CN100362147C - Process for preparing nano barium titanate and doped solid solution by low temperature solid state reaction - Google Patents
Process for preparing nano barium titanate and doped solid solution by low temperature solid state reaction Download PDFInfo
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- CN100362147C CN100362147C CNB2006100126452A CN200610012645A CN100362147C CN 100362147 C CN100362147 C CN 100362147C CN B2006100126452 A CNB2006100126452 A CN B2006100126452A CN 200610012645 A CN200610012645 A CN 200610012645A CN 100362147 C CN100362147 C CN 100362147C
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Abstract
The present invention relates to a method for preparing nanometer barium titanate with low-temperature solid-state reaction, which is characterized in that A TiCl4 is used as raw materials to be hydrolyzed under the condition that PH value is from 6 to 8 to obtain filter cakes of metatitanic acid H2 TiO3; B the filter cakes and solid Ba (OH) 2.8H2O are mixed to be ground fully for 30 to 60 minutes at room temperature and directly dried at the temperature from 80 to 120 DEG C to obtain the powder of BaTiO3. The method for preparing nanometer barium titanate doping solid solution comprises that A and B sites of barium titanate are doped to be synthesized, Sr, Ca, Zn, Cu, etc. can be selected as A-site doping raw materials, and Zr, Sn, Si, Ce, etc. can be selected as B-site doping raw materials. The present invention has the advantages of simple process, short reaction time, high yield and low energy consumption. The phenomenon of forceful agglomeration of products is avoided effectively, solvent is not used, the environmental pollution is little, the atomic saving reaction is realized, and the present invention is consistent with the idea of green chemistry. The dielectric constant of barium titanate ceramic prepared by the present invention at room temperature can reach more than 4000, the dielectric performance is increased greatly by the barium titanate doping solid solution prepared by doping modification, and the present invention has high theory and use value.
Description
Technical field
The present invention relates to the method that a kind of low temperature solid state reaction prepares nano barium phthalate and sosoloid, belong to chemosynthesis purification techniques field.
Background technology
BaTiO
3As a kind of ferroelectric material of excellent performance, it has unusual high specific inductivity.Except basic masterbatch as electronic devices and components such as monolithic ceramic capacitor, multi-layered ceramic electricradiator, PTCR thermistors, and also be widely used at aspects such as dielectric amplifier, frequency modulation and storing devices, become one of most popular material of electronic ceramic fields gradually, be described as " pillar of electronic ceramics industry ".
The synthetic method of nano barium phthalate is varied, and using many is solid phase method and liquid phase method.Conventional solid-state method is meant and will forms the oxide compound (TiO of each metallic element of barium titanate
2, BaO) or their acid-salt (TiO
2, BaCO
3Or Ba (NO
3)
2) mix, levigate, calcining for a long time about 1250 ℃ then forms required powder by solid state reaction.This method has that technology is simple, ripe, equipment is reliable; Cost of material is more cheap, and production cost is lower; Can regulate advantages such as chemical constitution as requested arbitrarily.But the chemical ingredients skewness of the barium carbonate powder that the use solid phase method obtains; Easily reunite through the barium carbonate powder that high temperature forms, particle thick (general＞1m), size-grade distribution is inhomogeneous; Easily introduce impurity in the production process, product purity is low.So can not satisfy the requirement that hyundai electronics components and parts volume is little, performance is high.
Summary of the invention
The objective of the invention is to provides a kind of brand-new synthetic method at the prior art defective, and the low temperature solid state reaction is prepared nano barium phthalate and doped solid solution thereof.
The object of the present invention is achieved like this: this low temperature solid state reaction prepares the method for nano barium phthalate, and its feature comprises:
A, with TiCl
4Be hydrolysis under the condition of 6-8 in the pH value for raw material, decompress filter is cleaned chlorion and is obtained metatitanic acid H
2TiO
3Filter cake;
B, with filter cake and solid Ba (OH)
28H
2O mixes with mol ratio at 1: 1, at room temperature fully grinds 30～60min, in 80-120 ℃ of directly oven dry, obtains median size 50-70nm, and crystal formation is the BaTiO of cube phase
3Powder.
Described low temperature solid state reaction prepares the method for nano barium phthalate, it is characterized in that the described TiCl of steps A
4Hydrolysis is the TiCl with 11ml 0.1mol
4Splash in the 100-200ml deionized water, transferring pH with ammoniacal liquor then is 6-8, makes soup compound, and decompress filter is drained behind the clean chlorion.
