradually become milky white colloid. Then, after the dropwise addition of the sodium hydroxide-ammonia water is finished, stirring is continued for 10min;
secondly, transferring the white emulsion obtained in the first step into a high-pressure reaction kettle with a Teflon lining, and then putting the reaction kettle into a high-temperature oven, wherein the temperature range is 160-220 ℃, and the reaction time is 12-36 hours;
thirdly, centrifugally separating the product obtained in the second step, alternately washing the product with ethanol and water for 3 times respectively to remove impurities and residual solvent, dispersing the product with ultrapure water, and freeze-drying the product to obtain white one-dimensional gamma-hydroxy alumina nanowires;
fourthly, calcining the one-dimensional gamma-hydroxy alumina nano wire obtained in the third step at the temperature of 400-500 ℃ (preferably 500 ℃) for 1-360 min, and finally obtaining the amorphous alumina nano wire, the two-phase alumina nano wire and the gamma-Al nano wire respectively according to the difference of the calcining temperature and the calcining time 2 O 3 A nanowire;
fifthly, ultrasonically dispersing graphene oxide in deionized water to prepare 2-4 mg/mL Graphene Oxide (GO) dispersion liquid; taking 1-10 mg of biphase alumina nano-wire to be ultrasonically dispersed in deionized water to obtain the concentration of 0.2-2 mg/mL; weighing solid polyvinyl alcohol (PVA), heating in a water bath at 75 ℃ for 4h, and gradually dissolving and dispersing in deionized water under stirring to obtain a polyvinyl alcohol solution with the concentration of 2.5mg/mL; dispersing 50wt% of glutaraldehyde in deionized water to obtain glutaraldehyde diluent with the concentration of 0.5 mg/mL;
and sixthly, adding 2-20mg of aluminum oxide nanowires into 5mL of GO solution on the basis of the fifth step, stirring for 12-36 h, fully mixing the aluminum oxide nanowires with GO, and adsorbing wires on the surface of GO. Then, firstly carrying out ultrasonic treatment for 20-30 min, sequentially adding 4mL of 2.5mg/mL polyvinyl alcohol and 0.2mL of 0.5mg/mL glutaraldehyde, then stirring for 12-18 h, then carrying out ultrasonic treatment for 20-30 min, and then obtaining the alumina nanowire reinforced shell-like composite material with the sandwich structure by a vacuum-assisted suction filtration method.
In the present invention, no special statement is made on the preparation conditions (such as temperature, humidity, apparatus, materials, processes, methods, etc.) which are common in the art or can be easily obtained by a person of ordinary skill in the art according to the conventional techniques in the art.
In the present invention, the temperature of dissolution or reaction is not particularly specified, and is 15 to 35 ℃ at normal temperature, normal pressure, or the like.
In the invention, the graphene oxide is synthesized by a modified Hummers method, the preparation method can be referred to, the thickness of the graphene is below 1nm, and the transverse dimension of the graphene is 10-50 μm, but the graphene oxide is not limited to the thickness of the graphene.
Furthermore, the length range of the gamma-hydroxy aluminum oxide nanowire prepared by the invention is 0.5-1.2 mu m, the diameter range is 25-30 nm, and the specific length and diameter are determined by reaction conditions and can be adjusted.
Furthermore, the length range of the biphase aluminum oxide nano wire prepared by the invention is 0.5-1.2 μm, the diameter range is 20-25 nm, and the specific length and diameter are determined by reaction conditions and can be adjusted.
Furthermore, the length range of the gamma-alumina nano wire prepared by the invention is 0.5-1.2 μm, the diameter range is 20-25 nm, and the specific length and diameter are determined by reaction conditions and can be adjusted.
Furthermore, the thickness of the GO-based shell-like composite material with a sandwich structure and enhanced by the one-dimensional two-phase (crystal-amorphous) alumina nanowires prepared by the method is determined by the amount of a sample added during vacuum-assisted suction filtration and the diameter of a sand core suction filtration device, and the transverse size is determined by the diameter of the sand core suction filtration device. The typical diameter of the GO-based shell-like composite material with a sandwich structure is-5 cm, and the thickness is 5-20 μm, but the thickness and the diameter are not limited thereto.
