CN109055928A - A kind of high distortion structure black nano titania coating and preparation method thereof - Google Patents
A kind of high distortion structure black nano titania coating and preparation method thereof Download PDFInfo
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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
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Abstract
A kind of high distortion structure black nano titania coating and preparation method thereof, object are mutually Rutile Type, and particle has high distortion inner core, and form is coated in the coating on matrix；The preparation method comprises the following steps: sheet metal is fixed on ball milling pot bottom by (1), it is put into abrading-ball and titanium dioxide powder；(2) it is filled with inert gas air is discharged, or vacuumizes, then put shake ball mill with three-dimensional and carry out ball milling, obtain high distortion structure black nano titania coating in matrix surface deposition.Method raw material of the invention is easy to get；Ordinary titanium dioxide light abstraction width can be extended near infrared region by simple process, but significant effect, product, and narrow particle size distribution, ingredient is pure, preparation process no pollution to the environment, it is easy to accomplish industrialization.
Description
Technical field
The invention belongs to catalysis material technical field, in particular to a kind of high distortion structure black nano titania coating
And preparation method thereof.
Background technique
In numerous semiconductor light-catalysts, titanium oxide is due to cheap, abundance, biological nontoxic, chemically
The advantages that matter is stable, redox ability is strong, it is considered to be one of most potential semiconductor light-catalyst is widely used in ring
The various fields such as border pollution control, solar battery, antibiotic self-cleaning material, cosmetics sun-screening agent；However, titanium oxide band gap is big
In 3.0eV, corresponding light absorption wavelength range is narrow, can only absorbing wavelength be less than the ultraviolet light of 387nm, and cannot be to accounting for the sun
The visible light part of light about 50% makes full use of.In addition, titania photocatalyst is usually to be existed in solution with suspension system
It is reacted, but suspended particles will affect the radiation depth of absorption and the illumination of light, and suspended particulate is in aqueous solution
Easily cohesion, recycles difficulty after reaction, various unfavorable factors limit the practical application of titanium oxide suspension system；How oxidation is improved
Titanium, in order to recycle, reuse, just becomes titanium oxide research field in visible range absorbability, and being fixed
Hot issue.
For the low problem of visible light utilization efficiency, other ion pair titanium oxide are generallyd use at present and are doped modification, with drop
Low band gaps width；And titanium oxide auto-dope technology is different from conventional ion doping, particular by reduction mode by particle surface
Ti4+It is reduced into Ti3+, do not change the chemical component of particle but；It can be simultaneously to titanium oxide valence band, conduction band energy by auto-dope method
Grade carries out controllable adjustment, band gap width is reduced, to improve it to visible light utilization efficiency；Chen in 2011 etc. is reported for the first time to be passed through
High-pressure hydrogenation reduction method prepare auto-dope titanium oxide, and by Germicidal efficacy discovery with processing the time extension, titanium oxide color by
Gradually by leucismus depth, black nano titanium oxide is finally obtained；The various black nano titanium oxide preparation methods reported after this are all
It is similar, it is by chemical method by titan oxide particles surface Ti4+It is reduced into Ti3+, to reach auto-dope purpose；But change
Method complex process, low yield, product quality are also difficult to keep stable, further apply to limit it.
In conclusion black nano titanium oxide can be significantly improved to can be by the utilization rate of light, but it is limited to production technology
Complexity problem is difficult to be used widely；In addition, similar to common titanium oxide, black nano titanium oxide, which similarly faces, to be difficult to
Recycling, recycling problem.How to find that a kind of simple process, yield be high, method of stable product quality prepares black nano
Titanium oxide, and carrier surface is fixed in reach recycling, recycling effect, just become the main of current titanium oxide research
Project.
Summary of the invention
For doping vario-property nano-titanium oxide in the above problem present on technology of preparing, the present invention provides a kind of high distortion
Structure black nano titania coating is by preparation method, and by using surface mechanical attrition treatment mode, black is made in a step
Nano-titanium oxide is simultaneously fixed on matrix.
For high distortion structure black nano titania coating thickness of the invention at 20~50 μm, microcosmic group becomes diameter 10
The particle of~20nm, appearance of coat are black, and object is mutually Rutile Type, and particle has amorphous shell and high distortion inner core.
The purity of above-mentioned high distortion structure black nano titania coating is 99.9% or more.
