CN104692796A - Dielectric material for temperature compensation and method of preparing the same - Google Patents
Dielectric material for temperature compensation and method of preparing the same Download PDFInfo
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Abstract
The present invention provides a dielectric material for temperature compensation of the chemical formula 1 and a method for its production. Chemical formula 1 (Ba1-a-b-3c/2SraMgbLac) (Ti1-xSnx) O3. In the above Chemical Formula 1, 0 <=a<0.20; 0 <b<0.05; 0 <c<0.01; and 0 <x<0.20 as defined in the detailed description.
Description
related application
This application claims right of priority and the rights and interests of No. 10-2013-0152539th, the korean patent application being filed in Korean Intellectual Property Office on December 9th, 2013, at this, its full content is incorporated herein by reference.
Invention field
The present invention relates to the quite high and relative permittivity of a kind of lead-free temperature factor quite high for temperature compensation dielectric materials with and preparation method thereof.
Background technology
Comprise the LC tuning circuit of inductor block (inductor) mainly as the driving circuit in ultrasonic piezoelectric transducer.But, when LC tune drive circuit is used in the auxiliary ultrasonic transducer of such as vehicle parking in the wide temperature range of about-40 DEG C to about 80 DEG C, electrostatic capacitance change based on the piezoelectric transducer of temperature needs to be compensated, to keep drive waveforms in LC tune drive circuit and drive efficiency.
Capacitance temperature factor (TCC) represents the temperature compensation rate of electrostatic capacitance temperature compensation material for reference temperature 25 DEG C, provides as follows:
TCC(ppm/℃)＝10
6X(C
T-C
25/C
25)/(T-25)
Wherein, T represents centigradetemperature (DEG C), each C
tor C
25represent the electrostatic capacitance at each temperature of T or about 25 DEG C.
Piezoelectric for ultrasonic piezoelectric transducer generally includes the large and soft piezoelectric based on plumbous zirconate titanate (or PZT)-5 that frequency aging is little of piezoelectric constant.But, approximately there is scope at about 2,500ppm/ DEG C extremely about 4 under-40 DEG C to the temperature of about 25 DEG C and about 25 DEG C to about 80 DEG C based on the soft piezoelectric of PZT-5, the quite high TCC of 000ppm/ DEG C, in addition, have about 2, the quite high relative permittivity of 000 or higher.
Piezo-electric device for ultrasonic transducer can use tackiness agent such as epoxy resin (epoxy) etc. to stick to the material of such as aluminium, polymer plastic etc. usually.Therefore, such piezo-electric device can have more much bigger TCC owing to depending on the changes in hardness of Adhesive temp.Such as, depend on that the TCC of Adhesive temp characteristic can in the scope of about 6,000ppm/ DEG C to about 10,000ppm/ DEG C.In ultrasonic transducer piezo-electric device can with temperature-compensating device parallel coupled.Therefore, electrostatic capacitance compensation system can have by considering the electrostatic capacitance scope that cancellation ratio is suitably selected, and vibrates reduction characteristic and minimizes, and keep the receiving sensitivity of ultrasonic transducer to make transmitting wave mode.Therefore, compensation system can have the electrostatic capacitance of scope at about 30% to about 70% of piezo-electric device electrostatic capacitance.
Persisting exploitation is able to for the temperature-compensating device in the ultrasonic transducer of vehicle.In an example, such temperature-compensating device can be built in sensor construction, and electric wire can be directly welded on it.Because ultrasonic transducer needs about 400V/mm to the driving voltage of about 600V/mm, pressure, distance of separation etc. in the insulation considering insulation continuous surface, when relative permittivity is less, increasing electrostatic capacitance by increase thickness may be restricted.In addition, when by reducing thickness and increasing electrostatic capacitance, temperature-compensating device can have quite low intensity, and becomes and be difficult to process, and then is difficult to make conglomerate together with ultrasonic transducer.