Further, the preferable concentration range of sodium hydroxide in the second step is 0.4 to 0.6mol/L, and the preferable concentration range of ammonia water is 0.4 to 0.6mol/L.
Further, the temperature range of the hydrothermal process in the fourth step is 180 to 200 ℃, the preferred reaction time is 24 to 36 hours, and any combination thereof is acceptable.
Furthermore, the preferable calcining temperature of the seventh step is 500 ℃, and the calcining time is 1-5 min, so that the biphase aluminum oxide nanowire can be obtained.
The invention has the following advantages:
the invention provides a method for preparing gamma-hydroxy alumina nano wire, which is simple and easy to popularize, the gamma-hydroxy alumina nano wire can not be converted into gamma-alumina after being calcined for more than 12 hours at 350 ℃, the thermal stability is good, and the yield of the gamma-hydroxy alumina nano wire is up to more than 70 percent by calculating the mole number (namely, more than 0.7mol of hydroxy alumina can be obtained by adding 1mol of aluminum chloride hexahydrate), so that the gamma-hydroxy alumina nano wire is hopeful to realize industrial application and batch production.
The invention provides a method for preparing biphase alumina nano-wire and gamma-alumina nano-wire with extremely simple structure. Specifically, the gamma-hydroxy aluminum oxide nanowires prepared by the method only need to be thermally treated at 500 ℃ for 1-120 min, and the dual-phase aluminum oxide nanowires with different crystallinities can be obtained. The gamma-hydroxy aluminum oxide nano-wire prepared by the method can be completely crystallized when being thermally treated for more than 360 minutes at 500 ℃. The mole number of the biphase alumina or fully crystallized gamma-alumina nano-wire obtained by the heat treatment is not changed.
3, the GO-based shell-like composite material with a sandwich structure and enhanced by the alumina nanowires is creatively constructed, the method is simple and convenient, and convenient to popularize, components of the GO-based shell-like composite material can be replaced by combinations with similar shapes, and the GO-based shell-like composite material with a sandwich structure can also be prepared, such as one-dimensional hydroxyapatite nanowires, MXene two-dimensional sheets and polymer carboxymethyl cellulose sodium combinations.
4, the GO-based shell-like composite material with a sandwich structure is creatively constructed by reinforcing the alumina nanowires, so that the mechanical property and the long-term service stability of the GO-based shell-like composite material are obviously improved, and the GO-based shell-like composite material has a good application prospect in the fields of engineering, aerospace and the like.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of the dual-phase alumina nanowires obtained in example 1 of the present invention;
FIG. 2 is an X-ray diffraction pattern (XRD) of the dual-phase alumina nanowire obtained in example 1 of the present invention;
fig. 3 is an SEM photograph of the dual-phase alumina nanowire reinforced GO-based shell-like composite material with a sandwich structure obtained in example 1 of the present invention;
FIG. 4 shows the results of mechanical testing in example 1 of the present invention;
Detailed Description
The present invention will be further described in detail with reference to the drawings and examples, wherein the solvents, drugs and instruments used in the following are not specifically illustrated but are generally considered to be available in the laboratory or in the market. Furthermore, the examples in this embodiment are intended only for the understanding of the reader as to specific details of the invention, not all, and are not intended to limit the scope of the invention in any way. Further, optimization or regulation that can be conceived by those skilled in the art is included in the present invention within a scope not departing from the idea of the present invention.
