CN106381461B - The preparation method of petal accordion nano-sized iron oxide coating - Google Patents
The preparation method of petal accordion nano-sized iron oxide coating Download PDFInfo
- Publication number
- CN106381461B CN106381461B CN201610816900.2A CN201610816900A CN106381461B CN 106381461 B CN106381461 B CN 106381461B CN 201610816900 A CN201610816900 A CN 201610816900A CN 106381461 B CN106381461 B CN 106381461B
- Authority
- CN
- China
- Prior art keywords
- nano
- stainless steel
- iron oxide
- steel wire
- accordion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of petal accordion nano-sized iron oxide coating, it is after being air-dried stainless steel wire or iron wire ultrasonic cleaning, isolation, it is submerged initially in strong acid solution and performs etching, then stainless steel wire or iron wire ultrapure water will be obtained after etching, isolation is air-dried；It is subsequently placed in and is put into combustion oxidation in flame, nano-sized iron oxide is obtained in stainless steel wire or iron wire surface；Finally by after combustion oxidation stainless steel wire or iron wire use ultra-pure water, methanol to rinse successively, isolation is air-dried, and uniform petal accordion nano-sized iron oxide coating is obtained in stainless steel wire or iron wire surface.Its fold spacing of nano-sized iron oxide coating prepared by the present invention is 100 ~ 250 nm, and for the thickness of coating in 1.2 ~ 1.4um, structure is in petal accordion, and is evenly distributed；Large specific surface area, adsorption capacity is strong, is applied to extracting head coating material in solid phase micro-extraction technique, energy extracting polyaromatic hydrocarbon class, extraction efficiency is high, and stability is strong.
Description
Technical field
The present invention relates to a kind of preparations of nano-sized iron oxide coating more particularly to a kind of petal accordion nano-sized iron oxide to apply
The preparation of layer is applied in solid phase micro-extraction technique, belongs to mainly as the coating material of extracting head in solid phase micro-extraction technique
Field of nanometer material technology and environmental analysis field.
Background technology
In environmental analysis field, since the diversity, complexity and content of sample are very low, just needed to sample before analysis
Product carry out pre-treatment.And solid phase micro-extraction technique（Solid Phase Microextraction, SPME）With very high extraction
And accumulation ability, it quickly grew in recent years, since its unique advantage is widely used.But current solid phase is micro-
The shortcomings of it is mainly vitreous silica fiber to extract coating, and there are expensive, short life, poor stability.Thus, development efficiently,
Inexpensively, the coating material of long-life has very important research significance and application value.
The nano-sized iron oxide metal oxide important as one kind in nanometer new material, since its chemical property is stablized,
Catalytic activity is high, also has the characteristics that good light resistance and weatherability, catalyst, fine ceramics, coating, plastic products,
Magnetic material and bioengineering and medicine etc. have a wide range of applications value and development prospect, and nano-sized iron oxide also has
There is nontoxic, cheap characteristic, therefore study nano-sized iron oxide to have very important meaning.However nano-sized iron oxide is as solid phase
The application of micro-extraction coat layer is not yet reported.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of petal accordion nano-sized iron oxide coating, reduce fiber and apply
The manufacturing cost of layer, and improve stability and the service life of fiber coat.
The present invention prepares the preparation method of petal accordion nano-sized iron oxide coating, is that stainless steel wire or iron wire ultrasound is clear
After washing, completely cutting off and be air-dried, it is submerged initially in strong acid solution and performs etching, keep stainless steel wire or iron wire surface roughening, to increase
Specific surface area；Stainless steel wire or iron wire are obtained after etching again uses ultra-pure water, methanol to rinse successively, and isolation is air-dried；Then it sets
In being put into combustion oxidation in flame, nano-sized iron oxide is obtained in stainless steel wire or iron wire surface；Finally by after combustion oxidation not
Rust steel wire or iron wire use ultra-pure water, methanol to rinse successively, and isolation is air-dried, is obtained uniformly in stainless steel wire or iron wire surface
Petal accordion nano-sized iron oxide coating.
The specification of the stainless steel wire or iron wire is the mm of Φ=0.15 ~ 0.45；Stainless steel wire or iron wire be cleaned by ultrasonic for according to
It is secondary to use weak caustic solution（Sodium hydroxide, the potassium hydroxide solution of a concentration of 1.0 ~ 1.5 M）, acetone, ultra-pure water cleaning.
