CN107244650A - A kind of preparation method and applications of two-dimensional layer compound/zinc-oxide nano rod composite material - Google Patents
A kind of preparation method and applications of two-dimensional layer compound/zinc-oxide nano rod composite material Download PDFInfo
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Abstract
A kind of preparation method and applications of two-dimensional layer compound/zinc-oxide nano rod composite material, belong to field of nanometer material technology.The present invention will improve MXene electro-magnetic wave absorption performance technical problems.The present invention method be:First, zinc oxide seed solution is prepared using acetic acid dihydrate zinc and sodium hydroxide;2nd, two-dimensional layer MXene powders are immersed in zinc oxide seed solution, grows Seed Layer, through separation, dried, three, repeat step two at least 2 times;4th, it is then added in zinc oxide growth liquid prepared by hexamethylenetetramine and zinc nitrate hexahydrate, after heating response, through washing, dries, obtain two-dimensional layer compound oxidation zinc nanometer rod composite material.The preparation method of the present invention is simple, and reaction condition is gentle, prepares effect preferable.The obtained composite excellent electrochemical performance of the present invention, meanwhile, conductive channel is added there is provided bigger surface area, can be applied to electro-magnetic wave absorption field.
Description
Technical field
The invention belongs to field of nanometer material technology;Specifically related to a kind of two-dimensional layer compound/zinc oxide nano rod composite wood
The preparation method and applications of material.
Background technology
MXene is a kind of new two-dimensional material, and this material is typically to be removed the Al layers etching in MAX phases using acid
Fall, form a kind of two-dimensional layer material similar to graphene.MAX represents that Mn+1AXn, wherein M represent transition metal, and A represents A
Race's element, A is usually Al or Si elements, and X represents C or N element, wherein n=1,2,3.
MXene has the layer structure similar with graphene, and big specific surface area makes it have excellent chemical property,
Interlamellar spacing is adjustable to make it have the significant advantage for being different from other two-dimensional layer materials, and there are some researches show with unique and excellent
Mechanics, electronics, magnetic performance, be a kind of electromagnetic wave absorbent material for having very much researching value and a research potential.However, by
Ti after etching3C2With O, OH and F functional group, these functional groups can also change Ti3C2Characteristic electron, MXene is presented half
Conductor nature, has a strong impact on its electric conductivity.
The content of the invention
The invention aims to provide a kind of preparation side of two-dimensional layer compound/zinc-oxide nano rod composite material
Method and its application, expand MXene application field.The present invention etches MAX by chemical liquid phase etching method and prepares two-dimensional layer
MXene, by the use of surface functional group as chemical site, prepares MXene/ZnO nano composite materials, and then improve materials conductive
Rate, reaches raising wave-absorbing effect purpose, to promote the development of electromagnetic wave absorbent material to make certain contribution.
A kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material is by following steps in the present invention
Suddenly realize:
Step 1: acetic acid dihydrate zinc is dissolved in absolute ethyl alcohol, 30min is stirred under the conditions of 50~80 DEG C, is obtained
Solution A, sodium hydroxide is dissolved in absolute ethyl alcohol, and magnetic agitation 30min, obtains solution B under the conditions of 50~80 DEG C, 60
Solution A and solution B are mixed under the conditions of~80 DEG C, magnetic agitation 30min is subsequently placed in ice bath and is cooled to room temperature, stood
30min, obtains zinc oxide seed solution;
Step 2: MXene powders are added in the zinc oxide seed solution that step one is obtained, mix under magnetic stirring
10~30min, precipitates drying after separation;
Step 3: the operation of repeat step one at least 2 times;
Step 4: being 60~80 DEG C, under the conditions of stir speed (S.S.) is 500-1000r/min in bath temperature, step 2 is dried
Precipitation after dry, which is added in growth-promoting media, stirs 0.5-6.0h, takes precipitation to dry after centrifugation;Obtain two-dimensional layer compound/oxygen
Change zinc nanometer rod composite material;
Wherein, zinc source and alkali source are added in deionized water and are configured to by the growth-promoting media in step 4.