Example 1
Preparation method of two-phase aluminum oxide nanowire reinforced shell-like composite material with sandwich structure
In the first step, 0.875g of NaOH solution was weighed out and dissolved in 8.75mL of water to obtain 2.5mol/L NaOH solution, which was then added to an equal volume of 2.5mol/L ammonia to obtain 17.5mL of NaOH-ammonia buffer. 4.2g of aluminum chloride hexahydrate is dissolved in 17.5mL of water and stirred vigorously to obtain a clear and transparent aluminum chloride solution with the concentration of 1 mol/L. Subsequently, 17.5mL of NaOH-Ammonia buffer was added dropwise to 17.5mL of clear and transparent aluminum chloride solution using a constant pressure separatory funnel, and the solution gradually turned milky under vigorous stirring. After the buffer solution is added, stirring is continued for 10min;
and secondly, transferring the white emulsion obtained in the first step into a high-pressure reaction kettle with a Teflon lining, and then putting the reaction kettle into a high-temperature oven to react for 24 hours at the temperature of 200 ℃. After the reaction is finished, the product is transferred to a centrifuge tube for centrifugal separation, and a solid product is left. Then, alternately and centrifugally washing the nano-particles for 3 times by using ethanol and water to remove impurities and residual solvents in the nano-particles, then dispersing the nano-particles by using ultrapure water, and freeze-drying the dispersed nano-particles to obtain white gamma-hydroxy aluminum oxide nano-wires;
thirdly, calcining the gamma-hydroxy aluminum oxide nanowire obtained in the second step at 500 ℃ in air atmosphere for 1min-120min to obtain a dual-phase aluminum oxide nanowire;
fourthly, weighing solid polyvinyl alcohol (PVA), heating in a water bath at 75 ℃ for 4h, and gradually dissolving and dispersing in deionized water under the stirring condition to obtain a polyvinyl alcohol solution with the concentration of 2.5mg/mL; dispersing 50wt% of glutaraldehyde in deionized water to obtain glutaraldehyde diluent with the concentration of 0.5 mg/mL;
and fifthly, adding 7mg of biphase aluminum oxide nanowires into the 5mL of 4mg/mL GO solution on the basis of the fourth step, and then stirring for 36 hours to fully mix the biphase aluminum oxide nanowires with GO and fully adsorb the nanowires on the surface of GO. Then, firstly carrying out ultrasonic treatment for 30min, sequentially adding 4mL of 2.5mg/mL polyvinyl alcohol and 0.2mL of 0.5mg/mL glutaraldehyde, stirring for 12-18 h, then carrying out ultrasonic treatment for 20-30 min, and then obtaining the biphase alumina nanowire reinforced shell-like composite material with the sandwich structure by a vacuum-assisted suction filtration method. The composite material is a black film with the thickness of about 10 mu m and the diameter of 5cm, the microstructure of the black film presents a sandwich structure, and a two-phase aluminum oxide nanowire is sandwiched between graphene oxide sheets. It should be noted that the thickness and diameter, and thus the shape, can be adjusted depending on the amount of sample added, the concentration of the sample, and the size and shape of the suction filtration device;
and sixthly, stretching the two-phase aluminum oxide nanowire reinforced shell-like composite material with the sandwich structure prepared in the fifth step by using a universal stretching machine, wherein the strength and the strain of the shell-like composite material are respectively over 800MPa and 7 percent and are higher than the strength and the toughness of the existing steel for the bridge. In addition, the film can still maintain good self-supporting property and good structural stability after being soaked in solvents or solutions such as organic solvents, acids, alkalis, ethanol, water and the like, or standing or ultrasonic vibration.
