CN104525170A - Preparation method of titanium-dioxide powder with exposure of high-crystalline surface energy and spindle structure - Google Patents
Preparation method of titanium-dioxide powder with exposure of high-crystalline surface energy and spindle structure Download PDFInfo
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- CN104525170A CN104525170A CN201510022837.0A CN201510022837A CN104525170A CN 104525170 A CN104525170 A CN 104525170A CN 201510022837 A CN201510022837 A CN 201510022837A CN 104525170 A CN104525170 A CN 104525170A
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Abstract
The invention discloses a preparation method of exposure of a titanium-dioxide powder with high-crystalline surface energy and a spindle structure. The preparation method comprises the following steps: preparing a Ti-Cu-Pd amorphous alloy, carrying out ultrasonic treatment on a Ti-Cu-Pd amorphous alloy strip in absolute ethyl alcohol for 5 minutes, then cleaning with deionized water and putting in a drying box for drying; and putting into a sealed container containing corrosive liquid for carrying out reaction to obtain a product, washing the sample prepared after the reaction is finished by using the deionized water, and drying in the drying box to obtain the titanium-dioxide powder with the exposure of the high-crystalline surface energy and the spindle structure. The titanium-dioxide powder with the surface exposure of the high-crystalline surface energy (001) and the spindle structure, prepared by adopting the preparation method, is uniform in structure, and has the high specific surface area; and the high surface-exposed rate of the high-crystalline surface energy (001) is beneficial to improving the catalytic activity, and a catalyst with the titanium-dioxide powder has the good dyestuff degrading performance; and the preparation method is simple, the preparation condition and obtained products are easily controlled, and the preparation method is a high-efficiency and economic preparation method.
Description
Technical field
The present invention relates to a kind of preparation method with the titanium dioxide powder of the spindle structure that high crystal face can expose, particularly relate to a kind of nano porous titanium dioxide raw powder's production technology being applied to the high catalytic activity of catalytic field.
Background technology
Nanometer titanic oxide material has the special character such as stable chemical nature, nontoxic non-secondary pollution, abundance and has huge society and the benefit of economy in fields such as environmental protection, new energy development, biomedicines.Current available titanium dioxide nanostructure mainly contains nano particle, nanometer rods, nano wire, nanotube and nano flower, nanoporous etc.Its synthetic method is also various, as chemical deposition, hydro-thermal method, sol-gal process, de-alloyage and template etc.But himself also also exist that forbidden band is wider utilizes low and that electron-hole recombination rate high quantum production rate is low defect to solar energy, these defects strongly limit the application of nano titanium oxide in actual production, optically catalytic TiO 2 is made to meet the production demand that utilize extensive with life in order to overcome these problems, we need on the basis of previous work, and exploitation has the new multistage nanometer titanic oxide material of more excellent photocatalysis performance.
The surface energy of each crystal face varies in size, and therefore presents difformity, exposes different crystal faces, causes the difference of its catalytic activity, and the titanium dioxide in general exposing more high surface energy crystal face has good catalytic activity.But the crystal face with high surface energy easily disappears in crystal growing process, it is more low more stable that crystal growth always tends to stable process capability, and therefore how improving the ratio that the higher crystal face of surface energy exposes also is probe into nano-titanium dioxide modified important way.The preparation method of nano porous metal material has a variety of, de-alloyage prepares nano-porous materials, and to have technique simple, the manageable advantage of process, and obtained nano-material surface is even, greatly thus specific area becomes Application comparison one of method widely in recent years.But de-alloyage requires higher to virgin alloy materials microstructure and homogeneity of ingredients, and Ti alloy system has the intermetallic compound of Various Complex structure.
Summary of the invention
For prior art Problems existing, the invention provides a kind of spindle structure titanium dioxide raw powder's production technology that there is high crystal face and can expose, with Ti-Cu-Pd non-crystaline amorphous metal and red fuming nitric acid (RFNA) for raw material, the titanium dioxide powder that alloyage preparation has the spindle structure that high crystal face can expose is taken off by chemistry, the cost of this preparation method is lower, whole course of reaction is easy to operation, and reaction condition easily realizes.Gained spindle structure titanium dioxide powder has good photocatalysis performance.