The matrix of above-mentioned high distortion structure black nano titania coating attachment is sheet metal or abrading-ball, the material of matrix
For pure metal or alloy；The pure metal is titanium, aluminium, magnesium or iron, and purity >=99.9%, the alloy is titanium alloy, aluminium
Alloy, magnesium alloy or steel.
The preparation method of high distortion structure black nano titania coating of the invention the following steps are included:
1, sheet metal is fixed on ball milling pot bottom, then abrading-ball is placed in ball grinder, then titanium dioxide powder is placed in
In ball grinder and cover sheet metal；The sheet metal material be pure metal or alloy, the pure metal be titanium, aluminium or iron,
Purity >=99.9%, the alloy are titanium, aluminium alloy or steel；The titanium dioxide powder be Anatase titanium dioxide powder,
The mixture of rutile type titanium dioxide powder or both；
2, it is filled with inert gas into ball grinder air is discharged, or being evacuated to gauge pressure is -0.08MPa hereinafter, then
Ball grinder is mounted on three-dimensional pendulum shake ball mill, starts three-dimensional pendulum shake ball mill and ball milling is carried out to titanium dioxide powder, control ball
Revolving speed is ground in 300~3500rpm, 15~300min of Ball-milling Time after ball milling, obtains high distortion structure on sheet metal surface
Black nano titania coating.
In the above method, the material selection pure metal or alloy of abrading-ball, after ball milling, abrading-ball surface obtains high distortion knot
Structure black nano titania coating.
The above-mentioned preferred titanium alloy of ball grinder material.
The granularity of above-mentioned titanium dioxide powder is 10~220nm, and purity is greater than 99.9%.
Above-mentioned abrading-ball selects 3.5~10mm of diameter.
In above-mentioned step 1, the total volume of abrading-ball and titanium oxide powder in ball grinder accounts for the 1/2~1/ of ball grinder total measurement (volume)
5。
In above-mentioned step 1, the mass ratio of abrading-ball and titanium oxide powder in ball grinder is (10~80): 1.
Above-mentioned inert gas selects argon gas.
The principle of the present invention is: under height anaerobic condition, by the three-dimensional driving effect for putting shake ball mill, making ball grinder
Three-dimensional impact occurs for interior abrading-ball, and it is abnormal to generate high lattice inside the titan oxide particles that collision process can be mingled between abrading-ball
Become, while titan oxide particles outermost layer lattice can be ground into disordering, i.e. amorphous state by the three-dimensional rubbing action of sphere；This
In the high distortion structure refer to that lattice of nuclei high distortion in titan oxide particles, the amorphous shell refer to titan oxide particles
Outermost layer lattice highly disorderedization.
Compared with prior art, the present invention having the following advantages that and protruding effect: it is raw materials used sold by market it is common
Titanium dioxide, it is cheap and easy to get；Equipment used is cheap, simple process, but significant effect, can be by ordinary titanium dioxide light absorption model
It encloses and extends near infrared region；The high visible of preparation responds black nano titanium oxide powder narrow particle size distribution, and ingredient is pure, preparation
Process no pollution to the environment, it is easy to accomplish industrialization.
Detailed description of the invention
Fig. 1 is that titanium metal plate and surface are attached with high distortion structure black nano titania coating in the embodiment of the present invention 1
Titanium metal plate appearance photo figure；In figure, (a) is titanium metal plate, (b) is fixed with high distortion structure black nano oxidation for surface
The titanium metal plate of titanium coating；
Fig. 2 is the titanium metal plate X of the high distortion structure black nano titania coating coating front and back of the embodiment of the present invention 1
Ray diffraction spectra comparison diagram；In figure, ● it be the diffraction maximum , ﹡ of titanium is the diffraction maximum of rutile type titanium oxide；
Fig. 3 is the transmitted electron of the made high distortion structure black nano titania coating composition powder of the embodiment of the present invention 1
Microscope photo figure；In figure, left figure is low power, and right figure is high power；
Fig. 4 is the X-ray photoelectricity of the made high distortion structure black nano titania coating composition powder of the embodiment of the present invention 1
Sub- spectrogram；In figure, ● it is the high distortion structure black nano titanium oxide of powder, ▼ is raw material titanium dioxide powder；
Fig. 5 is the electron paramagnetic of the made high distortion structure black nano titania coating composition powder of the embodiment of the present invention 1
Resonance detection figure；In figure, ● it is the high distortion structure black nano titanium oxide of powder, ▼ is raw material titanium dioxide powder；
Fig. 6 is that different catalysts carry out rhodamine B solution degradation trial curve figure in the embodiment of the present invention 1；In figure, ■
For without using catalyst, ▼ is to use raw material titanium dioxide powder as degradation catalyst, ▲ it is to be fixed with high distortion using surface
The titanium metal plate of structure black nano titania coating is as degradation catalyst；
Fig. 7 is the high distortion structure black nano titania coating composition powder and original of powder in the embodiment of the present invention 1
Expect visible spectrum wavelength-absorption intensity curve graph of titanium dioxide powder；In figure, ● it is the high distortion structure black nano oxygen of powder
Change titanium, ▼ is raw material titanium dioxide powder.
