CN101213680A - Piezoelectric/electrostrictive film element production method - Google Patents
Piezoelectric/electrostrictive film element production method Download PDFInfo
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- CN101213680A CN101213680A CN 200680023734 CN200680023734A CN101213680A CN 101213680 A CN101213680 A CN 101213680A CN 200680023734 CN200680023734 CN 200680023734 CN 200680023734 A CN200680023734 A CN 200680023734A CN 101213680 A CN101213680 A CN 101213680A
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Abstract
A method for manufacturing a piezoelectric /electrostrictive element includes a step of subjecting the piezoelectric/electrostrictive film to a heat treatment and a polarization treatment after the film is allowed to stand until the value of an electric constant has converged after the heat treatment. The piezoelectric/electrostrictive element manufactured in this method has small stress remaining in the piezoelectric/electrostrictive film, and predetermined performance regarding, for example, a displacement amount, a displacement-generating force, and an electric power efficiency (consumed electric power) as a piezoelectric/electrostrictive element (piezoelectric/electrostrictive film) is never spoiled.
Description
Technical field
The present invention relates to the manufacture method of piezoelectric/electrostrictive film element.
Background technology
The piezoelectric/electrostrictive device that is called as " diaphragm element " is used as driver and various transducer all the time.For example as patent documentation 1 (Japanese kokai publication hei 8-201265 communique) is disclosed, be used for the characteristic measurement of the density, concentration, viscosity etc. of fluid as the piezoelectric/electrostrictive device of transducer.This piezoelectric/electrostrictive device utilization the amplitude of the oscillator that it had and with the viscous drag of oscillator fluid in contact between have relevant relation and be used as transducer.Mode of vibration in the such machinery of the vibration of oscillator is can be exchanged into the equivalent electric circuit at electricity system, in fluid, make the piezoelectric/electrostrictive device vibration, the viscous drag of this oscillator base flow body is subjected to mechanical resistance, thereby the situation that the electric constant of equivalent electric circuit that detect to constitute the piezoelectrics of oscillator changes, and then can measure the characteristic of the viscosity, density, concentration etc. of fluid.
The fluid that piezoelectric/electrostrictive device can be measured as transducer is liquids and gases.Be not only the liquid that constitutes by single component of water, alcohol, wet goods, also be included in dissolving in these liquid or mix or liquid, slip, the cream of the solvable or insoluble medium that suspends.Perhaps, as the electric constant that will detect can exemplify that loss constant, phase place, resistance, reactance, electricity are led, susceptance, inductance, static capacity (electric capacity) etc., especially preferably use near the resonance frequency of equivalent electric circuit, to have a very big or electric loss coefficient or a phase place of little change.Thus, not only can measure fluid viscosity and also can measure density and concentration, for example, can measure the sulfuric acid concentration in the aqueous sulfuric acid.Have again,, beyond the electric constant,, also can utilize the variation of resonance frequency if do not have special problem from the viewpoint of measuring precision, durability as the index of the variation that detects mode of vibration.
The piezoelectric/electrostrictive film element being subjected to displacement (vibration) part in the piezoelectric/electrostrictive device uses piezoelectric/electrostrictive material, this piezoelectric/electrostrictive material is in strong dielectric body phase usually at normal temperatures, at high temperature then becomes common dielectric body phase or anti-strong dielectric body phase.For example, with Pb (Zr
0.54Ti
0.46) O
3(lead zirconate titanate) be the piezoelectric/electrostrictive material of main component from being strong dielectric body phase near the normal temperature to 320 ℃, more than near 320 ℃, be common dielectric body phase.In addition, for example, with (Bi
0.5Na
0.5) O
3(sodium titanate bismuth) be the piezoelectric/electrostrictive material of main component from being strong dielectric body phase near the normal temperature to 200 ℃, from being anti-strong dielectric body phase near to 320 ℃ near the 200C, more than near 320 ℃, then be common dielectric body phase.
