CN109354487A - A kind of bismuth ferrite base nano ceramic and preparation method - Google Patents
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Abstract
The invention discloses a kind of bismuth ferrite base nano ceramic, the chemical formula of main constituents is Bi0.8Gd0.2Fe1‑xTixO3, wherein the value of x is Ti4+Doping ratio, 0.01≤x≤0.1, Bi0.8Gd0.2Fe1‑xTixO3Object be mutually orthorhombic phase.The spiralization cycle for having broken ferrous acid bismuth-based ceramics improves the ferromagnetism and ferroelectricity of bismuth ferrite ceramics, reduces dielectric loss and leakage current.The invention also discloses a kind of preparation methods of above-mentioned bismuth ferrite base nano ceramic, comprising the following steps: weighs bismuth source, source of iron, gadolinium source and configures mixed solution with titanium source, mixed dissolution in organic solvent, additive is added, stirs to obtain colloidal sol；Colloidal sol is dry, and fine gtinding obtains nano-powder；Nano-powder is inserted in graphite jig, plasma agglomeration, rubbing down removes the carbon paper on surface, and annealing obtains bismuth ferrite base nano ceramic.Using plasma agglomeration, the consistency of product is improved, so that ferromagnetism be made to be enhanced, and promotes the generation of orthorhombic phase in bismuth ferrite base nano ceramic.
Description
Technical field
The present invention relates to electrodeless nonmetallic materials preparation technical field, more particularly to a kind of bismuth ferrite base nano ceramic and
Preparation method.
Background technique
Bismuth ferrite (BiFeO3, BFO), it is a kind of triangle perovskite structure of distortion, Curie temperature with higher, Neil
Temperature and biggish residual polarization temperature, in Ferroelectric Random Access Memory, spin electric device, magnetoelectricity storage unit, photoelectric device
Equal fields have a good application prospect.
Volatile under Bi element high temperature in bismuth ferrite, pure phase not easily generated, Fe element, which easily appraises at the current rate, generates Fe2+, lead to electricity
Son is in Fe2+/Fe3+Between jump, keep the dielectric loss of system excessive, and its own structure there are the period be 62nm it is asymmetric
Helical structure, thus system macroscopically reflects that anti-ferromagnetism, the macroscopic magnetization of system are weaker.For said circumstances, can pass through
Other elements are adulterated into bismuth ferrite to be improved, had in the prior art by the way that lanthanide series is added into bismuth ferrite ceramics
(La, Dy, Ce and Nd), Ba or Cr significantly improve the ferromagnetism of bismuth ferrite ceramics.
Although the prior art improves the ferromagnetism of bismuth ferrite ceramics, does not change its anti-ferromagnetic structure when adulterating, leak
Electric current is larger, simultaneously as doped chemical in the prior art, is degrading its ferroelectricity, the residual polarization of bismuth ferrite ceramics is strong
Degree is substantially reduced, and remanent polarization is only 1 μ C/cm under partial condition2。
Summary of the invention
An object of the present invention is to provide a kind of ferromagnetism and the good bismuth ferrite base nano ceramic of ferroelectricity, and have
There are lower dielectric loss and leakage current.
A kind of bismuth ferrite base nano ceramic, the chemical formula of main constituents are Bi0.8Gd0.2Fe1-xTixO3, wherein x
Value is Ti4+Doping ratio, 0.01≤x≤0.1, Bi0.8Gd0.2Fe1-xTixO3Object be mutually orthorhombic phase.
The bismuth ferrite base nano ceramic proposed according to the present invention adulterates bismuth ferrite ceramics using Gd and Ti, and after doping
Product be orthorhombic phase, broken the spiralization cycle of ferrous acid bismuth-based ceramics, improved the ferromagnetism and ferroelectricity of bismuth ferrite ceramics,
Reduce dielectric loss and leakage current.