Example 2
Preparation method of gamma-alumina nanowire reinforced shell-like composite material with sandwich structure
In the first step, 0.875g of NaOH solution was weighed out and dissolved in 8.75mL of water to obtain 2.5mol/L NaOH solution, which was then added to an equal volume of 2.5mol/L ammonia to obtain 17.5mL of NaOH-ammonia buffer. 4.2g of aluminum chloride hexahydrate is dissolved in 17.5mL of water and stirred vigorously to obtain a clear and transparent aluminum chloride solution with the concentration of 1 mol/L. Subsequently, 17.5mL of NaOH-Ammonia buffer was added dropwise to 17.5mL of clear and transparent aluminum chloride solution using a constant pressure separatory funnel, and the solution gradually turned milky under vigorous stirring. After the buffer solution is added, stirring is continued for 10min;
and secondly, transferring the white emulsion obtained in the first step into a high-pressure reaction kettle with a Teflon lining, and then putting the reaction kettle into a high-temperature oven to react for 24 hours at the temperature of 200 ℃. After the reaction is finished, the product is transferred into a centrifuge tube and is subjected to centrifugal separation, and a solid product is left. Then, alternately and centrifugally washing the nano-particles for 3 times by using ethanol and water to remove impurities and residual solvents in the nano-particles, then dispersing the nano-particles by using ultrapure water, and freeze-drying the dispersed nano-particles to obtain white gamma-hydroxy aluminum oxide nano-wires;
thirdly, calcining the gamma-hydroxy aluminum oxide nanowire obtained in the second step at 500 ℃ in air atmosphere for 360min to obtain the gamma-aluminum oxide nanowire;
fourthly, weighing solid polyvinyl alcohol (PVA), heating in a water bath at 75 ℃ for 4h, and gradually dissolving and dispersing in deionized water under the stirring condition to obtain a polyvinyl alcohol solution with the concentration of 2.5mg/mL; dispersing 50wt% of glutaraldehyde in deionized water to obtain glutaraldehyde diluent with the concentration of 0.5 mg/mL;
and fifthly, on the basis of the fourth step, adding 7mg of gamma-alumina nanowires into 5mL of 4mg/mL GO solution, and then stirring for 36h to fully mix the gamma-alumina nanowires with GO and fully adsorb the gamma-alumina nanowires on the surface of GO. Then, firstly carrying out ultrasonic treatment for 30min, sequentially adding 4mL of 2.5mg/mL polyvinyl alcohol and 0.2mL of 0.5mg/mL glutaraldehyde, stirring for 12-18 h, then carrying out ultrasonic treatment for 20-30 min, and then carrying out vacuum-assisted suction filtration to obtain the gamma-alumina nanowire reinforced shell-like composite material with a sandwich structure. The composite material is a black film with the thickness of about 10 mu m and the diameter of 5cm, the microstructure of the composite material presents a sandwich structure, and gamma-alumina nanowires are intercalated between graphene oxide sheets. It should be noted that the thickness and diameter, and thus the shape, can be adjusted depending on the amount of sample added, the concentration of the sample, and the size and shape of the suction filtration device;
and sixthly, stretching the gamma-alumina nanowire reinforced shell-like composite material with the sandwich structure prepared in the fifth step by using a universal stretching machine, and measuring that the strength and the strain of the shell-like composite material are respectively more than 500MPa and 5 percent. In addition, the film can still maintain good self-supporting property and good structural stability after being soaked in organic solvent, acid, alkali, ethanol, water and other solvents or solutions, or standing or ultrasonic vibration.
Example 3
Preparation method of shell-like composite material with sandwich structure and reinforced by amorphous alumina nanowires
In the first step, 0.875g of NaOH solution was weighed out and dissolved in 8.75mL of water to obtain 2.5mol/L NaOH solution, which was then added to an equal volume of 2.5mol/L ammonia to obtain 17.5mL of NaOH-ammonia buffer. 4.2g of aluminum chloride hexahydrate is dissolved in 17.5mL of water and stirred vigorously to obtain a clear and transparent aluminum chloride solution with the concentration of 1 mol/L. Subsequently, 17.5mL of NaOH-Ammonia buffer was added dropwise to 17.5mL of clear and transparent aluminum chloride solution using a constant pressure separatory funnel, and the solution gradually turned milky under vigorous stirring. After the buffer solution is added, stirring is continued for 10min;
