CN108441957A - A kind of preparation method of bismuth ferrite photocatalysis film - Google Patents
A kind of preparation method of bismuth ferrite photocatalysis film Download PDFInfo
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- CN108441957A CN108441957A CN201711298836.4A CN201711298836A CN108441957A CN 108441957 A CN108441957 A CN 108441957A CN 201711298836 A CN201711298836 A CN 201711298836A CN 108441957 A CN108441957 A CN 108441957A
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- bismuth ferrite
- bismuth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
Abstract
The invention belongs to Material growth technical fields, and in particular to a kind of preparation method of bismuth ferrite photocatalysis film includes the following steps, step 1：It weighs nine water ferric nitrates and five water bismuth nitrates is spare；Step 2：The nine water ferric nitrates finished being weighed in step 1 and five water bismuth nitrates being uniformly mixed, ethylene glycol monomethyl ether then is added to the inside, obtains mixed liquor；Step 3：A certain amount of citric acid complexing agent is added in the mixed liquor obtained to step 2, suitable ethylene glycol monomethyl ether is then added and adjusts solution, then continues to stir at room temperature；Step 4：The solution that step 3 obtains is aged at room temperature, obtains bismuth ferrite precursor liquid；Step 5：Take a certain size SiO2/ Si substrates；Step 6：The bismuth ferrite precursor liquid that step 4 obtains is dropped in into SiO2In/Si substrate surfaces；Then it is prepared into film with sol evenning machine；Step 7：The film that step 6 obtains is preheated on hot plate, mahjong sample, which is placed in Muffle furnace, after preheating anneals, and bismuth ferrite photocatalysis film is obtained after annealing.
Description
Technical field
The invention belongs to Material growth technical fields, and in particular to a kind of preparation method of bismuth ferrite photocatalysis film.
Background technology
As a kind of single-phase multi-ferroic material, bismuth ferrite material is more in high density, low-power consumption, non-volatile novel sensor
State magnetoelectricity memory, the fields such as spintronics and photoelectric device are with important application prospects.
Physical deposition method and chemical deposition can be used respectively by preparing bismuth ferrite thin film；Physical deposition method is mainly
Refer to magnetron sputtering method, pulsed laser deposition and molecular beam epitaxy etc.；Chemical deposition is primarily referred to as chemical vapor deposition
Method, metal-organic decomposition method, sol-gel processing and hydro-thermal method etc.；Wherein, sol-gel processing is at present more
Relatively simple method, advantage：(1) at low cost, it is easy to operate；(2) stoichiometric ratio is easily controllable, and it is easy to be doped；
(3) energy large area does film.It is exactly first the compounds of needs in suitable solvent that sol-gel processing, which prepares bismuth ferrite thin film,
Middle dissolving simultaneously adds a small amount of additive, and ageing forms uniform colloidal sol, then colloid is uniformly spin-coated on substrate with sol evenning machine,
By hydrolysis, polymerisation forms gel, is then preheated and made annealing treatment to obtain the film of required thickness.
Invention content
The purpose of the present invention is be to control ferric nitrate and bismuth nitrate molal weight ratio and annealing temperature by sol-gal process
Degree, annealing time, at room temperature in SiO2/ Si substrate surfaces are prepared into pure phase bismuth ferric photocatalysis film.
