CN106381461A - Preparation method for petal-fold-shaped nanometer iron oxide coating - Google Patents
Preparation method for petal-fold-shaped nanometer iron oxide coating Download PDFInfo
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- CN106381461A CN106381461A CN201610816900.2A CN201610816900A CN106381461A CN 106381461 A CN106381461 A CN 106381461A CN 201610816900 A CN201610816900 A CN 201610816900A CN 106381461 A CN106381461 A CN 106381461A
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/12—Oxidising using elemental oxygen or ozone
- C23C8/14—Oxidising of ferrous surfaces
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- 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
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Abstract
The invention discloses a preparation method for a petal-fold-shaped nanometer iron oxide coating. After being subjected to ultrasonic cleaning and dried in an air-insulated manner, a stainless steel wire or an iron wire is firstly soaked into a strong acid solution to be etched, and then the stainless steel wire or the iron wire obtained after being etched is washed with ultrapure water and dried in the air-insulated manner; then the stainless steel wire or the iron wire is placed in flames to be combusted and oxidized, and nanometer iron oxide is obtained on the surface of the stainless steel wire or the iron wire; and finally, the combusted and oxidized stainless steel wire or iron wire is sequentially washed with ultrapure water and methanol, and is dried in the air-insulated manner, and the uniform petal-fold-shaped nanometer iron oxide coating is obtained on the surface of the stainless steel wire or the iron wire. The fold interval of the nanometer iron oxide coating prepared through the method is 100-250 nanometers, the thickness of the coating is 1.2-1.4 microns, the structure is in a petal fold shape, and distribution is uniform; and the specific surface area is large, the adsorption capacity is high, the nanometer iron oxide coating is applied to an extraction head coating material in a solid phase microextraction technology, polycyclic aromatic hydrocarbons can be extracted, the extraction efficiency is high, and stability is high.
Description
Technical field
The present invention relates to a kind of preparation of nano-sized iron oxide coating, more particularly, to a kind of petal accordion nano-sized iron oxide painting
The preparation of layer, mainly as the coating material of extracting head in solid phase micro-extraction technique, is applied in solid phase micro-extraction technique, belongs to
Field of nanometer material technology and environmental analysis field.
Background technology
In environmental analysis field, due to the diversity of sample, complexity and content is very low, it is accomplished by sample before analysis
Product carry out pre-treatment.And solid phase micro-extraction technique（Solid Phase Microextraction, SPME）There is very high extraction
And accumulation ability, quickly grew in the last few years, because its unique advantage is widely used.But current solid phase is micro-
Extraction coating is mainly vitreous silica fiber, there is the shortcomings of expensive, short life, stability are poor.Thus, development efficiently,
Inexpensively, long-life coating material has very important Research Significance and using value.
Nano-sized iron oxide as the important metal oxide of the class in nanometer new material, due to its stable chemical nature,
Catalysis activity is high, also has the features such as good light resistance and weatherability, catalyst, fine ceramics, coating, plastic products,
The aspect such as magnetic material and bioengineering and medical science has a wide range of applications and is worth and development prospect, and nano-sized iron oxide also has
There is nontoxic, cheap characteristic, therefore research nano-sized iron oxide has very important meaning.But nano-sized iron oxide is as solid phase
The application of micro-extraction coat layer has not yet to see report.
Content of the invention
It is an object of the invention to provide a kind of preparation method of petal accordion nano-sized iron oxide coating, reduce fiber and apply
The preparation cost of layer, and improve stability and the life-span of fiber coat.
The present invention prepares the preparation method of petal accordion nano-sized iron oxide coating, is will be ultrasonic to stainless steel wire or iron wire clear
Wash, completely cut off air be dried after, be submerged initially in strong acid solution and perform etching, make stainless steel wire or iron wire surface roughening, with increase
Specific surface area；Stainless steel wire will be obtained again after etching or iron wire will use ultra-pure water, methyl alcohol to rinse successively, isolation air will be dried；Then put
In putting into combustion oxidation in flame, obtain nano-sized iron oxide in stainless steel wire or iron wire surface；Finally by after combustion oxidation not
Rust steel wire or iron wire use ultra-pure water, methyl alcohol to rinse successively, and isolation air is dried, and obtains uniformly in stainless steel wire or iron wire surface
Petal accordion nano-sized iron oxide coating.