Use the situation of this piezoelectric/electrostrictive material as piezoelectric/electrostrictive film element, usually, after piezoelectric/electrostrictive material and electrode material are configured as intended shape, integrated by heat treated, thereafter, by being that the low temperature of the phase transition temperature of principal phase is implemented polarization and handled mutually than near the strong dielectric body the normal temperature, thereby obtain desired piezoelectric characteristic.At this moment, in the front and back that polarization is handled, the electric constant of change piezoelectric/electrostrictive film element is the numerical value of static capacity for example.This is because handle by polarization, makes the orientation unanimity of the crystallographic axis of piezoelectric/electrostrictive material, usually, the rate of change of the electric constant of the piezoelectric/electrostrictive film element before and after polarization is handled, each piezoelectric/electrostrictive material is the value of almost fixed.Also have, implemented piezoelectric/electrostrictive film element after polarization is handled, can reset into the state of implementing before polarization is handled by being heated to be the Regeneration Treatment more than the phase transition temperature.The electric constant of the piezoelectric/electrostrictive film element after the Regeneration Treatment turns back to the value that polarization is handled, if polarize processing once more, then becomes with initial polarization and handles the roughly the same electric constant in back.Like this, handle and Regeneration Treatment, the electric constant of piezoelectric/electrostrictive film element is reversibly changed by polarization.
The piezoelectric/electrostrictive film element that piezoelectric/electrostrictive device possessed that uses as aforesaid transducer, desired characteristic can not fluctuate, and is relative therewith, in existing piezoelectric/electrostrictive film element, has the situation of initial stage characteristic because of the individual difference fluctuation.At this problem, patent documentation 2 (TOHKEMY 2004-23688 communique) has proposed to have in the finished product stage manufacture method of the piezoelectricity part of the instrument of placing at normal temperatures after heat ageing, but in order to make the stability of characteristics of piezoelectric/electrostrictive film element, polarization is handled very important, but because the polarization meeting becomes unstable because of heat ageing, so disclosed method may not necessarily obtain specific piezoelectric/electrostrictive film element after stable.
The present invention is in view of above-mentioned thing, and purpose is to provide the scheme that obtains the piezoelectric/electrostrictive film element after the initial stage stability of characteristics.
The result that the present inventor studies repeatedly, found to be expressed as follows the situation of movement, promptly when carrying out that piezoelectric/electrostrictive film element is heated to processing more than the phase transition temperature, even if make piezoelectric/electrostrictive film element turn back to normal temperature after the heat treated, but directly do not turn back to strong dielectric body phase, and turn back to strong dielectric body phase gradually through several minutes～a few hours.Promptly, turn back to normal temperature after, inside at piezoelectric/electrostrictive film element, be in the strong dielectric body on the microcosmic mutually and the state that mixes mutually of common dielectric body, the together variation gradually of elapsed time after their ratio and the heating reprocessing, finally reaching with the strong dielectric body is the microstructure of principal phase mutually.Indeterminate organizing of this movement, and think that stress that piezoelectric/electrostrictive film element inside is produced and effluxion together discharge gradually because be accompanied by heating.
The electric constant of the present piezoelectric/electrostrictive film element of change list of this phase structure that is accompanied by the elapsed time after the heat treated is the value of static capacity for example.The electric constant of piezoelectric/electrostrictive film element sharply changes after heat treated, and thereafter, variation gradually diminishes, and near fixed value.So, can hold the done state of phase transformation according to the variation of electric constant.
Have again, as mentioned above, when implementing the polarization processing under the inadequate state of phase transformation of strong dielectric body phase, it is specific then can not obtain sufficient piezoelectric after piezoelectric/electrostrictive film element is carried out heat treated for present inventor's discovery, and characteristic can fluctuate.Promptly, under the inadequate state of the phase transformation after the heat treated, when piezoelectric/electrostrictive film element had been implemented polarization and handled, the variation of the electric constant of piezoelectric/electrostrictive film element before and after polarization is handled was with different in the situation of fully having carried out having implemented under the state after the phase transformation polarization processing.Especially the piezoelectric/electrostrictive material that has, when in phase transformation being implements polarization to handle under insufficient state, the magnitude relationship that then has the electric constant of polarization before and after handling with in phase transformation be the opposite situation of situation of having carried out the polarization processing under the sufficient state.This situation, the piezoelectric after polarization is handled is specific very low, because of implementing the timing that polarization is handled, causes characteristic to have than great fluctuation process.
In the manufacturing process of piezoelectric/electrostrictive film element, except with piezoelectric/electrostrictive material and the incorporate operation of polarization material, also have the situation of under removing unwanted organic substance, implementing heat treated in operation and dewatered operation etc., impact except the piezoelectric characteristic of the elapsed time of operation during the treatment process that polarizes after the polarization processing from these heating.
On the basis of above-mentioned opinion, as the scheme of the stability of characteristicsization of piezoelectric/electrostrictive film element having been finished the present invention as follows.
