CN114229892B - Ion implantation doped bismuth oxide and preparation method and application thereof - Google Patents
Ion implantation doped bismuth oxide and preparation method and application thereof Download PDFInfo
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- CN114229892B CN114229892B CN202111590671.4A CN202111590671A CN114229892B CN 114229892 B CN114229892 B CN 114229892B CN 202111590671 A CN202111590671 A CN 202111590671A CN 114229892 B CN114229892 B CN 114229892B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/10—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce uniformly-coloured transparent products
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses an ion implantation doped bismuth oxide and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing bismuth nitrate with citric acid to obtain a mixture, adding the mixture into water to obtain slurry, heating the slurry in water bath to obtain sol, evaporating water from the solThen obtaining gel, calcining the gel to obtain nano bismuth oxide particles, pressing the nano bismuth oxide particles to form a bismuth oxide green sheet, sintering the bismuth oxide green sheet to obtain a bismuth oxide sheet, placing the bismuth oxide sheet on a substrate of an ion implanter, and injecting doping ions into the bismuth oxide sheet to obtain doped bismuth oxide, wherein Na is doped in the bismuth oxide by the method + The invention can obviously improve the hydrophilic property of bismuth oxide, greatly improve the application of bismuth oxide in glass coloring, and the invention is more original to lead the nonmetallic ion Si to be 4+ Doped into bismuth oxide to dope Si 4+ Can greatly improve the performances of the catalyst in catalyzing and degrading organic wastewater, high-temperature superconductivity and the like.
Description
Technical Field
The invention relates to a doped powder material, in particular to an ion implantation doped bismuth oxide, a preparation method and application thereof.
Background
Bismuth oxide is also called bismuth trioxide, is one of the most important compounds of bismuth, has alpha, beta, gamma and delta crystal forms, has very wide application, is not only an organic synthesis catalyst, a ceramic colorant and a glass additive, but also can be used for manufacturing nuclear engineering glass and nuclear reactor fuel, and nano bismuth oxide can be used for special occasions such as semiconductor electronic materials, special functional ceramic materials, cathode ray tube inner wall coatings and the like; the particle size and uniformity of bismuth oxide have great influence on the catalytic performance and the like, meanwhile, bismuth oxide is an important doped powder material in the electronic industry, ion doping is mainly used for surface modification of semiconductor materials, the bismuth oxide doped by different metals has obvious change in photoelectric properties and the like, such as doping Cu 2+ 、Fe 3+ 、Co 2+ The absorption spectrum and sunlight spectrum matching property of the bismuth oxide of the plasma are obviously improved, and the photocatalysis performance of the bismuth oxide is improved.
The current methods for ion doping bismuth oxide include coprecipitation method, impregnation method, sol-gel method, etc., wherein the coprecipitation method comprises Bi 3+ Slowly adding the solution doped with ions into the solution containing the excessive precipitant, stirring to obtain a relatively uniform precipitate, and performing heat treatment to obtain a required material; the impregnation method is to prepare the bismuth oxide by immersing the bismuth oxide in a salt solution containing metal ions, and the sol-gel method is to add metal ion inorganic salt into bismuth oxide sol and then obtain the bismuth oxide with final doped ions through subsequent treatment; the methods have large defects such as uneven ion doping distribution and no ion dopingThe method for controlling the bismuth oxide crystal form, the particle size and the like finally influences the use effect of the finished product, and the method can not dope C into the bismuth oxide + 、Si 4+ Non-metal ions; and the dopant ion concentration cannot be precisely controlled.
Disclosure of Invention
In view of the problems existing in the prior art, the invention aims to provide ion implantation doped bismuth oxide, and a preparation method and application thereof. The invention dopes metal ion Na into the nanometer bismuth oxide film by ion implantation method + Nonmetallic ion Si 4+ Thereby remarkably improving the photocatalysis performance and conductivity of bismuth oxide and improving the application performance of bismuth oxide in glass coloring, catalytic degradation of organic wastewater, superconductive and the like. The method has low power consumption, saves materials, has no toxicity and byproducts, and is beneficial to environmental protection.
In order to achieve the above object, the technical solution of the present invention is:
the invention discloses a preparation method of ion implantation doped bismuth oxide, which comprises the following steps: mixing bismuth nitrate and citric acid to obtain a mixture, adding the mixture into water to obtain slurry, heating the slurry in water bath to obtain sol, evaporating the sol to obtain gel, calcining the gel to obtain nano bismuth oxide particles, pressing the nano bismuth oxide particles to form a bismuth oxide green sheet, sintering the bismuth oxide green sheet to obtain a bismuth oxide sheet, placing the bismuth oxide sheet on a substrate of an ion implanter, and injecting doping ions into the bismuth oxide sheet to obtain the doped bismuth oxide.
