CN104557026A - BaTiO3/Ba(Fe0.5Nb0.5)O3 lamellar ferroelectric composite material as well as preparation method thereof - Google Patents
BaTiO3/Ba(Fe0.5Nb0.5)O3 lamellar ferroelectric composite material as well as preparation method thereof Download PDFInfo
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- CN104557026A CN104557026A CN201510018787.9A CN201510018787A CN104557026A CN 104557026 A CN104557026 A CN 104557026A CN 201510018787 A CN201510018787 A CN 201510018787A CN 104557026 A CN104557026 A CN 104557026A
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- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 229910002113 barium titanate Inorganic materials 0.000 title abstract 4
- 239000000843 powder Substances 0.000 claims abstract description 119
- 230000004888 barrier function Effects 0.000 claims abstract description 16
- 238000000748 compression moulding Methods 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 225
- 229910052742 iron Inorganic materials 0.000 claims description 41
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 39
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 39
- 239000003795 chemical substances by application Substances 0.000 claims description 32
- 239000000126 substance Substances 0.000 claims description 31
- 150000001875 compounds Chemical class 0.000 claims description 15
- 238000005469 granulation Methods 0.000 claims description 13
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 3
- 230000005621 ferroelectricity Effects 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 16
- 238000005245 sintering Methods 0.000 description 15
- 239000000463 material Substances 0.000 description 11
- 238000000227 grinding Methods 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000010287 polarization Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
The invention relates to a BaTiO3/Ba(Fe0.5Nb0.5)O3 lamellar ferroelectric composite material as well as a preparation method thereof. The preparation method comprises the following steps: firstly preparing Ba(Fe0.5Nb0.5)O3 powder and BaTiO3 powder; then granulating the powder and screening the powder to obtain the Ba(Fe0.5Nb0.5)O3 powder and BaTiO3 powder; and carrying out compression moulding on the two powder in a 2-2 composite barrier layer superposition and arrangement manner in a die, cofiring ferro-electric phases in a way of lamellar composition. Interaction of the two phases can be effectively inhibited so as to maintain the characteristics, so that the prepared composite material not only has relatively good ferroelectricity, but also effectively reduces the dielectric loss. According to the prepared lamellar ferroelectric composite material provided by the invention, the dielectric loss is just 0.1-0.2 when the frequency is 100Hz.
Description
Technical field
The invention belongs to material science, relate to a kind of BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite and preparation method thereof.
Background technology
Along with continuing to bring out of electronic message unit Large and middle scale IC and portable communications instrument, ferrite device is to the even integrated future development of miniaturization, microminiaturization, chip type, more and more higher requirement is proposed to the dielectric properties of electronic material, wish to obtain the having superior novel electron material of the over-all properties such as high-dielectric coefficient, low-loss, easily processing, this is difficult to realize in one-component.Ferroelectric Composites just can use less resource, takies less volume.Therefore, research and develop efficient Ferroelectric Composites and have very important meaning for the development of large-scale integrated circuit technology.
Ba (Fe
0.5nb
0.5) O
3belong to composite perofskite material.What this kind of material had has supraconductivity, ionic conductivity and high specific inductivity.But this kind of pottery still also exists obvious shortcoming in the application, under such as room temperature, dielectric loss is comparatively large, and this is the key hindering the practical application of huge dielectric constant material.
Under electrostatic field, the dielectric loss of ceramic dielectic is only caused by the conductance process of dielectric material, and that is dielectric loss only depends on specific conductivity and the strength of electric field of material; Under action of alternative electric field, the dielectric loss of ceramic dielectic is except the specific conductivity that depends on material and strength of electric field, some is caused by dielectric polarization, and mainly in stiff polarization process of establishing, charging point absorbs the thermal motion that a part of electric field energy is converted into particle and loses.Dielectric loss is all very sensitive to factors such as chemical constitution, phase composite, structures, and every factor affecting conductance and polarization all has impact to the dielectric dielectric loss of energy storage ceramic.Dielectric loss not only consumes electric energy, and the device temperature rising caused by dielectric loss can affect the normal work of device, needs to control dielectric loss, make it the smaller the better when therefore preparing energy storage dielectric ceramics.
