CN109536903A - A kind of ceric oxide nanorod and its preparation method and application - Google Patents

A kind of ceric oxide nanorod and its preparation method and application Download PDF

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Publication number
CN109536903A
CN109536903A CN201811486302.9A CN201811486302A CN109536903A CN 109536903 A CN109536903 A CN 109536903A CN 201811486302 A CN201811486302 A CN 201811486302A CN 109536903 A CN109536903 A CN 109536903A
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ceric oxide
oxide nanorod
preparation
glancing incidence
magnetron sputtering
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安涛
窦春月
鞠金宁
魏文龙
纪全增
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Changchun University
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Changchun University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Catalysts (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to field of nano material preparation more particularly to a kind of preparation methods of ceric oxide nanorod, and the preparation method comprises the following steps: in Ar and O2Mixed atmosphere in, using Si (100) single-chip as substrate, using Ce as target, carry out glancing incidence magnetron sputtering, obtain ceric oxide nanorod.The present invention is the ceric oxide nanorod of triangular pyramid by the available surface of glancing incidence magnetically controlled sputter method, contact angle >=107.5 ° of the ceric oxide nanorod and water that are prepared using preparation method provided by the invention, it is maximum 143.2 ° reachable, it is the Maximum Contact angle value of current ceria material.

Description

A kind of ceric oxide nanorod and its preparation method and application
Technical field
The present invention relates to technical field of nano material more particularly to a kind of ceric oxide nanorod and preparation method thereof and answer With.
Background technique
Wellability is one of important feature of the surface of solids, again to national defence troops from daily life to industrial and agricultural production Thing equipment field, wellability are all a kind of very important property.The application of wetability is extremely extensive: super-hydrophobic boundary material is used It, can be with the anti-accumulated snow of waterproof, to guarantee the reception of high-quality signal on exterior aerial；Super-amphiphobic boundary material can be coated in steamer On the shells of naval vessels, fuel reserve tank, anti-pollution, etch-proof effect can achieve；It is transported in petroleum pipeline in petroleum During defeated, petroleum can be prevented viscous in duct wall, to reduce the loss and energy consumption in transportational process, and prevent pipe Road blocking；For means of transport in water or underwater nuclear submarine, it is possible to reduce the resistance of water improves travel speed；For micro On syringe needle point, viscous and thus bring needle point pollution of the expensive drug on needle point can be completely eliminated；It can also be with With it come finishing textiles, it is made into waterproof and antipollution clothes etc..Therefore, the wellability of material is in each neck of national economy There is very important application in domain and national defense construction.The micromechanism for determining material wellability is explored, preparation has high (super) The material of hydrophobic performance becomes the great demand of numerous areas.
Currently, there are two the factor for influencing surface of solids wellability is main: first is that the surface free energy of solid；Second is that solid Surface roughness.The surface of super-hydrophobic (150 ° of water contact angle >) material will also have certain other than having low-surface-energy Roughness.The main method for preparing super hydrophobic surface is that coarse surface is modified with the material of low-surface-energy.Minami et al. The Al of rough porous is prepared for using sol-gel method2O3Then film modifies this film with silicon fluoride, obtain connecing with water The super-hydrophobic Al that feeler is 165 °2O3Film.McCarthy group is prepared using the method for photoengraving with micron order column battle array The silicon face of array structure carries out hydrophobic treatment with silylating reagent and obtains super hydrophobic surface；Yoshimitsu et al. utilizes machine The method of tool etching, obtaining the pattern silicon face for having well-regulated micron order roughness can obtain after silicon fluoride is handled To about 150 ° of super hydrophobic surface of contact angle.The method of Bartell and Shepard Mechanical lithography is prepared for tetrahedroid The contact angle of the coarse paraffin surface of structure, this surface and water is about 160 °.
Although above-mentioned many research achievements all obtain ideal hydrophobic surface, these research achievements there is also One restricts its widely applied common problem: that coating material for being exactly these low-surface-energies is largely that high temeperature chemistry is stablized Property lower, the polymer or high molecular material of poor mechanical property.These polymer materials or high molecular material in hot conditions or It is likely to phenomena such as decomposing, remove and falling off in the more harsh working environment such as mechanical shock, to influence reality Hydrophobic effect in.On the other hand, the studies above is all made of the coating of low-surface-energy to modify rough surface, so that it is made Standby technique is considerably complicated.
