CN104496471A - High-Curie-temperature lead-free pyroelectric ceramic material and preparation method thereof - Google Patents

High-Curie-temperature lead-free pyroelectric ceramic material and preparation method thereof Download PDF

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CN104496471A
CN104496471A CN201410696783.1A CN201410696783A CN104496471A CN 104496471 A CN104496471 A CN 104496471A CN 201410696783 A CN201410696783 A CN 201410696783A CN 104496471 A CN104496471 A CN 104496471A
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ceramic material
unleaded
curie temperature
ball
pyroelectric ceramic
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毛朝梁
薛鲁
董显林
王根水
曹菲
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention relates to a high-Curie-temperature lead-free pyroelectric ceramic material and a preparation method thereof; the high-Curie-temperature lead-free pyroelectric ceramic material has the composition chemical formula of CaxSr0.3-xBa0.7Nb2O6, wherein 0<x<=0.3.

Description

Unleaded pyroelectric ceramic material of a kind of high-curie temperature and preparation method thereof
Technical field
The present invention relates to unleaded pyroelectric ceramic material of a kind of high-curie temperature and preparation method thereof, specifically, relate to unleaded pyroelectric ceramic material of a kind of strontium barium niobate base and preparation method thereof, belong to pyroelectric ceramic material technical field.
Background technology
Pyroelectric ceramics is one of responsive first material of key of non-brake method infrared detection technique, and the ferroelectric ceramic material as intrinsic pyroelectricity work pattern generally is perovskite structure containing Pb material.There is the non-strontium barium niobate base ferroelectric material (Sr filling up type quadratic tungsten bronze structure xba 1-xnb 2o 6be called for short SBN) due to have not leaded, volatilize without Pb, environmentally friendly, and strong mechanical property, physical strength is good, the detection figure of merit is higher, and thermal diffusivity is lower and become the huge intrinsic pyroelectricity material of a kind of application potential by the series of advantages such as composition regulation electric property changing material.
At present, the Curie temperature of strontium barium niobate base ferroelectric ceramic(s) is generally on the low side, and after polarization, ceramics sample very easily causes high temperature umpolarization in the course of processing, how to become by the temperature stability introducing new element raising strontium barium niobate ceramics the problem that is needed badly solution.
Summary of the invention
The Curie temperature that the present invention is intended to overcome existing strontium barium niobate base ferroelectric ceramic(s) generally very easily causes the defect of high temperature umpolarization after on the low side, polarization in the course of processing, the invention provides unleaded pyroelectric ceramic material of a kind of high-curie temperature and preparation method thereof.
The invention provides the unleaded pyroelectric ceramic material of a kind of high-curie temperature, the constitutional chemistry formula of the unleaded pyroelectric ceramic material of described high-curie temperature is Ca xsr 0.3-xba 0.7nb 2o 6, wherein 0 < x≤0.3.
Preferably, the unleaded pyroelectric ceramic material of described high-curie temperature Curie temperature be 190-230 DEG C.
Preferably, in the unleaded pyroelectric ceramic material of described high-curie temperature, grain-size is 2-5 microns.
Preferably, the unleaded pyroelectric ceramic material of described high-curie temperature uses in 20-130 DEG C, and high temperature umpolarization can not occur.
Again, present invention also offers the preparation method of the unleaded pyroelectric ceramic material of a kind of above-mentioned high-curie temperature, described method comprises:
1) CaCO is taken according to the constitutional chemistry formula of the unleaded pyroelectric ceramic material of described high-curie temperature 3powder, BaCO 3powder, SrCO 3powder and Nb 2o 5powder, carry out first time ball milling mixing, briquetting successively, be incubated at 1150-1250 DEG C, pulverize, sieve, second time ball milling, obtain the unleaded pyroelectric ceramic material powder of high-curie temperature;
2) in step 1) add binding agent in the unleaded pyroelectric ceramic material powder of high-curie temperature prepared after, through granulation, ageing, sieve, shaping, plastic removal, obtain the ceramic body of the unleaded pyroelectric ceramic material of high-curie temperature;
3) by step 2) ceramic body prepared, at 1300-1400 DEG C of sintering, obtain the unleaded pyroelectric ceramic material of described high-curie temperature.