Therefore, how reduced the dielectric loss of this kind of material by the method for replacing or adulterate, and strengthen its temperature stability while maintenance huge dielectric constant, be one and significantly work.
Summary of the invention
The object of the present invention is to provide a kind of BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite and preparation method thereof, the method can prepare the lower Ferroelectric Composites of dielectric loss.
For achieving the above object, the present invention adopts following technical scheme:
A kind of BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite, the chemical formula of this lamina-like iron composite is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and 11.1%≤x≤33.3%.
The chemical formula of this lamina-like iron composite is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=11.1%, 22.2% or 33.3%.
A kind of BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, comprises the following steps:
1) by chemical formula Ba (Fe
0.5nb
0.5) O
3by analytically pure BaCO
3, Fe
2o
3, Nb
2o
5mixed by ball milling after preparation, then sieve, briquetting, then through 1150 ~ 1200 DEG C of pre-burnings 4 ~ 6 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain Ba (Fe
0.5nb
0.5) O
3powder;
2) by chemical formula BaTiO
3by analytically pure BaCO
3, TiO
2mixed by ball milling after preparation, then sieve, then through 1150 ~ 1200 DEG C of pre-burnings 4 ~ 6 hours, obtain bulk product, cross 120 mesh sieves after then being pulverized by gained bulk sample, obtain BaTiO
3powder;
3) respectively to Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3add granulation after PVA tackiness agent in powder, then sieve through 60 eye mesh screens, obtain Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3powder;
4) by chemical formula x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and 11.1%≤x≤33.3%, by Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3powder is arranged under the overlay mode according to the barrier layer of 2-2 compound, in a mold compression moulding; Then get rid of PVA tackiness agent, then at 1330 ~ 1350 DEG C, sinter 2 ~ 4 hours one-tenth porcelain, obtain BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite.
Described step 1), step 2) in Ball-milling Time be 4 ~ 6 hours.
To Ba (Fe
0.5nb
0.5) O
3the quality adding PVA tackiness agent in powder is Ba (Fe
0.5nb
0.5) O
38 ~ 15% of powder quality; To BaTiO
3the quality adding PVA tackiness agent in powder is BaTiO
38 ~ 15% of powder quality.
Described PVA tackiness agent is the polyvinyl alcohol water solution of mass concentration 10%.
The barrier layer of described 2-2 compound is arranged under the overlay mode and is specially: according to being followed successively by BaTiO from the top down
3powder, Ba (Fe
0.5nb
0.5) O
3powder, BaTiO
3the order of powder stacks together; Or according to being followed successively by BaTiO from the top down
3powder, Ba (Fe
0.5nb
0.5) O
3powder, BaTiO
3powder, Ba (Fe
0.5nb
0.5) O
3powder, BaTiO
3the order of powder stacks together.
Described eliminating PVA tackiness agent is specifically: at temperature is 550-600 DEG C, be incubated 3-5 hour.
Compared with prior art, the beneficial effect that has of the present invention: the present invention first prepares Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3powder, sieves after then two kinds of powders being carried out granulation, obtains Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3powder, then two kinds of powder are arranged under the overlay mode according to the barrier layer of 2-2 compound, in a mold after compression moulding, ferroelectric phase is burnt together altogether in the mode of lamellar composite, effectively can suppress reacting to each other thus keeping respective characteristic between two-phase, make the matrix material obtained not only have good ferroelectricity but also can effectively reduce its dielectric loss.The present invention passes through at Ba (Fe
0.5nb
0.5) O
3middle doping BaTiO
3, significantly reduce the dielectric loss of matrix material.
The lamina-like iron composite that the present invention obtains is when frequency is 100Hz, and dielectric loss is only 0.1 ~ 0.2, when being 100Hz well below frequency, and BFN (Ba (Fe
0.5nb
0.5) O
3) dielectric loss 3 ~ 4 of pure phase, and matrix material compactness is good, exists, two-phase even grain size, all at systems, without obvious interface atoms diffusion phenomena without obvious gross blow hole.