and secondly, transferring the white emulsion obtained in the first step into a high-pressure reaction kettle with a Teflon lining, and then putting the reaction kettle into a high-temperature oven to react for 24 hours at the temperature of 200 ℃. After the reaction is finished, the product is transferred to a centrifuge tube for centrifugal separation, and a solid product is left. Then, alternately and centrifugally washing the nano-particles for 3 times by using ethanol and water to remove impurities and residual solvents in the nano-particles, then dispersing the nano-particles by using ultrapure water, and freeze-drying the dispersed nano-particles to obtain white gamma-hydroxy aluminum oxide nano-wires;
thirdly, calcining the gamma-hydroxy alumina nanowire obtained in the second step at 500 ℃ in air atmosphere for 10s to obtain an amorphous alumina nanowire;
fourthly, weighing solid polyvinyl alcohol (PVA), heating in a water bath at 75 ℃ for 4h, and gradually dissolving and dispersing in deionized water under the stirring condition to obtain a polyvinyl alcohol solution with the concentration of 2.5mg/mL; dispersing 50wt% of glutaraldehyde in deionized water to obtain glutaraldehyde diluent with the concentration of 0.5 mg/mL;
and fifthly, on the basis of the fourth step, adding 7mg of amorphous alumina nanowires into a 5 mL-4 mg/mL GO solution, and then stirring for 36 hours to fully mix the amorphous alumina nanowires with GO and fully adsorb the amorphous alumina nanowires on the surface of GO. Then, firstly carrying out ultrasonic treatment for 30min, sequentially adding 4mL of 2.5mg/mL polyvinyl alcohol and 0.2mL of 0.5mg/mL glutaraldehyde, stirring for 12-18 h, carrying out ultrasonic treatment for 20-30 min, and carrying out vacuum-assisted suction filtration to obtain the amorphous alumina nanowire-reinforced shell-like composite material with a sandwich structure. The composite material is a black film with the thickness of about 10 mu m and the diameter of 5cm, the microstructure of the black film presents a sandwich structure, and amorphous alumina nanowires are sandwiched between graphene oxide sheets. It should be noted that the thickness and diameter, and thus the shape, can be adjusted depending on the amount of sample added, the concentration of the sample, and the size and shape of the suction filtration device.
And sixthly, stretching the amorphous alumina nanowire reinforced shell-like composite material with the sandwich structure prepared in the fifth step by using a universal stretching machine, and measuring that the strength and the strain of the shell-like composite material exceed 600MPa and 5 percent respectively (figure 4). In addition, the film can still maintain good self-supporting property and good structural stability after being soaked in organic solvent, acid, alkali, ethanol, water and other solvents or solutions, or standing or ultrasonic vibration.
Claims (8)
1. A preparation method of a shell-like composite material with a sandwich structure is characterized by comprising the following steps:
firstly, adjusting the concentration range of aluminum chloride hexahydrate to be 0.1-2 mol/mL, and preferably, the concentration is 0.9-1.1 mol/mL; the NaOH-ammonia water mixed solution is used as a precipitator, wherein the debugging concentration range of ammonia water is 0.5-3.5 mol/mL, the debugging concentration range of NaOH solution is 0.5-3.5 mol/mL, the optimal concentration of the two alkaline solutions is 2.5-2.6 mol/m, the ammonia water and the NaOH solution with equal volumes are fully mixed with the optimal concentration finally, and the obtained mixture can be used as the precipitator for precipitating aluminum salt in aluminum chloride solution;
and secondly, dripping 17.5mL of the preferable NaOH-ammonia water mixed solution prepared in the first step into 17.5mL of aluminum chloride solution with preferable concentration, stirring for 5-60 min, and then transferring to a high-temperature reaction kettle for reaction at 140-240 ℃ for 12-48 h. Particularly, the adding volume is proportionally controlled according to the size of a reaction kettle and the amount of a sample to be prepared, for example, a 100mL reaction kettle is selected, and a mixed alkali liquor of NaOH-ammonia water with a preferred concentration and an aluminum chloride solution with a preferred concentration in equal volume can be added, wherein the preferred concentration is not more than 40 mL;
removing the solution in the sample after the reaction in the second step (common solid-liquid separation means such as filtration and centrifugation can be adopted), then alternately washing the sample by using ethanol and deionized water for 3 times, then ultrasonically dispersing the obtained product into the deionized water, and then freeze-drying the product to obtain clean white gamma-hydroxy aluminum oxide nanowires;