Solution A and solution B press 1 in step one:2 molar concentration rate mixing.
Magnetic agitation is 600r/min in step one.
0.2gMXene powders are added in the zinc oxide seed solution that 125ml steps one are obtained in step 2.
In step 2 2-5h is dried at 70~100 DEG C.
Zinc source described in step 4 is zinc nitrate hexahydrate;The alkali source is hexamethylenetetramine;Zinc source and alkali source rub
You are than being 2:1.
Precipitation is dried into 12h-15h under the conditions of 70~100 DEG C in step 4.
Two-dimensional layer compound/zinc-oxide nano rod composite material prepared by the above method is led applied to electro-magnetic wave absorption
Domain.
The present invention prepares nano composite material by the way that MXene and ZnO are combined, and brings more excellent electrical
It can wait, there are some researches show zinc oxide has certain application value inhaling ripple field, while MXene possesses good electrical property,
Therefore it is compound by both, application field can be expanded with combination property.
The preparation method of the present invention is simple, and reaction condition is gentle, prepares effect preferable.The composite chemical property is excellent
It is good, meanwhile, conductive channel is added there is provided bigger surface area, can be applied in electro-magnetic wave absorption field.
Brief description of the drawings
Fig. 1 is the Flied emission scanning electricity of MXene zinc-oxide nano rod composite materials prepared by the method for embodiment one
Mirror photo;Fig. 2 is Fig. 1 partial enlarged drawings;Fig. 3 is MXene zinc-oxide nano rod composite material electro-magnetic wave absorption curve maps.
Embodiment
Embodiment one, present embodiment are a kind of two-dimensional layer compound oxidation zinc nanometer rod composite material, two
Tie up lamellar compound zinc-oxide nano rod composite material through the following steps that realize:
Step 1: the ethanol solution and concentration for the two nitric hydrate zinc that compound concentration is 1mmol/L are respectively
The ethanol solution of 2mmol/L sodium hydroxide, takes 125mL respectively, at 60 DEG C, magnetic agitation under the conditions of 600r/min
30min, then ice bath is to room temperature, and standing 30min obtains zinc oxide seed solution.
Acetic acid dihydrate zinc is dissolved in absolute ethyl alcohol, 30min is stirred under the conditions of 80 DEG C, obtains solution A,
Sodium hydroxide is dissolved in absolute ethyl alcohol, magnetic agitation 30min, obtains solution B under the conditions of 80 DEG C,
Step 2: 0.2g MXene powders are added in the zinc oxide seed solution that step one is obtained, in magnetic agitation
Lower mixing 30min, is then centrifuged for separation, will be deposited in 80 DEG C of drying 2h;
Step 3: the operation of repeat step one 3 times;
Step 4: be 70 DEG C, under the conditions of stir speed (S.S.) is 600r/min in bath temperature, the precipitation after step 2 is dried
It is added in growth-promoting media and stirs 1.0h, precipitation is taken after centrifugation, 12h is dried under the conditions of 80 DEG C;Obtain two-dimensional layer compound/
Zinc-oxide nano rod composite material
Growth-promoting media described in step 4 is by 12.5mmol zinc nitrate hexahydrates and the addition of 12.5mmol hexamethylenetetramines
Mixing is stirred into 500mL deionized water.
Fig. 1 is the scanning electron microscope (SEM) photograph for preparing MXene/ZnO nano composite materials, it can be seen that MXene and ZnO is successfully answered
Close.Fig. 2 is Fig. 1 Regional High Resolution electron microscope, it can be seen that ZnO is in nano bar-shape structure.
Fig. 3 be MXene/ZnO nano composite materials electro-magnetic wave absorption curve map, it can be seen that the composite have compared with
Good wave-absorbing effect.