Preferably, step 1) in, ball milling comprises wet ball grinding for the first time, and the mass ratio of ball milling material, ball-milling medium and dehydrated alcohol is 1:1.0:0.6 ~ 1:1.5:1.2, and Ball-milling Time is 12 ~ 24 hours, and described ball-milling medium is agate ball; First time ball milling post-drying, sieve, then carry out briquetting.
Preferably, step 1) in, second time ball milling comprises wet ball grinding, and the mass ratio of ball milling material and ball-milling medium and dehydrated alcohol is 1:1.5:0.4 ~ 1:2.0:0.8, and Ball-milling Time is 24 ~ 48 hours, and described ball-milling medium is agate ball; Second time ball milling post-drying.
Preferably, step 1) in, with the ramp of 1-4 DEG C/min to 1150-1250 DEG C, be incubated 2 ~ 4 hours.
Preferably, step 2) in, binding agent to be massfraction be 5 ~ 6% polyvinyl alcohol water solution, the add-on of described polyvinyl alcohol solution is 6 ~ 8% of the unleaded pyroelectric ceramic material powder quality of high-curie temperature; Digestion time is 22 ~ 26 hours; Plastic removal condition is plastic removal 1 ~ 2 hour at 750 ~ 850 DEG C.
Preferably, step 3) in, with ramp to 1300 ~ 1400 DEG C of 1 ~ 4 DEG C/min, be then incubated 2 ~ 4 hours.
Beneficial effect of the present invention:
1, the unleaded pyroelectric ceramic material of prepared high-curie temperature not only has grain-size little (2 ~ 5 μm), specific inductivity is moderate, at room temperature in typical ferroelectric phase advantage, Curie temperature can reach 220 DEG C, can be comparable with PZT system leaded pyroelectric ceramics;
2, preparation method of the present invention have technique simple, without the need to specific installation, low cost and other advantages, be applicable to large-scale production, meet industrialization production requirements.
Accompanying drawing explanation
Fig. 1 shows the stereoscan photograph of the obtained stupalith of embodiment 2;
Fig. 2 shows the X-ray diffractogram of comparative example 1 and the stupalith obtained by embodiment 1 ~ 6;
Fig. 3 shows the specific inductivity and dielectric loss variation with temperature graphic representation that comparative example 1 and the obtained stupalith of embodiment 1 ~ 6 record under 100Hz frequency;
Fig. 4 shows the obtained pyroelectric ceramics of embodiment 3 after hyperpolarization, its pyroelectric coefficient variation with temperature curve.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
The problems referred to above existed for prior art and demand, the object of this invention is to provide a kind of microstructure fine and close, crystal grain is tiny, Curie temperature is high, unleaded pyroelectric ceramic material of strontium barium niobate base that temperature stability is good and preparation method thereof, for the application of strontium barium niobate sill in thermoelectric type infrared eye lays the foundation.
Described unleaded pyroelectric ceramic material has and forms general formula as follows: Ca xsr 0.3-xba 0.7nb 2o 6, wherein: 0 < x≤0.3.
Unleaded pyroelectric ceramic material provided by the invention can adopt traditional solid phase method powder process and air calcination technique to be prepared from.It is little that prepared unleaded pyroelectric ceramic material not only has grain-size, and specific inductivity is moderate, and at room temperature in typical ferroelectric phase advantage, and Curie temperature is higher, and temperature stability is good.In addition, preparation method of the present invention have technique simple, without the need to specific installation, low cost and other advantages, be applicable to large-scale production, meet industrialization production requirements.
The invention provides the method for the unleaded pyroelectric ceramic material of a kind of above-mentioned high-curie temperature, comprise the steps:
A) by general formula: Ca xsr 0.3-xba 0.7nb 2o 6, 0 < x≤0.3, takes the CaCO of stoichiometric ratio 3, BaCO 3, SrCO 3and Nb 2o 5each powder, ball milling makes to mix;
B) mixed powder step a) obtained dries rear briquetting, synthesizes, obtain consisting of Ca under air atmosphere in 1150 ~ 1250 DEG C xsr 0.3-xba 0.7nb 2o 6powder;
C) by step b) Ca that obtains xsr 0.3-xba 0.7nb 2o 6powder carries out pulverizing, sieving, and ball milling makes to mix again;
D) by step c) powder that obtains dries, and adds binding agent, through granulation, ageing, sieve, shaping, plastic removal, obtain ceramic body;
E) by steps d) ceramic body that obtains sinters in atmosphere: with ramp to 1300 ~ 1400 DEG C of 1 ~ 4 DEG C/min, be then incubated 2 ~ 3 hours; Cool to room temperature with the furnace, obtain described unleaded pyroelectric ceramic material.