Therefore, a kind of intrinsic hydrophobic material with preferable hydrophobic effect, which how is prepared, becomes the weight of people's research Point.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of ceric oxide nanorod with good hydrophobic effect and It is applied.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of ceric oxide nanorod, comprising the following steps:
In Ar and O2Mixed atmosphere in, using Si (100) single-chip as substrate, using Ce as target, carry out glancing incidence Magnetron sputtering obtains ceric oxide nanorod.
Preferably, the Ar and O2Volume ratio be (25~35): 10.
Preferably, the glancing angle of the glancing incidence magnetron sputtering is 45~55 °.
Preferably, the pressure of the glancing incidence magnetron sputtering is 0.8~2Pa.
Preferably, the temperature of the glancing incidence magnetron sputtering is 200~600 DEG C.
Preferably, the radio-frequency power of the glancing incidence magnetron sputtering is 90~110W, and sputtering time is 80~180 minutes.
The present invention also provides the ceric oxide nanorod that the preparation method is prepared, the cerium dioxide nano Contact angle >=107.5 ° of stick and water.
The present invention also provides the ceric oxide nanorods to prepare the application in hydrophobic ceramic material.
The present invention provides a kind of preparation methods of ceric oxide nanorod, comprising the following steps: in Ar and O2Mixing In atmosphere, using Si (100) single-chip as substrate, using Ce as target, glancing incidence magnetron sputtering is carried out, ceria is obtained and receives Rice stick.The present invention is the ceric oxide nanorod of triangular pyramid by the available surface of glancing incidence magnetically controlled sputter method, utilizes this Contact angle >=107.5 ° of ceric oxide nanorod and water that the preparation method that invention provides is prepared, it is maximum reachable 143.2 °, be the Maximum Contact angle value of current ceria material.
Detailed description of the invention
Fig. 1 is the cross-sectional scans electron microscope for the ceric oxide nanorod that embodiment 1 is prepared；
Fig. 2 is the flat scanning electron microscope for the ceric oxide nanorod that embodiment 1 is prepared；
Fig. 3 is the cross-sectional scans electron microscope for the ceric oxide nanorod that embodiment 2 is prepared；
Fig. 4 is the flat scanning electron microscope for the ceric oxide nanorod that embodiment 2 is prepared；
Fig. 5 is the cross-sectional scans electron microscope for the ceric oxide nanorod that embodiment 3 is prepared；
Fig. 6 is the flat scanning electron microscope for the ceric oxide nanorod that embodiment 3 is prepared；
Fig. 7 is the cross-sectional scans electron microscope for the ceric oxide nanorod that embodiment 4 is prepared；
Fig. 8 is the flat scanning electron microscope for the ceric oxide nanorod that embodiment 4 is prepared.
Specific embodiment
The present invention provides a kind of preparation methods of ceric oxide nanorod, comprising the following steps:
In Ar and O2Mixed atmosphere in, using Si (100) single-chip as substrate, using Ce as target, carry out glancing incidence Magnetron sputtering obtains ceric oxide nanorod.
In the present invention, if without specified otherwise, all raw material components are commercial product well known to those skilled in the art.
In the present invention, before carrying out glancing incidence magnetron sputtering, preferably the Si (100) single-chip and Ce target are carried out pre- Processing；The Si (100) single-chip is preferably cut into 2cm × 2cm's by the pretreatment to the Si (100) single-chip After size, successively ultrasound 10 minutes, hair dryer are dried up respectively in acetone, alcohol and deionized water.
The pretreatment to Ce target preferably uses Ar ion sputtering, washes the pollutant on target material surface；This Invention does not have any special restriction to the condition of the Ar ion sputtering, using sputtering condition well known to those skilled in the art Progress.
In the present invention, the Ar is sputter gas, the O2For reaction gas.
In the present invention, the Ar and O2Volume ratio be preferably (25~35): 10, more preferably (28~32): 10, most Preferably (29~31): 10.
In the present invention, the pressure of the glancing incidence magnetron sputtering is preferably 0.8~2Pa, more preferably 1~1.8Pa, most Preferably 1.2~1.6Pa.
In the present invention, the glancing angle of the glancing incidence magnetron sputtering is preferably 45~55 °, and more preferably 48~52 °, most Preferably 49~51 °.
In the present invention, the temperature of the glancing incidence magnetron sputtering is preferably 200~600 DEG C, more preferably 300~500 DEG C, most preferably 350~450 DEG C.
In the present invention, the radio-frequency power of the glancing incidence magnetron sputtering is preferably 90~110W, more preferably 95~ 105W, most preferably 98~102W；The sputtering time is preferably 80~180 minutes, more preferably 100~160 minutes, optimal It is selected as 120~140 minutes.
In the present invention, the condition of the glancing incidence magnetron sputtering can obtain the maximum CeO of roughness2Nanometer rods, can So that CeO2The surface particles of nanometer rods are more uniform, and shape is more complete, uniform, and then the surface for improving nanometer rods and water connects Feeler.