To realize the above-mentioned technical purpose, the technical solution adopted by the present invention is as follows：
A kind of preparation method of bismuth ferrite photocatalysis film, includes the following steps,
Step 1：Weigh nine water ferric nitrate [Fe (NO3)3·9H2O] and five water bismuth nitrate [Bi (NO3)3·5H2O] it is spare,
Wherein the molal quantity ratio of ferric nitrate and bismuth nitrate is 1：(0.95~1.05)；
Step 2：The nine water ferric nitrates finished will be weighed in the step 1 and five water bismuth nitrates are uniformly mixed, then to
Ethylene glycol monomethyl ether is added in the inside, then stirs 30min~60min, until nine water ferric nitrates and five water bismuth nitrates are completely dissolved, obtains
To mixed liquor；
Step 3：A certain amount of citric acid complexing agent is added in the mixed liquor obtained to the step 2, and continues to stir,
Then suitable ethylene glycol monomethyl ether is added and adjusts solution, makes a concentration of 0.20-0.35mol/L of bismuth ferrite solution, then in room
Continue to stir 3h~4h under temperature；
Step 4：The solution that the step 3 obtains is aged for 24 hours~72h at room temperature, obtains bismuth ferrite precursor liquid；
Step 5：Take a certain size SiO2/ Si substrates, then by SiO2/ Si substrates clean up, and are dried for standby；
Step 6：The bismuth ferrite precursor liquid that the step 4 obtains is dropped in into the SiO that the step 5 obtains2/ Si substrates
On face；Then it is prepared into film with sol evenning machine；
Step 7：The film that the step 6 obtains is preheated into 3min~5min, mahjong after preheating on hot plate
Sample is placed in Muffle furnace and anneals, and bismuth ferrite photocatalysis film is obtained after annealing.
As a preferred embodiment of the present invention, SiO is cleaned in the step 52When/Si substrates, first by SiO2/ Si substrates
It is placed in the container equipped with acetone, then uses ultrasonic cleaning 10min, then SiO2/ Si substrates are rinsed well with deionized water
2min~5min, then dry up, absolute ethyl alcohol ultrasonic cleaning 10min, the SiO that will finally take out are used later2/ Si substrates are used again
Deionized water ultrasonic cleaning 10min.
As a preferred embodiment of the present invention, in the step 6, the spin coating rate of sol evenning machine be 3000r/min~
4000r/min。
As a preferred embodiment of the present invention, in the step 6, the time of sol evenning machine is 20s~30s.
As a preferred embodiment of the present invention, in the mixed liquor that the step 3 obtains, the concentration of citric acid complexing agent
For 15g/L.
As a preferred embodiment of the present invention, in the step 7, the temperature of heating plate is 200 DEG C.
As a preferred embodiment of the present invention, in the step 7, preheating on hot plate repeats 10~20 times.
As a preferred embodiment of the present invention, annealing temperature is 500 DEG C~650 DEG C in the step 7.
Annealing time of annealing as a preferred embodiment of the present invention, in the step 7 is 2min~30min.
Beneficial effects of the present invention：
1, using five water bismuth nitrate [Bi (NO3)3·5H2O] and nine water ferric nitrate [Fe (NO3)3·9H2O] as initial former
Material, ethylene glycol monomethyl ether prepare bismuth ferrite precursor liquid, in room temperature as complexing agent as solvent, citric acid by sol-gal process
Lower acquisition bismuth ferrite precursor liquid breaches the bismuth ferrite precursor liquid that document is reported and needs to heat and could prepare, to reduce reality
Test process；
2, in SiO2/ Si substrate surfaces control annealing temperature and annealing time is thin come the photocatalysis bismuth ferrite for preparing monocrystalline
Film provides a kind of new method for later industrial production.
Description of the drawings
The present invention can be further illustrated by the nonlimiting examples that attached drawing provides；
Fig. 1 is the XRD diagram for the sample that annealing time of the embodiment of the present invention is 10min；
Fig. 2 is 500 DEG C of annealing temperature of the embodiment of the present invention, the sample SEM figures that annealing time is 10min；
Fig. 3 is that the photocatalysis effect for the sample that annealing time of the embodiment of the present invention is 10min changes over time tendency chart；
Specific implementation mode
In order to make those skilled in the art that the present invention may be better understood, with reference to the accompanying drawings and examples to this hair
Bright technical solution further illustrates.