A kind of manufacture method of piezoelectric/electrostrictive film element promptly, at first is provided, be that a kind of manufacturing stacks gradually lower electrode, piezoelectric film, and the method for the piezoelectric/electrostrictive film element of upper electrode, wherein, have the piezoelectric film is carried out heat treated, place thereafter, and after the value of the electric constant after the heat treated of the piezoelectric film convergence, the operation that the piezoelectric film is polarized and handles.Here, the convergence magnitude relationship of value before and after polarization is handled that be meant electric constant (for example static capacity) is consistent with the magnitude relationship of the situation of having implemented the polarization processing after having placed the sufficient time after the heat treated.In other words, polarization is handled preceding and after magnitude relationship and the heat treated of value of electric constant (for example static capacity) after to have placed the magnitude relationship of value of electric constant (for example static capacity) of the situation of having implemented the polarization processing after the sufficient time inconsistent at the placement initial stage, but it is consistent along with the process of time, is judged as convergence when it is consistent.
Usually, the piezoelectric film that is made of piezoelectric/electrostrictive material is if carry out heat treated with the temperature more than the transformation temperature, and then the piezoelectric film undergoes phase transition, and crystalline texture changes.Think if be placed into temperature descend then internal stress discharge, the in opposite directions phase transfer of regulation of piezoelectric thereafter.If having carried out polarization before the phase transfer of such regulation handles, then cause in the piezoelectric film, taking place bigger internal stress, can't obtain the characteristic (for example piezoelectric constant) of the regulation that the piezoelectric film had, so this is the reason of incipient surge.Its result, there is fluctuation in the characteristic that is inferred as piezoelectric/electrostrictive film element with this piezoelectric film and piezoelectric/electrostrictive device.Here, regulation be meant mutually the strong dielectric body mutually with the common dielectric body mutually or anti-strong dielectric body on microcosmic with the state of the regulation mixed that is suitable for this piezoelectric film.In relating to the manufacture method of piezoelectric/electrostrictive film element of the present invention, think that the value of the electric constant after the heat treated of piezoelectric film finishes the transfer of the phase after the heat treated of piezoelectric film with the state of convergence, thereafter, to the processing that polarizes of piezoelectric film, the piezoelectric film of handling so implement to polarize is in the state of regulation phase, treatment characteristic can not fluctuate even polarize, and the numerical value that can be used as fixed range can reliably be guaranteed.Therefore, in piezoelectric/electrostrictive film element and piezoelectric/electrostrictive device, be difficult to the characteristics fluctuation of early period of origination.The characteristic of piezoelectric/electrostrictive device for example is meant at transducer and is meant that load takes place in institute when vibrating under the same conditions, is meant displacement, displacement generating capacity, electrical efficiency (consumption electric power) at driver.
In relating to the manufacture method of piezoelectric/electrostrictive film element of the present invention, the temperature when preferably placing is the phase point temperature of above-mentioned piezoelectric film or following.According to this optimal way, can promote the piezoelectric film to stipulate the transfer of phase mutually, can shorten the stand-by period between the polarization after the heat treated is handled.
In relating to the manufacture method of piezoelectric/electrostrictive film element of the present invention, preferably to the additional at least pulsatile once shape voltage of piezoelectric film and the processing that polarizes.According to this optimal way, can be more with the stability of characteristicsization of piezoelectric/electrostrictive device.
In relating to the manufacture method of piezoelectric/electrostrictive film element of the present invention, preferred electric constant is electrostatic capacitance or loss coefficient.Have again, as electric constant can be fit to use that resistance, reactance, the electricity of piezoelectric film are led, susceptance, inductance etc.
Have again, make the situation of piezoelectric/electrostrictive film element, in order to boost productivity, the employing a plurality of element of ining succession of producing once, be divided into each method, but there is internal stress in this situation in the piezoelectric/electrostrictive film element inside that is divided between each, if when polarizing in this state, the regulation ability of then losing the piezoelectric film is displacement, displacement generation power for example.For this reason, preferably use dicer to be divided into each, internal stress is discharged after, polarize.
Secondly, the manufacture method of making piezoelectric/electrostrictive device is provided, this piezoelectric/electrostrictive device is possessing the piezoelectric/electrostrictive film element that stacks gradually lower electrode, piezoelectric film and upper electrode at least and constitute by having heavy section at periphery and having on the substrate that the pottery of thin-walled diaphragm portion constitutes, wherein, has following operation, promptly, after obtaining the substrate that constitutes by pottery, on the substrate that constitutes by this pottery, utilize the above-mentioned manufacture method that relates to arbitrary piezoelectric/electrostrictive film element of the present invention to form piezoelectric/electrostrictive film element.
