CN102249676A - Preparation method of low dielectric loss BaFe0.5Nb0.5O3 ceramics - Google Patents
Preparation method of low dielectric loss BaFe0.5Nb0.5O3 ceramics Download PDFInfo
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- CN102249676A CN102249676A CN2011101272635A CN201110127263A CN102249676A CN 102249676 A CN102249676 A CN 102249676A CN 2011101272635 A CN2011101272635 A CN 2011101272635A CN 201110127263 A CN201110127263 A CN 201110127263A CN 102249676 A CN102249676 A CN 102249676A
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Abstract
The invention relates to a preparation method of low dielectric loss BaFe0.5Nb0.5O3 ceramics. The method comprises the steps of: compounding analytically pure BaCO3, Fe2O3 and Nb2O5 and conducting ball milling for 4 hours, after stoving, sieving, briquetting and presintering, thus obtaining low dielectric loss BaFe0.5Nb0.5O3 powder; taking analytically pure BaCO3 and TiO2 for ball milling, then conducting stoving, sieving, briquetting and presintering, thus obtaining low dielectric loss BaFe0.5Nb0.5O3 powder; mixing the BaFe0.5Nb0.5O3 and BaTio3 powder uniformly and adding a PVA (polyvinyl alcohol) adhesive so as to obtain low dielectric loss BaFe0.5Nb0.5O3 mixed powder; subjecting the mixed powder to compression molding according to needs, then performing sintering, thus obtaining the low dielectric loss BaFe0.5Nb0.5O3 ceramics characterized by huge dielectric constant and very low dielectric loss. The dielectric constant of 1kHz of BaFe0.5Nb0.5O3 ceramics ranges from 13300-21000, while the dielectric loss ranges from 0.14-0.32. Able to be sintered at a temperature of 1350DEG C, the low dielectric loss BaFe0.5Nb0.5O3 ceramics provided in the invention has a simple preparation process.
Description
Technical field
The invention belongs to material science, relate to a kind of low-dielectric loss iron niobic acid titanate ceramics and preparation method thereof
Background technology
Since nineteen forty-seven invention transistor, particularly after the invention unicircuit in 1958, the microelectronics development is extremely rapid.Microelectronic industry has based on this become one of most important mainstay industry in the national economy.Needs based on new application requiring and raising share of market and competitive power must improve constantly the performance of integrated circuits and the ratio of performance to price.For this reason, need the characteristic dimension of continuous reduction of device, improve the integrated level of chip and the area of increase silicon chip, this also is the main path of microelectronics development.Dennard had invented very important circuit one dynamic RAM (DRAM) of being made up of two basic devices in 1967, the design of traditional DRAM has utilized the silicon-dioxide amorphous layer that forms naturally at silicon face as dielectric substance very cleverly, and technology is simple and ripe.But along with the integrated level of silicon industry constantly improves, the storage density of DRAM also needs continuous raising, and this also just requires information storage at littler area.If wherein when area reduces, reduce dielectric thickness simultaneously, can keep the constant of capacitance.Traditional processing method also improves the integrated level and the performance of device just by the thickness that constantly reduces silicon-dioxide, but present dielectric thickness approaches the electron tunneling zone just rapidly, along with the reducing of thickness, is exponential growth at this regional leakage current.For this reason, in order to continue to improve the storage density of memory period, from the eighties in 20th century researcher two kinds of possible approach have been proposed.One changes original electrode structure, becomes the spatial three-dimensional structure by the two-dimensional plane structure, uses the spatial electrode structure, can effectively increase the surface-area of electrode in limited area.Second kind of approach is to adopt than the medium layer of the bigger dielectric substance of present dielectric specific inductivity as electrical condenser, thereby reaches the requirement that improves integrated level.To the nineties in 20th century, semiconductor makers find, just progressively move towards the limit by changing technologic methods such as electrode structure,, its advantage continues to use the simple maturation process of tradition though being to change dielectric layer, but complicated three-dimensional arrangement is accomplished on the existing processes level to be unusual difficulty, and its expense also is very huge.Particularly importantly, along with the develop rapidly of science and technology, the development of microelectronic process engineering exceeds people's expection, and this makes that seeking new high dielectric-constant dielectric material becomes a very urgent research work at present.