Embodiment one
Step 1：Weigh nine water ferric nitrate [Fe (NO3)3·9H2O] 3.31695g and five water bismuth nitrate [Bi (NO3)3·
5H2O] 2.626g is spare；
Step 2：The nine water ferric nitrates finished will be weighed in the step 1 and five water bismuth nitrates are uniformly mixed, then to
12mL ethylene glycol monomethyl ethers are added in the inside, then stir 30min~60min, until nine water ferric nitrates and five water bismuth nitrates are completely molten
Solution, obtains mixed liquor；
Step 3：0.3g citric acid complexing agents are added in the mixed liquor obtained to the step 2, and continue to stir, then
Suitable ethylene glycol monomethyl ether is added and adjusts solution, makes a concentration of 0.20-0.35mol/L of bismuth ferrite solution, then at room temperature
Continue to stir 3h~4h；
Step 4：The solution that the step 3 obtains is aged for 24 hours~72h at room temperature, obtains bismuth ferrite precursor liquid；
Step 5：Take a certain size SiO2/ Si substrates, then by SiO2/ Si substrates clean up, and are dried for standby；
Step 6：The bismuth ferrite precursor liquid that the step 4 obtains is dropped in into the SiO that the step 5 obtains2/ Si substrates
On face；Then it is prepared into film with sol evenning machine；
Step 7：The film that the step 6 obtains is preheated into 3min~5min, mahjong after preheating on hot plate
Sample is placed in Muffle furnace and anneals, and annealing temperature selects 450 DEG C, and annealing time is 2~30min, and bismuth ferrite light is obtained after annealing and is urged
Change film.
Embodiment two
Step 1：Weigh nine water ferric nitrate [Fe (NO3)3·9H2O] 3.31695g and five water bismuth nitrate [Bi (NO3)3·
5H2O] 2.626g is spare；
Step 2：The nine water ferric nitrates finished will be weighed in the step 1 and five water bismuth nitrates are uniformly mixed, then to
12mL ethylene glycol monomethyl ethers are added in the inside, then stir 30min~60min, until nine water ferric nitrates and five water bismuth nitrates are completely molten
Solution, obtains mixed liquor；
Step 3：0.3g citric acid complexing agents are added in the mixed liquor obtained to the step 2, and continue to stir, then
Suitable ethylene glycol monomethyl ether is added and adjusts solution, makes a concentration of 0.20-0.35mol/L of bismuth ferrite solution, then at room temperature
Continue to stir 3h~4h；
Step 4：The solution that the step 3 obtains is aged for 24 hours~72h at room temperature, obtains bismuth ferrite precursor liquid；
Step 5：Take a certain size SiO2/ Si substrates, then by SiO2/ Si substrates clean up, and are dried for standby；
Step 6：The bismuth ferrite precursor liquid that the step 4 obtains is dropped in into the SiO that the step 5 obtains2/ Si substrates
On face；Then it is prepared into film with sol evenning machine；
Step 7：The film that the step 6 obtains is preheated into 3min~5min, mahjong after preheating on hot plate
Sample is placed in Muffle furnace and anneals, and annealing temperature selects 500 DEG C, and annealing time is 2~30min, and bismuth ferrite light is obtained after annealing and is urged
Change film.
Embodiment three
Step 1：Weigh nine water ferric nitrate [Fe (NO3)3·9H2O] 3.31695g and five water bismuth nitrate [Bi (NO3)3·
5H2O] 2.626g is spare；
Step 2：The nine water ferric nitrates finished will be weighed in the step 1 and five water bismuth nitrates are uniformly mixed, then to
12mL ethylene glycol monomethyl ethers are added in the inside, then stir 30min~60min, until nine water ferric nitrates and five water bismuth nitrates are completely molten
Solution, obtains mixed liquor；
Step 3：0.3g citric acid complexing agents are added in the mixed liquor obtained to the step 2, and continue to stir, then
Suitable ethylene glycol monomethyl ether is added and adjusts solution, makes a concentration of 0.20-0.35mol/L of bismuth ferrite solution, then at room temperature
Continue to stir 3h~4h；
Step 4：The solution that the step 3 obtains is aged for 24 hours~72h at room temperature, obtains bismuth ferrite precursor liquid；
Step 5：Take a certain size SiO2/ Si substrates, then by SiO2/ Si substrates clean up, and are dried for standby；
Step 6：The bismuth ferrite precursor liquid that the step 4 obtains is dropped in into the SiO that the step 5 obtains2/ Si substrates
On face；Then it is prepared into film with sol evenning machine；
Step 7：The film that the step 6 obtains is preheated into 3min~5min, mahjong after preheating on hot plate
Sample is placed in Muffle furnace and anneals, and annealing temperature selects 550 DEG C, and annealing time is 2~30min, and bismuth ferrite light is obtained after annealing and is urged
Change film.