Claims (10)
1. a kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material, it is characterised in that this method is logical
Cross following step realization:
Step 1: acetic acid dihydrate zinc is dissolved in absolute ethyl alcohol, 30min is stirred under the conditions of 50~80 DEG C, solution is obtained
A, sodium hydroxide is dissolved in absolute ethyl alcohol, and magnetic agitation 30min, obtains solution B under the conditions of 50~80 DEG C, 60~80
Solution A and solution B are mixed under the conditions of DEG C, magnetic agitation 30min is subsequently placed in ice bath and is cooled to room temperature, stand, obtain oxygen
Change zinc seed solution;
Step 2: MXene powders are added in the zinc oxide seed solution that step one is obtained, mix 10 under magnetic stirring~
30min, precipitates drying after separation;
Step 3: the operation of repeat step one at least 2 times;
Step 4: being 60~80 DEG C, under the conditions of stir speed (S.S.) is 500-1000r/min in bath temperature, after step 2 is dried
Precipitation be added in growth-promoting media and stir 0.5-6.0h, take precipitation to dry after centrifugation;Obtain two-dimensional layer compound/zinc oxide
Nanometer rod composite material;
Wherein, zinc source and alkali source are added in deionized water and are configured to by the growth-promoting media in step 4.
2. a kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material according to right wants 1, it is special
Levy and be that solution A and solution B are by 1 in step one:2 molar concentration rate mixing.
3. a kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material according to right wants 1, it is special
Levy and be in step one that magnetic agitation is 600r/min.
4. a kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material according to right wants 1, it is special
Levy and be in step 2 0.2gMXene powders being added in the zinc oxide seed solution that 125ml steps one are obtained.
5. a kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material according to right wants 1, it is special
Levy and be in step 2 to dry 2-5h at 70~100 DEG C.
6. a kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material according to right wants 1, it is special
Levy and be that zinc source described in step 4 is zinc nitrate hexahydrate.
7. a kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material according to right wants 6, it is special
Levy and be that alkali source described in step 4 is hexamethylenetetramine.
8. a kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material according to right wants 7, it is special
Levy and be that the mol ratio of zinc source and alkali source in step 4 is 2:1.
9. a kind of preparation method of two-dimensional layer compound/zinc-oxide nano rod composite material according to right wants 1, it is special
Levy and be in step 4 under the conditions of 70~100 DEG C precipitation drying 12h-15h.
10. a kind of application of two-dimensional layer compound/zinc-oxide nano rod composite material, it is characterised in that in claim 1-9
Two-dimensional layer compound/zinc-oxide nano rod composite material prepared by any one methods described is led applied to electro-magnetic wave absorption
Domain.
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Cited By (11)
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CN108811478A (en) * | 2018-06-12 | 2018-11-13 | 西北工业大学 | A kind of three-layer laminated MXene electromagnetic shielding foam and preparation method |
CN110053229A (en) * | 2019-04-22 | 2019-07-26 | 成都新柯力化工科技有限公司 | One kind anti-fog haze function waterproof roll for building and preparation method |
CN110828671A (en) * | 2019-11-30 | 2020-02-21 | 华南理工大学 | Organic solar cell with organic-inorganic cathode modification layer material and preparation method thereof |
CN110931643A (en) * | 2019-11-30 | 2020-03-27 | 华南理工大学 | Ti3C2TxOrganic solar cell with doped ZnO as cathode modification layer material and preparation method thereof |