Accompanying drawing explanation
Fig. 1 is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=11.1%, the structure iron of composite ceramics when 1350 DEG C of sintering.
Fig. 2 is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=22.2%, the structure iron of composite ceramics when 1350 DEG C of sintering.
Fig. 3 is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=33.3%, the structure iron of composite ceramics when 1350 DEG C of sintering.
Fig. 4 is x Ba (Fe under room temperature
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=11.1%, composite ceramics is at the SEM figure of 1350 DEG C of sintering rear interfaces.
Fig. 5 is x Ba (Fe under room temperature
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=22.2%, composite ceramics is at the SEM figure of 1350 DEG C of sintering rear interfaces.
Fig. 6 is x Ba (Fe under room temperature
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=33.3%, composite ceramics is at the SEM figure of 1350 DEG C of sintering rear interfaces.
Fig. 7 is x Ba (Fe under room temperature
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=11.1%, the dielectric and magnetic of composite ceramics after 1350 DEG C of sintering.
Fig. 8 is x Ba (Fe under room temperature
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=22.2%, the dielectric and magnetic of composite ceramics after 1350 DEG C of sintering.
Fig. 9 is x Ba (Fe under room temperature
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=33.3%, the dielectric and magnetic of composite ceramics after 1350 DEG C of sintering.
In figure, 1 is BaTiO
3powder, 2 is Ba (Fe
0.5nb
0.5) O
3powder.
Embodiment
Be described in detail below in conjunction with the drawings and specific embodiments.
Embodiment 1
A kind of BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the chemical formula of lamina-like iron composite is xBa (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=11.1%.
Above-mentioned BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, comprises the following steps:
1) by chemical formula Ba (Fe
0.5nb
0.5) O
3by analytically pure BaCO
3, Fe
2o
3, Nb
2o
5within 4 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1150 DEG C of pre-burnings 6 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain Ba (Fe
0.5nb
0.5) O
3powder;
2) by chemical formula BaTiO
3by analytically pure BaCO
3, TiO
2within 6 hours, mixed by wet ball grinding after preparation, then dry, sieve, then through 1180 DEG C of pre-burnings 5 hours, obtain bulk product, cross 120 mesh sieves after then being pulverized by gained bulk sample and obtain BaTiO
3powder;
3) to Ba (Fe
0.5nb
0.5) O
3add in powder and account for Ba (Fe
0.5nb
0.5) O
3granulation after the PVA tackiness agent of powder quality 10%, then sieve through 60 eye mesh screens, obtain Ba (Fe
0.5nb
0.5) O
3powder; To BaTiO
3add in powder and account for BaTiO
3granulation after the PVA tackiness agent of powder quality 10%, then sieve through 60 eye mesh screens, obtain BaTiO
3powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of mass concentration 10%.
4) by chemical formula x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=11.1%, by Ba (Fe
0.5nb
0.5) O
3and BaTiO
3powder is arranged under the overlay mode according to the barrier layer of 2-2 compound, in a mold compression moulding; Then at temperature is 560 DEG C, be incubated 4 hours, get rid of PVA tackiness agent, then at 1350 DEG C, sinter 2 hours one-tenth porcelain, obtain BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite.Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: according to being followed successively by BaTiO from the top down
3powder 1, Ba (Fe
0.5nb
0.5) O
3powder 2, BaTiO
3the order of powder 1 stacks together.
Fig. 1 is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=11.1%, the structure iron of composite ceramics when 1350 DEG C of sintering.
From figure, 4 can find out, good in the material compactness of 1350 DEG C of sintering, exist, two-phase even grain size, all at systems, without obvious interface atoms diffusion phenomena without obvious gross blow hole.As seen from Figure 7, matrix material dielectric loss within the scope of 100 ~ 1MHz is 0.2 ~ 0.3.
Embodiment 2
A kind of BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the chemical formula of lamina-like iron composite is xBa (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=22.2%.
