CN100455538C - Lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic and its prepn process - Google Patents
Lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic and its prepn process Download PDFInfo
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- CN100455538C CN100455538C CNB2006101194230A CN200610119423A CN100455538C CN 100455538 C CN100455538 C CN 100455538C CN B2006101194230 A CNB2006101194230 A CN B2006101194230A CN 200610119423 A CN200610119423 A CN 200610119423A CN 100455538 C CN100455538 C CN 100455538C
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Abstract
The present invention is one kind of lead-less piezoelectric sodium bismuth titanate-barium titanate ceramic, and belongs to the field of lead-less piezoelectric ceramic. The lead-less piezoelectric sodium bismuth titanate-barium titanate ceramic has the chemical formula of (Na1/2Bi1/2)1-xBaxTiO3, where, x is 0.05-0.1, and has ceramic crystal grains parallel to the grain boundary. Its preparation process includes the following steps: molten salt procedure to synthesize Bi4Ti3O12 template or solid phase reaction procedure to synthesize Na0.5Bi4.5Ti4O15 precursor material powder; preparing slurring with Na2CO3, BaCO3, Bi2O3 and nanometer TiO2; silk screen printing to obtain thick ceramic film; cutting, superposing and sintering.
Description
Technical field
The present invention relates to a kind of lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic and preparation method thereof, belong to the leadless piezoelectric ceramics preparation field.
Background technology
Ferroelectric piezoelectric ceramics and device thereof all have widely in industry, the product for civilian use and military affairs and use, and are that a class is important, irreplaceable, the hi-tech material that international competition is very fierce.At present, piezoelectric ceramics commonly used is leaded pottery mostly, and as PZT etc., these lead base potteries have all shown very excellent performance near its accurate homotype phase boundary.But plumbous toxicity and environmental pollution thereof have caused more and more to human society and have seriously influenced.Therefore, the leadless piezoelectric ceramics of the friendly type of development environment be one urgent and have a problem of great Practical significance.
In numerous leadless piezoelectric ceramics systems, bismuth-sodium titanate Na
0.5Bi
0.5TiO
3(NBT) be considered to most important one of the candidate material that replaces the lead base piezoelectric ceramics that is expected.Wherein, the bismuth sodium titanate-barium titanate pottery has shown excellent performance near its accurate homotype phase boundary, is a kind of up-and-coming leadless piezoelectric material material.People have done big quantity research by doping vario-property, but its performance still has gap with leaded ceramic phase ratio.Result of study in recent years shows that texturing technology has obtained extensive studies and concern at home and abroad as a kind of effective ways that improve the piezoelectric ceramics performance.
The texturing technology is meant by technology controlling and process, and the ceramic crystalline grain of script random orientation is aligned, and makes it to reach the performance that has near monocrystalline.The texturing technology is a kind of structurally-modified, compares with traditional doping vario-property, has the advantage that does not change ceramic Curie temperature.
At present, the more ceramic texturing technology of research has heat treatment technics and template grain growth technology.Though the heat treatment technics directional effect is obvious, complex process, cost are higher, only use to some extent in the laboratory.Though adopt the template grain growth technology can prepare the pottery of high-orientation, one of them committed step is the anisotropic template crystal grain of preparation, and this just makes its technology complicated.In addition, because template crystal grain does not belong to mutually same with parent, this also will inevitably make the character of material produce inconsistent phenomenon.
In addition, because the pottery of perovskite structure has higher symmetry, crystal grain develops into cubic when spontaneous growth easily, thereby is difficult to obtain anisotropic pattern.Therefore, in the prior art, the texturing technology of perovskite structure pottery is very complicated.
Summary of the invention
The present invention can make the material of high-density, high-orientation, thereby simplify this type of ceramic preparation technology greatly adding template or not having under the template condition.
The chemical formula of the texturing lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic of the present invention's preparation is: (Na
1/2Bi
1/2)
1-xBa
xTiO
3, x=0.05-0.1 wherein, ceramic crystalline grain is parallel to the crystal boundary direction.