It is another object of the present invention to the preparation method for proposing a kind of above-mentioned bismuth ferrite base nano ceramic, including it is following
Step:
(1) according to the molar ratio of doped chemical weigh bismuth source, source of iron, gadolinium source and and titanium source, mixed dissolution is in organic solvent
In, it is configured to the mixed solution of 0.05~0.2mol/L of concentration；
(2) it is added additive into mixed solution, the molar ratio of additive and mixed solution is 0.5~2:1, stirring 3~5
Hour, obtain colloidal sol；
(3) colloidal sol is 10~15 hours dry, drying temperature is 100~150 DEG C, and fine gtinding obtains nano-powder；
(4) nano-powder is inserted in graphite jig, plasma agglomeration is carried out to nano-powder, rubbing down removes the carbon on surface
Paper, annealing, obtains bismuth ferrite base nano ceramic.
The preparation method of the bismuth ferrite base nano ceramic proposed according to the present invention, the beneficial effect is that:
Using bismuth source, source of iron, gadolinium source and with titanium source mix, by be added additive colloidal sol is made, be conducive to the burning in later period
Knot uses plasma agglomeration after dry again, improves the consistency of product, so that ferromagnetism be made to be enhanced, and promote iron
The generation of orthorhombic phase in sour bismuthino nano ceramics improves the probability of orthorhombic phase generation.
In addition, the preparation method of the bismuth ferrite base nano ceramic provided according to the present invention, can also have following additional
Technical characteristic:
Further, the bismuth source in the step (1) is Bi (NO3)3·5H2O, source of iron are Fe (NO3)3·9H2O, gadolinium source
For Gd (NO3)3·6H2O, titanium source C16H36O4Ti, wherein titanium source selects organic solution, can be effectively controlled the content of Ti element, and
Promote to generate orthorhombic phase in subsequent sintering process.
Further, the organic solvent in the step (1) is ethylene glycol monomethyl ether, glacial acetic acid, ethylene glycol, one in ethyl alcohol
Various elements are mixed into solution by kind or a variety of combinations, are used for subsequent processing.
Further, the additive in the step (2) is one of tartaric acid, acetylacetone,2,4-pentanedione, citric acid or a variety of
Combination, be added additive after mixed solution will form colloidal sol, wherein when additive be tartaric acid when, it is molten claret to be formed
Glue easily brings it about distortion of lattice when being sintered to the colloidal sol, improves the generation probability of orthorhombic phase.
Further, further include that nano-powder is subjected to pre-burning between the step (3) and step (4), burnt in plasma
Pre-burning is first carried out before knot can improve the consistency of final sintering products therefrom, improve the ferromagnetism and ferroelectricity of product.
Further, the pre-burning is to be sintered 1~3 hour under the conditions of 400~500 DEG C.
Further, it is as follows that sintering parameter is controlled during the plasma agglomeration in the step (4):
Sintering temperature is 500~700 DEG C, and when sintering is 10~15 minutes a length of.
Further, it is 2~10Pa that the sintering parameter, which further includes the vacuum degree of control sintering environment, in certain vacuum degree
Under be sintered, can be further improved the consistency of sintering, while orthorhombic phase is more also easy to produce in plasma agglomeration.
Further, the annealing process in the step (4) is to anneal 1~3 hour in 400~600 DEG C of air.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Above-mentioned and/or additional aspect of the invention and advantage will become from the description of the embodiment in conjunction with the following figures
Obviously and it is readily appreciated that, in which:
Fig. 1 is the bismuth ferrite base nano ceramic of the embodiment of the present invention 1 and the XRD curve comparison figure of normal orthogonal phase；
Fig. 2 is the ferroelectric hysteresis loop of the bismuth ferrite base nano ceramic of the embodiment of the present invention 1；
Fig. 3 is the M-H curve graph of the bismuth ferrite base nano ceramic of the embodiment of the present invention 1；
Fig. 4 is the ferroelectric hysteresis loop of 1 gained bismuth ferrite base nano ceramic of reference examples.
Specific embodiment
To keep objects, features and advantages of the present invention more obvious and easy to understand, with reference to the accompanying drawing to tool of the invention
Body embodiment is described in detail.Several embodiments of the invention are given in attached drawing.But the present invention can be with many not
With form realize, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes to this
The disclosure of invention is more thorough and comprehensive.