Above-mentioned BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, comprises the following steps:
1) by chemical formula Ba (Fe
0.5nb
0.5) O
3by analytically pure BaCO
3, Fe
2o
3, Nb
2o
5within 5 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1200 DEG C of pre-burnings 4 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain Ba (Fe
0.5nb
0.5) O
3powder;
2) by chemical formula BaTiO
3by analytically pure BaCO
3, TiO
2within 4 hours, mixed by wet ball grinding after preparation, then dry, sieve, then through 1170 DEG C of pre-burnings 5.5 hours, obtain bulk product, cross 120 mesh sieves after then being pulverized by gained bulk sample and obtain BaTiO
3powder;
3) to Ba (Fe
0.5nb
0.5) O
3add in powder and account for Ba (Fe
0.5nb
0.5) O
3granulation after the PVA tackiness agent of powder quality 12%, then sieve through 60 eye mesh screens, obtain Ba (Fe
0.5nb
0.5) O
3powder; To BaTiO
3add in powder and account for BaTiO
3granulation after the PVA tackiness agent of powder quality 12%, then sieve through 60 eye mesh screens, obtain BaTiO
3powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of mass concentration 10%.
4) by chemical formula x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=22.2%, by Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3powder is arranged under the overlay mode according to the barrier layer of 2-2 compound, in a mold compression moulding; Then at temperature is 570 DEG C, be incubated 3.5 hours, get rid of PVA tackiness agent, then at 1350 DEG C, sinter 3 hours one-tenth porcelain, obtain BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite.Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: according to being followed successively by BaTiO from the top down
3powder, Ba (Fe
0.5nb
0.5) O
3powder, BaTiO
3powder, Ba (Fe
0.5nb
0.5) O
3powder, BaTiO
3the order of powder stacks together.
Fig. 2 is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=22.2%, the structure iron of composite ceramics when 1350 DEG C of sintering.
From figure, 5 can find out, good in the material compactness of 1350 DEG C of sintering, exist, two-phase even grain size, all at systems, without obvious interface atoms diffusion phenomena without obvious gross blow hole.As seen from Figure 8, matrix material dielectric loss is in 0.1 ~ 0.4.
Embodiment 3
A kind of BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the chemical formula of lamina-like iron composite is xBa (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=33.3%.
Above-mentioned BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, comprises the following steps:
1) by chemical formula Ba (Fe
0.5nb
0.5) O
3by analytically pure BaCO
3, Fe
2o
3, Nb
2o
5within 6 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1160 DEG C of pre-burnings 5 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain Ba (Fe
0.5nb
0.5) O
3powder;
2) by chemical formula BaTiO
3by analytically pure BaCO
3, TiO
2within 5 hours, mixed by wet ball grinding after preparation, then dry, sieve, then through 1200 DEG C of pre-burnings 4 hours, obtain bulk product, cross 120 mesh sieves after then being pulverized by gained bulk sample and obtain BaTiO
3powder;
3) to Ba (Fe
0.5nb
0.5) O
3add in powder and account for Ba (Fe
0.5nb
0.5) O
3granulation after the PVA tackiness agent of powder quality 15%, then sieve through 60 eye mesh screens, obtain Ba (Fe
0.5nb
0.5) O
3powder; To BaTiO
3add in powder and account for BaTiO
3granulation after the PVA tackiness agent of powder quality 15%, then sieve through 60 eye mesh screens, obtain BaTiO
3powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of mass concentration 10%.
4) by chemical formula x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=33.3%, by Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3powder is arranged under the overlay mode according to the barrier layer of 2-2 compound, in a mold compression moulding; Then at temperature is 550 DEG C, be incubated 5 hours, get rid of PVA tackiness agent, then at 1350 DEG C, sinter 4 hours one-tenth porcelain, obtain BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite.Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: according to being followed successively by BaTiO from the top down
3powder 1, Ba (Fe
0.5nb
0.5) O
3powder 2, BaTiO
3the order of powder 1 stacks together.
Fig. 3 is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3in component as x=33.3%, the structure iron of composite ceramics when 1350 DEG C of sintering.