Specific embodiment
The following examples are a further detailed description of the invention.
The high distortion structure black nano titania coating prepared in the embodiment of the present invention carries out structure by the following means
Characterization: using X ' the Pert Pro PW3040/60 type X-ray diffractometer of PANalytical company of Holland production to product object phase
It is characterized；The TECNNAI G produced using FEI Co. of the U.S.220 type transmission electron microscopes carry out product microscopic appearance
Observation；Being combined using the x-ray photoelectron spectrometer of U.S. Thermo VG production to product Ti2p orbital electron can be carried out test.
Ball milling 60~the 100mL of tank volume, 50~65mm of internal diameter used in the embodiment of the present invention.
Sheet metal 50~the 60mm of diameter, 0.5~7.8mm of thickness used in the embodiment of the present invention.
The Anatase titanium dioxide powder used in the embodiment of the present invention is Shandong Linyi You Suo Chemical Industry Science Co., Ltd
Product, or be the Anatase titanium dioxide powder into the production of Nanjing titanium white Chemical Co., Ltd..
The R-902 micron order that the rutile type titanium dioxide powder used in the embodiment of the present invention produces for DuPont Corporation
Rutile type titanium dioxide powder.
The three-dimensional pendulum shake ball mill used in the embodiment of the present invention is the production of Hefei ,Anhui Ke Jing Materials Technology Ltd.
MSK-SFM-3 type three-dimensional pendulum shake ball mill, or be SPEX-8000M type ball mill.
The abrading-ball used in the embodiment of the present invention is the titanium alloy ball of Baoji Chuan Xin metal material Co., Ltd.
The argon gas-sealed tank body for being 99.99% with purity after ball grinder charging in the embodiment of the present invention.
Raw material partial size after ball milling is constant in the embodiment of the present invention.
Material quality of grinding balls selects TC4 titanium alloy ball in the embodiment of the present invention.
Ball grinder is fixed in ball mill by fixture in the embodiment of the present invention, and the operating rate of fixture is 400~1750
Secondary/min.
The following are the preferred embodiment of the present invention.
Embodiment 1
Sheet metal is fixed on ball milling pot bottom, then abrading-ball is placed in ball grinder；The TC4 titanium that abrading-ball is Φ 10mm closes
Gold；Titanium dioxide powder is placed in ball grinder again and covers sheet metal；Sheet metal is the TA2 titanium sheet of Φ 50mm × 3mm；Titanium oxide
Powder is Anatase titanium dioxide powder；Ball grinder material is TC4 titanium alloy；The granularity of titanium dioxide powder is 35nm, and purity is big
In 99.9%；The total volume of abrading-ball and titanium oxide powder in ball grinder accounts for the 1/3 of ball grinder total measurement (volume)；Abrading-ball in ball grinder and
The mass ratio of titanium oxide powder is 50:1；
It is filled with argon gas into ball grinder air is discharged, then ball grinder is mounted on ball mill, starts ball mill pair
Titanium dioxide powder carries out ball milling, and control drum's speed of rotation is in 1000rpm, Ball-milling Time 100min, after ball milling, in sheet metal
And abrading-ball surface can obtain high distortion structure black nano titania coating simultaneously；25 μm of coating layer thickness；
After being coated with the sheet metal taking-up of high distortion structure black nano titania coating, remaining material in ball grinder
Abrading-ball is screened out, then powder is immersed in dehydrated alcohol, then applies ultrasonic wave and carries out Ultrasonic Pulverization 1h, further take out and use hole
The hydrophilic filter membrane that 0.22 μm of diameter filter out partial size be greater than 220nm part, surplus material after organic solvent volatilization after, obtain with
Made high distortion structure black nano titania coating forms the identical titanium oxide powder of powder, and (i.e. the high distortion structure of powder is black
Color nano-titanium oxide), kernel is high distortion structure, and shell is amorphous state；Wherein the frequency of ultrasonic wave is 20kHz, using JY92-
IIDN ultrasonic cell disruptor；
Titanium metal plate and the titanium metal plate appearance photo such as Fig. 1 institute for being deposited with high distortion structure black nano titania coating
Show；