Embodiment 1
The present embodiment proposes that ferrous acid bismuthino nano ceramics, the chemical formula of main constituents are Bi0.8Gd0.2Fe1- xTixO3, wherein the value of x is Ti4+Doping ratio, x=0.05, Bi0.8Gd0.2Fe1-xTixO3Object be mutually orthorhombic phase.
The preparation method of above-mentioned bismuth ferrite base nano ceramic the following steps are included:
(1) according to the molar ratio of doped chemical weigh bismuth source, source of iron, gadolinium source and and titanium source, mixed dissolution is in organic solvent
In, it is configured to the mixed solution of concentration 0.1mol/L；
(2) it is added additive into mixed solution, the molar ratio of additive and mixed solution is 1:1, stirs 4 hours, obtains
Colloidal sol；
(3) colloidal sol is 12 hours dry, drying temperature is 120 DEG C, and fine gtinding obtains nano-powder；
(4) nano-powder is inserted in graphite jig, plasma agglomeration is carried out to nano-powder, rubbing down removes the carbon on surface
Paper, annealing, obtains bismuth ferrite base nano ceramic.
In the present embodiment, the bismuth source in the step (1) is Bi (NO3)3·5H2O, source of iron are Fe (NO3)3·9H2O,
Gadolinium source is Gd (NO3)3·6H2O, titanium source C16H36O4The titanium source of Ti, the present embodiment select organic solution, can be effectively controlled Ti member
The content of element, and promote to generate orthorhombic phase in subsequent sintering process.
Organic solvent in the step (1) is ethylene glycol, and various elements are mixed into solution, is used for subsequent processing, institute
Stating the additive in step (2) is tartaric acid, when additive is tartaric acid, can form claret colloidal sol, carry out to the colloidal sol
When sintering, distortion of lattice is easily brought it about, improves the generation probability of orthorhombic phase.
Further include that nano-powder is subjected to pre-burning between the step (3) and step (4), is first carried out before plasma agglomeration
Pre-burning can improve the consistency of final sintering products therefrom, improve the ferromagnetism and ferroelectricity of product, and pre-burning is in 450 DEG C of conditions
Lower sintering 2 hours.
Sintering parameter is controlled during plasma agglomeration in the step (4) includes:
Sintering temperature is 650 DEG C, 10 minutes a length of, vacuum degree 5Pa when sintering.
It is sintered under certain vacuum degree, can be further improved the consistency of sintering, while in plasma agglomeration more
It is also easy to produce orthorhombic phase.
Annealing process in the step (4) is to anneal 2 hours in 600 DEG C of air.
The consistency of the resulting bismuth ferrite base nano ceramic of the present embodiment is 98.5%.
Referring to Fig. 1, the present embodiment verifies sample structure using XRD diagram spectrum analysis, each peak of map
All there is good corresponding relationship (standard diffraction map card number with the standard diffraction map card of the orthorhombic phase structure of theoretical calculation
JCPDS is 16-6040), it was demonstrated that the object of the bismuth ferrite ceramics in the present embodiment is mutually orthorhombic phase structure.
From figure 2 it can be seen that the resulting ferrous acid bismuth-based ceramics of the present embodiment are smaller by influence of leakage current, curve obtained exists
It is almost continuous state in all ranges of voltage, then when the voltage increases, it is existing that breakdown will not occur in ferrous acid bismuth-based ceramics
As.
From figure 3, it can be seen that this area of hysteresis loop for implementing resulting ferrous acid bismuth-based ceramics is smaller, it was demonstrated that its is ferromagnetic
Property is preferable.