Secondly, providing a kind of piezoelectric/electrostrictive film element, stack gradually lower electrode, piezoelectric film and upper electrode, is to utilize the above-mentioned piezoelectric/electrostrictive film element that relates to the manufacture method of arbitrary piezoelectric/electrostrictive film element of the present invention and make.Promptly, relating to piezoelectric/electrostrictive film element of the present invention limits with two important documents.First is to the processing (polarization) that polarizes of piezoelectric film as thing.Second is that polarization is handled in that the piezoelectric film is carried out heat treated, place thereafter, after the electric constant convergence after the heat treated of piezoelectric film again to the piezoelectric/electrostrictive film element processing (so manufacturing) that polarizes.Piezoelectric/electrostrictive film element according to second polarized processing of important document, as a result of, the static capacity of this piezoelectric film with polarize handle before or fully place after the magnitude relationship of the static capacity of piezoelectric/electrostrictive film element after the Regeneration Treatment and the Regeneration Treatment after polarization when having carried out polarization to handle the magnitude relationship of static capacity of front and back identical.
Secondly, provide piezoelectric/electrostrictive device, wherein, possessing the above-mentioned piezoelectric/electrostrictive film element of the present invention that relates to by having heavy section at periphery and having on the substrate that the pottery of thin-walled diaphragm portion constitutes.
Summary of the invention
Description of drawings
Fig. 1 is the vertical view that expression relates to the execution mode of piezoelectric/electrostrictive device of the present invention.
Fig. 2 is the figure that expression relates to the execution mode of piezoelectric/electrostrictive device of the present invention, is the cutaway view of the AA section in the presentation graphs 1.
Fig. 3 is the figure that expression relates to the execution mode of piezoelectric/electrostrictive device of the present invention, is the cutaway view of the BB section in the presentation graphs 1.
Fig. 4 is the key diagram that expression relates to other execution mode of piezoelectric/electrostrictive device of the present invention, is the expression cutaway view suitable with Fig. 2.
Fig. 5 is the stereogram that expression relates to the execution mode of piezoelectric/electrostrictive film element of the present invention.
Fig. 6 is the cutaway view that expression relates to the execution mode of piezoelectric/electrostrictive film element of the present invention.
Fig. 7 is the chart of execution mode that expression relates to the manufacture method of piezoelectric/electrostrictive film element of the present invention, is to have adopted expression in the situation of static capacity the piezoelectric film to be carried out the figure of relation of the static capacity (relative value, the longitudinal axis) of standing time after the heat treated (transverse axis) and piezoelectric film as electric constant.
Fig. 8 is the chart of execution mode that expression relates to the manufacture method of piezoelectric/electrostrictive device of the present invention, is to have adopted expression in the situation of static capacity the piezoelectric film to be carried out the figure of relation of the static capacity (relative value, the longitudinal axis) of standing time after the heat treated (transverse axis) and piezoelectric film as electric constant.
Among the figure:
The 1-ceramic substrate; The 2-heavy section; 3-thin-walled diaphragm portion; The 4-lower electrode; 5-piezoelectric film; The 6-upper electrode; The incomplete joint portion of 7A, 7B-, 7C-binder course; The 8-auxiliary electrode; The 9-through hole; 10-cavity portion; The 11-extension; The 15-piezoelectric/electrostrictive body; The 20-connection electrode.
Embodiment
Fig. 1, Fig. 2 and Fig. 3 represent to relate to the transducer piezoelectric/electrostrictive device of the execution mode of piezoelectric/electrostrictive device of the present invention.This piezoelectric/electrostrictive device (diaphragm element) is to utilize common film shape method to stack gradually lower electrode 4, piezoelectric film 5 and upper electrode (part that is equivalent to piezoelectric/electrostrictive film element) and the structure that forms as one on the ceramic substrate 1 that is made of thin-walled diaphragm portion 3 and heavy section 2 (be equivalent to be made of pottery substrate).One end of auxiliary electrode 8 sides of lower electrode 4 is with the length of the position that is no more than thin-walled diaphragm portion 3 and form.With lower electrode 4 with on the one side with its independently on the position in the mode of the downside that enters piezoelectric film 5 and with from forming auxiliary electrode 8 continuously with the heavy section 2 of the opposition side of lower electrode 4 to the specific length of thin-walled diaphragm portion 3.