The present invention also provides the ceric oxide nanorod that the preparation method is prepared, the cerium dioxide nano Contact angle >=107.5 ° of stick and water.
The present invention also provides the ceric oxide nanorods to prepare the application in hydrophobic ceramic material.
Ceric oxide nanorod provided by the invention and its preparation method and application is carried out below with reference to embodiment detailed Explanation, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
After Si (100) single-chip is cut into the size of 2cm × 2cm, successively in acetone, alcohol and deionized water respectively Ultrasound 10 minutes, hair dryer drying；
Using Ar ion sputtering, the pollutant on target material surface is washed；
In the Ar and O that volume ratio is 30:102Mixed atmosphere in carry out glancing incidence magnetron sputtering, glancing angle be 50 °, splash Penetrating pressure is 0.8Pa, and radio-frequency power 100W, sputter temperature is 400 DEG C, and sputtering time is 120 minutes, obtains ceria and receives Rice stick.
Fig. 1 is the cross-sectional scans electron microscope of the ceric oxide nanorod, and Fig. 2 is the plane of the ceric oxide nanorod Scanning electron microscope (SEM) photograph, ceric oxide nanorod is independent of one another it can be seen from Fig. 1 and Fig. 2, does not occur agglomeration, and its top The pattern of triangular pyramid is presented, most triangular pyramid sizes are almost equal, have a little little particle to be distributed in the intersection of triangular pyramid.
Embodiment 2
After Si (100) single-chip is cut into the size of 2cm × 2cm, successively in acetone, alcohol and deionized water respectively Ultrasound 10 minutes, hair dryer drying；
Using Ar ion sputtering, the pollutant on target material surface is washed；
In the Ar and O that volume ratio is 30:102Mixed atmosphere in carry out glancing incidence magnetron sputtering, glancing angle be 50 °, splash Penetrating pressure is 0.8Pa, and radio-frequency power 100W, sputter temperature is 200 DEG C, and sputtering time is 120 minutes, obtains ceria and receives Rice stick.
Fig. 3 is the cross-sectional scans electron microscope of the ceric oxide nanorod, and Fig. 4 is the plane of the ceric oxide nanorod Scanning electron microscope (SEM) photograph, ceric oxide nanorod arrangement is more loose it can be seen from Fig. 3 and Fig. 4.
Embodiment 3
After Si (100) single-chip is cut into the size of 2cm × 2cm, successively in acetone, alcohol and deionized water respectively Ultrasound 10 minutes, hair dryer drying；
Using Ar ion sputtering, the pollutant on target material surface is washed；
In the Ar and O that volume ratio is 30:102Mixed atmosphere in carry out glancing incidence magnetron sputtering, glancing angle be 50 °, splash Penetrating pressure is 0.8Pa, and radio-frequency power 100W, sputter temperature is 600 DEG C, and sputtering time is 120 minutes, obtains ceria and receives Rice stick.
Fig. 5 is the cross-sectional scans electron microscope of the ceric oxide nanorod, and Fig. 6 is the plane of the ceric oxide nanorod Scanning electron microscope (SEM) photograph, ceric oxide nanorod is independent of one another it can be seen from Fig. 5 and Fig. 6, does not occur agglomeration, and its top The pattern of triangular pyramid is presented, the triangular pyramid size big absolutely is almost equal, has a little little particle to be distributed in the intersection of triangular pyramid.
Embodiment 4
After Si (100) single-chip is cut into the size of 2cm × 2cm, successively in acetone, alcohol and deionized water respectively Ultrasound 10 minutes, hair dryer drying；
Using Ar ion sputtering, the pollutant on target material surface is washed；
In the Ar and O that volume ratio is 30:102Mixed atmosphere in carry out glancing incidence magnetron sputtering, glancing angle be 50 °, splash Penetrating pressure is 0.8Pa, and radio-frequency power 100W, sputter temperature is 400 DEG C, and sputtering time is 180 minutes, obtains ceria and receives Rice stick.
Fig. 7 is the cross-sectional scans electron microscope of the ceric oxide nanorod, and Fig. 8 is the plane of the ceric oxide nanorod Scanning electron microscope (SEM) photograph, ceric oxide nanorod is independent of one another it can be seen from Fig. 7 and Fig. 8, does not occur agglomeration, and its top The pattern of triangular pyramid is presented, the triangular pyramid size big absolutely is almost equal, has a little little particle to be distributed in the intersection of triangular pyramid.
Embodiment 5
Using Krus-DSA30 contact angle tester, the titanium dioxide that the 2 pure water droplets of μ L are prepared in Examples 1 to 4 Cerium nanorod surfaces test the contact angle of water droplet and sample surfaces after water droplet form stable, then take pictures, and obtain contact angle figure Piece.Each sample tests no less than 6 points, is averaged.
Specific contact angle is as shown in table 1:
Table 1: the contact angle of ceric oxide nanorod and water that Examples 1 to 4 is prepared
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Contact angle 143.2° 107.5° 137.9° 140.6°
Above it is found that the ceric oxide nanorod that preparation method provided by the invention is prepared has excellent hydrophobicity Energy.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (8)