The iron niobic acid barium (BaFe of composite perofskite type structure
0.5Nb
0.5O
3) cause investigator's extensive concern because of having the huge dielectric constant effect.It is at first obtained by solid phase method is synthetic in 2002 by Saha and Sinha etc.Present correlative study work mainly is to adopt different synthetic and preparation technology (sol-gel method, microwave-assisted synthesis method, FeNbO
4Precursor solid sintering technology etc.) its Effect on Performance of preparation iron niobic acid titanate ceramics, and research processing method.Sum up pertinent literature, we can find that iron niobic acid barium shortcoming is that dielectric loss is bigger, dielectric loss under the room temperature is about 4.29 (1kHz), this shortcoming has seriously restricted the practical application of this stupalith, the high-k that how to keep iron niobic acid barium reduces its dielectric loss and seems particularly urgent.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of low-dielectric loss iron niobic acid titanate ceramics, the iron niobic acid titanate ceramics of process modification still has huge dielectric constant, yet its dielectric loss has obtained remarkable reduction.
For achieving the above object, the technical solution used in the present invention is:
1) presses chemical general formula BaFe
0.5Nb
0.5O
3, get analytically pure BaCO
3, Fe
2O
3And Nb
2O
5Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1250 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
2) press chemical general formula BaTiO
3, get analytically pure BaCO
3And TiO
2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1200 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
3) chemical general formula is (1-x) BaFe
0.5Nb
0.5O
3-xBaTiO
3Mass ratio with BaFe
0.5Nb
0.5O
3And BaTiO
3Powder mixes, and wherein x is BaTiO
3Massfraction, and 0.1≤x≤0.4;
4) the PVA tackiness agent that adds mixture quality 8%～15% in the mixture of step 3) sieves through 60 orders and 120 eye mesh screens, obtains the mixed powder of required low-dielectric loss iron niobic acid barium;
5) with mixed powder compression moulding on demand, at 550 ℃, be incubated 4 hours and get rid of tackiness agent PVA, obtained low-dielectric loss iron niobic acid titanate ceramics in 0.5～2 hour at 1350 ℃ of following sintering then.
Described PVA tackiness agent is to be meant that mass concentration is 5% polyvinyl alcohol water solution.
The low-dielectric loss iron niobic acid titanate ceramics of the present invention preparation have huge dielectric constant and a low-down dielectric loss, specific inductivity is 13300～21000 during 1kHz, dielectric loss is 0.14～0.32.This low-dielectric loss iron niobic acid titanate ceramics can be under 1350 ℃ condition sintering.The preparation technology of this low-dielectric loss iron niobic acid titanate ceramics is simple.
Description of drawings
Fig. 1 is x=0.1, and promptly chemical general formula is 0.9BaFe
0.5Nb
0.5O
3-0.1BaTiO
3The time, the X-ray diffractogram of iron niobic acid titanate ceramics.
Fig. 2 is x=0.2, and promptly chemical general formula is 0.8BaFe
0.5Nb
0.5O
3-0.2BaTiO
3The time, the X-ray diffractogram of iron niobic acid titanate ceramics.
Fig. 3 is x=0.3, and promptly chemical general formula is 0.7BaFe
0.5Nb
0.5O
3-0.3BaTiO
3The time, the X-ray diffractogram of iron niobic acid titanate ceramics.
Fig. 4 is x=0.4, and promptly chemical general formula is 0.6BaFe
0.5Nb
0.5O
3-0.4BaTiO
3The time, the X-ray diffractogram of iron niobic acid titanate ceramics.
Fig. 5 is x=0.1, and promptly chemical general formula is 0.9BaFe
0.5Nb
0.5O
3-0.1BaTiO
3The time, the dielectric properties of iron niobic acid titanate ceramics.As seen from the figure, the specific inductivity of 1kHz iron niobic acid titanate ceramics and dielectric loss are respectively 21000 and 0.31.