Therefore, in order to reduce the size of temperature-compensating device and make it be easy to process or manufacture, or the significant temp obtaining ultrasonic piezoelectric transducer in wide temperature range compensates, need temperature compensation rate for about-5,000ppm/ DEG C to approximately-30,000ppm/ DEG C and relative permittivity are more than or equal to the dielectric materials of about 1000.
The dielectric materials for circuit common temperature compensation of current use can comprise based on calcium titanate (CaTiO
3)-zirconia titanate (ZrTiO
3)-strontium titanate (SrTiO
3) material, but its temperature compensation rate is approximately-5,000ppm/ DEG C to approximately-6000ppm/ DEG C to the maximum, and relative permittivity is about 200 to about 800.In some instances, developed capacitance temperature factor (TCC) for approximately-5,000ppm/ DEG C to approximately-15,000ppm/ DEG C based on barium titanate (BaTiO
3)-calcium zirconate (CaZrO
3)-zinc oxide (ZnO)-silicate (SiO
3) material, but its relative permittivity can be about 700 to about 1,100.In another example, developed capacitance temperature factor (TCC) for approximately-2,500ppm/ DEG C and relative permittivity be less than or equal to about 500 based on plumbous oxide (Pb
3o
4)-strontium oxide (SrO)-calcium oxide (CaO)-titanium oxide (TiO
2)-bismuth oxide (Bi
2o
3the material of)-magnesium oxide (MgO).But these materials may comprise poisonous lead (Pb).In another example, reported capacitance temperature factor for approximately-8,700ppm/ DEG C based on calcium titanate (CaTiO
3)-lead titanate (PbTiO
3)-lanthanum trioxide (La
2o
3)-titanium oxide (TiO
2) material.But its relative permittivity for being less than or equal to about 1,000, and also can comprise Pb.
Above-mentioned information disclosed in this part is only for strengthening the understanding to background of the present invention, and therefore, it can containing the information not being formed in the prior art that those of ordinary skill in the art have known in this country.
Summary of the invention
The present invention one illustrative embodiments provides a kind of lead-free specific inductivity high and the dielectric materials for temperature compensation that temperature compensation rate is high; And this dielectric materials can optimize the temperature compensation of ultrasonic piezoelectric transducer in wide temperature range, thus can reduce the size of temperature-compensating device.
The present invention one illustrative embodiments provides a kind of dielectric materials for temperature compensation of chemical formula 1.
Chemical formula 1
(Ba
1-a-b-3c/2Sr
aMg
bLa
c)(Ti
1-xSn
x)O
3
In above chemical formula 1, a is 0≤a<0.20; B is 0<b<0.05; C is 0<c<0.01; And x is 0<x<0.20.
In another illustrative embodiments, the capacitance temperature factor (TCC) that the dielectric materials for temperature compensation is obtained by equation 1 in about-40 DEG C extremely about 25 DEG C with two temperature ranges of about 25 DEG C to about 80 DEG C can be negative (-) value.In addition, capacitance temperature factor can be approximately-5,000ppm/ DEG C to approximately-30,000ppm/ DEG C.
Equation 1
Capacitance temperature factor (TCC) (ppm/ DEG C)=10
6x (C
t-C
25/ C
25)/(T-25)
In equation 1, T represents centigradetemperature (DEG C), and each C
tor C
25represent the electrostatic capacitance at each temperature of T or about 25 DEG C.
In another illustrative embodiments, the dielectric materials (under the reference temperature of 25 DEG C) for temperature compensation can be about 1 according to the relative permittivity of equation 2,000 to about 3,000.
Equation 2
Relative permittivity (K)=ε/ε
0
In equation 2, ε represents the specific inductivity of the dielectric materials for temperature compensation, and ε
0represent permittivity of vacuum.
Another illustrative embodiments of the present invention provides a kind of preparation method of the dielectric materials for temperature compensation, and it comprises: the proportion of composing preparation according to providing in chemical formula 1 comprises barium carbonate (BaCO
3), titanium dioxide (TiO
2), tindioxide (SnO
2), lanthanum trioxide (La
2o
3) and magnesium oxide (MgO) and optional Strontium carbonate powder (SrCO
3) mixture; With at the temperature of about 1280 DEG C to about 1360 DEG C by about for mixture sintering 1 to about 3 hours.
