CN1321901C - Coprecipitation process of preparing relation base niobate ferroelectric powder - Google Patents
Coprecipitation process of preparing relation base niobate ferroelectric powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 54
- 238000000975 co-precipitation Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title abstract description 26
- 239000010955 niobium Substances 0.000 claims abstract description 65
- 239000000047 product Substances 0.000 claims abstract description 24
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 13
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 13
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 7
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 3
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- 238000005119 centrifugation Methods 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 12
- 238000004448 titration Methods 0.000 claims description 12
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- 239000012071 phase Substances 0.000 abstract description 17
- 239000000126 substance Substances 0.000 abstract description 6
- -1 niobium alkoxide Chemical class 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 2
- 239000007791 liquid phase Substances 0.000 abstract 1
- 239000012716 precipitator Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000002341 toxic gas Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 238000005245 sintering Methods 0.000 description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 239000002253 acid Substances 0.000 description 8
- JMAHHHVEVBOCPE-UHFFFAOYSA-N [Fe].[Nb] Chemical compound [Fe].[Nb] JMAHHHVEVBOCPE-UHFFFAOYSA-N 0.000 description 7
- HWHWBMBTCNLBGY-UHFFFAOYSA-N [Pb].[Ni].[Nb] Chemical compound [Pb].[Ni].[Nb] HWHWBMBTCNLBGY-UHFFFAOYSA-N 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002821 niobium Chemical class 0.000 description 1
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention belongs to the field of dielectric ceramics materials. The existing liquid phase chemical method has the disadvantages that chloride impurities remain in products, and toxic gas is generated; the price of niobium alkoxide is high, and the niobium alkoxide dissolves in water easily. The present invention comprises the following steps: mixture of Nb2O5 and KOH with the mol ratio of 1: 8 is calcined for one to two hours at the temperature of 340 to 380 DEG C and is dissolved in deionized water, nitric acid is used for titrating the pH value between two and three to obtain precipitates, the precipitates are separated and are dissolved in oxalic acid solution, and oxalic acid solution A which comprises niobium is obtained after stirring; the pH value of the solution A is titrated between 10 and 11 by ammonia water, and precipitates B are obtained after separation and washing; the precipitates B are dissolved in nitric acid solution, and Pb (NO3) 2 and nitrate of M are added according to stoichiometric ratio of the ultimate compound Pb (M, Nb) O3; hydrogen peroxide with 1 to 10 times of molal quantity of niobium is dripped, and precursor solution C is obtained after stirring for 10 to 30 min; ammonia water or diethylamine is used as precipitator for regulating the pH value of the solution to 10 to 13, and coprecipitation products are obtained; the products D are centrifuged and washed, and after dried at the temperature of 80 to 100 DEG C, the products D are calcined for one to four hours at the temperature of 800 to 900 DEG C to obtain the Pb (M, Nb) O3 powder. The process of the present invention is simple and harmless, the products have pure perovskite phases and uniform particle diameters, and the cost is lowered.
Description
Technical field
The present invention relates to a kind of coprecipitation method for preparing the relaxation base niobate ferroelectric powder, belong to the preparing technical field of dielectric ceramic material.
Background technology
Relaxor based ferroelectrics has the performance more better than common ferroelectrics, as high specific inductivity, low relatively sintering temperature, fast etc. by the low temperature coefficient of capacitance of disperse phase transformation decision, big electrostrictive effect and small strain hysteresis and zero restoring ability and favorable reproducibility, response, thereby be widely used in many fields, obtained the concern of investigator and industry member.Niobium iron acid lead Pb (Fe
1/2Nb
1/2) O
3, lead scandate columbate Pb (Sc
1/2Nb
1/2) O, niobium nickel lead plumbate Pb (Ni
1/3Nb
2/3) O
3And lead magnoniobate Pb (Mg
1/3Nb
2/3) O
3Deng being typical leaded relaxation base niobate ferroelectric.Prepare the higher calcining temperature of leaded relaxation base niobate ferroelectric needs with traditional solid reaction process, be difficult to obtain the powder of pure perovskite phase, and particle size distribution is inhomogeneous.