Fig. 6 is x=0.2, and promptly chemical general formula is 0.8BaFe
0.5Nb
0.5O
3-0.2BaTiO
3The time, the dielectric properties of iron niobic acid titanate ceramics.As seen from the figure, the specific inductivity of 1kHz iron niobic acid titanate ceramics and dielectric loss are respectively 14600 and 0.18.
Fig. 7 is x=0.3, and promptly chemical general formula is 0.7BaFe
0.5Nb
0.5O
3-0.3BaTiO
3The time, the dielectric properties of iron niobic acid titanate ceramics.As seen from the figure, the specific inductivity of 1kHz iron niobic acid titanate ceramics and dielectric loss are respectively 13600 and 0.17.
Fig. 8 is x=0.4, and promptly chemical general formula is 0.6BaFe
0.5Nb
0.5O
3-0.4BaTiO
3The time, the dielectric properties of iron niobic acid titanate ceramics.As seen from the figure, the specific inductivity of 1kHz iron niobic acid titanate ceramics and dielectric loss are respectively 13300 and 0.13.
Fig. 9 is x=0.1, and promptly chemical general formula is 0.9BaFe
0.5Nb
0.5O
3-0.1BaTiO
3The time, the microstructure photograph of iron niobic acid titanate ceramics.
Figure 10 is x=0.2, and promptly chemical general formula is 0.8BaFe
0.5Nb
0.5O
3-0.2BaTiO
3The time, the microstructure photograph of iron niobic acid titanate ceramics.
Figure 11 is x=0.3, and promptly chemical general formula is 0.7BaFe
0.5Nb
0.5O
3-0.3BaTiO
3The time, the microstructure photograph of iron niobic acid titanate ceramics.。
Figure 12 is x=0.4, and promptly chemical general formula is 0.6BaFe
0.5Nb
0.5O
3-0.4BaTiO
3The time, the microstructure photograph of iron niobic acid titanate ceramics.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1:
1) presses chemical general formula BaFe
0.5Nb
0.5O
3, get analytically pure BaCO
3, Fe
2O
3And Nb
2O
5Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1250 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
2) press chemical general formula BaTiO
3, get analytically pure BaCO
3And TiO
2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1200 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
3) chemical general formula is 0.9BaFe
0.5Nb
0.5O
3-0.1BaTiO
3Mass ratio with BaFe
0.5Nb
0.5O
3And BaTiO
3Powder mixes, and wherein x is BaTiO
3Massfraction;
4) the PVA tackiness agent that adds mixture quality 8% in the mixture of step 3) sieves through 60 orders and 120 eye mesh screens, obtains the mixed powder of required low-dielectric loss iron niobic acid barium;
Described PVA tackiness agent is to be meant that mass concentration is 5% polyvinyl alcohol water solution.
5) with mixed powder compression moulding on demand, at 550 ℃, be incubated 4 hours and get rid of tackiness agent PVA, obtained low-dielectric loss iron niobic acid titanate ceramics in 0.5 hour at 1350 ℃ of following sintering then, the X-ray diffractogram of the low-dielectric loss iron niobic acid titanate ceramics of present embodiment preparation as described in Figure 1, as seen from Figure 1, prepared pottery is the monocline perovskite structure.Dielectric properties as shown in Figure 5, as seen from Figure 5, the specific inductivity and the dielectric loss of 1kHz iron niobic acid titanate ceramics are respectively 21000 and 0.31, microstructure photograph such as Fig. 9, prepared as seen from Figure 9 ceramic structure densification.
Embodiment 2:
1) presses chemical general formula BaFe
0.5Nb
0.5O
3, get analytically pure BaCO
3, Fe
2O
3And Nb
2O
5Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1250 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
2) press chemical general formula BaTiO
3, get analytically pure BaCO
3And TiO
2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1200 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
3) chemical general formula is 0.8BaFe
0.5Nb
0.5O
3-0.2BaTiO
3Mass ratio with BaFe
0.5Nb
0.5O
3And BaTiO
3Powder mixes, and wherein x is BaTiO
3Massfraction;
4) the PVA tackiness agent that adds mixture quality 10% in the mixture of step 3) sieves through 60 orders and 120 eye mesh screens, obtains the mixed powder of required low-dielectric loss iron niobic acid barium;
Described PVA tackiness agent is to be meant that mass concentration is 5% polyvinyl alcohol water solution.