The method that described low temperature solid state reaction prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, and its feature comprises:
A, with the filter cake and the solid Ba (OH) of steps A gained
28H
2O and the element consistent with the plain valence state of barium titanate A bit are doped raw material mixed grinding 30～60min, in 80-120 ℃ of directly oven dry, preparation Ba
1-xM
xTiO
3Barium phthalate base is nanocrystalline;
Or
B, be doped raw material and TiCl with the element consistent with barium titanate B position valence state
4Common hydrolysis adds the ammoniacal liquor making beating, and accent pH is 6-8, and decompress filter is cleaned chlorion and obtained filter cake, with filter cake and solid Ba (OH)
28H
2O mixes with mol ratio 1: 1, at room temperature fully grind 30～60min after, in 80-120 ℃ of oven dry, preparation BaTi
1-xN
xO
3Barium phthalate base is nanocrystalline;
Or
C, be doped raw material and TiCl with the element consistent with barium titanate B position valence state
4Common hydrolysis adds the ammoniacal liquor making beating, and accent pH is 6-8, and decompress filter is cleaned chlorion and obtained filter cake, with filter cake and solid Ba (OH)
28H
2O reaches and the consistent element doping mixed grinding 30～60min of the plain valence state of barium titanate A bit, in 80-120 ℃ of directly oven dry, preparation Ba
1-xM
xTi
1-yN
yO
3The series barium phthalate base is nanocrystalline.
The method that described low temperature solid state reaction prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, the described preparation barium titanate of step a A position doped solid solution Ba
1-xM
xTiO
3The metallic element M that selects comprises Sr, Ca, Zn or Cu etc.
The method that described low temperature solid state reaction prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, the described filter cake of step a, solid Ba (OH)
28H
2The blending ratio of O and A position doped raw material is a mol ratio 1: (1-X): X, and wherein the value of X is 0,0.03,0.05,0.08 ..., between 1.0.
The method that described low temperature solid state reaction prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, it is characterized in that the described preparation barium titanate of step b B position doped solid solution BaTi
1-xN
xO
3The metallic element N that selects comprises Zr, Sn, Si or Ce etc.
The method that described low temperature solid state reaction prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, the described B of step b position doped raw material, filter cake, solid Ba (OH)
28H
2The blending ratio of O is mol ratio X: (1-X): 1, and wherein the value of X is
0.02,0.03 ..., until 0.3.
The method that described low temperature solid state reaction prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, the described preparation barium titanate of step c A, B position doped solid solution Ba
1-xM
xTi
1-yN
yO
3The metallic element M that selects comprises Sr, Ca, Zn or Cu etc.; N comprises Zr, Sn, Si or Ce etc.
The method that described low temperature solid state reaction prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, the described B of step c position doped raw material, filter cake, solid Ba (OH)
28H
2The blending ratio of O and A position doped raw material is mol ratio Y: 1-Y: 1-X: X, and wherein the value of X and Y is respectively 0.01,0.02,0.03 ..., until between 1.0.
The method that described low temperature solid state reaction prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, and the described preparation barium titanate of step c A, B position doped solid solution are to be doped raw material and TiCl with the element consistent with barium titanate B position valence state
4Common hydrolysis adds the ammoniacal liquor making beating, and accent pH is 6-8, and decompress filter is cleaned chlorion and obtained filter cake, with filter cake and solid Ba (OH)
28H
2O reaches and plain consistent element of valence state of barium titanate A bit and the composite mixed mixed grinding 30～60min of rare earth element, in 80-120 ℃ of directly oven dry, preparation Ba
1-xM
xTi
1-yN
yO
3ZLn
2O
3The series barium phthalate base is nanocrystalline.
The method and technology progress effect that low temperature solid state reaction provided by the invention prepares nano barium phthalate and doped solid solution shows: technology is simple, and the reaction times is short, the productive rate height; Energy consumption is low; Not only effectively avoided the hard aggregation phenomenon of product, and do not used solvent, environmental pollution is little, has realized the atomic economics reaction, meets the Green Chemistry theory.Adopt the barium titanate ceramics of method preparation of the present invention, room temperature dielectric constant can reach more than 4000.Obtaining on the basis of pure barium titanate, the barium titanate doped solid solution that adopts the inventive method to carry out the doping vario-property preparation makes that dielectric properties have obtained increasing substantially, and very high theory and practical value are arranged.
