CN104692796B - Dielectric material and preparation method thereof for temperature-compensating - Google Patents
Dielectric material and preparation method thereof for temperature-compensating Download PDFInfo
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Abstract
The dielectric material and preparation method thereof for temperature-compensating of present invention offer chemical formula 1.Chemical formula 1:(Ba1‑a‑b‑3c/ 2SraMgbLac)(Ti1‑xSnx)O3.In the 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, as defined in being described in detail.
Description
Related application
This application claims on December 9th, 2013 to be filed in the South Korea patent application 10-2013- of Korean Intellectual Property Office
Entire contents, are incorporated herein by reference by No. 0152539 priority and right herein.
Invention field
The present invention relates to a kind of lead-free temperature coefficient, quite high and relative permitivity is quite high is used for temperature-compensating
Dielectric material with and preparation method thereof.
Background technique
LC tuning circuit including inductor (inductor) is mainly used as the driving circuit in ultrasonic piezoelectric transducer.
But when LC tune drive circuit is used for such as vehicle parking in about -40 DEG C to about 80 DEG C of wide temperature range
When in auxiliary ultrasonic sensor, the electrostatic capacitance change needs of piezoelectric transducer based on temperature are compensated, to keep
Drive waveforms and drive efficiency in LC tune drive circuit.
Capacitance temperature factor (TCC) indicates electrostatic capacitance temperature-compensating material for 25 DEG C of reference temperature of temperature-compensating
Rate provides as follows:
TCC (ppm/ DEG C)=106X(CT-C25/C25)/(T-25)
Wherein, T indicates Celsius temperature (DEG C), each CTOr C25Indicate the electrostatic electricity at T or about 25 DEG C of each temperature
Hold.
Piezoelectric material for ultrasonic piezoelectric transducer generally includes that piezoelectric constant is big and frequency aging is small based on lead
The soft piezoelectric material of zirconium titanate (or PZT) -5.But the soft piezoelectric material based on PZT-5 at about -40 DEG C to about
Have range at about 2,500ppm/ DEG C to about 4,000ppm/ DEG C at a temperature of 25 DEG C and about 25 DEG C to about 80 DEG C
Quite high TCC, in addition, having about 2,000 or higher quite high relative permitivity.
The adherency such as adhesive such as epoxy resin (epoxy) usually can be used in piezo-electric device for ultrasonic sensor
On such as material of aluminium, polymer plastic etc..Therefore, such piezo-electric device becomes due to depending on the hardness of Adhesive temp
Change and can have much larger TCC.For example, the TCC for depending on Adhesive temp characteristic can be at about 6,000ppm/ DEG C
To in the range of about 10,000ppm/ DEG C.Piezo-electric device can coupling in parallel with temperature compensation means in ultrasonic sensor
It closes.Therefore, electrostatic capacitance compensation device can have the electrostatic capacitance range suitably selected by considering cancellation ratio, so that
Emitting wave mode vibration reduces characteristic minimum, and keeps the receiving sensitivity of ultrasonic sensor.Therefore, compensation device can have
There is range in the electrostatic capacitance of about 30% to about 70% of piezo-electric device electrostatic capacitance.
Persisting exploitation has been able to for the temperature compensation means in the ultrasonic sensor of vehicle.In an example, in this way
Temperature compensation means can be built in sensor structure, and electric wire can be directly welded in thereon.Due to supersonic sensing
The driving voltage of device needs about 400V/mm to about 600V/mm, it is contemplated that the insulation internal pressure of insulation continuous surface separates
Distance etc. may be restricted by increasing thickness to increase electrostatic capacitance when relative permitivity is smaller.In addition, when passing through
Thickness is reduced come when increasing electrostatic capacitance, temperature compensation means there can be rather low intensity, and becomes difficult to handle, Jin Ernan
In conglomerate is made together with ultrasonic sensor.
Therefore, in order to reduce the size of temperature compensation means and make it easier to handle or manufacture, or in wider temperature
The effective temperature compensation that ultrasonic piezoelectric transducer is obtained in range, need temperature-compensating rate be about -5,000ppm/ DEG C extremely
About -30,000ppm/ DEG C and dielectric material of the relative permitivity more than or equal to about 1000.