1. a kind of preparation method of ceric oxide nanorod, comprising the following steps:
In Ar and O2Mixed atmosphere in, using Si (100) single-chip as substrate, using Ce as target, carry out glancing incidence magnetic control splash It penetrates, obtains ceric oxide nanorod.
2. preparation method as described in claim 1, which is characterized in that the Ar and O2Volume ratio be (25~35): 10.
3. preparation method as described in claim 1, which is characterized in that the glancing angle of the glancing incidence magnetron sputtering be 45~ 55°。
4. preparation method as described in claim 1, which is characterized in that the pressure of the glancing incidence magnetron sputtering be 0.8~ 2Pa。
5. preparation method as described in claim 1, which is characterized in that the temperature of the glancing incidence magnetron sputtering is 200~600 ℃。
6. preparation method as described in claim 1, which is characterized in that the radio-frequency power of the glancing incidence magnetron sputtering be 90~ 110W, sputtering time are 80~180 minutes.
7. the ceric oxide nanorod that the described in any item preparation methods of claim 1~6 are prepared, which is characterized in that institute State contact angle >=107.5 ° of ceric oxide nanorod and water.
8. ceric oxide nanorod as claimed in claim 7 is preparing the application in hydrophobic ceramic material.
CN201811486302.9A 2018-12-06 2018-12-06 A kind of ceric oxide nanorod and its preparation method and application Pending CN109536903A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104080728A (en) * 2011-09-28 2014-10-01 康涅狄格大学 Metal oxide nanorod arrays on monolithic substrates

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104080728A (en) * 2011-09-28 2014-10-01 康涅狄格大学 Metal oxide nanorod arrays on monolithic substrates

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
TAO AN ET AL: ""Growth and roughness dependent wetting properties of CeO2 films prepared__by glancing angle deposition"", 《CERAMICS INTERNATIONAL》 *
TAO AN ET AL: ""Preparation of highly hydrophobic CeO2 films using glancing angle deposition"", 《MATERIALS LETTERS》 *

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Application publication date: 20190329