The specification of described stainless steel wire or iron wire is Φ=0.15 ~ 0.45 mm；Stainless steel wire or iron wire be cleaned by ultrasonic be according to
Secondary use weak caustic solution（Concentration is the NaOH of 1.0 ~ 1.5 M, potassium hydroxide solution）, acetone, ultra-pure water cleaning.
Described strong acid solution is hydrochloric acid, sulfuric acid or the hydrofluoric acid solution of mass concentration 20% ~ 40%；Stainless steel wire or iron wire exist
In strong acid solution, etch period is 20 ~ 60 min, and etching temperature is 30 ~ 50 DEG C.
The described stainless steel wire or iron wire burning time in flame is 10 ~ 50 second；Wherein flame source is alcohol
Lamp, lighter or candle；There are flame core, internal flame or flame envelope in the position that flame put into by stainless steel wire or iron wire.
By Energy dispersive x-ray spectrometer（EDS）Data analysis shows, above-mentioned stainless steel wire or iron wire surface life
The product becoming is iron oxide.Scan sub micro- Electronic Speculum（SEM）Analysis shows, the nano-sized iron oxide of present invention preparation is in uniformly, causes
Close petal accordion, between 100 nm ~ 250 nm, the thickness of coating is between 1.2um ~ 1.4um for fold spacing.
Hinge structure of the present invention has advantages below：
1st, using wire as carrier, good mechanical stability and repeatability, energy are shown compared with vitreous silica fiber
Multiring aromatic hydrocarbon in extraction environmental sample（PAHs）, extraction efficiency height, stability is strong；
2nd, prepare nano-sized iron oxide coating with flame method, process is simple, strong operability, easily controllable；
3rd, preparation cost is cheap, efficiency high, environmental protection.
Brief description
Fig. 1 is the SEM figure of embodiment 1 products therefrom.
Fig. 2 is the SEM figure of embodiment 2 products therefrom.
Fig. 3 is the SEM figure of embodiment 3 products therefrom.
Fig. 4 is the SEM figure of embodiment 4 products therefrom.
Fig. 5 is the SEM figure of embodiment 4 products therefrom thickness.
Fig. 6 is the EDS figure of embodiment 4 products therefrom.
Specific embodiment
Make further below by the method that specific embodiment prepares petal accordion nano-sized iron oxide coating to the present invention
Explanation.
Embodiment 1
（1）Take the iron wire of one section of Φ=0.25 mm, be first cleaned by ultrasonic 20 min with 1.0 M sodium hydroxide solutions, then surpassed with acetone
Sound cleans 10 min, is finally cleaned by ultrasonic 10 min with ultra-pure water again；
（2）At 30 DEG C, in the sulfuric acid solution iron wire of cleaning being immersed mass concentration 30%, etch 60 min；Iron after etching
Silk ultrapure water, isolation air is dried, standby；
（3）Light lighter manually, etched iron wire one end is put into the flame core position of flame, burn 30 s, in iron wire table
Face is obtained nano-sized iron oxide；
（4）Iron wire will be obtained after burning uses ultra-pure water, methyl alcohol to rinse successively, and isolation air is dried, prepared uniform on iron wire surface
Petal accordion nano-sized iron oxide coating.
The SEM figure of the nano-sized iron oxide coating of above-mentioned preparation is shown in Fig. 1（The SEM figure that left figure is 20,000 times for multiplication factor, right
Figure is the SEM figure that multiplication factor is 50,000 times.）.Good surface shape is had by the nano-sized iron oxide coating that Fig. 1 can draw preparation
State, in petal fold-like structures, and coating is evenly distributed, and specific surface area is big.
Embodiment 2
（1）Take the iron wire of one section of Φ=0.35 mm, be first cleaned by ultrasonic 20 min with 1.2 M potassium hydroxide solutions, then surpassed with acetone
Sound cleans 15 min, is then cleaned by ultrasonic 10 min with ultra-pure water, isolation air is dried, standby；
（2）At 50 DEG C, in the hydrochloric acid solution stainless steel wire of cleaning being immersed mass concentration 30%, etch 30 min；After etching
Iron wire cleaned with ultra-pure water, isolation air be dried, standby；
（3）Light lighter manually, iron wire one end of etching processing is put into the internal flame position of flame, burn 20 s, in iron wire
Surface is obtained nano-sized iron oxide；
（4）Iron wire ultra-pure water after burning, methyl alcohol are rinsed respectively, isolation air is dried, be obtained on iron wire surface uniform
Petal accordion nano-sized iron oxide coating.