In addition, be provided with the connection electrode 20 that upper electrode 6 and auxiliary electrode 8 is electrically connected.Thus, upper electrode 6 and auxiliary electrode 8 are electrically connected with independently a plurality of paths each other (in Fig. 1, Fig. 2 and the mode shown in Figure 3 is two paths).Have again,,, preferably be connected position away from auxiliary electrode 8 position of two paths (promptly, further from) as Fig. 1, Fig. 2 and shown in Figure 3 though an end of upper electrode 6 sides of connection electrode 20 can be connected arbitrary position of upper electrode 6.This is because resulting from insulating properties low of piezoelectric film 5, takes place in the situation of destruction of a part of upper electrode 6, and the possibility of keeping the connection at least one path in above-mentioned two paths uprises.
As the material of ceramic substrate 1, preferably has the material of thermal endurance, chemical stability, insulating properties.This is because as described later, the part that will be equivalent to piezoelectric/electrostrictive film element promptly, lower electrode 4, piezoelectric film 5, and upper electrode 6 integrated when, have heat treated situation and situation and this liquid that characteristics of liquids carries out sensing had conductivity and corrosive situation as the piezoelectric/electrostrictive device of transducer.Spendable from this viewpoint pottery can exemplify zirconia, aluminium oxide, magnesium oxide, mullite, aluminium nitride, silicon nitride and the glass etc. after the stabilisation.This wherein the zirconia after the stabilisation in the situation that forms the thin-walled diaphragm portion than unfertile land based on guaranteeing higher mechanical strength, the reason of good-toughness, can preferably use.
The thickness of the thin-walled diaphragm portion 3 of ceramic substrate 1 is typically 50 μ m for the vibration that does not hinder piezoelectric film 5, and expectation is 30 μ m or following, is preferably 15 μ m or following.Have again; though the flat shape of thin-walled diaphragm portion 3 can adopt arbitrary shape of rectangle, square, triangle, ellipse, circle etc.;, can select rectangle and circle as required as the transducer that must make the resonance mode simplification that is energized; the situation of applying piezoelectric/electrostrictive device.
On the surface of this ceramic substrate 1, form lower electrode 4 and auxiliary electrode 8.This lower electrode 4 equates or littler given size and forming from end of ceramic substrate 1 and with the size that should be formed with piezoelectric film 5 on the thin-walled diaphragm portion 3.On the other hand, auxiliary electrode 8 is from forming continuously with the end of the opposition side of the lower electrode of ceramic substrate 1 assigned position to thin-walled diaphragm portion 3.The upper end of the heavy section 2 of lower electrode 4 and auxiliary electrode 8 is as the lead-in wire terminal.
Known various film formation method is used in the formation of lower electrode 4 and auxiliary electrode 8.Concrete, though can use the film method of formationing, the screen printing of ion beam, splash, vacuum evaporation, CVD, ion plating, plating etc., the caudacoria method of formationing of impregnating, therein, the suitable selection of sputtering method and stencil printing.
Between lower electrode 4 and auxiliary electrode 8, be provided with situation about being used in conjunction with the binder course of piezoelectric film 5 and thin-walled diaphragm portion 3, before formation piezoelectric film 5, as shown in Figure 4, on the position of incomplete joint portion 7B, be formed with binder course 7C.As the binder course 7C that constitutes by insulator, as long as both sides' adhesiveness, the associativity of raising and piezoelectric film 5 and ceramic substrate 1 can be arbitrary materials of organic material, inorganic material.Have, the material coefficient of thermal expansion coefficient that uses as binder course 7C has the median of the material coefficient of thermal expansion coefficient and the piezoelectric film 5 employed material coefficient of thermal expansion coefficients of ceramic substrate 1 again, so more preferred owing to obtaining the high associativity of reliability.The situation that is used for sintering piezoelectric film 5 and heat-treats, as the material that constitutes binder course 7C, because the both sides' of glass material and piezoelectric film 5 and ceramic substrate 1 adhesiveness, associativity height, so be fit to use, wherein, glass material with the above softening point of the heat treatment temperature of piezoelectric film 5 can make piezoelectric film 5 and ceramic substrate 1 combination more securely, or because so softening point is higher can suppress because of heat treated distortion, so more suitable use.
