CN107417951A - A kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional - Google Patents
A kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional Download PDFInfo
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- CN107417951A CN107417951A CN201710280807.9A CN201710280807A CN107417951A CN 107417951 A CN107417951 A CN 107417951A CN 201710280807 A CN201710280807 A CN 201710280807A CN 107417951 A CN107417951 A CN 107417951A
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Abstract
The invention provides a kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional, yttrium nitrate, urea and anion salt are weighed first, prepare growth-promoting media, the concentration for controlling ruthenium ion in growth-promoting media is 0.05~0.2mol/L, the concentration of urea is 0.2~0.8mol/L, and the concentration of anion salt is 0.01~0.03mol/L；Then using acetone and the aqueous solution of lauryl sodium sulfate processing PET film, finally the PET film after processing is placed on the surface of growth-promoting media, PET film is set to float on growth-promoting media surface without sinking, 80~90 DEG C of controlling reaction temperature, react 12~72h, nano thin-film is obtained after drying, the anion salt is sodium sulphate, dibastic sodium phosphate, sodium sulfite, sodium fluoride, one kind of sodium metasilicate.The inventive method cost is cheap, reaction condition is gently controllable, preparation technology is simple, can prepare the yittrium oxide nano thin-film of the sequential 2 D of large area, and obtained nano thin-film is carried out ordered arrangement perpendicular to PET film surface by nano wire or nanometer rods and formed.
Description
Technical field
The invention belongs to rare earth nano material field, is related to a kind of preparation method of yittrium oxide nano thin-film, more particularly to
A kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional.
Background technology
Rare earth nano material research work is from the research to zero-dimension nano particle, gradually to one-dimensional (nanotube, nanometer
Line, nanometer rods), two-dimentional (nanometer film) and three-dimensional nanometer material development, from rare-earth nanometer particles are initially simply prepared, to system
The standby rare earth nano material with specific form is simultaneously carried out compound with assembling.Rare earth nanometer film is in electricity, magnetics, optics, warm
Learn etc. all has distinctive performance, and its performance and microstructure are influenceed by preparation method, prepare rare earth nano at present
The method of thin-film material mainly include spray pyrolysis, inert-gas condensation method, sol-gel process, critical hydrothermal synthesis method and
Precipitation method etc., these methods prepare rare earth nanometer film material, although the film consistency being prepared having is high,
The investment of equipment is big, and cost is high；Although what is had is cheap, investment is small, the poor performance of the rare earth nanometer film obtained.Urgently
It need to study that a kind of cost is cheap, gentle controllable, the simple preparation method of preparation technology of reaction condition carrys out controllable preparation sequential 2 D
Rare earth nanometer film.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional, this method
Cost is cheap, reaction condition is gently controllable, preparation technology is simple, can be used to prepare the yittrium oxide nanometer of the sequential 2 D of large area
Film.
To realize above-mentioned purpose, the technical solution adopted by the present invention is：
A kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional, comprises the following steps：
(1) growth-promoting media is prepared：It is accurate to weigh yttrium nitrate and urea, deionized water dissolving is added, is then added thereto cloudy
Ion salt, stirring are completely dissolved it, form growth-promoting media, and the concentration for controlling ruthenium ion in growth-promoting media is 0.05~0.2mol/L,
The concentration of urea is 0.2~0.8mol/L, and the concentration of anion salt is 0.01~0.03mol/L；
(2) thin-film carrier is handled：PET film is immersed in acetone, ultrasonic 20min, then immerse lauryl sodium sulfate
In the aqueous solution, ultrasonic 10min, finally with alcohol flushing 2 times, naturally dry；
(3) preparation of nano thin-film：PET film after step (2) processing is placed in the table of growth-promoting media made from step (1)
On face, PET film is floated on growth-promoting media surface without sinking, and be brought into close contact with growth-promoting media liquid level, then put growth-promoting media
In baking oven, 80~90 DEG C of controlling reaction temperature, 12~72h is reacted, PET film is finally taken out, dries, received at 80 DEG C
Rice film.
The nano thin-film be by nano wire, nanometer rods or nanometer sheet perpendicular to PET film surface carry out ordered arrangement and
The film of formation.
The area of the nano thin-film is 1~100cm2。
The anion salt is sodium sulphate, dibastic sodium phosphate, sodium sulfite, sodium fluoride, one kind of sodium metasilicate.
The concentration of the aqueous solution of the lauryl sodium sulfate is 0.1~1mol/L.
Beneficial effect possessed by the present invention：
(1) preparation method of the present invention has the characteristics of cost is cheap, reaction condition is gentle and technique is simple, is easy to promote；
(2) nano thin-film prepared by the present invention is arranged in order perpendicular to PET film surface by nano wire or nanometer rods
Arrange and formed, regularity is good, and area is big；
(3) the invention provides a kind of method for preparing large-area nano film, for the system of large-area nano film material
It is standby to open a kind of variation route.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the nano thin-film of embodiment 1；
Fig. 2 is the X ray diffracting spectrum of the nano thin-film of embodiment 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of the nano thin-film of embodiment 2；
Fig. 4 is the scanning electron microscope (SEM) photograph of the nano thin-film of embodiment 3；
Fig. 5 is the scanning electron microscope (SEM) photograph of the nano thin-film of embodiment 4.