Purpose of the present invention can realize by the following technical solutions:
With molten-salt growth method synthetic sheet Bi
4Ti
3O
12Be template, with Na
2CO
3, BaCO
3, Bi
2O
3And nano-TiO
2For other raw material powder, press chemical formula (Na
1/2Bi
1/2)
1-xBa
xTiO
3The preparation raw material powder, wherein, x=0.05-0.1, sheet Bi
4Ti
3O
12The Ti that template provides accounts for the 10-30% of required Ti amount mol ratio;
Perhaps adopt solid reaction process, with Na
2CO
3, Bi
2O
3And nano-TiO
2Synthetic Na
0.5Bi
4.5Ti
4O
15Be prepared as forerunner's material powder, with this forerunner's material powder and Na
2CO
3, BaCO
3, Bi
2O
3And nano-TiO
2For other raw material powders, press chemical formula (Na
1/2Bi
1/2)
1- xBa
xTiO
3The preparation raw material powder, wherein, x=0.05-0.1, Na
0.5Bi
4.5Ti
4O
15The Ti that template provides accounts for the 10-30% of required Ti amount mol ratio.
Selecting ethyl cellulose, methylcellulose gum, soluble cotton for use is binding agent, selecting Terpineol 350, ethylene glycol, Terpineol 350 for use is solvent, earlier with binding agent and solvent 80 ℃ of heated and stirred until forming clear solution, material powder is added in the above-mentioned solution, mixed in ball milling 2-4 hour, and continued ball milling 15-30 branch and can obtain slurry.
Slurry is directly printed onto on the substrate by silk screen printing, dries in 100-120 ℃ baking oven.Repeat above-mentioned steps repeatedly, can obtain the ceramic thick film of desired thickness, general thickness is at 0.10-0.20mm.At last with ceramic membrane in 90-100 ℃ the oven dry 12-20 hour, standby.
Above-mentioned ceramic membrane is cut into the ceramic diaphragm of desired size, after taking off from substrate, is stacked on compression moulding in the mould, the biscuit after the moulding places in the heat treatment furnace in 500-800 ℃ of eliminating organism wherein.
Sintering process is: heat-up rate 5-10 ℃/min is warming up to 700-900 ℃ of insulation 2-8 hour, and the speed with 5-10 ℃/mi n is warming up to 1100-1200 ℃ of sintered specimen again, is incubated 2-10 hour.
The present invention has successfully prepared textured lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic, shows that by XRD and sem analysis to pottery prepared ceramic crystalline grain aligns, and has tangible texturing feature.Adopt the Lotgering method to calculate, pottery is 92% and 32% in the orientation degree of adding template or do not have under the template condition clearly.
Compare with existing texturing technology, the present invention has the following advantages:
1, the present invention can prepare the textured lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic of perovskite structure by two step hybrid systems under no template condition.
2, slurry preparation of the present invention and printing process are easy, and it is long that the slurry usage period is joined by institute, and good stability is with low cost.
3, adopt the textured lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic of the perovskite structure of the present invention's preparation can obtain high-density and high-orientation simultaneously.
Description of drawings
Fig. 1 is for adding Bi
4Ti
3O
12Template, the XRD figure of the NBBT pottery (1180 ℃, 5 hours) of silk screen printing preparation.(a) be powdered sample; (b) be that the texturing samples vertical is in the surface of silk screen printing; (c) be parallel to the surface of silk screen printing for the texturing sample.As we can see from the figure, the diffraction peak of texturing sample both direction is obviously different, and (h00) peak that is parallel to the silk screen printing surface is strong significantly to be strengthened, and has very strong texturing feature.
Fig. 2 is for adding Bi
4Ti
3O
12Template, the SEM photo of the pottery (1180 ℃, 5 hours) of silk screen printing preparation, ceramic crystalline grain is brick-shaped and aligns as can be seen.
Fig. 3 is the XRD figure of the pottery (1200 ℃, 10 hours) of no template silk screen printing preparation.(a) be powdered sample; (b) be that the texturing samples vertical is in the surface of silk screen printing; (c) be parallel to the surface of silk screen printing for the texturing sample.As we can see from the figure, the diffraction peak difference of texturing sample both direction, (100), (200) peak of being parallel to the silk screen printing surface strengthen by force, and (200) become highest peak, show certain texturing feature.