In order to solve the problems of the technologies described above, a kind of spindle structure titanium dioxide raw powder's production technology having high crystal face and can expose that the present invention proposes, comprises the following steps:
Step one, prepare Ti-Cu-Pd non-crystaline amorphous metal according to following component and atom percentage content, wherein: the content of the content of Ti to be the content of 20%-40%, Cu be 60%-70%, Pd is 0%-10%;
Step 2, Ti-Cu-Pd non-crystaline amorphous metal obtained for step one is cut into thickness is 10 μm-30 μm, and width is 3mm-5mm, and length is the Ti-Cu-Pd AMORPHOUS ALLOY RIBBONS of 20-30mm; This Ti-Cu-Pd AMORPHOUS ALLOY RIBBONS is dry in drying box by washed with de-ionized water juxtaposition after ultrasonic 5min in absolute ethyl alcohol;
Step 3, the Ti-Cu-Pd AMORPHOUS ALLOY RIBBONS of step 2 gained is put into the closed container filling corrosive liquid react, the concentrated nitric acid solution of described corrosive liquid to be molar concentration be 13-15mol/L; Reaction temperature is 50-90 DEG C, and the reaction time is 30-70h, reaction is terminated rear obtained sample deionized water rinsing, and in drying box, is the spindle structure titanium dioxide powder having high crystal face and can expose after drying.
Further, in the step one of above-mentioned preparation method, in Ti-Cu-Pd non-crystaline amorphous metal each component atom percentage content have one of following several situation:
(1) content of the content of Ti to be the content of 30%, Cu be 60%, Pd is 10%;
(2) content of the content of Ti to be the content of 30%, Cu be 62%, Pd is 8%;
(3) content of the content of Ti to be the content of 30%, Cu be 64%, Pd is 6%;
(4) content of the content of Ti to be the content of 30%, Cu be 66%, Pd is 4%.
Process conditions in the step 3 of above-mentioned preparation method have one of following several situation:
(1) molar concentration of described corrosive liquid red fuming nitric acid (RFNA) is 14.8mol/L, and reaction temperature is 50 DEG C, reaction time 50h;
(2) molar concentration of described corrosive liquid red fuming nitric acid (RFNA) is 14.4mol/L, and reaction temperature is 70 DEG C, reaction time 50h;
(3) molar concentration of described corrosive liquid red fuming nitric acid (RFNA) is 13.6mol/L, and reaction temperature is 70 DEG C, reaction time 60h.
(4) molar concentration of described corrosive liquid red fuming nitric acid (RFNA) is 13.6mol/L, and reaction temperature is 90 DEG C, reaction time 40h.
What the present invention prepared have spindle structure titanium dioxide powder that high crystal face can expose
Preparation method prepare there is the spindle structure titanium dioxide powder that high crystal face can expose, its even structure, there is high specific area, and high crystal face can expose the high raising being conducive to catalytic activity of ratio in (001) face, the catalyst degradation dyestuff of this titanium dioxide powder is functional, can be applicable in the catalyst material of light degradation dyestuff.
Compared with prior art, the invention has the beneficial effects as follows:
Ti base noncrystal alloy is adopted to make original material in preparation method of the present invention, compared with crystal alloy, in non-crystaline amorphous metal, each element is all exist with solid solution state, and the character of amorphous alloy can change along with the change of element in alloy, in addition, the composition of amorphous alloy is easy to regulate, eliminate the impact of intermetallic compound alloy composition and structural homogenity, therefore the application of non-crystaline amorphous metal is conducive to carrying out smoothly of de-alloy process.The advantage of what the present invention prepared the have titanium dioxide powder of the spindle structure that high crystal face can expose is: implementation method prepared by (1) this titanium dioxide powder has simple to operate, easily carries out the advantages such as manual control to the pattern of product and structure; (2) improve and there is high crystal face can be enhanced by the exposure ratio in (001) face catalytic performance that is conducive to catalyst.