From figure, 6 can find out, good in the material compactness of 1350 DEG C of sintering, exist, two-phase even grain size, all at systems, without obvious interface atoms diffusion phenomena without obvious gross blow hole.As seen from Figure 9, matrix material dielectric loss is 0.2 ~ 0.5.
Embodiment 4
A kind of BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the chemical formula of lamina-like iron composite is xBa (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=16%.
Above-mentioned BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, comprises the following steps:
1) by chemical formula Ba (Fe
0.5nb
0.5) O
3by analytically pure BaCO
3, Fe
2o
3, Nb
2o
5within 4.5 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1180 DEG C of pre-burnings 4.5 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain Ba (Fe
0.5nb
0.5) O
3powder;
2) by chemical formula BaTiO
3by analytically pure BaCO
3, TiO
2within 5.5 hours, mixed by wet ball grinding after preparation, then dry, sieve, then through 1150 DEG C of pre-burnings 6 hours, obtain bulk product, cross 120 mesh sieves after then being pulverized by gained bulk sample and obtain BaTiO
3powder;
3) to Ba (Fe
0.5nb
0.5) O
3add in powder and account for Ba (Fe
0.5nb
0.5) O
3granulation after the PVA tackiness agent of powder quality 8%, then sieve through 60 eye mesh screens, obtain Ba (Fe
0.5nb
0.5) O
3powder; To BaTiO
3add in powder and account for BaTiO
3granulation after the PVA tackiness agent of powder quality 8%, then sieve through 60 eye mesh screens, obtain BaTiO
3powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of mass concentration 10%.
4) by chemical formula x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=16%, by Ba (Fe
0.5nb
0.5) O
3and BaTiO
3powder is arranged under the overlay mode according to the barrier layer of 2-2 compound, in a mold compression moulding; Then at temperature is 580 DEG C, be incubated 5.5 hours, get rid of PVA tackiness agent, then at 1330 DEG C, sinter 3.5 hours one-tenth porcelain, obtain BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite.Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: according to being followed successively by BaTiO from the top down
3powder 1, Ba (Fe
0.5nb
0.5) O
3powder 2, BaTiO
3the order of powder 1 stacks together.
Embodiment 5
A kind of BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the chemical formula of lamina-like iron composite is xBa (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=27%.
Above-mentioned BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, comprises the following steps:
1) by chemical formula Ba (Fe
0.5nb
0.5) O
3by analytically pure BaCO
3, Fe
2o
3, Nb
2o
5within 5.5 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1190 DEG C of pre-burnings 4 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain Ba (Fe
0.5nb
0.5) O
3powder;
2) by chemical formula BaTiO
3by analytically pure BaCO
3, TiO
2within 4.5 hours, mixed by wet ball grinding after preparation, then dry, sieve, then through 1160 DEG C of pre-burnings 4 hours, obtain bulk product, cross 120 mesh sieves after then being pulverized by gained bulk sample and obtain BaTiO
3powder;
3) to Ba (Fe
0.5nb
0.5) O
3add in powder and account for Ba (Fe
0.5nb
0.5) O
3granulation after the PVA tackiness agent of powder quality 14%, then sieve through 60 eye mesh screens, obtain Ba (Fe
0.5nb
0.5) O
3powder; To BaTiO
3add in powder and account for BaTiO
3granulation after the PVA tackiness agent of powder quality 14%, then sieve through 60 eye mesh screens, obtain BaTiO
3powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of mass concentration 10%.
4) by chemical formula x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=27%, by Ba (Fe
0.5nb
0.5) O
3and BaTiO
3powder is arranged under the overlay mode according to the barrier layer of 2-2 compound, in a mold compression moulding; Then at temperature is 600 DEG C, be incubated 3 hours, get rid of PVA tackiness agent, then at 1340 DEG C, sinter 2.5 hours one-tenth porcelain, obtain BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite.Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: according to being followed successively by BaTiO from the top down
3powder 1, Ba (Fe
0.5nb
0.5) O
3powder 2, BaTiO
3the order of powder 1 stacks together.