Forming these binder courses 7C uses common thick-film methods, especially stamped method, stencil printing or should form suitable use of occasion ink-jet method that part is of a size of tens of μ m～several 100 μ m degree.Have again, must carry out the heat treated situation of binder course 7C, can heat-treat before piezoelectric film 5 formation secondarily, also can after the formation that forms piezoelectric film 5, heat-treat.
Have, lower electrode 4 and auxiliary electrode 8 use platinum or with the situation of platinum as the alloy of main component, better with its associativity, the characteristics fluctuation of minimizing element obtains higher reliability, so (Bi again
0.5Na
0.5) TiO
3Or be the material of main component with it.Therein, especially (1-x) (Bi
0.5Na
0.5) TiO
3-xKNbO
3So (x is molar fraction, 0≤x≤0.06) or be that the material of main component has higher piezoelectric property with it is more suitable use.The phase transition temperature of this material exists with ... material to be formed, and from being strong dielectric body phase near normal temperature to 100～200 ℃, from being anti-strong dielectric body phase near 250～320 ℃ near 100～200 ℃, then is common dielectric body phase more than near 250～320 ℃.
This piezoelectric/electrostrictive material is as piezoelectric film 5, and is same with lower electrode 4 and auxiliary electrode 8, forms method by known various films and forms.Wherein, from the viewpoint of low composition, screen printing is fit to use.
The piezoelectric film 5 of Xing Chenging is heat-treated as required thus, and lower electrode 4, auxiliary electrode 8 and binder course 7C is integrally formed.Need make the more firm situation of zygosity of piezoelectric film 4, lower electrode 5, auxiliary electrode 8 and binder course 7C for the characteristics fluctuation that suppresses piezoelectric/electrostrictive device improves reliability, use (Bi
0.5Na
0.5) TiO
3Or be the material of main component with it, especially use (1-x) (Bi
0.5Na
0.5) TiO
3-xKNbO
3(x is molar fraction, 0≤x≤0.06) or be the material of main component with it is especially preferred to heat-treat from 1000 ℃ to 1300 ℃ temperature from 900 ℃～1400 ℃.Use the situation of PZT based material also identical.At this moment, can stablize when the high temperature, and the evaporation source of expectation and piezoelectric/electrostrictive material is heat-treated when together carrying out environment control in order to make piezoelectric film 5.
Have again, on the piezoelectric film 5 that so forms, stride across auxiliary electrode 8 and form upper electrode 6 continuously from piezoelectric film 5.As the material of this upper electrode 6, use the high conductive material of zygosity with piezoelectric film 5, form by forming method with the same film of lower electrode 4 and auxiliary electrode 8.Have, the needs after upper electrode 6 corresponding films form are heat-treated again, and engage with piezoelectric film 5 and auxiliary electrode 8, thereby constitute integrative-structure.This heat treatment may not be necessary, and is identical with lower electrode 4.
Have, the situation that lower electrode 4, knitting layer, piezoelectric film 5, upper electrode 6 engage by heat treatment can be with each leisure be heat-treated after film forms successively simultaneously with heat-treating also by the formation degree separately again.When heat-treating, rotten for what suppress that diffusion because of good zygosity and composed component causes, certainly select suitable heat treatment temperature.Have again, in Fig. 1, Fig. 2 and mode shown in Figure 3, form through holes 9 in cavity portion 10, but the structure of the part that contacts with fluid in the piezoelectric/electrostrictive device can be do not have a cap simple inner-cavity structure any structure all can, do not do qualification.Have, the length that is no more than thin-walled diaphragm portion 3 is made in the end of auxiliary electrode 8 sides of piezoelectric film 5 again, also can not stride across the structure of heavy section 2 for piezoelectric film 5.
To the processing that polarizes of the additional multiple pulses shape voltage of this piezoelectric/electrostrictive device (particularly, piezoelectric film 5), thereby can improve polarizability at short notice.This situation, the size of pulse-like voltage becomes big mode extra-pulse shape voltage with the carrying out according to additional number of times, then can improve polarizability in shorter time.This polarizes based on the stress that relaxes between the inside of piezoelectric film 5 time and handles and infer.