The above-mentioned SEM figure preparing nano-sized iron oxide coating is shown in Fig. 2（The SEM figure that left figure is 20,000 times for multiplication factor, right figure
The SEM figure being 50,000 times for multiplication factor.）.Good configuration of surface is had by the nano-sized iron oxide coating that Fig. 2 can draw preparation,
Structure petal accordion, and coating is evenly distributed, specific surface area is big.
Embodiment 3
（1）Take the iron wire of one section of Φ=0.35 mm, be first cleaned by ultrasonic 15 min with 1.5 M potassium hydroxide solutions, then surpassed with acetone
Sound cleans 15 min, is then cleaned by ultrasonic 15 min with ultra-pure water, isolation air is dried, standby；
（2）At 50 DEG C, in the hydrochloric acid solution stainless steel wire of cleaning being immersed mass concentration 30%, etch 30 min；After etching
Iron wire cleaned with ultra-pure water, isolation air be dried, standby；
（3）The internal flame position of the flame of alcolhol burner is put in iron wire one end of just etching, and burn 40 s, is obtained on iron wire surface and receives
Rice iron oxide；
（4）Iron wire ultra-pure water after burning, methyl alcohol are rinsed respectively, isolation air is dried, be obtained on iron wire surface uniform
Petal accordion nano-sized iron oxide coating.
The SEM figure of the nano-sized iron oxide coating of above-mentioned preparation is shown in Fig. 3（The SEM figure that left figure is 20,000 times for multiplication factor, right
Figure is the SEM figure that multiplication factor is 50,000 times.）.Good surface shape is had by the nano-sized iron oxide coating that Fig. 3 can draw preparation
State, structure petal accordion, and coating are evenly distributed, and specific surface area is big.
Embodiment 4
（1）Take the stainless steel wire of one section of Φ=0.25 mm, be first cleaned by ultrasonic 20 min with 1.0 M NaOH, then surpassed with acetone
Sound cleans 10 min, is finally cleaned by ultrasonic 10 min with ultra-pure water, isolation air is dried, standby；
（2）At 40 DEG C, in the hydrochloric acid solution stainless steel wire of cleaning being immersed mass concentration 40%, etch 60 min；After etching
Iron wire cleaned with ultra-pure water, isolation air be dried, standby；
（3）Flame envelope position in the candle flame lighted is put in stainless steel wire one end after etching, burn 10 s, in stainless steel wire
Surface is obtained nano-sized iron oxide；
（4）Iron wire ultra-pure water after burning, methyl alcohol are rinsed respectively, isolation air is dried, be obtained on iron wire surface uniform
Petal accordion nano-sized iron oxide coating.
The SEM figure of the nano-sized iron oxide coating of above-mentioned preparation is shown in Fig. 4（The SEM figure that left figure is 20,000 times for multiplication factor, right
Figure is the SEM figure that multiplication factor is 50,000 times.）.Can show that prepared nano-sized iron oxide coating has good surface by Fig. 4
Form, structure is in petal accordion, and coating is evenly distributed, and specific surface area is big.
Fig. 5 is the SEM figure of nano-sized iron oxide coating layer thickness prepared by above-described embodiment 4.Can be drawn by Fig. 5, above-mentioned institute
The thickness of the nano-sized iron oxide coating of preparation is between 1.2um ~ 1.4um.
Fig. 6 is the EDS figure of product prepared by above-described embodiment 4.Can show that prepared coating mainly contains iron by Fig. 6
Element, oxygen element.Table 1 is the gamma-spectrometric data of product prepared by embodiment 4.By table 1 quantitative analysis must tap a blast furnace and oxygen atomic ratio
For 2:3, therefore prepare is iron oxide.
Claims (9)
1. the preparation method of petal accordion nano-sized iron oxide coating, is to be cleaned by ultrasonic, completely cut off air stainless steel wire or iron wire
After drying, it is submerged initially in strong acid solution and performs etching, then stainless steel wire or iron wire ultrapure water after etching, will be obtained, isolation is empty
Gas is dried；It is subsequently placed in and puts into combustion oxidation in flame, obtain nano-sized iron oxide in stainless steel wire or iron wire surface；Finally will fire
Burn the stainless steel wire after oxidation or iron wire uses ultra-pure water, methyl alcohol to rinse successively, isolation air is dried, in stainless steel wire or iron wire table
Face obtains uniform petal accordion nano-sized iron oxide coating.