As a kind of preferred version, step a) in ball milling be wet ball grinding, the mass ratio of ball milling material and ball-milling medium and dehydrated alcohol is 1:1.0:0.6 ~ 1:1.5:1.2, and Ball-milling Time is 12 ~ 24 hours, and described ball-milling medium is agate ball.
As a kind of preferred version, step b) described in mixed powder cross 40 mesh sieves after the drying.
As a kind of preferred version, step c) described in sieve be 40 mesh sieves.
As a kind of preferred version, step c) in ball milling be wet ball grinding, the mass ratio of ball milling material and ball-milling medium and dehydrated alcohol is 1:1.5:0.4 ~ 1:2.0:0.8, and Ball-milling Time is 24 ~ 48 hours, and described ball-milling medium is agate ball.
As a kind of preferred version, steps d) in binding agent to be massfraction be 5 ~ 6% polyvinyl alcohol water solution, the add-on of described polyvinyl alcohol solution is Ca xsr 0.3-xba 0.7nb 2o 66 ~ 8% of powder quality.
As a kind of preferred version, steps d) in digestion time be 22 ~ 26 hours.
As a kind of preferred version, steps d) described in sieve be 20 mesh sieves.
As a kind of preferred version, steps d) in plastic removal condition be plastic removal 1 ~ 2 hour at 750 ~ 850 DEG C.
Compared with prior art, the present invention has following beneficial effect:
1, the unleaded pyroelectric ceramic material of prepared high-curie temperature not only has grain-size little (2 ~ 5 μm), specific inductivity is moderate, at room temperature in typical ferroelectric phase advantage, Curie temperature can reach 220 DEG C, can be comparable with PZT system leaded pyroelectric ceramics;
2, preparation method of the present invention have technique simple, without the need to specific installation, low cost and other advantages, be applicable to large-scale production, meet industrialization production requirements.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Comparative example 1
First according to general formula Sr 0.3ba 0.7nb 2o 6[x=0.00, referred to as CSBN (0.00)] takes the BaCO of stoichiometric ratio 3, SrCO 3and Nb 2o 5each powder, makes all powders mix by wet ball grinding technique; Ball milling condition is: ball milling material, agate ball and dehydrated alcohol mix by the mass ratio of 1:1.2:1.0, ball milling 24h;
Gained mixed powder to be dried and after crossing 40 mesh sieves, briquetting, synthesizes under air atmosphere, and synthesis temperature is 1200 DEG C, and generated time is 3h, obtains consisting of Sr 0.3ba 0.7nb 2o 6powder; Pulverize, cross 40 mesh sieves, again by wet ball grinding technique, powder is mixed; Ball milling condition is: ball milling material, agate ball and dehydrated alcohol mix by the mass ratio of 1:1.8:0.7, ball milling 48h;
Gained CSBN (0.00) powder is dried, the massfraction adding powder quality 7% be polyvinyl alcohol (PVA) aqueous solution of 5% as binding agent, granulation, ageing 24h, crosses 20 mesh sieves, shaping, at 800 DEG C of plastic removals, i.e. obtained Sr 0.3ba 0.7nb 2o 6base substrate; Base substrate is sintered in atmosphere: with the ramp of 2 DEG C/min to 1360 DEG C, be then incubated 4h;
Cool to room temperature with the furnace, obtain pyroelectric ceramic material Sr 0.3ba 0.7nb 2o 6, referred to as CSBN (0.00);
Gained pyroelectric ceramics sample is polished, cleans, dries, silk screen printing silver slurry, then dry, silver ink firing 20 ~ 40min at 650 ~ 750 DEG C, make ceramic component to measure dielectric properties;
Gained ceramic component is placed in silicone oil, is heated to 180 ~ 200 DEG C of insulations, then with the polarized electric field intensity of 5kV/mm, ceramic component is polarized 60min.Sample after polarization is surveyed it and does not add outer pyroelectric property after the match.
Embodiment 1
The difference of the present embodiment and comparative example 1 is only: according to general formula Ca 0.05sr 0.25ba 0.7nb 2o 6[x=0.05, referred to as CSBN (0.05)] takes the CaCO of stoichiometric ratio 3, BaCO 3, SrCO 3and Nb 2o 5each powder;
All the other contents of the present embodiment are all identical with described in comparative example 1.