Liquid chemical method can overcome the deficiency of traditional solid reaction process to a certain extent, reduces the temperature and time of synthetic leaded relaxation base niobate ferroelectric, reduces energy consumption.As the coprecipitation method of one of liquid chemical method, be the optional method of synthetic high-purity multi-component material, can when guaranteeing the stoichiometric ratio of prepared material, its chemical composition be evenly distributed.During the synthetic leaded relaxation base niobate ferroelectric powder of liquid chemical method, normal compound niobium source of adopting comprises niobium chloride (NbCl
5), niobium alkoxides ((C
nH
2n+1O)
5Nb) etc.But there is certain shortcoming: NbCl separately in they
5Can cause residual chloride thing impurity in the final product, influence the electrical property of ceramic body, produce deleterious HCl gas in addition in the building-up process, be unfavorable for environment protection; Niobium alkoxides is usually used in hydrothermal method or sol-gel method craft, has good solubility, and still, it costs an arm and a leg, and very easily hydrolysis, is difficult for preserving, and promotes the use of to have difficulties in industry.
Summary of the invention
The objective of the invention is with Niobium Pentxoxide (Nb
2O
5) be converted on the basis of solubility niobium salt, provide the co-precipitation preparation method of the leaded relaxation base niobate ferroelectric powder of the simple perovskite structure of a kind of production technique, to obtain to have the relaxation base niobate ferroelectric powder of pure perovskite structure, the tiny homogeneous of particle diameter.
The co-precipitation preparation method of relaxation base niobate ferroelectric powder of the present invention is characterized in that, may further comprise the steps:
(1) with mol ratio is 1: 8 Nb
2O
5-KOH mixture is dissolved in deionized water through the product that 340-380 ℃ of calcining 1-2h obtains; Then with nitric acid titration pH value to 2-3, produce white precipitate; The white precipitate of centrifugation gained also is dissolved in oxalic acid solution, and what obtain clear after the stirring contains niobium oxalate solution A;
(2) be 10-11 with niobium oxalate solution A to the pH value that contains that obtains in the ammonia water titration step 1, obtain white depositions B through centrifugation and deionized water wash;
(3) white depositions B is dissolved in the salpeter solution that concentration is 2-4mol/l, and by final compound Pb (M, Nb) O
3Stoichiometric ratio, add Pb (NO
3)
2And and final compound Pb (M, Nb) O
3The nitrate of corresponding metal ions M, wherein M is divalence or trivalent metal ion, comprises Mg
2+, Ni
2+, Sc
3+, Fe
3+Simultaneously, dropping is equivalent to niobium molar weight 1-10 hydrogen peroxide doubly, stirs 10-30min, obtains transparent clarifying precursor solution C;
(4) with ammoniacal liquor or diethylamine as precipitation agent, the pH value of regulating precursor solution C obtains coprecipitated product D to 10-13;
(5) with the centrifugal collection of above-mentioned gained coprecipitated product D, use deionized water wash, after 80-100 ℃ of drying,, obtain final compound Pb (M, Nb) O of uhligite phase at 800-900 ℃ of calcining 1-4h
3Powder.
The present invention adopts more cheaply, the Nb of easier acquisition
2O
5Replace NbCl
5Or niobium alkoxides, by simple chemical conversion process, obtain containing the niobium salpeter solution, thereby greatly reduce the production cost of the leaded relaxation base niobate ferroelectric powder of preparation.Coprecipitation method provided by the invention can be used to prepare multiple relaxation base niobate ferroelectric powder, comprises Pb (Mg
1/3Nb
2/3) O
3, Pb (Ni
1/3Nb
2/3) O
3, Pb (Sc
1/2Nb
1/2) O
3Or Pb (Fe
1/2Nb
1/2) O
3Deng.Simple with respect to the solid phase method production technique, coprecipitation method provided by the invention has reduced one-tenth phase temperature and calcination time, and products therefrom has pure perovskite phase structure and homogeneous particle diameter.This powder has high specific inductivity and lower dielectric loss, can be used for as all kinds of ceramic condensers of preparation, as laminated ceramic capacitor, monolithic capacitor etc.
Description of drawings
Fig. 1 is powder x-ray diffraction (XRD) collection of illustrative plates of different products.Used instrument is Bruker D-8 Advance powder diffractometer (Cu K
αRadiation, λ=1.5406 ).Wherein, the Pb (Fe of curve a for obtaining by embodiment 1
1/2Nb
1/2) O
3XRD figure spectrum, the Pb (Sc of b for obtaining by embodiment 4
1/2Nb
1/2) O
3XRD figure spectrum, the Pb (Ni of c for obtaining by embodiment 8
1/3Nb
2/3) O
3XRD figure spectrum.
Fig. 2 is the Pb (Fe that obtains by embodiment 1
1/2Nb
1/2) O
3The scanning electron microscope shape appearance figure of powder.Used instrument is a HitachiS-3500N type scanning electronic microscope.