The ray diffraction spectra of the titanium metal plate X of high distortion structure black nano titania coating coating front and back is as shown in Figure 2；
The transmission electron microscope photo of high distortion structure black nano titania coating composition powder as shown in figure 3, from
Fig. 3 visual hull is amorphous (in two white dashed lines of right figure), and kernel is high distortion structure (right figure lower section white dashed line arrow
It is signified)；
The x-ray photoelectron spectroscopy of high distortion structure black nano titania coating composition powder and raw material titanium dioxide powder
Figure is as shown in Figure 4；
The electron paramagnetic resonance of high distortion structure black nano titania coating composition powder and raw material titanium dioxide powder
Testing result is as shown in figure 5, wherein high distortion structure black nano titania coating composition powder has obvious Ti3+Resonance effects；
The visible spectrum wavelength-of high distortion structure black nano titania coating composition powder and raw material titanium dioxide powder
Absorption intensity curve is as shown in Figure 7；
High distortion structure black nano titania coating and the comparison of raw material titanium oxide are carried out to the degradation of rhodamine B solution
Test, testing program are as follows:
The 100mL rhodamine B solution of concentration 10mg/L is respectively placed in two 150mL quartz curettes, and with it is ultraviolet-can
See that spectrophotometer tests the absorbance C of solution at this time0；
20mg raw material titanium oxide and high distortion structure black nano titania coating titanium sheet is taken to be added separately to two quartz
In cup, marking cup body respectively is A and B；
Two quartz curettes are respectively placed under 30W xenon light etc., starts timing, is sampled every 1h and use UV-vis spectroscopy
Photometer tests its absorbance, is recorded as CA1、CA2、…CA5、CB1、CB2、…CB5, the sample solution after test is all refunded every time
In former quartz curette；
Absorption intensity-time graph is drawn according to each absorbance data as shown in fig. 6, high distortion structure black nano aoxidizes
The photocatalytic degradation capability of titanium coating titanium sheet is at least 2~3 times of raw material titanium oxide powder.
Embodiment 2
With embodiment 1, difference is method:
(1) sheet metal is the 42CrMo steel disc of Φ 50mm × 0.5mm；The granularity of titanium dioxide powder is 30nm；In ball grinder
Abrading-ball and the total volume of titanium oxide powder account for the 1/2 of ball grinder total measurement (volume)；The mass ratio of abrading-ball and titanium oxide powder in ball grinder
For 10:1；Titanium dioxide powder is rutile type titanium dioxide powder；Ball radius 10mm；
(2) drum's speed of rotation is in 1200rpm；
(3) it is -0.08MPa hereinafter, rotational speed of ball-mill is in 300rpm, Ball-milling Time 300min that ball grinder, which is evacuated to gauge pressure,；
(4) 50 μm of coating layer thickness.
Embodiment 3
With embodiment 1, difference is method:
(1) sheet metal material is the technical pure iron plate of Φ 60mm × 3.5mm；The granularity of titanium dioxide powder is 220nm；Ball milling
The total volume of abrading-ball and titanium oxide powder in tank accounts for the 1/5 of ball grinder total measurement (volume)；The matter of abrading-ball and titanium oxide powder in ball grinder
Amount is than being 80:1；Titanium dioxide powder is the equal mass mixings object of Anatase titanium dioxide powder and rutile type titanium dioxide powder；
Ball radius 3.5mm；
(2) drum's speed of rotation is in 3500rpm；Ball-milling Time 15min；
(3) 20 μm of coating layer thickness.
Embodiment 4
With embodiment 1, difference is method:
(1) sheet metal is the technical pure aluminium flake of Φ 60mm × 7.8mm；The granularity of titanium dioxide powder is 60nm；In ball grinder
Abrading-ball and the total volume of titanium oxide powder account for the 1/4 of ball grinder total measurement (volume)；The mass ratio of abrading-ball and titanium oxide powder in ball grinder
For 40:1；Titanium dioxide powder is the mixture of Anatase titanium dioxide powder and rutile type titanium dioxide powder mass ratio 1:3；Mill
Bulb diameter 4mm；
(2) it is -0.08MPa hereinafter, drum's speed of rotation is in 2000rpm, Ball-milling Time that ball grinder, which is evacuated to gauge pressure,
30min；
(3) 29 μm of coating layer thickness.