Description of drawings
Fig. 1: the transmission electron microscope of pure barium titanate powder (TEM) figure
Fig. 2: pure barium titanate powder XRD diffractogram
Fig. 3: Ba
1-xSr
xTiO
3Room temperature dielectric constant ε (a) and dissipation loss tan δ (b) and the relation of forming
Fig. 4: a-Ba
0.9Sr
0.1TiO
3, b-BaTiO
3The specific inductivity of differing temps (ε)
Fig. 5: BaTi
1-xSn
xO
3Room temperature dielectric constant (ε) and dissipation loss (tan δ) and the relation of forming
Fig. 6: a-BaTi
0.9Sn
0.1O
3, b-BaTiO
3The specific inductivity of differing temps (ε)
Fig. 7: Ba
1-xSr
xTi
1-ySn
yO
3Dielectric properties figure
Fig. 8: pure sample BaTiO under the a-differing temps
3Specific inductivity
Ba under the b-differing temps
0.9Sr
0.1Ti
0.9Sn
0.1O
3Specific inductivity
Embodiment
Embodiment 1: prepare pure nano barium phthalate sosoloid
1, the generation of metatitanic acid
TiCl with 11ml (0.1mol)
4Splash in 100～200ml deionized water, transferring pH with ammoniacal liquor then is 6-8, makes soup compound, and decompress filter is drained behind the clean chlorion, and obtaining filter cake is metatitanic acid (H
2TiO
3Or TiO
2H
2O).
2, grind oven dry
With filter cake according to effective content and solid Ba (OH)
28H
2O mixes with mol ratio at 1: 1, at room temperature fully grinds 30～60min, and 100 ℃ of directly oven dry can obtain median size 50～70nm then, and crystal formation is the BaTiO of cube phase
3Powder, as shown in Figure 1 and Figure 2.With the barium titanate ceramics of the present invention's preparation, room temperature dielectric constant can reach more than 4000.And adopt its specific inductivity of barium titanate that the prior art high temperature sintering obtains between 2000-4000 and unstable.
Embodiment 2: to BaTiO
3(ABO
3) sosoloid carries out the A position synthetic Ba that mixes
1-xM
xTiO
3
To mix strontium (Ba
0.9Sr
0.1TiO
3) be example: TiCl
4Hydrolytic process is with embodiment 1, with the filter cake of flush away chlorion according to effective content and fresh solid Ba (OH)
28H
2O and Sr (OH)
28H
2O mixes with mol ratio 1: 0.9: 0.1, at room temperature fully grind 30～60min after, move into crucible, 120 ℃ of oven dry, promptly obtain cube phase Ba of median size 30～50nm
0.9Sr
0.1TiO
3Powder.At Ba
1-xM
xTiO
3In the system, the value of X is, 0,0.03,0.05,0.08 ..., between 1.0, X is value or interruption value continuously.
Potting test confirms, in barium titanate, mix an amount of strontium with the inventive method after, the material room temperature dielectric constant can reach more than 10000, its correlation technique index as shown in Figure 3, Figure 4.
3. couples of BaTiO of embodiment
3Sosoloid carries out the adulterated synthetic BaTi in B position
0.9N
0.1O
3
To mix tin (BaTi
0.9Sn
0.1O
3) be example: with 9.9mlTiCl
4, 3.5058g SnCl
45H
2Add the ammoniacal liquor making beating after the common hydrolysis of O, accent pH is 6-8, and decompress filter is cleaned chlorion, then with filter cake according to effective content and fresh solid Ba (OH)
28H
2O mixes with mol ratio 1: 1, at room temperature fully grind 30～60min after, put into 120 ℃ of baking ovens and directly dry.Can make nanometer BaTi
0.9Sn
0.1O
3Solid-solution powder.BaTi
1-xN
xO
3The value of middle x is: 0.01,0.02,0.03 ..., 0.1,0.15,0.2,0.25,0.3.X is value or interruption value continuously.
Potting test confirms, in barium titanate, mix an amount of tin with the inventive method after, the material room temperature dielectric constant can reach more than 9000, its correlation technique index such as Fig. 5, shown in Figure 6.