Accompanying drawing explanation
Fig. 1 is the microscopic appearance photo (SEM S4800, Hitachi Japan) of the spindle structure titanium dioxide powder that embodiment of the present invention 1-4 prepares;
Fig. 2 is XRD figure (XRD tester RIGAKU/DMAX2500, Japan) of the spindle structure titanium dioxide powder that embodiment of the present invention 1-4 prepares;
The curve of the light degradation rhodamine B of titanium dioxide prepared by embodiment of the present invention 1-4 has been shown in Fig. 3.
Detailed description of the invention
Tell about detailed content of the present invention by the following examples, provide embodiment to be convenience in order to understand, is never restriction the present invention.
The de-alloyage of embodiment 1, use prepares a kind of titanium dioxide powder with the spindle structure that high crystal face can expose, and comprises the following steps:
Step one, be Ti respectively according to atom percentage content be 30%, Cu be 62%, Pd8%, prepare Ti
30-Cu
62-Pd
8non-crystaline amorphous metal;
Step 2, the Ti that step one is obtained
30-Cu
62-Pd
8it is 25 μm that non-crystaline amorphous metal is cut into thickness, and width is 5mm, and length is the Ti of 25mm
30-Cu
62-Pd
8aMORPHOUS ALLOY RIBBONS; By this Ti
30-Cu
62-Pd
8aMORPHOUS ALLOY RIBBONS is dry in drying box by washed with de-ionized water juxtaposition after ultrasonic 5min in absolute ethyl alcohol;
Step 3, by the Ti of step 2 gained
30-Cu
62-Pd
8aMORPHOUS ALLOY RIBBONS is put into the closed container filling corrosive liquid and is reacted, the concentrated nitric acid solution of described corrosive liquid to be molar concentration be 14.4mol/L; Reaction temperature is 70 DEG C, and the reaction time is 50h, reaction is terminated rear obtained sample deionized water rinsing, and in drying box, is the spindle structure titanium dioxide powder having high crystal face and can expose after drying.
The titanium dioxide powder surface that embodiment 1 prepares is spindle pattern, and (a) in Fig. 1 shows the SEM figure with spindle structure titanium dioxide.(a) in Fig. 2 shows the XRD result of the titanium dioxide powder that the preparation-obtained high crystal face of embodiment 1 can expose.The even structure of this spindle structure titanium dioxide powder, there is high specific area, and high crystal face can expose the high raising being conducive to catalytic activity of ratio in (001) face, therefore, this spindle structure titanium dioxide powder catalyst degradation dyestuff is functional.The curve of the light degradation rhodamine B of titanium dioxide prepared by embodiment 1 has been shown in Fig. 3.
The de-alloyage of embodiment 2, use prepares a kind of titanium dioxide powder with the spindle structure that high crystal face can expose, its preparation process is substantially the same manner as Example 1, its difference is only: in step 3, the molar concentration of described corrosive liquid red fuming nitric acid (RFNA) is 13.6mol/L, reaction temperature is 90 DEG C, reaction time 40h.The titanium dioxide powder surface that embodiment 2 prepares is spindle pattern, and (b) in Fig. 1 shows the SEM figure with spindle structure titanium dioxide.(b) in Fig. 2 shows the XRD result of the titanium dioxide powder that the preparation-obtained high crystal face of embodiment 2 can expose.The curve of the light degradation rhodamine B of titanium dioxide prepared by embodiment 2 has been shown in Fig. 3.