Have again, carry out again or not after above-mentioned polarization is handled that above-mentioned polarization is handled and (piezoelectric/electrostrictive film element) piezoelectric film 5 of piezoelectric/electrostrictive device is carried out heat treated, at normal temperatures place thereafter, electric constant after the heat treated of piezoelectric film 5 (for example, static capacity (electric capacity), loss coefficient) value convergence after (moment after the convergence is the moment of convergency value finally promptly), handle by the polarization of carrying out piezoelectric film 5, thereby can guarantee the regulation ability of piezoelectric film 5 reliably.This is because after the phase transfer after the heat treated of piezoelectric film 5 finishes, to piezoelectric film 5 processing that polarizes, so can residual useless stress in the inside of piezoelectric film 5, therefore do not have the situation that the piezoelectric/electrostrictive material characteristic is reduced because of this stress.Promptly, after the placement under heating, the normal temperature, if with the processing that polarizes of the timing by the value decision of the electric constant of piezoelectric film 5, then not being that such situation is compared, bigger displacement and displacement generation power can be found, the piezoelectric/electrostrictive device (piezoelectric/electrostrictive film element) of crooked relatively height output can be obtained when using as transducer simultaneously.
Above-mentioned polarization after the placement is handled in the situation of having carried out the polarization processing before heat treated, can add pulsatile once shape voltage and get final product, and can make the stability of characteristicsization of piezoelectric/electrostrictive device with this processing.
Use with (Bi as piezoelectric film 5
0.5Na
0.5) TiO
3Material for main component, as the zirconia after the ceramic substrate 1 use stabilisation, to carrying out repeatedly implementing the thermal regenerations processing with 350 ℃ while changing standing time according to Fig. 1, the Fig. 2 of said method making and the piezoelectric/electrostrictive device of mode shown in Figure 3, and implement polarization after (25 ℃) are placed at normal temperatures in the set time and handle, handle the static capacity of front and back every standing time with LCR measuring appliance measurement polarization, thereby obtain handling the data of the static capacity numerical value of front and back with respect to the polarization of standing time.Fig. 8 ecbatic.Fig. 8 represent as electric constant adopted static capacity situation piezoelectric film 5 is carried out the standing time (transverse axis) after the heat treated and the relation of static capacity (relative value, the longitudinal axis).In Fig. 8, the static capacity before " * " symbolic representation polarization is handled, the static capacity after " zero " symbolic representation polarization is handled is with arrow represent to polarize change direction before and after handling.
As can be known: in standing time is among the 0hr, the static capacity of having carried out the piezoelectric film 5 after polarization is handled is bigger relatively than the static capacity of the piezoelectric film 5 before handling that polarizes, relative therewith, 2hr is the boundary with standing time, after standing time 3hr, it is relatively littler to have carried out the static capacity that the static capacity of the piezoelectric film 5 after polarization is handled handles preceding piezoelectric film 5 than polarizing.As can be known: the value relative time of static capacity and changing, by placing the stipulated time, thereby the internal stress that can infer piezoelectric film 5 by the numerical value convergence diminishes, in this piezoelectric film 5, place the above processing that polarizes afterwards of 3hr, then can reliably be guaranteed the good piezoelectric/electrostrictive device of the regulation ability of piezoelectric film 5.
Have again, because the thermal expansion ratio of the piezoelectric film that forms with above-mentioned material is 13.5 * 10
-6/ ℃, the thermal expansion ratio of ceramic substrate 1 is 9.2 * 10
-6/ ℃, so in piezoelectric film 5 thermal stress takes place because of the thermal expansion difference that increases when the heat.The stress that causes because of this heat discharges by placement, can guarantee the regulation ability easily so can infer.
Fig. 7 represents not to be in being assembled into piezoelectric/electrostrictive device and makes in the piezoelectric/electrostrictive film element monomer, the piezoelectric film carried out the chart of the relation of standing time after the heat treated (transverse axis) and static capacity (relative value, the longitudinal axis).Employed piezoelectric/electrostrictive film element such as Fig. 5 and shown in Figure 6, owing to be monomer, so thickening piezoelectric film, make rectangular-shaped piezoelectric film (being referred to as " piezoelectric/electrostrictive body 15 "), with this piezoelectric/electrostrictive body 15 of positive and negative electrode (upper electrode 6 and lower electrode 7) clamping.Have again, in Fig. 5, omit the thickness of upper electrode 6, do not represent.
Fig. 5 and piezoelectric/electrostrictive film element shown in Figure 6 are made in such a way.At first, piezoelectric with (Bi
0.5Na
0.5) TiO
3(sodium titanate bismuth) is mixed adhesive in the powder of main component, and the working pressure machine is configured as cuboid and burns till after granulation.And, use the cuboid after fret saw will burn till to be cut into given size, obtain piezoelectric/electrostrictive body 15.Secondly, on this piezoelectric/electrostrictive body 15, use electrode material (Au) and use the splash method to form upper electrode 6 and lower electrode 4.