Embodiment 4
Step 1：Weigh nine water ferric nitrate [Fe (NO3)3·9H2O] 3.31695g and five water bismuth nitrate [Bi (NO3)3·
5H2O] 2.626g is spare；
Step 2：The nine water ferric nitrates finished will be weighed in the step 1 and five water bismuth nitrates are uniformly mixed, then to
12mL ethylene glycol monomethyl ethers are added in the inside, then stir 30min~60min, until nine water ferric nitrates and five water bismuth nitrates are completely molten
Solution, obtains mixed liquor；
Step 3：0.3g citric acid complexing agents are added in the mixed liquor obtained to the step 2, and continue to stir, then
Suitable ethylene glycol monomethyl ether is added and adjusts solution, makes a concentration of 0.20-0.35mol/L of bismuth ferrite solution, then at room temperature
Continue to stir 3h~4h；
Step 4：The solution that the step 3 obtains is aged for 24 hours~72h at room temperature, obtains bismuth ferrite precursor liquid；
Step 5：Take a certain size SiO2/ Si substrates, then by SiO2/ Si substrates clean up, and are dried for standby；
Step 6：The bismuth ferrite precursor liquid that the step 4 obtains is dropped in into the SiO that the step 5 obtains2/ Si substrates
On face；Then it is prepared into film with sol evenning machine；
Step 7：The film that the step 6 obtains is preheated into 3min~5min, mahjong after preheating on hot plate
Sample is placed in Muffle furnace and anneals, and annealing temperature selects 600 DEG C, and annealing time is 2~30min, and bismuth ferrite light is obtained after annealing and is urged
Change film.
Above-described embodiment is merely exemplary to illustrate the principle of the present invention and its effect, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, all those of ordinary skill in the art are completed without departing from the spirit and technical ideas disclosed in the present invention
All equivalent modifications or change, should by the present invention claim be covered.
Claims (9)
1. a kind of preparation method of bismuth ferrite photocatalysis film, it is characterised in that：Include the following steps,
Step 1：Weigh nine water ferric nitrate [Fe (NO3)3·9H2O] and five water bismuth nitrate [Bi (NO3)3·5H2O] it is spare, wherein
The molal quantity ratio of ferric nitrate and bismuth nitrate is 1：(0.95~1.05)；
Step 2：The nine water ferric nitrates finished will be weighed in the step 1 and five water bismuth nitrates are uniformly mixed, then to the inside
Ethylene glycol monomethyl ether is added, then stirs 30min~60min, until nine water ferric nitrates and five water bismuth nitrates are completely dissolved, is mixed
Close liquid；
Step 3：A certain amount of citric acid complexing agent is added in the mixed liquor obtained to the step 2, and continues to stir, then
Suitable ethylene glycol monomethyl ether is added and adjusts solution, makes a concentration of 0.20-0.35mol/L of bismuth ferrite solution, then at room temperature
Continue to stir 3h~4h；
Step 4：The solution that the step 3 obtains is aged for 24 hours~72h at room temperature, obtains bismuth ferrite precursor liquid；
Step 5：Take a certain size SiO2/ Si substrates, then by SiO2/ Si substrates clean up, and are dried for standby；
Step 6：The bismuth ferrite precursor liquid that the step 4 obtains is dropped in into the SiO that the step 5 obtains2In/Si substrate surfaces；
Then it is prepared into film with sol evenning machine；
Step 7：The film that the step 6 obtains is preheated into 3min~5min on hot plate, mahjong sample after preheating
It is placed in Muffle furnace and anneals, bismuth ferrite photocatalysis film is obtained after annealing.