Please refer to Fig. 2 and Fig. 3, under different electric field conditions, the resulting ferrous acid bismuth-based ceramics of the present embodiment all have compared with
Good effect,
The present embodiment is to adulterate Gd element again on the basis of adulterating Ti, atomic radius of the Gd element when ligancy is 9
ForIts value is less than replaced Bi element radius, BiFeO3Tolerance factor t when undoped0=0.954, and this
Bi in embodiment0.8Gd0.2Fe1-xTixO3Tolerance factor be t=0.941, i.e. t < t0, it was demonstrated that the doping is easy induction
Distortion of lattice.Tetragonal phase and orthorhombic phase can be randomly generated when distortion of lattice, in the doping ratio and preparation method of the present embodiment
Under the conditions of, the accounting for the orthorhombic phase that lattice mutation generates can be improved.
Embodiment 2
The present embodiment and embodiment 1 are almost the same, the difference is that, x=0.01, the orthorhombic phase that lattice mutation generates
Accounting be 67.9%.
Embodiment 3
The present embodiment and embodiment 1 are almost the same, the difference is that, x=0.1, the orthorhombic phase that lattice mutation generates
Accounting be 76.4%.
Embodiment 4
The present embodiment and embodiment 1 are almost the same, the difference is that, additive is acetylacetone,2,4-pentanedione.
Embodiment 5
The present embodiment and embodiment 1 are almost the same, the difference is that, the sintering temperature in plasma agglomeration is 700 DEG C.
Reference examples 1
This reference examples and embodiment 1 are almost the same, the difference is that, adjustment preparation method makes gained ferrous acid bismuthino nanometer
The object of ceramics is mutually mainly tetragonal phase.
Reference examples 2
This reference examples and embodiment 1 are almost the same, the difference is that, plasma agglomeration is replaced with into conventional calcination, is had
Body are as follows: add raw materials into ball grinder, deionized water is added and carries out ball milling, drying, pre-fired powder, then carries out second of ball
Mill, is granulated to obtain green compact, puts the green body into high temperature furnace, keeps the temperature dumping, bismuth ferrite base nano ceramic of annealing to obtain.
Reference examples 3
This reference examples and embodiment 1 are almost the same, the difference is that, the Ti element in bismuth ferrite base nano ceramic is replaced
It is changed to Sr element.
The relevant parameter of above-mentioned gained bismuth ferrite base nano ceramic is measured, structure is shown in Table 1, is judged using saturation magnetization
Ferromagnetism, numerical value is bigger, illustrates that its ferromagnetism is better, judges ferroelectricity using remanent polarization, and numerical value is bigger, illustrates its iron
It is electrically better.
Table 1
Table 1 is please referred to, the measurement result of comparative example 1~4,1 products therefrom of embodiment is best, then embodiment 1 can be made
For most highly preferred embodiment of the invention, mesotartaric acid can be obviously promoted the generation of orthorhombic phase, and strengthen ferromagnetism and ferroelectricity.
Comparative example 1 and reference examples 1, referring to Fig. 4, as can be seen that curve obtained is apparent discontinuous curve, then
Products therefrom can puncture because of voltage change, at the same from table 1 it can be seen that, ferromagnetism, the ferroelectricity of 1 products therefrom of embodiment
Property and leakage current density are much better than reference examples 1, then when product object is mutually orthorhombic phase, have to the quality of product and significantly mention
It rises.
Comparative example 1 and reference examples 2,1 parameters obtained of embodiment be better than reference examples 2, therefore, the present invention in using etc. from
It is more excellent that son is sintered more traditional sintering products therefrom.
Comparative example 1 and reference examples 3, when the Ti element in embodiment 1 individually being replaced with Sr element, products therefrom
Select Ti element more excellent compared with Sr element compared with the quality of reference examples 1 and reference examples 2 height, but in the present invention.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
Centainly refer to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be any
One or more embodiment or examples in can be combined in any suitable manner.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of bismuth ferrite base nano ceramic, which is characterized in that the chemical formula of its main constituents is Bi0.8Gd0.2Fe1- xTixO3, wherein the value of x is Ti4+Doping ratio, 0.01≤x≤0.1, Bi0.8Gd0.2Fe1-xTixO3Object be mutually orthorhombic phase.