The de-alloyage of embodiment 3, use prepares a kind of titanium dioxide powder with the spindle structure that high crystal face can expose, and its preparation process is substantially the same manner as Example 1, and its difference is only: in step one, and that prepare is Ti
30-Cu
64-Pd
6non-crystaline amorphous metal; In step 3, the molar concentration of described corrosive liquid red fuming nitric acid (RFNA) is 14.8mol/L, and reaction temperature is 50 DEG C, reaction time 50h.The titanium dioxide powder surface that embodiment 3 prepares is spindle pattern, and (c) in Fig. 1 shows the SEM figure with spindle structure titanium dioxide.(c) in Fig. 2 shows the XRD result of the titanium dioxide powder that the preparation-obtained high crystal face of embodiment 3 can expose.The curve of the light degradation rhodamine B of titanium dioxide prepared by embodiment 3 has been shown in Fig. 3.
The de-alloyage of embodiment 4, use prepares a kind of titanium dioxide powder with the spindle structure that high crystal face can expose, and its preparation process is substantially the same manner as Example 1, and its difference is only: in step one, and that prepare is Ti
30-Cu
66-Pd
4non-crystaline amorphous metal; In step 3, the molar concentration of described corrosive liquid red fuming nitric acid (RFNA) is 13.6mol/L, and reaction temperature is 70 DEG C, reaction time 60h.The titanium dioxide powder surface that embodiment 4 prepares is spindle pattern, and (d) in Fig. 1 shows the SEM figure with spindle structure titanium dioxide.(d) in Fig. 2 shows the XRD result of the titanium dioxide powder that the preparation-obtained high crystal face of embodiment 4 can expose.The curve of the light degradation rhodamine B of titanium dioxide prepared by embodiment 4 has been shown in Fig. 3.
The de-alloyage of embodiment 5, use prepares a kind of titanium dioxide powder with the spindle structure that high crystal face can expose, and its preparation process is substantially the same manner as Example 1, and its difference is only: in step one, and that prepare is Ti
30-Cu
60-Pd
10non-crystaline amorphous metal; In step 3, the molar concentration of described corrosive liquid red fuming nitric acid (RFNA) is 14.4mol/L, and reaction temperature is 50 DEG C, reaction time 50h.
To sum up, along with increasing of Pd element in non-crystaline amorphous metal, the catalytic performance of prepared nano titanium oxide strengthens gradually, and too lowly too highly all reduces catalytic performance to being chosen as of corrosive liquid concentration and temperature.Corrosive liquid concentration and moderate temperature, when Pd content is 8%, catalytic performance is best.
Although invention has been described by reference to the accompanying drawings above; but the present invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; instead of it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; when not departing from present inventive concept, can also make a lot of distortion, these all belong within protection of the present invention.
Claims (7)
1. there is the spindle structure titanium dioxide raw powder's production technology that high crystal face can expose, it is characterized in that, comprise the following steps:
Step one, prepare Ti-Cu-Pd non-crystaline amorphous metal according to following component and atom percentage content, wherein: the content of the content of Ti to be the content of 20%-40%, Cu be 60%-70%, Pd is 0%-10%;
Step 2, Ti-Cu-Pd non-crystaline amorphous metal obtained for step one is cut into thickness is 10 μm-30 μm, and width is 3mm-5mm, and length is the Ti-Cu-Pd AMORPHOUS ALLOY RIBBONS of 20-30mm; This Ti-Cu-Pd AMORPHOUS ALLOY RIBBONS is dry in drying box by washed with de-ionized water juxtaposition after ultrasonic 5min in absolute ethyl alcohol;
Step 3, the Ti-Cu-Pd AMORPHOUS ALLOY RIBBONS of step 2 gained is put into the closed container filling corrosive liquid react, the concentrated nitric acid solution of described corrosive liquid to be molar concentration be 13-15mol/L; Reaction temperature is 50-90 DEG C, and the reaction time is 30-70h, reaction is terminated rear obtained sample deionized water rinsing, and in drying box, is the spindle structure titanium dioxide powder having high crystal face and can expose after drying.