2. a kind of preparation method of bismuth ferrite photocatalysis film according to claim 1, it is characterised in that：The step 5
Middle cleaning SiO2When/Si substrates, first by SiO2/ Si substrates are placed in the container equipped with acetone, then use ultrasonic cleaning 10min,
Again SiO2/ Si substrates rinse 2min~5min well with deionized water, then dry up, and use absolute ethyl alcohol ultrasonic cleaning later
10min, the SiO that will finally take out2/ Si substrates use deionized water ultrasonic cleaning 10min again.
3. a kind of preparation method of bismuth ferrite photocatalysis film according to claim 2, it is characterised in that：The step 6
In, the spin coating rate of sol evenning machine is 3000r/min~4000r/min.
4. a kind of preparation method of bismuth ferrite photocatalysis film according to claim 3, it is characterised in that：The step 6
In, the time of sol evenning machine is 20s~30s.
5. a kind of preparation method of bismuth ferrite photocatalysis film according to claim 4, it is characterised in that：The step 3
In obtained mixed liquor, a concentration of 15g/L of citric acid complexing agent.
6. a kind of preparation method of bismuth ferrite photocatalysis film according to claim 5, it is characterised in that：The step 7
In, the temperature of heating plate is 200 DEG C.
7. a kind of preparation method of bismuth ferrite photocatalysis film according to claim 6, it is characterised in that：The step
In rapid seven, preheating on hot plate repeats 10~20 times.
8. a kind of preparation method of bismuth ferrite photocatalysis film according to claim 7, it is characterised in that：The step 7
Middle annealing temperature is 500 DEG C~650 DEG C.
9. a kind of preparation method of bismuth ferrite photocatalysis film according to claim 8, it is characterised in that：The step 7
Middle annealing annealing time is 2min~30min.
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Cited By (6)
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| CN109702186A (en) * | 2019-01-28 | 2019-05-03 | 合肥学院 | A kind of bismuth metal nanometer shell material and preparation method thereof |
| CN111074244A (en) * | 2018-10-19 | 2020-04-28 | 营口理工学院 | Nickel-cerium co-doped bismuth ferrite film material and preparation method thereof |
| CN112226808A (en) * | 2020-09-10 | 2021-01-15 | 清华大学 | Bismuth ferrite nano single crystal array, preparation method thereof and electronic element containing bismuth ferrite nano single crystal array |
| CN114229911A (en) * | 2021-12-31 | 2022-03-25 | 湖南大学 | Preparation method of bismuth ferrite film |
| CN114808194A (en) * | 2022-04-06 | 2022-07-29 | 山东大学 | Preparation method and application of single-phase bismuth ferrite ceramic fiber |
| CN115432738A (en) * | 2022-09-05 | 2022-12-06 | 南京理工大学 | BiFeO for depositing amorphous layer 3 Film and method for producing same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111074244A (en) * | 2018-10-19 | 2020-04-28 | 营口理工学院 | Nickel-cerium co-doped bismuth ferrite film material and preparation method thereof |
| CN109702186A (en) * | 2019-01-28 | 2019-05-03 | 合肥学院 | A kind of bismuth metal nanometer shell material and preparation method thereof |
| CN112226808A (en) * | 2020-09-10 | 2021-01-15 | 清华大学 | Bismuth ferrite nano single crystal array, preparation method thereof and electronic element containing bismuth ferrite nano single crystal array |
| CN112226808B (en) * | 2020-09-10 | 2021-12-07 | 清华大学 | Bismuth ferrite nano single crystal array, preparation method thereof and electronic element containing bismuth ferrite nano single crystal array |
| CN114229911A (en) * | 2021-12-31 | 2022-03-25 | 湖南大学 | Preparation method of bismuth ferrite film |
| CN114229911B (en) * | 2021-12-31 | 2022-08-12 | 湖南大学 | Preparation method of bismuth ferrite film |
| CN114808194A (en) * | 2022-04-06 | 2022-07-29 | 山东大学 | Preparation method and application of single-phase bismuth ferrite ceramic fiber |
| CN115432738A (en) * | 2022-09-05 | 2022-12-06 | 南京理工大学 | BiFeO for depositing amorphous layer 3 Film and method for producing same |
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