Embodiment 2
The difference of the present embodiment and comparative example 1 is only: according to general formula Ca 0.1sr 0.2ba 0.7nb 2o 6[x=0.10, referred to as CSBN (0.10)] takes the CaCO of stoichiometric ratio 3, BaCO 3, SrCO 3and Nb 2o 5each powder;
All the other contents of the present embodiment are all identical with described in comparative example 1.
Embodiment 3
The difference of the present embodiment and comparative example 1 is only: according to general formula Ca 0.15sr 0.15ba 0.7nb 2o 6[x=0.15, referred to as CSBN (0.15)] takes the CaCO of stoichiometric ratio 3, BaCO 3, SrCO 3and Nb 2o 5each powder;
All the other contents of the present embodiment are all identical with described in comparative example 1.
Embodiment 4
The difference of the present embodiment and comparative example 1 is only: according to general formula Ca 0.2sr 0.1ba 0.7nb 2o 6[x=0.20, referred to as CSBN (0.20)] takes the CaCO of stoichiometric ratio 3, BaCO 3, SrCO 3and Nb 2o 5each powder;
All the other contents of the present embodiment are all identical with described in comparative example 1.
Embodiment 5
The difference of the present embodiment and comparative example 1 is only: according to general formula Ca 0.25sr 0.05ba 0.7nb 2o 6[x=0.25, referred to as CSBN (0.25)] takes the CaCO of stoichiometric ratio 3, BaCO 3, SrCO 3and Nb 2o 5each powder;
All the other contents of the present embodiment are all identical with described in comparative example 1.
Embodiment 7
The difference of the present embodiment and comparative example 1 is only: according to general formula Ca 0.3ba 0.7nb 2o 6[x=0.30, referred to as CSBN (0.30)] takes the CaCO of stoichiometric ratio 3, BaCO 3and Nb 2o 5each powder;
All the other contents of the present embodiment are all identical with described in comparative example 1.
Fig. 1 is the stereoscan photograph of the strontium barium niobate calcium pyroelectric ceramics that the present embodiment 2 obtains, as seen from Figure 1: most of grain-size of pottery is less, between 2-5 μm.
The X-ray diffractogram of the pyroelectric ceramic material of Fig. 2 obtained by comparative example 1 and embodiment 1 ~ 6, as seen from Figure 2: the pyroelectric ceramic material that above-mentioned comparative example and embodiment obtain is all in tungsten bronze phase completely.
Fig. 3 is the specific inductivity that records under 100Hz frequency of the obtained pyroelectric ceramics of comparative example 1 and embodiment 1 ~ 6 and dielectric loss variation with temperature graphic representation, as seen from Figure 3: the pyroelectric ceramic material that above-mentioned comparative example and embodiment obtain is with change of component (change of x value), transformation temperature first increases rear reduction, wherein CSBN (0.20) Curie temperature is the highest, reaches 223 DEG C.And along with the increase of Ca content, dielectric peak is more and more narrow.
Fig. 4 be the obtained pyroelectric ceramics of embodiment 3 after hyperpolarization, its pyroelectric coefficient variation with temperature curve.Temperature range is 20 DEG C ~ 130 DEG C, and temperature rise rate is 2 DEG C/min.Measure twice, the repeatability of result is fine, illustrates at this temperature, and the temperature stability of pyroelectric ceramics is fine, and high temperature umpolarization does not occur.
The pyroelectric ceramic material of table 1 obtained by comparative example 1 and embodiment 1 ~ 6 be (~ 25 DEG C) performance data of testing at room temperature.
Table 1
From table 1: the specific inductivity of pyroelectric ceramic material adopting the inventive method to prepare is moderate, at room temperature in typical ferroelectric phase, Curie temperature can be comparable with PZT system leaded pyroelectric ceramics.
Visible in sum: unleaded pyroelectric ceramic material provided by the invention not only has size of microcrystal less (about 3 ~ 5 μm), and Curie temperature is high; And preparation method of the present invention is simple, low without the need to specific installation, cost, be applicable to large-scale production, industrialization demand can be met.

Claims (10)

1. the unleaded pyroelectric ceramic material of high-curie temperature, is characterized in that, the constitutional chemistry formula of the unleaded pyroelectric ceramic material of described high-curie temperature is Ca xsr 0.3-xba 0.7nb 2o 6, wherein 0 < x≤0.3.