2. a kind of preparation method with the titanium dioxide powder of the spindle structure that high crystal face can expose according to claim 1, wherein:
In step one, the content of the content of Ti to be the content of 30%, Cu be 62%, Pd is 8%;
In step 3, the molar concentration of corrosive liquid red fuming nitric acid (RFNA) is 14.4mol/L, and reaction temperature is 70 DEG C, reaction time 50h.
3. a kind of preparation method with the titanium dioxide powder of the spindle structure that high crystal face can expose according to claim 1, wherein,
In step one, the content of the content of Ti to be the content of 30%, Cu be 62%, Pd is 8%;
In step 3, the molar concentration of corrosive liquid red fuming nitric acid (RFNA) is 13.6mol/L, and reaction temperature is 90 DEG C, reaction time 40h.
4. a kind of preparation method with the titanium dioxide powder of the spindle structure that high crystal face can expose according to claim 1, wherein,
In step one, the content of the content of Ti to be the content of 30%, Cu be 64%, Pd is 6%;
In step 3, the molar concentration of corrosive liquid red fuming nitric acid (RFNA) is 14.8mol/L, and reaction temperature is 50 DEG C, reaction time 50h.
5. a kind of preparation method with the titanium dioxide powder of the spindle structure that high crystal face can expose according to claim 1, wherein,
In step one, the content of the content of Ti to be the content of 30%, Cu be 66%, Pd is 4%;
In step 3, the molar concentration of corrosive liquid red fuming nitric acid (RFNA) is 13.6mol/L, and reaction temperature is 70 DEG C, reaction time 60h.
6. a kind of preparation method with the titanium dioxide powder of the spindle structure that high crystal face can expose according to claim 1, wherein,
In step one, the content of the content of Ti to be the content of 30%, Cu be 60%, Pd is 10%;
In step 3, the molar concentration of corrosive liquid red fuming nitric acid (RFNA) is 14.4mol/L, and reaction temperature is 50 DEG C, reaction time 50h.
7. one kind according to any one of claim 1 to 6, have that spindle structure titanium dioxide raw powder's production technology that high crystal face can expose prepares there is the application of spindle structure titanium dioxide powder in the catalyst material of light degradation dyestuff that high crystal face can expose.
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Cited By (4)
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| CN108686662A (en) * | 2018-05-28 | 2018-10-23 | 国网山东省电力公司电力科学研究院 | Nano TiO 2-amorphous zirconium-base alloy composite photocatalyst material and preparation method thereof and purposes |
| CN110449154A (en) * | 2019-07-21 | 2019-11-15 | 内蒙古农业大学 | A kind of copper oxide and titanium dioxide heterogeneous knot composite catalyst and its preparation method and application |
| CN110614091A (en) * | 2019-09-30 | 2019-12-27 | 华东理工大学 | Fusiform mesogenic TiO2Composite photocatalyst, preparation method and application thereof |
| CN115073070A (en) * | 2022-05-31 | 2022-09-20 | 河海大学 | Preparation method and application of antibacterial mortar coating |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108686662A (en) * | 2018-05-28 | 2018-10-23 | 国网山东省电力公司电力科学研究院 | Nano TiO 2-amorphous zirconium-base alloy composite photocatalyst material and preparation method thereof and purposes |
| CN110449154A (en) * | 2019-07-21 | 2019-11-15 | 内蒙古农业大学 | A kind of copper oxide and titanium dioxide heterogeneous knot composite catalyst and its preparation method and application |
| CN110614091A (en) * | 2019-09-30 | 2019-12-27 | 华东理工大学 | Fusiform mesogenic TiO2Composite photocatalyst, preparation method and application thereof |
| CN110614091B (en) * | 2019-09-30 | 2023-05-30 | 华东理工大学 | Spindle-shaped mesogenic TiO 2 Composite photocatalyst, preparation method and application thereof |
| CN115073070A (en) * | 2022-05-31 | 2022-09-20 | 河海大学 | Preparation method and application of antibacterial mortar coating |
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Application publication date: 20150422 |