Preferably, the ratio of the bismuth nitrate to the citric acid is 1:1-1.5.
Preferably, the solid-liquid mass volume ratio of the mixture to water is 59.5g:100-200ml.
In a preferred scheme, the temperature of the water bath heating is 90-95 ℃, and the time of the water bath heating is 3-5h.
In a preferred scheme, the gel is calcined at 350-450 ℃ for 1-2 hours to obtain nano bismuth oxide particles.
In a preferred embodiment, the particle size of the nano bismuth oxide particles is 50nm-1.5 μm.
Preferably, the pressure of the compression molding is 2-4MPa.
The inventor finds that the more uniform the bismuth oxide flake is, the higher the uniformity of doped ions is after final ion implantation, so that the better the material performance is, the gel is firstly calcined at 350-450 ℃ to obtain nano bismuth oxide particles, the bismuth oxide green flake can be very flat and uniform after compression molding, and finally the bismuth oxide flake with excellent uniformity is obtained after calcination.
However, the pressure of the compression molding needs to be effectively controlled in the compression process, and even and complete bismuth oxide sheets can be obtained only within the scope of the invention.
Preferably, the sintering temperature is 700-750 ℃, and the sintering time is 30-60min.
In a preferred embodiment, the planar dimension of the bismuth oxide flake is 12×12-20×20mm, and the thickness is 1-1.2mm.
In a preferred scheme, when the doped ions are implanted, the temperature of the substrate is controlled to be 750-800 ℃, and the ion acceleration voltage is controlled to be 30-60KeV.
The inventors found that controlling the substrate temperature, as well as the acceleration voltage, within the above-described ranges, the final dopant ions are most uniformly distributed in the bismuth oxide, resulting in the best performance of the doped bismuth oxide.
Preferably, the implantation amount of the doped ions is 50-200ppm.
The inventors found that the performance of the finally obtained doped bismuth oxide is optimal by controlling the implantation amount of the doped ions within the above range.
Preferably, the doping ion is Na + Or Si (or) 4+ 。
The inventors found that doping Na in bismuth oxide + The invention can obviously improve the hydrophilic property of bismuth oxide, greatly improve the application of bismuth oxide in glass coloring, and the invention is more original to lead the nonmetallic ion Si to be 4+ Doped into bismuth oxide to dope Si 4+ Can greatly improve the performances of the catalyst in catalyzing and degrading organic wastewater, high-temperature superconductivity and the like.
The invention also provides the doped bismuth oxide prepared by the preparation method.
The invention also provides application of the doped bismuth oxide prepared by the preparation method.
Preferably, when the doping ion in the doped bismuth oxide is Na + When the doped bismuth oxide is applied to glass coloring.
Preferably, when the doping ion in the doped bismuth oxide is Si 4+ When the bismuth oxide doped catalyst is used for catalytic degradation of organic wastewater.
Advantageous effects
The invention discloses a method for doping metal ions Na into nano bismuth oxide thin blocks by an ion implantation method + Nonmetallic ion Si 4+ The inventors found that Na was doped in bismuth oxide + The invention can obviously improve the hydrophilic property of bismuth oxide, greatly improve the application of bismuth oxide in glass coloring, and the invention is more original to lead the nonmetallic ion Si to be 4+ Doped into bismuth oxide to dope Si 4+ Can greatly improve the performances of the catalyst in catalyzing and degrading organic wastewater, high-temperature superconductivity and the like. So that the performances of bismuth oxide in the aspects of glass coloring, catalytic degradation of organic wastewater, high-temperature superconductivity and other application can be widened.
Detailed Description
An ion implantation bismuth oxide doping method is to dope metal and nonmetal ions into bismuth oxide through an ion implantation method.
Example 1
Preparing 20g of citric acid and 39.5g of bismuth nitrate, uniformly mixing, adding into a 500ml beaker, adding 100ml of ultrapure water, heating in a water bath at 90 ℃ for 5 hours, evaporating water to obtain gel after sol is generated, calcining the gel at 400 ℃ for 1 hour to obtain nano bismuth oxide particles, pressing nano bismuth oxide into 12 x 1mm thin blocks under 2MPa, placing bismuth oxide into an ion injector, adjusting the substrate temperature to 780 ℃, adjusting the ion acceleration voltage to 50KeV, and injecting Na into the bismuth oxide + The obtained sodium-doped bismuth oxide reconstituted powder at a concentration of 100ppm was compared with pure bismuth oxide by a hydrophilicity test to obtain the results shown in Table 1:
TABLE 1 hydrophilia before and after bismuth oxide doping
| Material | Contact angle |
| Bi 2 O 3 | ＞90° |
| Doped with Na + Bi 2 O 3 | 0° |
The bismuth oxide doped with sodium ions has obvious improvement on hydrophilicity.