The 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
Etch period is 20 ~ 60 min in strong acid solution, and etching temperature is 30 ~ 50 DEG C.
The burning time of the stainless steel wire or iron wire 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 stainless steel wire or iron wire are put into flame.
Pass through Energy dispersive x-ray spectrometer（EDS）Data analysis shows above-mentioned to give birth on stainless steel wire or iron wire surface
At product be iron oxide.The micro- Electronic Speculum of scanning（SEM）Analysis shows nano-sized iron oxide prepared by the present invention is in uniform, cause
Close petal accordion, fold spacing is between the nm of 100 nm ~ 250, and the thickness of coating is between 1.2um ~ 1.4um.
The present invention has the following advantages compared with the prior art：
1, using wire as carrier, good mechanical stability is shown compared with vitreous silica fiber and is repeated
Property, multiring aromatic hydrocarbon in environmental sample can be extracted（PAHs）, extraction efficiency is high, and stability is strong；
2, nano-sized iron oxide coating is prepared with flame method, it is simple for process, strong operability, easily controllable；
3, manufacturing cost is cheap, efficient, environmentally protective.
Description of the drawings
Fig. 1 is the SEM figures of 1 products therefrom of embodiment.
Fig. 2 is the SEM figures of 2 products therefrom of embodiment.
Fig. 3 is the SEM figures of 3 products therefrom of embodiment.
Fig. 4 is the SEM figures of 4 products therefrom of embodiment.
Fig. 5 is the SEM figures of 4 products therefrom thickness of embodiment.
Fig. 6 is the EDS figures of 4 products therefrom of embodiment.
Specific implementation mode
Make below by the method that specific embodiment prepares petal accordion nano-sized iron oxide coating to the present invention further
Explanation.
Embodiment 1
（1）The iron wire of one section of mm of Φ=0.25 is taken, is first cleaned by ultrasonic 20 min with 1.0 M sodium hydroxide solutions, then with third
Ketone is cleaned by ultrasonic 10 min, is finally cleaned by ultrasonic 10 min with ultra-pure water again；
（2）At 30 DEG C, the iron wire of cleaning is immersed in the sulfuric acid solution of mass concentration 30% and etch 60 min；After etching
Iron wire ultrapure water, isolation is air-dried, spare；
（3）Lighter is lighted manually, etched iron wire one end is put into the flame core position of flame, burn 30 s, in iron
Nano-sized iron oxide is made in silk table face；
（4）Iron wire is obtained after burning uses ultra-pure water, methanol to rinse successively, and isolation is air-dried, and is made on iron wire surface
Even petal accordion nano-sized iron oxide coating.
The SEM figures of the nano-sized iron oxide coating of above-mentioned preparation are shown in Fig. 1（Left figure is the SEM figures that amplification factor is 20,000 times, right
Figure is the SEM figures that amplification factor is 50,000 times.）.It can show that the nano-sized iron oxide coating of preparation has good surface shape by Fig. 1
State is in petal fold-like structures, and coating is evenly distributed, large specific surface area.
Embodiment 2
（1）The iron wire of one section of mm of Φ=0.35 is taken, is first cleaned by ultrasonic 20 min with 1.2 M potassium hydroxide solutions, then with third
Ketone is cleaned by ultrasonic 15 min, is then cleaned by ultrasonic 10 min with ultra-pure water, isolation is air-dried, spare；
（2）At 50 DEG C, the stainless steel wire of cleaning is immersed in the hydrochloric acid solution of mass concentration 30% and etch 30 min；It carves
Iron wire after erosion is cleaned with ultra-pure water, and isolation is air-dried, spare；
（3）Lighter is lighted manually, iron wire one end of etching processing is put into the internal flame position of flame, burn 20 s,
Nano-sized iron oxide is made in iron wire surface；
（4）Iron wire after burning ultra-pure water, methanol are rinsed respectively, isolation is air-dried, and is made equal on iron wire surface
Even petal accordion nano-sized iron oxide coating.