Dielectric material used at present for circuit common temperature-compensating may include based on calcium titanate (CaTiO3)-
Zirconia titanate (ZrTiO3)-strontium titanates (SrTiO3) material, but its temperature-compensating rate is up to about -5,000ppm/ DEG C to big
About -6000ppm/ DEG C, relative permitivity is about 200 to about 800.In some instances, capacitance temperature system has been developed
Number (TCC) is about -5,000ppm/ DEG C to about -15,000ppm/ DEG C based on barium titanate (BaTiO3)-calcium zirconate
(CaZrO3)-zinc oxide (ZnO)-silicate (SiO3) material, but its relative permitivity can be about 700 to about 1,
100.In another example, developed that capacitance temperature factor (TCC) is about -2,500ppm/ DEG C and relative permitivity is small
In or equal to about 500 based on lead oxide (Pb3O4)-strontium oxide strontia (SrO)-calcium oxide (CaO)-titanium oxide (TiO2)-bismuth oxide
(Bi2O3The material of)-magnesia (MgO).But these materials may include toxic lead (Pb).In another example,
Reporting capacitance temperature factor is about -8,700ppm/ DEG C based on calcium titanate (CaTiO3)-lead titanates (PbTiO3)-lanthana
(La2O3)-titanium oxide (TiO2) material.But relative permitivity can be for less than or equal to about 1,000, and it can also
To include Pb.
Above- mentioned information disclosed in the part are used only for enhancing the understanding to background of the present invention, therefore, can be containing not
Be formed in those of ordinary skill in the art in the country it is known that the prior art information.
Summary of the invention
An of the invention illustrative embodiments provide that a kind of lead-free dielectric constant is high and temperature-compensating rate is high is used for
The dielectric material of temperature-compensating；And the dielectric material can optimize ultrasonic piezoelectric transducer in wider temperature range
Temperature-compensating, so as to reduce the size of temperature compensation means.
An illustrative embodiments of the invention provide a kind of dielectric material for temperature-compensating of chemical formula 1.
Chemical formula 1
(Ba1-a-b-3c/2SraMgbLac)(Ti1-xSnx)O3
In the 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 exemplary embodiment, for the dielectric material of temperature-compensating at about -40 DEG C to about 25 DEG C and
The capacitance temperature factor (TCC) obtained in about 25 DEG C to about 80 DEG C of two temperature ranges by equation 1 can be negative (-)
Value.In addition, capacitance temperature factor can be about -5,000ppm/ DEG C to about -30,000ppm/ DEG C.
Equation 1
Capacitance temperature factor (TCC) (ppm/ DEG C)=106X(CT-C25/C25)/(T-25)
In equation 1, T indicates Celsius temperature (DEG C), and each CTOr C25It indicates in T or about 25 DEG C of each temperature
Under electrostatic capacitance.
In another exemplary embodiment, for the dielectric material of temperature-compensating (under 25 DEG C of reference temperature) basis
The relative permitivity of equation 2 may be about 1,000 to about 3,000.
Equation 2
Relative permitivity (K)=ε/ε0
In equation 2, ε indicates the dielectric constant of the dielectric material for temperature-compensating, and ε0Indicate that vacuum dielectric is normal
Number.
Another exemplary embodiment of the invention provides a kind of preparation method of dielectric material for temperature-compensating,
It include: that barium carbonate (BaCO is included according to the composition ratio preparation provided in chemical formula 13), titanium dioxide (TiO2), stannic oxide
(SnO2), lanthana (La2O3) and magnesia (MgO) and optional strontium carbonate (SrCO3) mixture；With about 1280
DEG C at a temperature of about 1360 DEG C by mixture sintering about 1 to about 3 hour.
The present invention is provided without the lead dielectric material that still dielectric constant is high and temperature-compensating rate is high.Therefore, of the invention
Dielectric material can optimize piezoelectric ultrasonic sensing without using limitation material, that is, lead in wider temperature range
The temperature-compensating of device, and then the size of temperature compensation means can be reduced.
Specific embodiment
It should be understood that terms used herein " vehicle " or " vehicle " or other similar terms include common motor vehicle,
E.g., including sport utility vehicle (SUV), bus, truck, various commercial vehicles car, including various sailer and ships
Water carrier, aircraft etc., and including hybrid electric vehicle, electric vehicle, burning, plug-in hybrid electric vehicles, hydrogen power
Vehicle and other substitute fuel cars (for example, fuel of the resource other than petroleum).