Comparative example 1
Other conditions were the same as in example 1 except that the substrate temperature was 830 ℃, and as a result, the uniformity of the obtained sodium-doped bismuth oxide was lowered, and the hydrophilicity was lower than in example 1 (Table 2).
Table 2 bismuth oxide doped hydrophilic properties in example 1 and comparative example 1
Example 2
Preparing 20g of citric acid and 39.5g of bismuth nitrate, uniformly mixing, adding into a 500ml beaker, adding 100ml of ultrapure water, heating in a water bath at 90 ℃ for 5 hours, evaporating water to obtain gel after sol is generated, calcining the gel at 400 ℃ for 1 hour to obtain nano bismuth oxide particles, pressing nano bismuth oxide into 12 x 1mm thin blocks under 2MPa, placing bismuth oxide into an ion injector, adjusting the substrate temperature to 780 ℃, adjusting the ion acceleration voltage to 50KeV, and injecting Si into the bismuth oxide 4+ At a concentration of 150ppm, the resulting dopingThe results of rhodamine B photocatalytic degradation test of the silicon ion bismuth oxide reconstituted powder and pure bismuth oxide are shown in Table 3
Table 3 catalytic degradation test before and after bismuth oxide doping.
| Material | Time (min) | Degradation rate (%) |
| Bi 2 O 3 | 120 | 55 |
| Doped Si 4+ Bi 2 O 3 | 120 | 100 |
Comparative example 2
Other conditions were the same as in example 2 except that the substrate temperature was 830 ℃, and as a result, the uniformity of the obtained sodium-doped bismuth oxide was lowered, and the degradation efficiency was lower than in example 2 (table 4).
TABLE 4 photocatalytic degradation Rate doped with bismuth oxide in example 2 and comparative example 2
The foregoing description, for the convenience of the reader, has focused on a representative sample of all possible embodiments, that is presented to explain the principles of the invention and to illustrate the best mode for practicing the invention. This description is not intended to be exhaustive of all of the possible variations. Other variations or modifications not illustrated are also possible.
Claims (6)
1. A preparation method of ion implantation doped bismuth oxide is characterized in that: the method comprises the following steps: mixing bismuth nitrate and citric acid to obtain a mixture, adding the mixture into water to obtain slurry, heating the slurry in water bath to obtain sol, evaporating the sol to obtain gel, calcining the gel to obtain nano bismuth oxide particles, pressing the nano bismuth oxide particles to form a bismuth oxide green sheet, sintering the bismuth oxide green sheet to obtain a bismuth oxide sheet, placing the bismuth oxide sheet on a substrate of an ion implanter, and injecting doping ions into the bismuth oxide sheet to obtain doped bismuth oxide;
the pressure of the compression molding is 2-4MPa;
the sintering temperature is 700-750 ℃, and the sintering time is 30-60min;
the plane size of the bismuth oxide flake is 12 multiplied by 12 to 20 multiplied by 20mm, and the thickness is 1 to 1.2mm;
when the doping ions are injected, the temperature of the substrate is controlled to be 750-800 ℃, and the ion acceleration voltage is controlled to be 30-60KeV;
the implantation amount of the doped ions is 50-200ppm; the doped ion is Na + Or Si (or) 4+ 。
2. The method for preparing the ion implantation doped bismuth oxide according to claim 1, wherein the method comprises the following steps: the ratio of the bismuth nitrate to the citric acid is 1:1-1.5;
the solid-liquid mass volume ratio of the mixture to water is 59.5g:100-200mL.
3. The method for preparing the ion implantation doped bismuth oxide according to claim 1, wherein the method comprises the following steps: the temperature of the water bath heating is 90-95 ℃, and the time of the water bath heating is 3-5h.
4. The method for preparing the ion implantation doped bismuth oxide according to claim 1, wherein the method comprises the following steps: calcining the gel at 350-450 ℃ for 1-2h to obtain nano bismuth oxide particles;
the particle size of the nano bismuth oxide particles is 50nm-1.5 mu m.
5. A doped bismuth oxide prepared by the preparation method according to any one of claims 1 to 4.
6. The use of doped bismuth oxide prepared by the preparation method according to any one of claims 1 to 4, characterized in that: when the doping ion in the doped bismuth oxide is Na + When the bismuth oxide doped is applied to glass coloring;
when the doping ion in the doped bismuth oxide is Si 4+ When the bismuth oxide doped catalyst is used for catalytic degradation of organic wastewater.
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