2. the preparation method of bismuth ferrite base nano ceramic according to claim 1, which comprises the following steps:
(1) bismuth source, source of iron, gadolinium source are weighed according to the molar ratio of doped chemical and matched in organic solvent with titanium source, mixed dissolution
It is set to the mixed solution of 0.05~0.2mol/L of concentration；
(2) it is added additive into mixed solution, the molar ratio of additive and mixed solution is 0.5~2:1, and stirring 3~5 is small
When, obtain colloidal sol；
(3) colloidal sol is 10~15 hours dry, drying temperature is 100~150 DEG C, and fine gtinding obtains nano-powder；
(4) nano-powder to be inserted in graphite jig, plasma agglomeration is carried out to nano-powder, rubbing down removes the carbon paper on surface,
Annealing, obtains bismuth ferrite base nano ceramic.
3. the preparation method of bismuth ferrite base nano ceramic according to claim 2, which is characterized in that in the step (1)
Bismuth source be Bi (NO3)3·5H2O, source of iron are Fe (NO3)3·9H2O, gadolinium source are Gd (NO3)3·6H2O, titanium source C16H36O4Ti。
4. the preparation method of bismuth ferrite base nano ceramic according to claim 2, which is characterized in that in the step (1)
Organic solvent be one of ethylene glycol monomethyl ether, glacial acetic acid, ethylene glycol, ethyl alcohol or a variety of combinations.
5. the preparation method of bismuth ferrite base nano ceramic according to claim 2, which is characterized in that in the step (2)
Additive be one of tartaric acid, acetylacetone,2,4-pentanedione, citric acid or a variety of combinations.
6. the preparation method of bismuth ferrite base nano ceramic according to claim 2, which is characterized in that the step (3) and
It further include that nano-powder is subjected to pre-burning between step (4).
7. the preparation method of bismuth ferrite base nano ceramic according to claim 6, which is characterized in that the pre-burning be
It is sintered 1~3 hour under the conditions of 400~500 DEG C.
8. the preparation method of bismuth ferrite base nano ceramic according to claim 2, which is characterized in that in the step (4)
Plasma agglomeration during control sintering parameter it is as follows:
Sintering temperature is 500~700 DEG C, and when sintering is 10~15 minutes a length of.
9. the preparation method of bismuth ferrite base nano ceramic according to claim 8, which is characterized in that the sintering parameter is also
Vacuum degree including control sintering environment is 2~10Pa.
10. the preparation method of bismuth ferrite base nano ceramic according to claim 2, which is characterized in that in the step (4)
Annealing process be anneal 1~3 hour in 400~600 DEG C of air.
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| CN110451575A (en) * | 2019-09-11 | 2019-11-15 | 哈尔滨工业大学 | A method of bismuth ferrate nano powder magnetic is enhanced based on dimensional effect |
| CN110498676A (en) * | 2019-09-17 | 2019-11-26 | 江西科技学院 | A kind of nano ceramics and preparation method |
| CN113030518A (en) * | 2021-03-08 | 2021-06-25 | 淮阴工学院 | Analysis method for periodic strip domain structure of ferroelectric ceramic |
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| CN110272286A (en) * | 2019-07-23 | 2019-09-24 | 中国科学技术大学 | A method of improving ferrous acid bismuth-based ceramics ferromagnetism and magneto-electric coupled coefficient |
| CN110272286B (en) * | 2019-07-23 | 2020-10-27 | 中国科学技术大学 | Method for improving ferromagnetic and magnetoelectric coupling coefficient of bismuth ferrite-based ceramic |
| CN110451575A (en) * | 2019-09-11 | 2019-11-15 | 哈尔滨工业大学 | A method of bismuth ferrate nano powder magnetic is enhanced based on dimensional effect |
| CN110451575B (en) * | 2019-09-11 | 2022-04-05 | 哈尔滨工业大学 | Method for enhancing magnetic property of bismuth ferrite nanopowder based on size effect |
| CN110498676A (en) * | 2019-09-17 | 2019-11-26 | 江西科技学院 | A kind of nano ceramics and preparation method |
| CN113030518A (en) * | 2021-03-08 | 2021-06-25 | 淮阴工学院 | Analysis method for periodic strip domain structure of ferroelectric ceramic |
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