5) with mixed powder compression moulding on demand, at 550 ℃, be incubated 4 hours and get rid of tackiness agent PVA, obtained low-dielectric loss iron niobic acid titanate ceramics in 1.5 hours at 1350 ℃ of following sintering then.The X-ray diffractogram of the low-dielectric loss iron niobic acid titanate ceramics of present embodiment preparation as described in Figure 2, prepared as seen from Figure 2 pottery is the monocline perovskite structure.Dielectric properties as shown in Figure 6, as seen from Figure 6, the specific inductivity and the dielectric loss of 1kHz iron niobic acid titanate ceramics are respectively 14600 and 0.18, microstructure photograph such as Figure 10, prepared as seen from Figure 10 ceramic structure densification.
Embodiment 3:
1) presses chemical general formula BaFe
0.5Nb
0.5O
3, get analytically pure BaCO
3, Fe
2O
3And Nb
2O
5Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1250 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
2) press chemical general formula BaTiO
3, get analytically pure BaCO
3And TiO
2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1200 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
3) chemical general formula is 0.7BaFe
0.5Nb
0.5O
3-0.3BaTiO
3Mass ratio with BaFe
0.5Nb
0.5O
3And BaTiO
3Powder mixes, and wherein x is BaTiO
3Massfraction;
4) the PVA tackiness agent that adds mixture quality 12% in the mixture of step 3) sieves through 60 orders and 120 eye mesh screens, obtains the mixed powder of required low-dielectric loss iron niobic acid barium;
Described PVA tackiness agent is to be meant that mass concentration is 5% polyvinyl alcohol water solution.
5) with mixed powder compression moulding on demand, at 550 ℃, be incubated 4 hours and get rid of tackiness agent PVA, obtained low-dielectric loss iron niobic acid titanate ceramics in 2 hours at 1350 ℃ of following sintering then.The X-ray diffractogram of the low-dielectric loss iron niobic acid titanate ceramics of present embodiment preparation as described in Figure 3, prepared as seen from Figure 3 pottery is the monocline perovskite structure.Dielectric properties as shown in Figure 7, as seen from Figure 7, the specific inductivity and the dielectric loss of 1kHz iron niobic acid titanate ceramics are respectively 13600 and 0.17, microstructure photograph such as Figure 11, prepared as seen from Figure 11 ceramic structure densification.
Embodiment 4:
1) presses chemical general formula BaFe
0.5Nb
0.5O
3, get analytically pure BaCO
3, Fe
2O
3And Nb
2O
5Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1250 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
2) press chemical general formula BaTiO
3, get analytically pure BaCO
3And TiO
2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1200 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
3) chemical general formula is 0.6BaFe
0.5Nb
0.5O
3-0.4BaTiO
3Mass ratio with BaFe
0.5Nb
0.5O
3And BaTiO
3Powder mixes, and wherein x is BaTiO
3Massfraction;
4) the PVA tackiness agent that adds mixture quality 15% in the mixture of step 3) sieves through 60 orders and 120 eye mesh screens, obtains the mixed powder of required low-dielectric loss iron niobic acid barium;
Described PVA tackiness agent is to be meant that mass concentration is 5% polyvinyl alcohol water solution.
5) with mixed powder compression moulding on demand, at 550 ℃, be incubated 4 hours and get rid of tackiness agent PVA, obtained low-dielectric loss iron niobic acid titanate ceramics in 1 hour at 1350 ℃ of following sintering then.The X-ray diffractogram of the low-dielectric loss iron niobic acid titanate ceramics of present embodiment preparation as described in Figure 4, prepared as seen from Figure 4 pottery is the monocline perovskite structure.Dielectric properties as shown in Figure 8, as seen from Figure 8, the specific inductivity and the dielectric loss of 1kHz iron niobic acid titanate ceramics are respectively 13300 and 0.13, microstructure photograph such as Figure 12, prepared as seen from Figure 12 ceramic structure densification.