But the invention provides the high and dielectric materials that temperature compensation rate is high of not leaded specific inductivity.Therefore, dielectric materials of the present invention can optimize the temperature compensation of ultrasonic piezoelectric transducer in wide temperature range when not using limiting material to be plumbous, and then can reduce the size of temperature-compensating device.
Embodiment
Should understand, term used herein " vehicle " or " vehicle " or other similar terms comprise common motor vehicle, such as, comprise the passenger vehicle of Multifunctional bicycle (SUV), motorbus, truck, various commercial vehicle, comprise the water craft of various ship and boats and ships, aircraft etc., and comprise hybrid electric vehicle, power truck, burning, plug-in hybrid electric vehicles, hydrogen-powered vehicle and other fuel substitute car (such as, deriving from the fuel of the resource beyond oil).
Term used herein is only used to the object of explanation embodiment instead of is intended to limit the present invention.As used herein, singulative ", one (a, an) " and " being somebody's turn to do (the) " are also intended to comprise plural form, indicate unless clear in context.It will also be appreciated that, the term used in the description " comprises (comprises and/or comprising) " and refers to there are described feature, integer, step, operation, element and/or parts, but does not get rid of and exist or add one or more further feature, integer, step, operation, element, parts and/or its group.As used herein, term "and/or" comprises any of one or more relevant Listed Items and all combinations.
Unless expressly stated or from context clearly, as used herein, term " approximately " is understood as in the normal tolerable limit of this area, such as, in 2 standard deviations of mean value." approximately " can be understood as in 10%, 9%, 8%, 7%, 6%, 5%, 4%, 3%, 2%, 1%, 0.5%, 0.1%, 0.05% or 0.01% of described numerical value.Unless in addition by context clearly, all numerical value provided herein is modified by term " approximately ".
Hereinafter, embodiment is described in detail.But these embodiments are exemplary, and present disclosure is not limited thereto.
In an illustrative embodiments of the present invention, the dielectric materials for temperature compensation can be the material represented by chemical formula 1.
Chemical formula 1
(Ba
1-a-b-3c/2Sr
aMg
bLa
c)(Ti
1-xSn
x)O
3
In chemical formula 1, a is 0≤a<0.20; B is 0<b<0.05; C is 0<c<0.01; And x is 0<x<0.20.Ultrasonic transducer for vehicle works in the temperature range of about-40 DEG C to about 80 DEG C.In order to use based on BaTiO
3material temperature reduced compensate to quite low temperature, BaTiO
3curie temperature (Tc) can be reduced to and be less than or equal to approximately-40 DEG C.When using strontium (Sr) to reduce Tc, room temperature dielectric constant can reduce.Therefore, in an illustrative embodiments of the present invention, based on BaTiO
3material can use together with tin (Sn) and lanthanum (La).Therefore, Tc can reduce, and the reduction effect of specific inductivity can reduce.And, poisonous material such as plumbous (Pb) can not be used, thus the eco-friendly dielectric materials for temperature compensation is provided.
In another illustrative embodiments, the dielectric materials for temperature compensation with the composition of chemical formula 1 can be negative (-) value at about-40 DEG C extremely about 25 DEG C and the capacitance temperature factor (TCC) in the temperature range of about 25 DEG C to about 80 DEG C.Particularly, capacitance temperature factor can be approximately-5,000ppm/ DEG C to approximately-30,000ppm/ DEG C.When having the temperature factor within the scope of this when the dielectric materials for temperature compensation, it can have excellent temperature compensation characteristic in the wide temperature range of about-40 DEG C to about 80 DEG C.Therefore, dielectric materials of the present invention can optimize the temperature compensation of ultrasonic piezoelectric transducer, and can reduce the size of temperature-compensating device further.
In addition, capacitance temperature factor can obtain according to equation 1.
Equation 1
Capacitance temperature factor (TCC) (ppm/ DEG C)=10
6x (C
t-C
25/ C
25)/(T-25)
In equation 1, T represents temperature (DEG C), and each C
tor C
25represent the electrostatic capacitance at each temperature of T or about 25 DEG C.