Fig. 4 is the SEM photo of the pottery (1200 ℃, 10 hours) of no template silk screen printing preparation, and ceramic crystalline grain is brick-shaped, and certain orientations feature is arranged, and ceramic body is fine and close.
Embodiment
Embodiment 1
(1) the slurry preparation is dissolved in the 5.90g ethyl cellulose in the Terpineol 350 of 130.82g, in 80 ℃ of heated and stirred, dissolves the formation clear solution fully until ethyl cellulose.Take by weighing 7.02g Na
2CO
3, 3.33g BaCO
3, 10.32g Bi
2O
3With the 17.21g nano-TiO
2, adding in the above-mentioned solution, ball milling mixed in 2 hours.Again with 25.80g molten-salt growth method synthetic sheet Bi
4Ti
3O
12Add in the slurry, continued ball milling 15 minutes.
(2) on mylar, the baking oven of putting into 100 ℃ is dried with the prepared slurry silk screen printing in silk screen printing, repeats about above step 30 time, until the ceramic membrane that forms 0.15mm.
(3) moulding is cut into the square sheet of 12mm * 12mm with the ceramic membrane that obtains, and takes off diaphragm from substrate, and overlapping about 60 layers, compression moulding.
(4) the plastic removal sintering is put into heat treatment furnace in 650 ℃ of eliminatings organism wherein with above-mentioned biscuit of ceramics.Sample behind the plastic removal is put into High Temperature Furnaces Heating Apparatus, is warming up to 850 ℃ of insulations after 8 hours with the speed of 10 ℃/min, and the speed with 10 ℃/min is warming up to 1180 ℃ of sintered specimens again, is incubated 5 hours.
The XRD diffracting spectrum of the pottery that embodiment 1 makes calculates through the Loterging method as shown in Figure 1, and its orientation degree is 92%.On the direction perpendicular to silk screen printing, ceramic crystalline grain is brick-shaped and aligns (as shown in Figure 2).
Embodiment 2
(1) the slurry preparation is dissolved in the 5.90g ethyl cellulose in the Terpineol 350 of 130.82g, in 80 ℃ of heated and stirred, dissolves the formation clear solution fully until ethyl cellulose.Take by weighing 6.65g Na
2CO
3, 3.33g BaCO
3, 16.16g Bi
2O
3With the 18.01g nano-TiO
2, adding in the above-mentioned solution, ball milling mixed in 2 hours.Again with 19.46g solid reaction process synthetic Na
0.5Bi
4.5Ti
4O
15Add in the slurry, continued ball milling 15 minutes.
(2) on mylar, the baking oven of putting into 100 ℃ is dried with the prepared slurry silk screen printing in silk screen printing, repeats about above step 30 time, until the ceramic membrane that forms 0.15mm.
(3) moulding is cut into the square sheet of 12mm * 12mm with the ceramic membrane that obtains, and takes off diaphragm from substrate, and overlapping about 60 layers, compression moulding.
(4) the plastic removal sintering is put into heat treatment furnace in 650 ℃ of eliminatings organism wherein with above-mentioned biscuit of ceramics.Sample behind the plastic removal is put into High Temperature Furnaces Heating Apparatus, is warming up to 800 ℃ of insulations after 4 hours with the speed of 10 ℃/min, and the speed with 10 ℃/min is warming up to 1200 ℃ of sintered specimens again, is incubated 10 hours.
Embodiment 2 makes ceramic XRD diffracting spectrum as shown in Figure 3, calculates through the Loterging method, and its orientation degree is 32%.On the direction perpendicular to silk screen printing, ceramic crystalline grain is brick-shaped in the part and aligns.
Claims (7)
1, a kind of lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic is characterized in that its chemical formula is (Na
1/2Bi
1/2)
1-xBa
xTiO
3, x=0.05-0.1 wherein, ceramic crystalline grain is brick-shaped, has the texturing feature.