Embodiment
With reference to specific embodiment, the invention will be further described, but does not limit protection scope of the present invention.
Embodiment 1
A kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional, comprises the following steps：
(1) growth-promoting media is prepared：It is accurate to weigh yttrium nitrate and urea, deionized water dissolving is added, then adds phosphorus thereto
Sour hydrogen sodium, stirring are completely dissolved it, form growth-promoting media, the concentration for controlling ruthenium ion in growth-promoting media is 0.05mol/L, urea
Concentration is 0.2mol/L, and the concentration of dibastic sodium phosphate is 0.025mol/L；
(2) thin-film carrier is handled：PET film is immersed in acetone, ultrasonic 20min, then it is 0.5mol/L ten to immerse concentration
In the aqueous solution of sodium dialkyl sulfate, ultrasonic 10min, finally with alcohol flushing 2 times, naturally dry；
(3) preparation of nano thin-film：PET film after step (2) processing is placed in the table of growth-promoting media made from step (1)
On face, PET film is floated on growth-promoting media surface without sinking, and be brought into close contact in growth-promoting media liquid level, then put growth-promoting media
In baking oven, 85 DEG C of reaction 24h of controlling reaction temperature, PET film is taken out, is dried at 80 DEG C, obtains nano thin-film.
The product of the present embodiment is characterized, Fig. 1 is the scanning electron microscope (SEM) photograph of the nano thin-film of embodiment 1, and the upper right corner is small
The partial enlargement scanning electron microscope (SEM) photograph that figure is Fig. 1, it is seen that nano thin-film is arranged in order perpendicular to PET film surface by nano wire
Arrange and formed, nano thin-film uniform load is on pet vector；Fig. 2 is the X-ray diffractogram of the nano thin-film of the present embodiment
Spectrum, confirm that product is yittrium oxide after being compared with PDF standard cards.
Embodiment 2
A kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional, comprises the following steps：
(1) growth-promoting media is prepared：It is accurate to weigh yttrium nitrate and urea, deionized water dissolving is added, is then added thereto sub-
Sodium sulphate, stirring are completely dissolved it, form growth-promoting media, the concentration for controlling ruthenium ion in growth-promoting media is 0.1mol/L, urea
Concentration is 0.4mol/L, and the concentration of anion salt is 0.3mol/L；
(2) thin-film carrier is handled：PET film is immersed in acetone, ultrasonic 20min, then it is 0.5mol/L ten to immerse concentration
In the aqueous solution of sodium dialkyl sulfate, ultrasonic 10min, finally with alcohol flushing 2 times, naturally dry；
(3) preparation of nano thin-film：PET film after step (2) processing is placed in the table of growth-promoting media made from step (1)
On face, PET film is floated on growth-promoting media surface without sinking, and be brought into close contact in growth-promoting media liquid level, then put growth-promoting media
In baking oven, 90 DEG C of reaction 72h of controlling reaction temperature, PET film is taken out, is dried at 80 DEG C, obtains nano thin-film.
The product of the present embodiment is characterized, Fig. 3 is the scanning electron microscope (SEM) photograph of the nano thin-film of the present embodiment, and the upper right corner is small
The partial enlargement scanning electron microscope (SEM) photograph that figure is Fig. 3, it is seen that nano thin-film is arranged in order perpendicular to PET film surface by nanometer rods
Arrange and formed, nano thin-film uniform load is on pet vector.
Embodiment 3
A kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional, comprises the following steps：
(1) growth-promoting media is prepared：It is accurate to weigh yttrium nitrate and urea, deionized water dissolving is added, then adds sulphur thereto
Sour sodium, stirring are completely dissolved it, form growth-promoting media, and the concentration for controlling ruthenium ion in growth-promoting media is 0.05mol/L, urea it is dense
Spend for 0.2mol/L, the concentration of anion salt is 0.015mol/L；
(2) thin-film carrier is handled：PET film is immersed in acetone, ultrasonic 20min, then it is 1mol/L 12 to immerse concentration
In the aqueous solution of sodium alkyl sulfate, ultrasonic 10min, finally with alcohol flushing 2 times, naturally dry；
(3) preparation of nano thin-film：PET film after step (2) processing is placed in the table of growth-promoting media made from step (1)
On face, PET film is floated on growth-promoting media surface without sinking, and be brought into close contact in growth-promoting media liquid level, then put growth-promoting media
In baking oven, 85 DEG C of reaction 48h of controlling reaction temperature, PET film is taken out, is dried at 80 DEG C, obtains nano thin-film.
The product of the present embodiment is characterized, Fig. 4 is the scanning electron microscope (SEM) photograph of the nano thin-film of the present embodiment, and the upper right corner is small
The partial enlargement scanning electron microscope (SEM) photograph that figure is Fig. 4, it is seen that nano thin-film is arranged in order perpendicular to PET film surface by nanometer sheet
Arrange and formed, nano thin-film uniform load is on pet vector.