Embodiment
Further illustrate substantive distinguishing features of the present invention and remarkable advantage below by embodiment, the present invention only is confined to the embodiment that stated by no means.
Embodiment 1
This example is to prepare niobium iron acid lead Pb (Fe with coprecipitation method
1/2Nb
1/2) O
3Powder
(1) with mol ratio is 1: 8 Nb
2O
5-KOH mixture is dissolved in deionized water through the product that 360 ℃ of calcining 2h obtain; Then with nitric acid titration pH value to 2; The white precipitate that centrifugation is obtained is dissolved in oxalic acid solution, and what obtain clear after the stirring contains niobium oxalate solution A;
(2) be 10 with niobium oxalate solution A to the pH value that contains that obtains in the ammonia water titration step 1, obtain white depositions B through centrifugation and deionized water wash;
(3) white depositions B is dissolved in the salpeter solution that concentration is 2mol/l, and Pb: Fe: Nb=2 in molar ratio: 1: 1, add Pb (NO
3)
2And Fe (NO
3)
3Simultaneously, drip the hydrogen peroxide that is equivalent to 3 times of niobium element molar weights, behind the stirring 30min, obtain transparent clarifying precursor solution C;
(4) use ammoniacal liquor as precipitation agent, regulate the pH value to 12 of precursor solution C, obtain coprecipitated product D;
(5) the coprecipitated product D of centrifugation gained, behind deionized water wash, through 80 ℃ of dryings, 800 ℃ of calcining 2h obtain uhligite phase relaxor based ferroelectrics niobium iron acid lead Pb (Fe
1/2Nb
1/2) O
3Powder.Curve a is the XRD diffracting spectrum of this powder among Fig. 1.Fig. 2 is the scanning electron microscope shape appearance figure of this powder.
(6) sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
Experiment shows: the leaded relaxation base niobate product of gained is pure perovskite structure, and have size evenly, the granule-morphology of cubic.
The powder of all the other embodiment gained all has pure perovskite phase structure and similar granule-morphology.
Embodiment 2
This example is to prepare niobium iron acid lead Pb (Fe with coprecipitation method
1/2Nb
1/2) O
3Powder
PH value to 13 with ammonia water titration precursor solution C; Drying temperature is 100 ℃.All the other conditions are with embodiment 1.Obtain the niobium iron acid lead Pb (Fe of pure perovskite phase
1/2Nb
1/2) O
3Powder.
Sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
Embodiment 3
This example is to prepare niobium iron acid lead Pb (Fe with coprecipitation method
1/2Nb
1/2) O
3Powder
White depositions B is dissolved in the salpeter solution that concentration is 4mol/l; Dropping is equivalent to the hydrogen peroxide of 10 times of niobium element molar weights, stirs 10min, obtains the precursor solution C of clear.All the other conditions obtain the niobium iron acid lead Pb (Fe of pure perovskite phase with embodiment 1
1/2Nb
1/2) O
3Powder.
Niobium iron acid lead Pb (Fe
1/2Nb
1/2) O
3Powder.
Sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
Embodiment 4
This example is to prepare lead scandate columbate Pb (Sc with coprecipitation method
1/2Nb
1/2) O
3Powder
(1) with mol ratio is 1: 8 Nb
2O
5-KOH mixture is dissolved in deionized water through the product that 340 ℃ of calcining 2h obtain; Then with nitric acid titration pH value to 3; The white precipitate that centrifugation is obtained is dissolved in oxalic acid solution, and what obtain clear after the stirring contains niobium oxalate solution A;
(2) be 11 with niobium oxalate solution A to the pH value that contains that obtains in the ammonia water titration step 1, obtain white depositions B through centrifugation and deionized water wash;
(3) white depositions B is dissolved in the salpeter solution that concentration is 3mol/l, and Pb: Sc: Nb=2 in molar ratio: 1: 1, add Pb (NO
3)
2And Sc (NO
3)
3Simultaneously, drip the hydrogen peroxide that is equivalent to 8 times of niobium element molar weights, behind the stirring 20min, obtain the precursor solution C of clear;
(4) use ammoniacal liquor as precipitation agent, regulate the pH value to 10 of precursor solution C, obtain coprecipitated product D;
(5) centrifugation gained coprecipitated product D uses deionized water wash, 90 ℃ of dryings, and 800 ℃ of calcining 1h obtain uhligite phase lead scandate columbate Pb (Sc
1/2Nb
1/2) O
3Powder.Curve b is the XRD diffracting spectrum of gained powder among Fig. 1.