Terms used herein are merely to illustrate that the purpose of specific embodiment without being intended to the limitation present invention.Such as
Used herein, singular " one, a kind of (a, an) " and " being somebody's turn to do (the) " are also intended to including plural form, unless up and down
It is clearly indicated in text.It will also be appreciated that term used in the description " including (comprises and/or
Comprising) " refer to that there are the feature, integer, step, operations, elements, and/or components, but do not exclude the presence of or add
Add one or more of the other feature, integer, step, operation, component, assembly unit and/or its group.As it is used herein, term
"and/or" includes any and all combinations of one or more related listed items.
It is unless expressly stated or from context it is obvious that as used herein, term " about " be understood as this field just
In normal permissible range, for example, in 2 standard deviations of average value." about " can be understood as the numerical value 10%, 9%,
8%, in 7%, 6%, 5%, 4%, 3%, 2%, 1%, 0.5%, 0.1%, 0.05% or 0.01%.Unless in addition by context
It is obvious that all numerical value provided herein are modified by term " about ".
Hereinafter, embodiment is described in detail.But these embodiments are exemplary, in the disclosure
Hold without being limited thereto.
In an illustrative embodiments of the invention, the dielectric material for temperature-compensating be can be by 1 table of chemical formula
The material shown.
Chemical formula 1
(Ba1-a-b-3c/2SraMgbLac)(Ti1-xSnx)O3
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.For vehicle
Ultrasonic sensor work within the temperature range of about -40 DEG C to about 80 DEG C.BaTiO is based in order to use3Material
Temperature is reduced compensation to rather low temperature, BaTiO by material3Curie temperature (Tc) can be reduced to less than or equal to about-
40℃.When reducing Tc using strontium (Sr), room temperature dielectric constant can be reduced.Therefore, in an exemplary embodiment party of the invention
In formula, it is based on BaTiO3Material can be used together with tin (Sn) with lanthanum (La).Therefore, Tc can be reduced, and dielectric is normal
Several reduction effects can be reduced.Furthermore, it is possible to toxic material such as lead (Pb) not used, to provide environmental-friendly use
In the dielectric material of temperature-compensating.
In another exemplary embodiment, the dielectric material for temperature-compensating of the composition with chemical formula 1 is big
Capacitance temperature factor (TCC) within the temperature range of about -40 DEG C to about 25 DEG C and about 25 DEG C to about 80 DEG C can be negative
(-) value.Specifically, capacitance temperature factor can be about -5,000ppm/ DEG C to about -30,000ppm/ DEG C.When for temperature
It, can be in about -40 DEG C to about 80 DEG C of wide temperature model when the dielectric material of compensation has the temperature coefficient within the scope of this
There is excellent temperature compensation characteristic in enclosing.Therefore, dielectric material of the invention can optimize the temperature of ultrasonic piezoelectric transducer
Degree compensation, and be further able to reduce the size of temperature compensation means.
In addition, capacitance temperature factor can be obtained according to equation 1.
Equation 1
Capacitance temperature factor (TCC) (ppm/ DEG C)=106X(CT-C25/C25)/(T-25)
In equation 1, T indicates temperature (DEG C), and each CTOr C25It indicates in T or at about 25 DEG C of each temperature
Electrostatic capacitance.
In addition, the relative permitivity of the dielectric material (under 25 DEG C of reference temperature) for temperature-compensating can be about
1,000 to about 3,000.It, can be when the dielectric material for temperature-compensating has the relative permitivity within the scope of this
There is improved temperature compensation characteristic in about -40 DEG C to about 80 DEG C of wide temperature range.Therefore, dielectric material of the invention
The temperature-compensating of ultrasonic piezoelectric transducer can be optimized, and be further able to reduce the size of temperature compensation means.
Moreover, the relative permitivity under 25 DEG C of reference temperature can be obtained according to equation 2.
Equation 2
Relative permitivity (K)=ε/ε0
In equation 2, ε indicates the dielectric constant of the dielectric material for temperature-compensating, and ε0Indicate that vacuum dielectric is normal
Number.
In table 1 below, 7,8 and 10-12 of composition corresponds to the embodiment of illustrative embodiments according to the present invention, and forms
1-6 and 9 corresponds to the comparative example according to conventional material.In addition, each a, b, c or x in table 1 are respectively indicated and chemical formula 1
The corresponding composition ratio of each content of Sr, Mg, La or Sn.