In addition, the relative permittivity for the dielectric materials (under the reference temperature of 25 DEG C) of temperature compensation can be about 1,000 to about 3,000.When having the relative permittivity within the scope of this when the dielectric materials for temperature compensation, it can have the temperature compensation characteristic of improvement in the wide temperature range of about-40 DEG C to about 80 DEG C.Therefore, dielectric materials of the present invention can optimize the temperature compensation of ultrasonic piezoelectric transducer, and can reduce the size of temperature-compensating device further.
And the relative permittivity under the reference temperature of 25 DEG C can obtain according to equation 2.
Equation 2
Relative permittivity (K)=ε/ε
0
In equation 2, ε represents the specific inductivity of the dielectric materials for temperature compensation, and ε
0represent permittivity of vacuum.
In table 1 below, composition 7,8 and 10-12 correspond to the embodiment according to exemplary embodiment of the invention, and form 1-6 and 9 corresponding to the comparative example according to conventional material.In addition, each a, b, c or x in table 1 represent the proportion of composing corresponding to each content of Sr, Mg, La or Sn of chemical formula 1 respectively.
As shown in table 2 below, the content of Sn, Sr, Mg and La can suitably being regulated according in the scope of illustrative embodiments, so that the relative permittivity under the room temperature of 25 DEG C is about 1, and 500 to about 2,500; Capacitance temperature factor (TCC) at the temperature of about-40 DEG C to about 25 DEG C is approximately-9,200ppm/ DEG C to approximately-30,000ppm/ DEG C.If needed, can by the relative permittivity under regulating the room temperature according to the content increasing or reduce Sn or Sr in the scope of illustrative embodiments and capacitance temperature factor.Therefore, the dielectric materials for temperature compensation according to illustrative embodiments can not comprise Pb, but the high TCC of such high-k and about-40 DEG C to about 80 DEG C can be had, make compared with conventional dielectric materials time, the electrostatic capacitance of piezoelectric transducer reduces and can be able to effective compensation in wide temperature range.
As shown in Tables 1 and 2, when such as only using Sr in composition 1 and 2, Tc is low not; Even if but when a is about 0.5 or about 0.6, TCC may quite high (such as, being greater than threshold value).But when such as in composition 2, the content of Sr increases, room temperature dielectric constant may be sharply deteriorated, may be inappropriate for piezo-electric device compensative material.When such as only comprising Sn in composition 3-5, the composition only comprising Sn may have quite high TCC, or is similar to the specific inductivity that the composition only comprising Sr has sharply deterioration.
Add La and can suppress particle growth in sintering process, and except reducing Tc, the sharply deterioration of specific inductivity can also be prevented.When adding La, when the content c of La is more than or equal to about 0.01; Sintering characteristic may be sharply deteriorated, thus cause quite high dissipation loss.But when sintering temperature increases, most of La can be solidified into particle, and has minimal effect.Therefore, according to an illustrative embodiment of the invention, the content of La can in the scope of 0<c<0.01.
Add Mg and can reduce Tc, strengthen sintering characteristic, and reduce TCC.When such as form in 6 do not comprise Mg time, sintered density may reduce, and dissipation loss may increase.Therefore, the content of Mg can in the scope of about 0<b<0.05, to prevent the sharply deterioration of relative permittivity.Dielectric materials for temperature compensation can be prepared according to following methods.