2, by the preparation method of the described a kind of lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic of claim 1, may further comprise the steps:
(1) with Na
2CO
3, BaCO
3, Bi
2O
3And nano-TiO
2Be other raw material powder, with molten-salt growth method synthetic sheet Bi
4Ti
3O
12Be template, press chemical formula (Na
1/2Bi
1/2)
1-xBa
xTiO
3The preparation raw material powder, wherein, x=0.05-0.1, sheet Bi
4Ti
3O
12The Ti that template provides accounts for the 10-30% of required Ti amount mol ratio;
(2) selecting ethyl cellulose or methylcellulose gum or soluble cotton for use is binding agent, and selecting Terpineol 350 or ethylene glycol or Terpineol 350 for use is solvent;
(3) earlier binding agent and solvent heated and stirred are formed clear solution, material powder is added in the above-mentioned solution, ball milling mixes and obtains slurry;
(4) slurry is directly printed onto on the substrate and oven dry by silk screen printing, repeat above-mentioned steps repeatedly, obtain the ceramic thick film of desired thickness, the ceramic thick film that makes was dried 12-20 hour in 90-100 ℃, ceramic thick film is cut into the ceramic diaphragm of desired size, after taking off from substrate, be stacked on compression moulding in the mould, the biscuit after the moulding places in the heat treatment furnace gets rid of organism in 500-800 ℃;
(5) will get rid of organic biscuit after obtain required material behind the high temperature sintering.
3, by the preparation method of the described a kind of lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic of claim 2, it is characterized in that described by quality than binding agent: solvent: raw material powder=1: 12-25: 5-15 proportioning.
4, press the preparation method of the described a kind of lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic of claim 2, it is characterized in that described high temperature sintering condition is warming up to 700-900 ℃ of insulation 2-8 hour for the heat-up rate with 5-10 ℃/min, speed with 5-10 ℃/min is warming up to 1100-1200 ℃ of sintered specimen again, is incubated 2-10 hour.
5, by the preparation method of the described a kind of lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic of claim 1, may further comprise the steps:
(1) adopts solid reaction process, with Na
2CO
3, Bi
2O
3And nano-TiO
2Synthetic Na
0.5Bi
4.5Ti
4O
15Being forerunner's material powder, is the basic material powder with this forerunner's material powder, again with Na
2CO
3, BaCO
3, Bi
2O
3And nano-TiO
2For other raw material powders, press chemical formula (Na
1/2Bi
1/2)
1-xBa
xTiO
3The preparation raw material powder, wherein, x=0.05-0.1, Na
0.5Bi
4.5Ti
4O
15The Ti that template provides accounts for the 10-30% of required Ti amount mol ratio;
(2) selecting ethyl cellulose or methylcellulose gum or soluble cotton for use is binding agent, and selecting Terpineol 350 or ethylene glycol or Terpineol 350 for use is solvent;
(3) earlier binding agent and solvent heated and stirred are formed clear solution, material powder is added in the above-mentioned solution, ball milling mixes and obtains slurry;
(4) slurry is directly printed onto on the substrate and oven dry by silk screen printing, repeat above-mentioned steps repeatedly, obtain the ceramic thick film of desired thickness, the ceramic thick film that makes was dried 12-20 hour in 90-100 ℃, ceramic thick film is cut into the ceramic diaphragm of desired size, after taking off from substrate, be stacked on compression moulding in the mould, the biscuit after the moulding places in the heat treatment furnace gets rid of organism in 500-800 ℃;
(5) will get rid of organic biscuit after obtain required material behind the high temperature sintering.
6, by the preparation method of the described a kind of lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic of claim 5, it is characterized in that described by quality than binding agent: solvent: raw material powder=1: 12-25: 5-15 proportioning.
7, press the preparation method of the described a kind of lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic of claim 5, it is characterized in that described high temperature sintering condition is warming up to 700-900 ℃ of insulation 2-8 hour for the heat-up rate with 5-10 ℃/min, speed with 5-10 ℃/min is warming up to 1100-1200 ℃ of sintered specimen again, is incubated 2-10 hour.
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