(6) sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
Embodiment 5
This example is to prepare lead scandate columbate Pb (Sc with coprecipitation method
1/2Nb
1/2) O
3Powder
With the pH value of ammonia water titration precursor solution B 13; Coprecipitated product E is calcined 4h through 800 ℃.All the other conditions obtain the lead scandate columbate Pb (Sc of pure perovskite phase with embodiment 4
1/2Nb
1/2) O
3Powder.
Sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
Embodiment 6
This example is to prepare lead scandate columbate Pb (Sc with coprecipitation method
1/2Nb
1/2) O
3Powder
White depositions B is dissolved in the salpeter solution that concentration is 2mol/l; As precipitation agent, regulate the pH value to 12 of precursor solution C with diethylamine.All the other conditions obtain the lead scandate columbate Pb (Sc of pure perovskite phase with embodiment 4
1/2Nb
1/2) O
3Powder.
Sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
Embodiment 7
This example is to prepare lead scandate columbate Pb (Sc with coprecipitation method
1/2Nb
1/2) O
3Powder
Dropping is equivalent to the hydrogen peroxide of niobium element molar weight, stirs 30min; As precipitation agent, regulate the pH value to 13 of precursor solution C with diethylamine.All the other conditions obtain the lead scandate columbate Pb (Sc of pure perovskite phase with embodiment 4
1/2Nb
1/2) O
3Powder.
Sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
Embodiment 8
This example is to prepare niobium nickel lead plumbate Pb (Ni with coprecipitation method
1/3Nb
2/3) O
3Powder
(1) with mol ratio is 1: 8 Nb
2O
5-KOH mixture is dissolved in deionized water through the product that 380 ℃ of calcining 1h obtain; Then with nitric acid titration pH value to 2; The white precipitate that centrifugation obtained is dissolved in oxalic acid solution, and what obtain clear after the stirring contains niobium oxalate solution A;
(2) be 11 with niobium oxalate solution B to the pH value that contains that obtains in the ammonia water titration step 1, obtain white depositions B through centrifugation and deionized water wash;
(3) white depositions B is dissolved in the salpeter solution that concentration is 2mol/l, and Pb: Ni: Nb=3 in molar ratio: 1: 2, add Pb (NO
3)
2And Ni (NO
3)
2Simultaneously, drip the hydrogen peroxide that is equivalent to 3 times of niobium element molar weights, behind the stirring 10min, obtain clear precursor solution C;
(4) use diethylamine as precipitation agent, regulate the pH value to 10 of precursor solution C, obtain coprecipitated product E;
(5) the coprecipitated product D of centrifugation gained uses deionized water wash, 100 ℃ of dryings, and 900 ℃ of calcining 2h obtain uhligite phase relaxor based ferroelectrics niobium nickel lead plumbate Pb (Ni
1/3Nb
2/3) O
3Powder.Curve c is the XRD diffracting spectrum of this powder among Fig. 1.
(6) sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
Embodiment 9
This example is to prepare niobium nickel lead plumbate Pb (Ni with coprecipitation method
1/3Nb
2/3) O
3Powder
Regulate the pH value to 13 of precursor solution C with diethylamine.All the other conditions obtain the niobium nickel lead plumbate Pb (Ni of pure perovskite phase with embodiment 8
1/3Nb
2/3) O
3Powder.
Sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
Embodiment 10
This example is to prepare niobium nickel lead plumbate Pb (Ni with coprecipitation method
1/3Nb
2/3) O
3Powder
Dropping is equivalent to the hydrogen peroxide of 8 times of niobium element molar weights, stirs 20min.All the other conditions obtain the niobium nickel lead plumbate Pb (Ni of pure perovskite phase with embodiment 8
1/3Nb
2/3) O
3Powder.
Sinter resulting powder into pottery by the listed sintering schedule of table 1, and measure its dielectric properties and list in table 1.
The relaxation base niobate ferroelectric powder sintering that the method that table 1 provides by various embodiments of the present invention prepares
The dielectric properties of the pottery that forms
(measuring condition: room temperature, 1kHz)
| Embodiment | Sintering schedule | Relative permittivity ε r | Dielectric loss tangent value tan δ | Literature value ε r/tanδ |
| 1 | 1150℃/2h | 4826 | 0.129 | 2500～3000/ 0.03～0.04 [1] |
| 2 | 1150℃/2h | 5003 | 0.131 | |
| 3 | 1150℃/2h | 4899 | 0.135 | |
| 4 | 1200℃/2h | 6023 | 0.052 | 1500-2000/ 0.03-0.04 [2] |
| 5 | 1200℃/2h | 5892 | 0.051 | |
| 6 | 1200℃/2h | 5990 | 0.050 | |
| 7 | 1200℃/2h | 5723 | 0.050 | |
| 8 | 1200℃/2h | 1523 | 0.013 | 1400～1500/ 0.02～0.03 [3] |
| 9 | 1200℃/2h | 1498 | 0.017 | |
| 10 | 1200℃/2h | 1506 | 0.012 |
[1]S.B.Lee，S.H.Yoon，H.Kim，Positive temperature coeffcient ofresistivity in Pb(Fe
1/2Nb
1/2)O
3 ceramics，J.Euro.Ceram.Soc.24(2004)2465-2470.