Can according to the proportion of composing scope provided in chemical formula 1, preparation comprises BaCO
3, TiO
2, SnO
2, La
2o
3with MgO and optional SrCO
3mixture.Can be dry and calcine by the mixture obtained, to prepare synthetic powder, then carry out shaping and sintering.Particularly, sintering can carry out about 1 to about 3 hours at the temperature of about 1280 DEG C to about 1360 DEG C.Particularly, the dielectric materials for temperature compensation that can provide in preparation table 1.According to the proportion of composing provided in table 1, evenly can prepare by adding deionized water and dispersion agent wherein in masher and comprise BaCO
3, TiO
2, SnO
2, SrCO
3, La
2o
3with the mixture of MgO.Can by mixture vacuum filtration, and dry at about 80 DEG C to about 120 DEG C.Dispersion agent can comprise nonionic class dispersion agent etc. with the weight ratio of about 0.25%.The cake of drying can be broken, and at about 1,100 DEG C, calcine about 2 hours, with synthetic raw material.After the cake of calcining is broken, deionized water and dispersion agent can be added wherein, and mixture can be pulverized in masher, filter, and dry, prepare synthetic powder.The polyvinyl alcohol (PVA) of about 10w/w% can be added in synthetic powder.
Mixture mist projection granulating can be become be used for shaping particle, and particle can be suppressed and be shaped to the size of the about 12mm of diameter, the about 1mm of thickness.Then, by particulate mixtures respectively at about 1,300 DEG C and about 1,2 hours can be sintered at 340 DEG C, to prepare pill (pellet).The both sides silver paste of pill can be printed; Can be dry and heat 15 minutes, to produce silver electrode thereon at about 820 DEG C by the pill of printing; And potential electrode characteristic.Use electrostatic capacitance and the dissipation loss of LCR meter (Agilent, 4263B) potential electrode under 1kHz and 1V, and in constant temperature oven, in the temperature range of about-40 DEG C to about 80 DEG C, measure the cancellation ratio of dielectric materials.
Table 1
| Composition numbering | a | b | c | x | Remarks |
| 1 | 0.50 | 0 | 0 | 0 | Comparative example 1 |
| 2 | 0.60 | 0 | 0 | 0 | Comparative example 2 |
| 3 | 0 | 0 | 0 | 0.20 | Comparative example 3 |
| 4 | 0 | 0 | 0 | 0.25 | Comparative example 4 |
| 5 | 0 | 0 | 0 | 0.30 | Comparative example 5 |
| 6 | 0.08 | 0 | 0.006 | 0.10 | Comparative example 6 |
| 7 | 0.08 | 0.005 | 0.005 | 0.10 | Embodiment 1 |
| 8 | 0.08 | 0.005 | 0.0075 | 0.10 | Embodiment 2 |
| 9 | 0.08 | 0.005 | 0.01 | 0.10 | Comparative example 7 |
| 10 | 0.08 | 0.005 | 0.0083 | 0.10 | Embodiment 3 |
| 11 | 0.08 | 0.005 | 0.0065 | 0.125 | Embodiment 4 |
| 12 | 0.08 | 0.005 | 0.0065 | 0.15 | Embodiment 5 |
Table 2
Because comparative example 1 has the quite high Tc of approximately-27 DEG C, therefore TCC may do not provided in table 2.And the sintering characteristic shown due to comparative example 6 and 7 is not enough, the therefore non-prediction amount of its TCC.In addition, the TCC value in table 2 can calculate according to equation 1, and K value can calculate according to equation 2.
Reference table 1 and 2, contrary with comparative example 1-7, use and all in about-40 DEG C extremely about 25 DEG C with two temperature ranges of about 25 DEG C to about 80 DEG C, demonstrate scope about-5 according to each in the embodiment 1-10 of the dielectric materials for temperature compensation of the present invention one illustrative embodiments, 000ppm/ DEG C to about-30, the capacitance temperature factor of 000ppm/ DEG C, and about 1, the relative permittivity of 000 to about 3,000.Therefore, embodiment 1-10 can optimize the temperature compensation of ultrasonic piezoelectric transducer in wide temperature range, and can reduce the size of temperature-compensating device further.
In addition, when sintering temperature is greater than about 1360 DEG C, form new phase, and TCC increases.Meanwhile, when sintering temperature is less than about 1280 DEG C, sintering may be not enough, and may cause high dissipation loss inadequately.
Although present disclosure is described in conjunction with current taken as exemplary embodiment person, but should be appreciated that the present invention is not limited to disclosed embodiment, on the contrary, the invention is intended to contain various variation pattern and equivalent way, it includes within the spirit and scope of claims.