2. petal accordion nano-sized iron oxide coating as claimed in claim 1 preparation method it is characterised in that：Described stainless steel
The specification of silk or iron wire is Φ=0.15 ~ 0.45 mm.
3. petal accordion nano-sized iron oxide coating as claimed in claim 1 or 2 preparation method it is characterised in that：Stainless steel
Silk or iron wire are cleaned by ultrasonic for being cleaned with weak caustic solution, acetone, ultra-pure water successively.
4. petal accordion nano-sized iron oxide coating as claimed in claim 3 preparation method it is characterised in that：Described weak base
Solution is the NaOH of 1.0 ~ 1.5 M, potassium hydroxide solution for concentration.
5. petal accordion nano-sized iron oxide coating as claimed in claim 1 or 2 preparation method it is characterised in that：Described strong
Acid solution is hydrochloric acid, sulfuric acid or the hydrofluoric acid solution of mass concentration 20% ~ 40%.
6. petal accordion nano-sized iron oxide coating as claimed in claim 5 preparation method it is characterised in that：Described stainless steel
The silk or iron wire etch period in strong acid solution is 20 ~ 60 min, and etching temperature is 30 ~ 50 DEG C.
7. petal accordion nano-sized iron oxide coating as claimed in claim 1 or 2 preparation method it is characterised in that：Described not
The rust steel wire or iron wire burning time in flame is 10 ~ 50 s.
8. petal accordion nano-sized iron oxide coating as claimed in claim 7 preparation method it is characterised in that：Described flame source
For alcolhol burner, lighter or candle.
9. petal accordion nano-sized iron oxide coating as claimed in claim 8 preparation method it is characterised in that：Stainless steel wire or
The position that flame put into by iron wire is flame core, internal flame or flame envelope.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610816900.2A CN106381461B (en) | 2016-09-12 | 2016-09-12 | The preparation method of petal accordion nano-sized iron oxide coating |
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| CN201610816900.2A CN106381461B (en) | 2016-09-12 | 2016-09-12 | The preparation method of petal accordion nano-sized iron oxide coating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110735170A (en) * | 2019-10-23 | 2020-01-31 | 西北师范大学 | Preparation method of titanium dioxide nano thorn-shaped array fiber coatings |
| CN111423885A (en) * | 2020-05-08 | 2020-07-17 | 吉林大学 | Passivator for Cd and Pb pollution in farmland soil and preparation method and restoration method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817802A (en) * | 2006-01-10 | 2006-08-16 | 江苏天一超细金属粉末有限公司 | Production and producer for nanometer ferric oxide |
| US20060223052A1 (en) * | 2005-03-30 | 2006-10-05 | Kimberly-Clark Worldwide, Inc. | Technique for detecting microorganisms |
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2016
- 2016-09-12 CN CN201610816900.2A patent/CN106381461B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060223052A1 (en) * | 2005-03-30 | 2006-10-05 | Kimberly-Clark Worldwide, Inc. | Technique for detecting microorganisms |
| CN1817802A (en) * | 2006-01-10 | 2006-08-16 | 江苏天一超细金属粉末有限公司 | Production and producer for nanometer ferric oxide |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110735170A (en) * | 2019-10-23 | 2020-01-31 | 西北师范大学 | Preparation method of titanium dioxide nano thorn-shaped array fiber coatings |
| CN111423885A (en) * | 2020-05-08 | 2020-07-17 | 吉林大学 | Passivator for Cd and Pb pollution in farmland soil and preparation method and restoration method thereof |
| CN111423885B (en) * | 2020-05-08 | 2021-03-30 | 吉林大学 | Passivator for Cd and Pb pollution in farmland soil and preparation method and restoration method thereof |
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| CN106381461B (en) | 2018-11-02 |
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Effective date of registration: 20201231 Address after: No. 112-5, building 13, Tongyun Trade City, Guangling District, Yangzhou City, Jiangsu Province 225002 Patentee after: Yangzhou Oula Industrial Design Co.,Ltd. Address before: 730070 No. 967 Anning East Road, Anning District, Gansu, Lanzhou Patentee before: Northwest Normal University |
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