Claims (8)
1. a BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite, is characterized in that, the chemical formula of this lamina-like iron composite is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and 11.1%≤x≤33.3%.
2. a kind of BaTiO according to claim 1
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite, is characterized in that, the chemical formula of this lamina-like iron composite is x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and x=11.1%, 22.2% or 33.3%.
3. a BaTiO as claimed in claim 1
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, is characterized in that, comprises the following steps:
1) by chemical formula Ba (Fe
0.5nb
0.5) O
3by analytically pure BaCO
3, Fe
2o
3, Nb
2o
5mixed by ball milling after preparation, then sieve, briquetting, then through 1150 ~ 1200 DEG C of pre-burnings 4 ~ 6 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain Ba (Fe
0.5nb
0.5) O
3powder;
2) by chemical formula BaTiO
3by analytically pure BaCO
3, TiO
2mixed by ball milling after preparation, then sieve, then through 1150 ~ 1200 DEG C of pre-burnings 4 ~ 6 hours, obtain bulk product, cross 120 mesh sieves after then being pulverized by gained bulk sample, obtain BaTiO
3powder;
3) respectively to Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3add granulation after PVA tackiness agent in powder, then sieve through 60 eye mesh screens, obtain Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3powder;
4) by chemical formula x Ba (Fe
0.5nb
0.5) O
3/ (1-x) BaTiO
3, wherein x is Ba (Fe
0.5nb
0.5) O
3mass percent, and 11.1%≤x≤33.3%, by Ba (Fe
0.5nb
0.5) O
3powder and BaTiO
3powder is arranged under the overlay mode according to the barrier layer of 2-2 compound, in a mold compression moulding; Then get rid of PVA tackiness agent, then at 1330 ~ 1350 DEG C, sinter 2 ~ 4 hours one-tenth porcelain, obtain BaTiO
3/ Ba (Fe
0.5nb
0.5) O
3lamina-like iron composite.
4. BaTiO according to claim 3
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, is characterized in that, described step 1), step 2) in Ball-milling Time be 4 ~ 6 hours.
5. BaTiO according to claim 3
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, is characterized in that, to Ba (Fe
0.5nb
0.5) O
3the quality adding PVA tackiness agent in powder is Ba (Fe
0.5nb
0.5) O
38 ~ 15% of powder quality; To BaTiO
3the quality adding PVA tackiness agent in powder is BaTiO
38 ~ 15% of powder quality.
6. the BaTiO according to claim 3 or 5
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, is characterized in that, described PVA tackiness agent is the polyvinyl alcohol water solution of mass concentration 10%.
7. BaTiO according to claim 3
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, is characterized in that, the barrier layer of described 2-2 compound is arranged under the overlay mode and is specially: according to being followed successively by BaTiO from the top down
3powder, Ba (Fe
0.5nb
0.5) O
3powder, BaTiO
3the order of powder stacks together; Or according to being followed successively by BaTiO from the top down
3powder, Ba (Fe
0.5nb
0.5) O
3powder, BaTiO
3powder, Ba (Fe
0.5nb
0.5) O
3powder, BaTiO
3the order of powder stacks together.
8. BaTiO according to claim 3
3/ Ba (Fe
0.5nb
0.5) O
3the preparation method of lamina-like iron composite, is characterized in that, described eliminating PVA tackiness agent specifically: at temperature is 550-600 DEG C, be incubated 3-5 hour.
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CN108863348A (en) * | 2018-07-26 | 2018-11-23 | 陕西科技大学 | A kind of dielectric ceramic material and preparation method thereof of ultra-wide temperature stability |
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CN108863349A (en) * | 2018-07-26 | 2018-11-23 | 陕西科技大学 | A kind of barium titanate-based lead-free height Jie temperature-stable ceramic material and preparation method thereof |
CN108863348A (en) * | 2018-07-26 | 2018-11-23 | 陕西科技大学 | A kind of dielectric ceramic material and preparation method thereof of ultra-wide temperature stability |
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