Claims (5)
1. the dielectric materials for temperature compensation of a chemical formula 1:
(Ba
1-a-b-3c/2Sr
aMg
bLa
c)(Ti
1-xSn
x)O
3
Wherein, in chemical formula 1,
A is 0≤a<0.20; B is 0<b<0.05; C is 0<c<0.01; And x is 0<x<0.20.
2. the dielectric materials for temperature compensation according to claim 1, wherein said dielectric materials approximately in-40 DEG C to two temperature ranges of about 25 DEG C and about 25 DEG C to about 80 DEG C according to the capacitance temperature factor (TCC) of equation 1 for bearing (-) value:
Capacitance temperature factor (TCC) (ppm/ DEG C)=10
6x (C
t-C
25/ C
25)/(T-25); And
Wherein, in equation 1, T represents temperature (DEG C), and each C
tor C
25represent the electrostatic capacitance at each temperature of T or 25 DEG C.
3. the dielectric materials for temperature compensation according to claim 2, wherein said dielectric materials is being approximately about-5 according to the capacitance temperature factor (TCC) of equation 1 in-40 DEG C to two temperature ranges of about 25 DEG C and about 25 DEG C to about 80 DEG C, 000ppm/ DEG C to approximately-30,000ppm/ DEG C.
4. the dielectric materials for temperature compensation according to claim 1, wherein said dielectric materials is about 1 according to the relative permittivity of equation 2 under the reference temperature of 25 DEG C, 000 to about 3,000:
Relative permittivity (K)=ε/ε
0
Wherein, in equation 2, ε represents the specific inductivity of the described dielectric materials for temperature compensation, and ε
0represent permittivity of vacuum.
5., for a manufacture method for the dielectric materials of temperature compensation, it comprises:
Barium carbonate (BaCO is comprised with the proportion of composing provided in chemical formula 1 preparation
3), titanium dioxide (TiO
2), tindioxide (SnO
2), lanthanum trioxide (La
2o
3) and magnesium oxide (MgO) and optional Strontium carbonate powder (SrCO
3) mixture; With
Described mixture is sintered at the temperature of about 1280 DEG C to about 1360 DEG C about 1 to about 3 hours:
(Ba
1-a-b-3c/2Sr
aMg
bLa
c)(Ti
1-xSn
x)O3
Wherein, a is 0≤a<0.20; B is 0<b<0.05; C is 0<c<0.01; And x is 0<x<0.20.
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| CN111925199B (en) * | 2020-07-03 | 2022-07-01 | 成都宏科电子科技有限公司 | Low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
| CN112979314B (en) * | 2021-04-19 | 2022-05-10 | 清华大学 | Medium-dielectric-constant high-Q microwave dielectric ceramic material and preparation method thereof |
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| JPH0340962A (en) * | 1989-05-02 | 1991-02-21 | Japan Metals & Chem Co Ltd | Dielectric porcelain composition |
| JP3087657B2 (en) | 1996-07-26 | 2000-09-11 | 株式会社村田製作所 | Dielectric porcelain composition |
| US6268054B1 (en) | 1997-02-18 | 2001-07-31 | Cabot Corporation | Dispersible, metal oxide-coated, barium titanate materials |
| JP2000264724A (en) * | 1999-03-18 | 2000-09-26 | Murata Mfg Co Ltd | Dielectric ceramic composition and ceramic multilayered substrate |
| KR100646680B1 (en) | 2004-06-04 | 2006-11-23 | 익스팬테크주식회사 | Dielectric ceramic composition |
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| Title |
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| I.A.SOUZA ET AL.: "Structural and dielectric properties of Ba0.5Sr0.5(SnxTi1-x)O3 ceramics obtained by the soft chemical method", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| QI WEN ET AL.: "Microstructure of Ba0.615Sr0.35Mg0.035TiO3 dielectric ceramics via X-ray spectrum analysis", 《MATERIALS SCIENCE》 * |
| 沈彩等: "脉冲电流烧结掺杂Ba0.5Sr0.5TiO3陶瓷介电性能的研究", 《无机材料学报》 * |
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