4. couples of BaTiO of embodiment
3Sosoloid carries out A, the adulterated synthetic Ba in B position
0.9M
0.1Ti
0.9N
0.1O
3
With Ba
0.9Sr
0.1Ti
0.9Sn
0.1O
3Be example: with 9.9ml TiCl
4, 3.5058g SnCl
45H
2Add the ammoniacal liquor making beating after the common hydrolysis of O, accent pH is 6-8, and decompress filter is cleaned chlorion, then with filter cake according to effective content and fresh solid 28.350g Ba (OH)
28H
2O, 2.656gSr (OH)
28H
2O mixes with mol ratio 1: 1, at room temperature fully grind 30～60min after, put into 120 ℃ of baking ovens and directly dry.Can make nanometer Ba
0.9Sr
0.1Ti
0.9Sn
0.1O
3Solid-solution powder.Ba
1-xM
xTi
1-yN
yO
3In: the value of x, y is respectively: 0.01,0.02,0.03 ..., 0.1,0.15,0.2,0.25,0.3 ..., between 1.0.X, Y be value or interruption value continuously.
Potting test confirms, in barium titanate, mix an amount of strontium and tin with the inventive method after, the material room temperature dielectric constant can reach more than 14000, its correlation technique index such as Fig. 7, shown in Figure 8.
Embodiment 5, synthetic Ba
1-xSr
xTi
1-ySn (Zr)
yO
3ZLn
2O
3
With Ba
1-xSr
xTi
1-ySn (Zr)
yO
3ZLn
2O
3(Ln=rare earth element) is example: operation adds rare earth oxide with embodiment 4 during grinding, oven dry can make nanometer Ba
1-xSr
xTi
1-ySn (Zr)
yO
3ZLn
2O
3Solid-solution powder.
Experiment showed, after the foregoing description barium titanate sosoloid mixes to make that dielectric properties have obtained increasing substantially, very high theory and practical value are arranged.In the foregoing description: 1, the A position doped element Ba of barium titanate sosoloid
1-xM
xTiO
3, M can select Sr, Ca, Zn, Cu etc.2, the B position doped element BaTi of barium titanate sosoloid
1-xN
xO
3, N can select Zr, Sn, Si, Ce etc.3, the A of barium titanate sosoloid, B position doped element Ba
1-xM
xTi
1-yN
yO
3, M can select Sr, Ca, Zn, Cu etc.; N can select Zr, Sn, Si, Ce etc.4, the doped element of barium titanate sosoloid can also Application of composite, as it is nanocrystalline to adopt common hydrolysis of doped element more than two kinds or the doped element more than two kinds to grind a series of barium phthalate bases of preparation jointly.5, main raw material of the present invention uses commercially available analytical reagent, also can use industrial goods.
Listed examples of the present invention is intended to further illustrate the method that the low temperature solid state reaction prepares nano barium phthalate and doped solid solution, and protection scope of the present invention is not constituted any restriction.All can obtain than high dielectric property nano barium phthalate and doped solid solution product with the embodiment of the invention with via claims 1-10 of the present invention.
Claims (10)
1. the low temperature solid state reaction prepares the method for nano barium phthalate, and its feature comprises:
A, with TiCl
4Be hydrolysis under the condition of 6-8 in the pH value for raw material, decompress filter is cleaned chlorion and is obtained metatitanic acid H
2TiO
3Filter cake;
B, with filter cake and solid Ba (OH)
28H
2O mixes with mol ratio at 1: 1, at room temperature fully grinds 30～60min, in 80-120 ℃ of directly oven dry, obtains median size 50-70nm, and crystal formation is the BaTiO of cube phase
3Powder.
2. low temperature solid state reaction according to claim 1 prepares the method for nano barium phthalate, it is characterized in that the described TiCl of steps A
4Hydrolysis is the TiCl with 11ml 0.1mol
4Splash in the 100-200ml deionized water, transferring pH with ammoniacal liquor then is 6-8, makes soup compound, and decompress filter is drained behind the clean chlorion.