The above-mentioned SEM figures for preparing nano-sized iron oxide coating are shown in Fig. 2（Left figure is the SEM figures that amplification factor is 20,000 times, right figure
The SEM figures for being 50,000 times for amplification factor.）.It can show that the nano-sized iron oxide coating of preparation has good configuration of surface by Fig. 2,
Structure petal accordion, and coating is evenly distributed, large specific surface area.
Embodiment 3
（1）The iron wire of one section of mm of Φ=0.35 is taken, is first cleaned by ultrasonic 15 min with 1.5 M potassium hydroxide solutions, then with third
Ketone is cleaned by ultrasonic 15 min, is then cleaned by ultrasonic 15 min with ultra-pure water, isolation is air-dried, spare；
（2）At 50 DEG C, the stainless steel wire of cleaning is immersed in the hydrochloric acid solution of mass concentration 30% and etch 30 min；It carves
Iron wire after erosion is cleaned with ultra-pure water, and isolation is air-dried, spare；
（3）Iron wire one end of etching will be put into the internal flame position of the flame of alcolhol burner, burn 40 s, in iron wire surface system
Obtain nano-sized iron oxide；
（4）Iron wire after burning ultra-pure water, methanol are rinsed respectively, isolation is air-dried, and is made equal on iron wire surface
Even petal accordion nano-sized iron oxide coating.
The SEM figures of the nano-sized iron oxide coating of above-mentioned preparation are shown in Fig. 3（Left figure is the SEM figures that amplification factor is 20,000 times, right
Figure is the SEM figures that amplification factor is 50,000 times.）.It can show that the nano-sized iron oxide coating of preparation has good surface shape by Fig. 3
State, structure petal accordion, and coating is evenly distributed, large specific surface area.
Embodiment 4
（1）The stainless steel wire of one section of mm of Φ=0.25 is taken, is first cleaned by ultrasonic 20 min with 1.0 M sodium hydroxides, then with third
Ketone is cleaned by ultrasonic 10 min, is finally cleaned by ultrasonic 10 min with ultra-pure water, isolation is air-dried, spare；
（2）At 40 DEG C, the stainless steel wire of cleaning is immersed in the hydrochloric acid solution of mass concentration 40% and etch 60 min；It carves
Iron wire after erosion is cleaned with ultra-pure water, and isolation is air-dried, spare；
（3）Stainless steel wire one end after etching is put into flame envelope position in the candle flame lighted, burn 10 s, stainless
Nano-sized iron oxide is made in steel wire surface；
（4）Iron wire after burning ultra-pure water, methanol are rinsed respectively, isolation is air-dried, and is made equal on iron wire surface
Even petal accordion nano-sized iron oxide coating.
The SEM figures of the nano-sized iron oxide coating of above-mentioned preparation are shown in Fig. 4（Left figure is the SEM figures that amplification factor is 20,000 times, right
Figure is the SEM figures that amplification factor is 50,000 times.）.It 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, large specific surface area.
Fig. 5 is the SEM figures of nano-sized iron oxide coating layer thickness prepared by above-described embodiment 4.It can be obtained 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 figures of product prepared by above-described embodiment 4.It 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.The atomic ratio that must be tapped a blast furnace with oxygen by 1 quantitative analysis of table
It is 2:3, therefore what is be prepared is iron oxide.
Claims (6)
1. the preparation method of petal accordion nano-sized iron oxide coating, it is cleaned by ultrasonic stainless steel wire, after isolation is air-dried,
It is submerged initially in strong acid solution and performs etching, then by the stainless steel wire ultrapure water after etching, isolation is air-dried；Then it sets
In being put into combustion oxidation in flame, nano-sized iron oxide is obtained on stainless steel wire surface；Finally by the stainless steel wire after combustion oxidation
Ultra-pure water, methanol is used to rinse successively, isolation is air-dried, and it is nano oxidized to obtain uniform petal accordion on stainless steel wire surface
Iron coating；
The specification of the stainless steel wire is the mm of Φ=0.15 ~ 0.45；
The strong acid solution is hydrochloric acid, sulfuric acid or the hydrofluoric acid solution of mass concentration 20% ~ 40%；
Etch period of the stainless steel wire in strong acid solution is 20 ~ 60 min, and etching temperature is 30 ~ 50 DEG C.
2. the preparation method of petal accordion nano-sized iron oxide coating as described in claim 1, it is characterised in that：Stainless steel wire is super
Sound cleaning is to be cleaned successively with aqueous slkali, acetone, ultra-pure water.