fourthly, placing the gamma-hydroxy alumina nano wire obtained in the third step in a high temperature furnace for calcining for 1 to 10 seconds at the temperature of 500 ℃ to obtain an amorphous alumina nano wire, calcining the gamma-hydroxy alumina nano wire in the high temperature furnace for 1 to 120 minutes at the temperature of 500 ℃ to obtain a two-phase alumina nano wire with different crystallization degrees, wherein the crystallization proportion is improved along with the prolonging of time, placing the gamma-hydroxy alumina nano wire in the high temperature furnace for calcining for more than 360 minutes to obtain a fully crystallized gamma-alumina nano wire, and all the calcining processes can be carried out in air, oxygen or inert gas;
fifthly, dispersing the dried graphene oxide in deionized water by ultrasonic or (combined) stirring to obtain a graphene oxide solution with the concentration of 2-10 mg/mL, preferably 5mg/mL; heating and dispersing solid polyvinyl alcohol in deionized water, heating at 60-90 ℃ and violently stirring for 4 hours until the polyvinyl alcohol is completely dissolved, then stopping heating, and cooling to room temperature for later use while stirring to obtain a concentration of 0.5-4 mg/mL, preferably 2.5mg/mL; dispersing 50wt% of glutaraldehyde in deionized water to obtain glutaraldehyde diluent with the concentration of 0.5 mg/mL;
and sixthly, adding 2-20mg of alumina nanowires (preferably 7 mg) into 5mL of 2-10 mg/mL (preferably 4 mg/mL) GO solution on the basis of the fifth step, stirring for 12-36 h (preferably 36 h), fully mixing the alumina nanowires with GO, and adsorbing the nanowires on the surface of GO. Then, carrying out ultrasonic treatment for 20-30 min, sequentially adding 4mL of 2.5mg/mL polyvinyl alcohol and 0.2mL of 0.5mg/mL glutaraldehyde, stirring for 12-18 h, carrying out ultrasonic treatment for 20-30 min, and then obtaining the alumina nanowire reinforced shell-like composite material with a sandwich structure by a vacuum-assisted suction filtration method.
2. The method of preparing γ -aluminum oxyhydroxide nanowires according to claim 1, characterized in that: the nano-wire presents good linear morphology, the length range is 0.5-1.2 mu m, and the diameter range is 25-30 nm.
3. The method of preparing amorphous alumina nanowires of claim 1, wherein: the nano-wire presents good linear morphology, the length range is 0.5-1.2 μm, the diameter range is 20-25 nm, the calcination temperature is preferably 500 ℃, and the calcination time is 1-10 s.
4. The method of preparing crystalline-amorphous coexisting (dual phase) alumina nanowires with different degrees of crystallinity as claimed in claim 1, wherein: the nano-wire presents good linear morphology, the length range is 0.5-1.2 mu m, the diameter range is 20-25 nm, the calcination temperature is preferably 500 ℃, the calcination time is controllably regulated and controlled according to the requirement of the required crystallization proportion, and the controllable regulation and control range is 1-120 min.
5. The method of preparing fully crystallized γ -alumina nanowires of claim 1, wherein: the nano-wire presents good linear morphology, the length range is 0.5-1.2 μm, the diameter is 20-25 nm, the calcination temperature is preferably 500 ℃, and the calcination time is more than 360 min.
6. The method for preparing the shell-like composite material with a sandwich structure and enhanced by the aluminum oxide nanowires (comprising amorphous, dual-phase and gamma-phase aluminum oxide nanowires) according to claim 1 is characterized in that: the thickness, diameter (length or width) and shape of the slurry are determined by the quantity of the slurry and the shape and size of the suction filtration device; the composite material has excellent mechanical property and long-term stability in service under extreme environment; the chemical composition of the slurry can be changed according to requirements as long as the shape matching of the method is met, and the composite material with the sandwich structure can be constructed by combining the hydroxyl alumina nanowire, the sheet montmorillonite and the sodium carboxymethyl cellulose.
7. The aluminum oxide nanowire reinforced shell-like composite material with a sandwich structure as claimed in claim 1, wherein the tensile strength of the composite material is more than 800MPa, the breaking strain is more than 7%, and the breaking work is more than 30MJ/m when the composite material is used as a structural material -3 。
8. Use according to any of claims 1-7 in the fields of engineering, materials.
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