[2] Feng Chude, the W.A.Schulze. characteristic of the lead scandate columbate pottery (PSN) of chemical coprecipitation powder preparing. Journal of Inorganic Materials 3 (1990): 237-244
[3]E.F.Alberta，A.S.Bhalla.Low-temperature properties of lead nickelniobate ceramics.Mater.Lett.54(2002)：47-54.
Claims (1)
1, the co-precipitation preparation method of relaxation base niobate ferroelectric powder is characterized in that, may further comprise the steps:
1) with mol ratio is 1: 8 Nb
2O
5-KOH mixture is dissolved in deionized water through the product that 340-380 ℃ of calcining 1-2h obtains; Obtain white precipitate with nitric acid titration pH value to 2-3 then; The white precipitate of centrifugation gained also is dissolved in oxalic acid solution, and what obtain clear after the stirring contains niobium oxalate solution A;
2) be 10-11 with niobium oxalate solution A to the pH value that contains that obtains in the ammonia water titration step 1, obtain white depositions B through centrifugation and deionized water wash;
3) white depositions B is dissolved in the salpeter solution that concentration is 2-4mol/l, and by final compound Pb (M, Nb) O
3Stoichiometric ratio, add Pb (NO
3)
2And and final compound Pb (M, Nb) O
3The nitrate of corresponding metal ions M, wherein M is divalence or trivalent metal ion, comprises Mg
2+, Ni
2+, Sc
3+Or Fe
3+Simultaneously, dropping is equivalent to niobium molar weight 1-10 hydrogen peroxide doubly, stirs 10-30min, obtains transparent clarifying precursor solution C;
4) with ammoniacal liquor or diethylamine as precipitation agent, the pH value of regulating precursor solution C obtains coprecipitated product D to 10-13;
5) with the centrifugal collection of above-mentioned gained coprecipitated product D, use deionized water wash, after 80-100 ℃ of drying,, obtain final compound Pb (M, Nb) O of uhligite phase at 800-900 ℃ of calcining 1-4h
3Powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100579880A CN1321901C (en) | 2006-03-03 | 2006-03-03 | Coprecipitation process of preparing relation base niobate ferroelectric powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100579880A CN1321901C (en) | 2006-03-03 | 2006-03-03 | Coprecipitation process of preparing relation base niobate ferroelectric powder |
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| CN100429175C (en) * | 2006-11-21 | 2008-10-29 | 北京工业大学 | Method for preparing relaxation base ferroelectrics lead scandate columbate nano powder in low temperature |
| CN101613201B (en) * | 2009-06-25 | 2011-11-30 | 南京航空航天大学 | Method for synthesizing potassium-sodium niobate leadless piezoelectric ceramic powder by two hydro-thermal steps |
| CN103833082B (en) * | 2014-01-13 | 2015-10-28 | 陕西科技大学 | A kind of coprecipitation method prepares nanometer Ba (Fe 0.5nb 0.5) O 3the method of powder |
| CN104030684B (en) * | 2014-06-24 | 2015-09-30 | 陕西科技大学 | A kind of coprecipitation method prepares nanometer Sr (Fe 0.5nb 0.5) O 3the method of powder |
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| CN1227286A (en) * | 1999-02-11 | 1999-09-01 | 中国科学院上海硅酸盐研究所 | Method for preparing relaxing ferroelectric single crystal lead magnoniobate |
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Non-Patent Citations (3)
| Title |
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| "熔盐合成法制备铌铁酸铅粉末" 蔡君威等，《化学世界》，第12期 1993;"制备铅系弛豫铁电陶瓷的反应机理研究进展" 崔斌等，《材料导报》，第16卷第9期 2002 * |
| "制备铅系弛豫铁电陶瓷的反应机理研究进展" 崔斌等，《材料导报》，第16卷第9期 2002 * |
| "熔盐合成法制备铌铁酸铅粉末" 蔡君威等，《化学世界》，第12期 1993 * |
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