3. the method that low temperature solid state reaction according to claim 1 prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, and its feature comprises:
A, with the filter cake and the solid Ba (OH) of steps A gained
28H
2O and the element consistent with the plain valence state of barium titanate A bit are doped raw material mixed grinding 30～60min, in 80-120 ℃ of directly oven dry, preparation Ba
1-xM
xTiO
3Barium phthalate base is nanocrystalline, and wherein M is a barium titanate A position doped metallic elements, and X is the blending ratio value;
Or
B, be doped raw material and TiCl with the element consistent with barium titanate B position valence state
4Common hydrolysis adds the ammoniacal liquor making beating, and accent pH is 6-8, and decompress filter is cleaned chlorion and obtained filter cake, with filter cake and solid Ba (OH)
28H
2O mixes with mol ratio 1: 1, at room temperature fully grind 30～60min after, in 80-120 ℃ of oven dry, preparation BaTi
1-xN
xO
3Barium phthalate base is nanocrystalline, and wherein N is a barium titanate B position doped metallic elements, and X is the blending ratio value;
Or
C, be doped raw material and TiCl with the element consistent with barium titanate B position valence state
4Common hydrolysis adds the ammoniacal liquor making beating, and accent pH is 6-8, and decompress filter is cleaned chlorion and obtained filter cake, with filter cake and solid Ba (OH)
28H
2O reaches and the consistent element doping mixed grinding 30～60min of the plain valence state of barium titanate A bit, in 80-120 ℃ of directly oven dry, preparation Ba
1-xM
xTi
1-yN
yO
3The series barium phthalate base is nanocrystalline.
4. the method that low temperature solid state reaction according to claim 3 prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, it is characterized in that: the described preparation barium titanate of step a A position doped solid solution Ba
1-xM
xTiO
3The metallic element M that selects comprises Sr, Ca, Zn or Cu.
5. the method for preparing nano barium phthalate according to claim 3 or 4 described low temperature solid state reactions prepares the nano barium phthalate doped solid solution, it is characterized in that: the described filter cake of step a, solid Ba (OH)
28H
2The blending ratio of O and A position doped raw material is a mol ratio 1: (1-X): X.
6. the method that low temperature solid state reaction according to claim 3 prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, it is characterized in that the described preparation barium titanate of step b B position doped solid solution BaTi
1-xN
xO
3The metallic element N that selects comprises Zr, Sn, Si or Ce.
7. the method for preparing nano barium phthalate according to claim 3 or 6 described low temperature solid state reactions prepares the nano barium phthalate doped solid solution, it is characterized in that the described B of step b position doped raw material, filter cake, solid Ba (OH)
28H
2The blending ratio of O is mol ratio X: (1-X): 1.
8. the method that low temperature solid state reaction according to claim 3 prepares nano barium phthalate prepares the nano barium phthalate doped solid solution, it is characterized in that the described preparation barium titanate of step C A, B position doped solid solution Ba
1-xM
xTi
1-yN
yO
3The metallic element M that selects comprises Sr, Ca, Zn or Cu; N comprises Zr, Sn, Si or Ce.
9. the method for preparing nano barium phthalate according to claim 3 or 8 described low temperature solid state reactions prepares the nano barium phthalate doped solid solution, it is characterized in that the described B of step C position doped raw material, filter cake, solid Ba (OH)
28H
2The blending ratio of O and A position doped raw material is mol ratio Y: 1-Y: 1-X: X, and wherein X and Y are the blending ratio value.
10. the method for preparing nano barium phthalate according to claim 3 or 8 described low temperature solid state reactions prepares the nano barium phthalate doped solid solution, it is characterized in that the described preparation barium titanate of step C A, B position doped solid solution are is doped raw material and TiCl with the element consistent with barium titanate B position valence state
4Common hydrolysis adds the ammoniacal liquor making beating, and accent pH is 6-8, and decompress filter is cleaned chlorion and obtained filter cake, with filter cake and solid Ba (OH)
28H
2O reaches and plain consistent element of valence state of barium titanate A bit and the composite mixed mixed grinding 30～60min of rare earth element, in 80-120 ℃ of directly oven dry, preparation Ba
1-xM
xTi
1-yN
yO
3ZLn
2O
3The series barium phthalate base is nanocrystalline.
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| CN102718501B (en) * | 2012-06-19 | 2013-07-31 | 河北大学 | Preparation method of temperature stability type capacitor ceramic powder with high dielectric constant |
| CN105130425A (en) * | 2015-09-30 | 2015-12-09 | 桂林理工大学 | High-curie-point positive-temperature-coefficient resistive material Ba5ZnTi3O12 and preparation method thereof |
| CN108928854A (en) * | 2018-08-28 | 2018-12-04 | 江苏省农业科学院 | A kind of material and preparation method thereof with microwave heating effect |
| CN116217224B (en) * | 2023-02-10 | 2023-12-26 | 华中科技大学 | Nanometer BaTi 1-x Sn x O 3 Preparation method of powder |
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