As shown in table 2 below, the content of Sn, Sr, Mg and La can be fitted in range according to illustrative embodiments
Work as adjusting, so that the relative permitivity at room temperature at 25 DEG C is about 1,500 to about 2,500；At about -40 DEG C to about
Capacitance temperature factor (TCC) at a temperature of 25 DEG C is about -9,200ppm/ DEG C to about -30,000ppm/ DEG C.If needed
It wants, phase at room temperature can be adjusted by increasing or decreasing the content of Sn or Sr in range according to illustrative embodiments
To capacitivity and capacitance temperature factor.Therefore, the dielectric material according to illustrative embodiments for temperature-compensating can be with
Do not include Pb, but can have the high TCC of such high dielectric constant and about -40 DEG C to about 80 DEG C so that with it is normal
When rule dielectric material compares, the electrostatic capacitance reduction of piezoelectric transducer can effectively be mended in wider temperature range
It repays.
As shown in Tables 1 and 2, when such as when forming in 1 and 2 using only Sr, Tc is not low enough；Even if a is about 0.5 or big
When about 0.6, TCC may be quite high (for example, being greater than threshold value).But when such as when the content for forming Sr in 2 increases, room temperature is situated between
Electric constant may be deteriorated sharply, may be inappropriate for piezo-electric device compensating material.When such as composition 3-5 in only wrap
When including Sn, only the composition including Sn may have quite high TCC, or have similar to the composition for only including Sr and sharply deteriorate
Dielectric constant.
La, which is added, to inhibit particle to grow during the sintering process, and other than reducing Tc, can also prevent dielectric
The sharply deterioration of constant.When the content c of addition La, La are greater than or equal to about 0.01；Sintering characteristic may be deteriorated sharply, from
And lead to quite high dielectric absorption.But when sintering temperature increases, most of La can be solidified into particle, and have most
The effect of small limit.Therefore, according to an illustrative embodiment of the invention, the content of La can be in the range of 0 < c < 0.01.
Mg, which is added, can reduce Tc, enhance sintering characteristic, and reduce TCC.When not including Mg in such as composition 6, it is sintered close
Degree may be decreased, and dielectric absorption can increase.Therefore, the content of Mg can in the range of about 0 <b < 0.05, to prevent
The only sharply deterioration of relative permitivity.Dielectric material for temperature-compensating can be prepared according to following methods.
Can be according to the composition ratio range provided in chemical formula 1, preparing includes BaCO3、TiO2、SnO2、La2O3And MgO
And optional SrCO3Mixture.It by the drying of obtained mixture and can calcine, to prepare synthetic powder, then carry out
Molding and sintering.Specifically, sintering can about 1280 DEG C to about 1360 DEG C at a temperature of to carry out about 1 to about 3 small
When.Specifically, the dielectric material for temperature-compensating provided in table 1 can be provided.According to the composition ratio provided in table 1,
It can uniformly be prepared and deionized water and dispersing agent is added thereto including BaCO in grater3、TiO2、SnO2、
SrCO3、La2O3With the mixture of MgO.It can be dry by mixture vacuum filter, and at about 80 DEG C to about 120 DEG C.Point
Powder can include nonionic class dispersing agent etc. with about 0.25% weight ratio.Dry cake can be ruptured, and about
It is calcined at 1,100 DEG C about 2 hours, with synthetic raw material.After the cake of calcining is ruptured, deionized water can be added thereto
And dispersing agent, and mixture can be crushed in grater, it filters, and dry, prepares synthetic powder.It can be to synthetic powder
The middle polyvinyl alcohol (PVA) that about 10w/w% is added.
Can be by mixture mist projection granulating at being used for molding particle, and particle can be suppressed and be shaped to diameter about
The size of 12mm, thickness about 1mm.It is then possible to by particulate mixtures respectively at about 1,300 DEG C and about 1,340 DEG C
Sintering 2 hours, to prepare pellet (pellet).The two sides of pellet can be printed with silver paste；It can be by the pellet of printing big
It dries and heats 15 minutes at about 820 DEG C, to generate silver electrode on it；And measuring electrode characteristic.It is counted using LCR
(Agilent, 4263B) at 1kHz and 1V measuring electrode electrostatic capacitance and dielectric absorption, and about -40 in constant temperature oven
DEG C to the cancellation ratio for measuring dielectric material within the temperature range of about 80 DEG C.