CN111574958A (en) * | 2020-05-19 | 2020-08-25 | 东华大学 | Carbide MXene/SiO of core-edge structure2Nano-plate-shaped ultrathin microwave absorbing material |
CN113025271A (en) * | 2021-03-25 | 2021-06-25 | 电子科技大学 | Ti3C2TxPreparation method of MXene @ ZnO composite wave-absorbing material |
CN114438773A (en) * | 2022-03-11 | 2022-05-06 | 北京理工大学 | Method for modifying bulletproof fiber fabric by using zinc oxide |
CN114725330A (en) * | 2022-03-04 | 2022-07-08 | 厦门大学 | Preparation method and application of two-dimensional titanium carbide-zinc oxide composite material |
CN114747593A (en) * | 2022-04-06 | 2022-07-15 | 湖南农业大学 | MXene-zinc oxide nano composite material, preparation method thereof and recyclable hydrophobic antibacterial material prepared by using MXene-zinc oxide nano composite material |
CN115282786A (en) * | 2022-01-21 | 2022-11-04 | 浙江师范大学 | MXene modified composite separation membrane and preparation method and application thereof |
CN116273103A (en) * | 2023-02-17 | 2023-06-23 | 南京信息工程大学 | Preparation method and application of zinc oxide-MXene composite pyroelectric catalyst |
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Cited By (17)
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CN108811478A (en) * | 2018-06-12 | 2018-11-13 | 西北工业大学 | A kind of three-layer laminated MXene electromagnetic shielding foam and preparation method |
CN108811478B (en) * | 2018-06-12 | 2019-08-09 | 西北工业大学 | A kind of three-layer laminated MXene electromagnetic shielding foam and preparation method |
CN110053229A (en) * | 2019-04-22 | 2019-07-26 | 成都新柯力化工科技有限公司 | One kind anti-fog haze function waterproof roll for building and preparation method |
CN110931643B (en) * | 2019-11-30 | 2022-03-29 | 华南理工大学 | Ti3C2TxOrganic solar cell with doped ZnO as cathode modification layer material and preparation method thereof |
CN110828671B (en) * | 2019-11-30 | 2021-08-06 | 华南理工大学 | Organic solar cell with organic-inorganic cathode modification layer material and preparation method thereof |
CN110931643A (en) * | 2019-11-30 | 2020-03-27 | 华南理工大学 | Ti3C2TxOrganic solar cell with doped ZnO as cathode modification layer material and preparation method thereof |
CN110828671A (en) * | 2019-11-30 | 2020-02-21 | 华南理工大学 | Organic solar cell with organic-inorganic cathode modification layer material and preparation method thereof |
CN111574958B (en) * | 2020-05-19 | 2023-03-21 | 东华大学 | Carbide MXene/SiO of core-edge structure 2 Nano-plate-shaped ultrathin microwave absorbing material |
CN111574958A (en) * | 2020-05-19 | 2020-08-25 | 东华大学 | Carbide MXene/SiO of core-edge structure2Nano-plate-shaped ultrathin microwave absorbing material |
CN113025271A (en) * | 2021-03-25 | 2021-06-25 | 电子科技大学 | Ti3C2TxPreparation method of MXene @ ZnO composite wave-absorbing material |
CN115282786A (en) * | 2022-01-21 | 2022-11-04 | 浙江师范大学 | MXene modified composite separation membrane and preparation method and application thereof |
CN115282786B (en) * | 2022-01-21 | 2023-12-08 | 浙江师范大学 | MXene modified composite separation membrane and preparation method and application thereof |
CN114725330A (en) * | 2022-03-04 | 2022-07-08 | 厦门大学 | Preparation method and application of two-dimensional titanium carbide-zinc oxide composite material |
CN114725330B (en) * | 2022-03-04 | 2024-06-11 | 厦门大学 | Preparation method and application of two-dimensional titanium carbide-zinc oxide composite material |
CN114438773A (en) * | 2022-03-11 | 2022-05-06 | 北京理工大学 | Method for modifying bulletproof fiber fabric by using zinc oxide |
CN114747593A (en) * | 2022-04-06 | 2022-07-15 | 湖南农业大学 | MXene-zinc oxide nano composite material, preparation method thereof and recyclable hydrophobic antibacterial material prepared by using MXene-zinc oxide nano composite material |
CN116273103A (en) * | 2023-02-17 | 2023-06-23 | 南京信息工程大学 | Preparation method and application of zinc oxide-MXene composite pyroelectric catalyst |
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Application publication date: 20171013 |