3. the preparation method of petal accordion nano-sized iron oxide coating as claimed in claim 2, it is characterised in that：The aqueous slkali
For sodium hydroxide, the potassium hydroxide solution of a concentration of 1.0 ~ 1.5 M.
4. the preparation method of petal accordion nano-sized iron oxide coating as described in claim 1, it is characterised in that：The stainless steel
Burning time of the silk in flame is 10 ~ 50 s.
5. the preparation method of petal accordion nano-sized iron oxide coating as claimed in claim 4, it is characterised in that：The flame source
For alcolhol burner, lighter or candle.
6. the preparation method of petal accordion nano-sized iron oxide coating as claimed in claim 5, it is characterised in that：Stainless steel wire is put
The position for entering flame is flame core, internal flame or flame envelope.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610816900.2A CN106381461B (en) | 2016-09-12 | 2016-09-12 | The preparation method of petal accordion nano-sized iron oxide coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610816900.2A CN106381461B (en) | 2016-09-12 | 2016-09-12 | The preparation method of petal accordion nano-sized iron oxide coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106381461A CN106381461A (en) | 2017-02-08 |
| CN106381461B true CN106381461B (en) | 2018-11-02 |
Family
ID=57935633
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610816900.2A Active CN106381461B (en) | 2016-09-12 | 2016-09-12 | The preparation method of petal accordion nano-sized iron oxide coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106381461B (en) |
Families Citing this family (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 |
| 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 |
Citations (1)
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060223052A1 (en) * | 2005-03-30 | 2006-10-05 | Kimberly-Clark Worldwide, Inc. | Technique for detecting microorganisms |
-
2016
- 2016-09-12 CN CN201610816900.2A patent/CN106381461B/en active Active
Patent Citations (1)
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106381461A (en) | 2017-02-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106381461B (en) | The preparation method of petal accordion nano-sized iron oxide coating | |
| JP6666438B2 (en) | Manufacturing method of local back contact solar cell | |
| CN102908908B (en) | Method for modifying modified ceramic microfiltration membrane by adopting graphite oxide | |
| CN102343352B (en) | Recovery method for solar silicon slice | |
| CN103394484B (en) | Cleaning after polysilicon solar cell silicon chip processed with acid floss | |
| CN105226112A (en) | A kind of preparation method of efficient crystal silicon solar batteries | |
| CN104261392B (en) | A kind of preparation method of the conductive graphene paper of borate ion crosslinking | |
| CN101409313A (en) | Method for preparing silicon solar battery pile face in magnetic field | |
| CN103613093B (en) | A kind of hydrogen reducing prepares the method for Graphene | |
| CN106373862A (en) | Processing method applicable to wet cleaning of heterojunction cell | |
| CN103337560A (en) | Preparation method of three-dimensional silicon nano structure for solar cell | |
| CN102383164A (en) | Titanium dioxide nano-honeycomb nested nanowire array film and preparation method thereof | |
| CN102009976A (en) | Method for preparing graphene film | |
| CN102703903A (en) | Alkali texture making technology | |
| CN109108524B (en) | Diamond-nano silver soldering paste heat conduction material and preparation method thereof | |
| CN104599949A (en) | Processing method of deep etching smooth surface based on SiC substrate slice | |
| CN100552986C (en) | The method of preparing polysilicon solar battery suede in magnetic field | |
| CN103014875A (en) | Method for treating synthetic sapphire wafer | |
| CN101319388A (en) | Preparation method of multicenter zinc aluminate nanometer pipe | |
| CN108821269B (en) | Preparation method of porous graphene | |
| CN106835077A (en) | A kind of preparation method of the porous Au coatings for suppressing Multipactor | |
| CN106282903B (en) | The technique that flame method prepares lumpy nanometer iron oxide coatings | |
| CN112758912A (en) | Method for preparing porous carbon material by non-noble metal auxiliary chemical etching | |
| CN108269884B (en) | A kind of preparation method of Buddha's warrior attendant wire cutting polycrystalline silicon solar battery suede | |
| CN103879995B (en) | The preparation method of carbon nanometer wall powder and the preparation method of graphene nanobelt |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
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 |
|
| TR01 | Transfer of patent right |