Claims (2)
1. the preparation method of a low-dielectric loss iron niobic acid titanate ceramics is characterized in that:
1) presses chemical general formula BaFe
0.5Nb
0.5O
3, get analytically pure BaCO
3, Fe
2O
3And Nb
2O
5Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1250 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
2) press chemical general formula BaTiO
3, get analytically pure BaCO
3And TiO
2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1200 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained low-dielectric loss iron niobic acid barium powder;
3) chemical general formula is (1-x) BaFe
0.5Nb
0.5O
3-xBaTiO
3Mass ratio with BaFe
0.5Nb
0.5O
3And BaTiO
3Powder mixes, and wherein x is BaTiO
3Massfraction, and 0.1≤x≤0.4;
4) the PVA tackiness agent that adds mixture quality 8%～15% in the mixture of step 3) sieves through 60 orders and 120 eye mesh screens, obtains the mixed powder of required low-dielectric loss iron niobic acid barium;
5) with mixed powder compression moulding on demand, at 550 ℃, be incubated 4 hours and get rid of tackiness agent PVA, obtained low-dielectric loss iron niobic acid titanate ceramics in 0.5～2 hour at 1350 ℃ of following sintering then.
2. the preparation method of low-dielectric loss iron niobic acid titanate ceramics according to claim 1 is characterized in that: described PVA tackiness agent is to be meant that mass concentration is 5% polyvinyl alcohol water solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557026A (en) * | 2015-01-14 | 2015-04-29 | 陕西科技大学 | BaTiO3/Ba(Fe0.5Nb0.5)O3 lamellar ferroelectric composite material as well as preparation method thereof |
| CN107215902A (en) * | 2017-05-26 | 2017-09-29 | 常熟理工学院 | A kind of preparation method of lithium ion battery negative material niobic acid iron |
Citations (2)
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|---|---|---|---|---|
| CN101792315A (en) * | 2010-04-07 | 2010-08-04 | 陕西科技大学 | Preparation method of low temperature sintered small-loss iron barium niobate ceramic |
| CN101792319A (en) * | 2010-04-07 | 2010-08-04 | 陕西科技大学 | Preparation method of low temperature sintered magnetoelectric composite ceramic material |
-
2011
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| CN101792315A (en) * | 2010-04-07 | 2010-08-04 | 陕西科技大学 | Preparation method of low temperature sintered small-loss iron barium niobate ceramic |
| CN101792319A (en) * | 2010-04-07 | 2010-08-04 | 陕西科技大学 | Preparation method of low temperature sintered magnetoelectric composite ceramic material |
Non-Patent Citations (2)
| Title |
|---|
| N.K.SINGH ET AL.: "study of structural, dielectric and electrical behavior of（1-x）Ba(Fe0.5Nb0.5)O3-xSrTiO3 ceramics", 《JOURNAL OF ALLOYS AND COMPOUNDS》, vol. 509, 30 November 2010 (2010-11-30), pages 2957 - 2963, XP027589792 * |
| URAINWAN INTATHA ET AL.: "Impedance study of giant dielectric permittivity in BaFe0.5Nb0.5O3 perovskite ceramic", 《CURRENT APPLIED PHYSICS》, vol. 10, 16 April 2009 (2009-04-16), pages 21 - 25, XP026546912, DOI: 10.1016/j.cap.2009.04.006 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557026A (en) * | 2015-01-14 | 2015-04-29 | 陕西科技大学 | BaTiO3/Ba(Fe0.5Nb0.5)O3 lamellar ferroelectric composite material as well as preparation method thereof |
| CN107215902A (en) * | 2017-05-26 | 2017-09-29 | 常熟理工学院 | A kind of preparation method of lithium ion battery negative material niobic acid iron |
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Application publication date: 20111123 |