Embodiment 5
With embodiment 1, difference is method:
(1) sheet metal is the TC4 titanium alloy piece of Φ 50mm × 3mm；The granularity of titanium dioxide powder is 80nm；In ball grinder
The total volume of abrading-ball and titanium oxide powder accounts for the 1/4 of ball grinder total measurement (volume)；The mass ratio of abrading-ball and titanium oxide powder in ball grinder is
60:1；Titanium dioxide powder is the mixture of Anatase titanium dioxide powder and rutile type titanium dioxide powder mass ratio 3:1；Abrading-ball
Diameter 5mm；
(2) drum's speed of rotation is in 800rpm；Ball-milling Time 220min；
(3) 42 μm of coating layer thickness.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention are limited by appended claims and its coordinate.
Claims (10)
1. a kind of high distortion structure black nano titania coating, it is characterised in that thickness becomes in 20~50 μm, microcosmic group
The particle of 10~20nm of diameter, appearance of coat are black, and object is mutually Rutile Type, and particle has amorphous shell and high distortion kernel
Structure.
2. a kind of high distortion structure black nano titania coating according to claim 1, it is characterised in that purity
99.9% or more.
3. a kind of high distortion structure black nano titania coating according to claim 1, it is characterised in that coating attachment
Matrix be sheet metal or abrading-ball, the material of matrix is pure metal or alloy；The pure metal is titanium, aluminium, magnesium or iron, purity
>=99.9%, the alloy is titanium alloy, aluminium alloy, magnesium alloy or steel.
4. a kind of preparation method of high distortion structure black nano titania coating described in claim 1, it is characterised in that packet
Include following steps:
(1) sheet metal is fixed on ball milling pot bottom, then abrading-ball is placed in ball grinder, then titanium dioxide powder is placed in ball milling
In tank and cover sheet metal；The sheet metal material be pure metal or alloy, the pure metal be titanium, aluminium, magnesium or iron, it is pure
Degree >=99.9%, the alloy are titanium alloy, aluminium alloy, magnesium alloy or steel；The titanium dioxide powder is Anatase oxygen
Change the mixture of titanium powder, rutile type titanium dioxide powder or both；
(2) it is filled with inert gas into ball grinder air is discharged, or being evacuated to gauge pressure is -0.08MPa hereinafter, then by ball
Grinding jar is mounted on three-dimensional pendulum shake ball mill, is started three-dimensional pendulum shake ball mill and is carried out ball milling to titanium dioxide powder, control ball milling turns
Speed is in 800~3500rpm, 15~300min of Ball-milling Time, after ball milling, obtains high distortion structure black on sheet metal surface
Nano-titanium oxide coating layer.
5. the preparation method of high distortion structure black nano titania coating according to claim 4, it is characterised in that institute
The material selection pure metal or alloy for the abrading-ball stated, after ball milling, abrading-ball surface obtains high distortion structure black nano oxidation
Titanium coating.
6. the preparation method of high distortion structure black nano titania coating according to claim 4, it is characterised in that institute
The granularity for the titanium dioxide powder stated is 10~220nm, and purity is greater than 99.9%.
7. the preparation method of high distortion structure black nano titania coating according to claim 4, it is characterised in that institute
The abrading-ball stated selects 3.5~10mm of diameter.
8. the preparation method of high distortion structure black nano titania coating according to claim 4, it is characterised in that step
Suddenly the total volume of the abrading-ball in (1) in ball grinder and titanium oxide powder accounts for the 1/2~1/5 of ball grinder total measurement (volume).
9. the preparation method of high distortion structure black nano titania coating according to claim 3, it is characterised in that step
Suddenly the mass ratio of the abrading-ball in (1) in ball grinder and titanium oxide powder is (10~80): 1.
10. the preparation method of high distortion structure black nano titania coating according to claim 3, it is characterised in that institute
The inert gas stated selects argon gas.
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| CN114606593A (en) * | 2022-02-16 | 2022-06-10 | 河北科技大学 | Preparation method of flaky carbonyl iron powder polypropylene flat flexible wave absorbing wire |
| CN115650285A (en) * | 2022-10-05 | 2023-01-31 | 复旦大学 | Mechanochemical method for quickly preparing rutile type titanium dioxide powder |
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| CN115650285A (en) * | 2022-10-05 | 2023-01-31 | 复旦大学 | Mechanochemical method for quickly preparing rutile type titanium dioxide powder |
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