Embodiment 4
A kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional, comprises the following steps：
(1) growth-promoting media is prepared：It is accurate to weigh yttrium nitrate and urea, deionized water dissolving is added, then adds sulphur thereto
Sour sodium, stirring are completely dissolved it, form growth-promoting media, and the concentration for controlling ruthenium ion in growth-promoting media is 0.2mol/L, urea it is dense
Spend for 0.8mol/L, the concentration of anion salt is 0.025mol/L；
(2) thin-film carrier is handled：PET film is immersed in acetone, ultrasonic 20min, then it is 1mol/L 12 to immerse concentration
In the aqueous solution of sodium alkyl sulfate, ultrasonic 10min, finally with alcohol flushing 2 times, naturally dry；
(3) preparation of nano thin-film：PET film after step (2) processing is placed in the table of growth-promoting media made from step (1)
On face, PET film is floated on growth-promoting media surface without sinking, and be brought into close contact in growth-promoting media liquid level, then put growth-promoting media
In baking oven, 85 DEG C of reaction 24h of controlling reaction temperature, PET film is taken out, is dried at 80 DEG C, obtains nano thin-film.
The product of the present embodiment is characterized, Fig. 5 is the scanning electron microscope (SEM) photograph of the nano thin-film of the present embodiment, and the upper right corner is small
The partial enlargement scanning electron microscope (SEM) photograph that figure is Fig. 5, it is seen that nano thin-film is arranged in order perpendicular to PET film surface by nanometer sheet
Arrange and formed, nano thin-film uniform load is on pet vector.
Above-described embodiment is only one of presently preferred embodiments of the present invention, is not limited the scope of the invention with this, therefore：
The equivalence changes that all structures under this invention, shape, principle are done, all should be covered by within protection scope of the present invention.
Claims (4)
1. a kind of preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional, it is characterised in that comprise the following steps：
(1) growth-promoting media is prepared：It is accurate to weigh yttrium nitrate and urea, deionized water dissolving is added, then adds anion thereto
Salt, stirring are completely dissolved it, form growth-promoting media, and the concentration for controlling ruthenium ion in growth-promoting media is 0.05~0.2mol/L, urea
Concentration be 0.2~0.8mol/L, the concentration of anion salt is 0.01~0.03mol/L；
(2) thin-film carrier is handled：PET film is immersed in acetone, ultrasonic 20min, then immerse the water-soluble of lauryl sodium sulfate
In liquid, ultrasonic 10min, finally with alcohol flushing 2 times, naturally dry；
(3) preparation of nano thin-film：PET film after step (2) processing is placed in the surface of growth-promoting media made from step (1)
On, PET film is floated on growth-promoting media surface without sinking, and be brought into close contact with growth-promoting media liquid level, then growth-promoting media is placed in
In baking oven, 80~90 DEG C of controlling reaction temperature, 12~72h is reacted, PET film is finally taken out, is dried at 80 DEG C, obtain nanometer
Film.
2. the preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional according to claim 1, it is characterised in that institute
It is the film for being carried out ordered arrangement perpendicular to PET film surface by nano wire, nanometer rods or nanometer sheet and being formed to state nano thin-film.
3. the preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional according to claim 1, it is characterised in that institute
Anion salt is stated as sodium sulphate, dibastic sodium phosphate, sodium sulfite, sodium fluoride, one kind of sodium metasilicate.
4. the preparation method of the orderly yittrium oxide nano thin-film of large-area two-dimensional according to claim 1, it is characterised in that institute
The concentration for stating the aqueous solution of lauryl sodium sulfate is 0.1~1mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113060753A (en) * | 2021-03-31 | 2021-07-02 | 陕西科技大学 | Low-dimensional layered yttrium oxide nanosheet and preparation method thereof |
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| JP2015036384A (en) * | 2013-08-10 | 2015-02-23 | 国立大学法人島根大学 | Manufacturing method of luminescent material |
| CN104556190A (en) * | 2013-10-09 | 2015-04-29 | 中国石油化工股份有限公司 | Ball follow-shaped yttrium oxide self-assembly thin film and preparation method thereof |
| CN106298455A (en) * | 2016-09-14 | 2017-01-04 | 齐鲁工业大学 | A kind of low temperature liquid phase method preparing high dielectric oxidation yttrium thin film |
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2017
- 2017-04-24 CN CN201710280807.9A patent/CN107417951A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2015036384A (en) * | 2013-08-10 | 2015-02-23 | 国立大学法人島根大学 | Manufacturing method of luminescent material |
| CN104556190A (en) * | 2013-10-09 | 2015-04-29 | 中国石油化工股份有限公司 | Ball follow-shaped yttrium oxide self-assembly thin film and preparation method thereof |
| CN106298455A (en) * | 2016-09-14 | 2017-01-04 | 齐鲁工业大学 | A kind of low temperature liquid phase method preparing high dielectric oxidation yttrium thin film |
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| 吴洪达等: "球形纳米氧化钇的制备与表征", 《无机盐工业》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113060753A (en) * | 2021-03-31 | 2021-07-02 | 陕西科技大学 | Low-dimensional layered yttrium oxide nanosheet and preparation method thereof |
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Application publication date: 20171201 |