Table 1
| Composition number | 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
Since comparative example 1 has about -27 DEG C of quite high Tc, TCC may not be provided in table 2.Moreover, because
The sintering characteristic that comparative example 6 and 7 is shown is insufficient, therefore the non-prediction amount of its TCC.In addition, the TCC value in table 2 can be according to side
Journey 1 calculates, and K value can be calculated according to equation 2.
Reference table 1 and 2, with comparative example 1-7 on the contrary, mending for temperature using an illustrative embodiments according to the present invention
Each of embodiment 1-10 for the dielectric material repaid is at about -40 DEG C to about 25 DEG C and about 25 DEG C to about 80 DEG C
Two temperature ranges in show capacitance temperature system of the range at about -5,000ppm/ DEG C to about -30,000ppm/ DEG C
Number, and about 1,000 to about 3,000 relative permitivity.Therefore, embodiment 1-10 can be in wider temperature range
Optimize the temperature-compensating of ultrasonic piezoelectric transducer, and is further able to reduce the size of temperature compensation means.
In addition, forming new phase, and TCC increases when sintering temperature is greater than about 1360 DEG C.Meanwhile when sintering temperature
When degree is less than about 1280 DEG C, being sintered may be insufficient, and may inadequately lead to high dielectric absorption.
It is regarded as illustrative embodiments person at present although present disclosure has combined and is described, it is to be understood that, this hair
It is bright to be not limited to disclosed embodiment, on the contrary, it is intended to cover various change mode and equivalent way, include
Within spirit and scope of the appended claims.
Claims (5)
1. a kind of dielectric material for temperature-compensating, it is characterised in that the structure with chemical formula 1:
(Ba1-a-b-3c/2SraMgbLac)(Ti1-xSnx)O3Chemical formula 1
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 material according to claim 1 for temperature-compensating, wherein the dielectric material is at -40 DEG C to 25 DEG C
With in 25 DEG C to 80 DEG C of two temperature ranges according to the capacitance temperature factor (TCC) of equation 1 be negative (-) value:
Capacitance temperature factor (TCC) (ppm/ DEG C)=106*(CT-C25/C25)/(T-25) equation 1；And
Wherein, in equation 1, T indicates temperature (DEG C), and each CTOr C25It indicates quiet at T or 25 DEG C of each temperature
Capacitor.
3. the dielectric material according to claim 2 for temperature-compensating, wherein the dielectric material is at -40 DEG C to 25 DEG C
With according to the capacitance temperature factor (TCC) of equation 1 be -5,000ppm/ DEG C to -30 in 25 DEG C to 80 DEG C of two temperature ranges,
000ppm/℃。
4. the dielectric material according to claim 1 for temperature-compensating, wherein reference of the dielectric material at 25 DEG C
At a temperature of according to the relative permitivity of equation 2 be 1,000 to 3,000:
Relative permitivity (K)=ε/ε0Equation 2
Wherein, in equation 2, ε indicates the dielectric constant of the dielectric material for temperature-compensating, and ε0Indicate that vacuum is situated between
Electric constant.
5. a kind of manufacturing method of the dielectric material for temperature-compensating comprising:
It include barium carbonate (BaCO with the composition ratio preparation provided in chemical formula 13), titanium dioxide (TiO2), stannic oxide
(SnO2), lanthana (La2O3) and magnesia (MgO) and optional strontium carbonate (SrCO3) mixture；With
By the mixture 1280 DEG C to 1360 DEG C at a temperature of be sintered 1 to 3 hour:
(Ba1-a-b-3c/2SraMgbLac)(Ti1-xSnx)O3Chemical formula 1
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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| Microstructure of Ba0.615Sr0.35Mg0.035TiO3 dielectric ceramics via X-ray spectrum analysis;QI Wen et al.;《Materials Science》;20121231;第57卷(第34期);第4510-4512页 |
| Structural and dielectric properties of Ba0.5Sr0.5(SnxTi1-x)O3 ceramics obtained by the soft chemical method;I.A.Souza et al.;《Journal of Alloys and Compounds》;20081117;第877-882页 |
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