2. the unleaded pyroelectric ceramic material of high-curie temperature according to claim 1, is characterized in that, the Curie temperature of the unleaded pyroelectric ceramic material of described high-curie temperature is 190-230 DEG C.
3. the unleaded pyroelectric ceramic material of high-curie temperature according to claim 1 and 2, is characterized in that, in the unleaded pyroelectric ceramic material of described high-curie temperature, grain-size is 2-5 microns.
4., according to the described unleaded pyroelectric ceramic material of high-curie temperature arbitrary in claim 1-3, it is characterized in that, the unleaded pyroelectric ceramic material of described high-curie temperature uses in 20-130 DEG C, and high temperature umpolarization can not occur.
5. the preparation method of the unleaded pyroelectric ceramic material of arbitrary described high-curie temperature in claim 1-4, it is characterized in that, described method comprises:
1) CaCO is taken according to the constitutional chemistry formula of the unleaded pyroelectric ceramic material of described high-curie temperature 3powder, BaCO 3powder, SrCO 3powder and Nb 2o 5powder, carry out first time ball milling mixing, briquetting successively, be incubated at 1150-1250 DEG C, pulverize, sieve, second time ball milling, obtain the unleaded pyroelectric ceramic material powder of high-curie temperature;
2) after adding binding agent in the unleaded pyroelectric ceramic material powder of high-curie temperature prepared in step 1), through granulation, ageing, sieve, shaping, plastic removal, obtain the ceramic body of the unleaded pyroelectric ceramic material of high-curie temperature;
3) by step 2) ceramic body prepared, at 1300-1400 DEG C of sintering, obtain the unleaded pyroelectric ceramic material of described high-curie temperature.
6. preparation method according to claim 5, is characterized in that, in step 1), ball milling comprises wet ball grinding for the first time, the mass ratio of ball milling material, ball-milling medium and dehydrated alcohol is 1:1.0:0.6 ~ 1:1.5:1.2, and Ball-milling Time is 12 ~ 24 hours, and described ball-milling medium is agate ball; First time ball milling post-drying, sieve, then carry out briquetting.
7. the preparation method according to claim 5 or 6, is characterized in that, in step 1), second time ball milling comprises wet ball grinding, the mass ratio of ball milling material and ball-milling medium and dehydrated alcohol is 1:1.5:0.4 ~ 1:2.0:0.8, and Ball-milling Time is 24 ~ 48 hours, and described ball-milling medium is agate ball; Second time ball milling post-drying.
8., according to described preparation method arbitrary in claim 5-7, it is characterized in that, in step 1), with the ramp of 1-4 DEG C/min to 1150-1250 DEG C, be incubated 2 ~ 4 hours.
9. according to described preparation method arbitrary in claim 5-8, it is characterized in that, step 2) in, binding agent to be massfraction be 5 ~ 6% polyvinyl alcohol water solution, the add-on of described polyvinyl alcohol solution is 6 ~ 8% of the unleaded pyroelectric ceramic material powder quality of high-curie temperature; Digestion time is 22 ~ 26 hours; Plastic removal condition is plastic removal 1 ~ 2 hour at 750 ~ 850 DEG C.
10., according to described preparation method arbitrary in claim 5-9, it is characterized in that, in step 3), with ramp to 1300 ~ 1400 DEG C of 1 ~ 4 DEG C/min, be then incubated 2 ~ 4 hours.
CN201410696783.1A 2014-11-26 2014-11-26 High-Curie-temperature lead-free pyroelectric ceramic material and preparation method thereof Pending CN104496471A (en)

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CN106365636A (en) * 2016-08-26 2017-02-01 中国科学院上海硅酸盐研究所 High-Curie-temperature strontium-barium niobate pyroelectric ceramic material and preparation method thereof
CN108516827A (en) * 2018-06-19 2018-09-11 哈尔滨工业大学 A kind of ceramic material and preparation method thereof of unleaded high dielectric energy storage density and high energy storage efficiency
CN114507064A (en) * 2020-11-16 2022-05-17 中国民航大学 Novel photochromic material and preparation method thereof

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CN102503410A (en) * 2011-11-02 2012-06-20 宁波大学 Barium strontium titanate-lead titanate pyroelectric ceramic and preparation method thereof
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Application publication date: 20150408