Fig. 5 of making like this and the piezoelectric/electrostrictive film element of mode shown in Figure 6 (monomer) are carried out implementing the thermal regeneration processing while changing standing time with 350 ℃ repeatedly, and implement polarization after (25 ℃) are placed at normal temperatures in the set time and handle, handle the static capacity of front and back every standing time with LCR measuring appliance measurement polarization, thereby obtain handling the data of the static capacity numerical value of front and back with respect to the polarization of standing time.Fig. 7 represents this result.In Fig. 7, the static capacity before " * " symbolic representation polarization is handled, the static capacity after " zero " symbolic representation polarization is handled is with arrow represent to polarize change direction before and after handling.
As can be known: in standing time is among the 0hr, the static capacity of having carried out the piezoelectric/electrostrictive body 15 after polarization is handled is bigger relatively than the static capacity of the piezoelectric/electrostrictive body 15 before handling that polarizes, relative therewith, 0.1hr is the boundary with standing time, after standing time 0.2hr, it is relatively littler to have carried out the static capacity that the static capacity of the piezoelectric/electrostrictive body 15 after polarization is handled handles preceding piezoelectric/electrostrictive body 15 than polarizing.As can be known: the value relative time of static capacity and changing, by placing the stipulated time, thereby the internal stress that can infer piezoelectric/electrostrictive body 15 by the numerical value convergence diminishes, in this piezoelectric/electrostrictive body 15, place the above processing that polarizes afterwards of 0.2hr, then can reliably be guaranteed the good piezoelectric/electrostrictive film element of the regulation ability of piezoelectric/electrostrictive body 15.
Have again, in relating to the manufacture method of piezoelectric/electrostrictive film element of the present invention, be not limited to manufacturing process, cutting-off method, electrode formation method, process for calcining, can in requisition for the change these process sequences.For example, can be fit to use the band forming process of scraping skill in using a kitchen knife in cookery etc. or extruding formation method etc., can be fit to use stencil printing or make method etc. firm by ramming, can be fit to use jackknife and food slicer etc. as cutting-off method as electrode formation method as manufacturing process.Have again, for example can also before burning till, cut off operation and electrode forming process.
Utilizability on the industry
The manufacture method that relates to piezoelectric of the present invention can be used as manufacturing as the driver that utilizes bending displacement or be used to measure the scheme of piezoelectric/electrostrictive device of the transducer etc. of acoustic pressure or fluid viscosity.
Claims (7)
1. the manufacture method of a piezoelectric/electrostrictive film element is made the piezoelectric/electrostrictive film element that lower electrode, piezoelectric film and upper electrode are stacked gradually, it is characterized in that,
Have above-mentioned piezoelectric film is carried out heat treated, place thereafter, and after the value of the electric constant after the above-mentioned heat treated of the above-mentioned piezoelectric film convergence, the operation that above-mentioned piezoelectric film is polarized and handles.
2. the manufacture method of piezoelectric/electrostrictive film element according to claim 1 is characterized in that, above-mentioned laying temperature is the phase point temperature of above-mentioned piezoelectric film or following.
3. the manufacture method of piezoelectric/electrostrictive film element according to claim 1 and 2 is characterized in that, above-mentioned piezoelectric film is added pulsatile once shape voltage at least and carries out above-mentioned polarization processing.
4. according to the manufacture method of each described piezoelectric/electrostrictive film element of claim 1～3, it is characterized in that above-mentioned electric constant is electrostatic capacitance or loss coefficient.
5. manufacture method of making piezoelectric/electrostrictive device, this piezoelectric/electrostrictive device has heavy section and has to possess on the substrate that is made of pottery of thin-walled diaphragm portion to major general's lower electrode, piezoelectric film and upper electrode at periphery and stacks gradually and the piezoelectric/electrostrictive film element that constitutes, it is characterized in that
Have following operation, promptly, after obtaining the substrate that constitutes by above-mentioned pottery, on the substrate that constitutes by this pottery, utilize manufacture method to form piezoelectric/electrostrictive film element according to each described piezoelectric/electrostrictive film element of claim 1～4.
6. a piezoelectric/electrostrictive film element stacks gradually lower electrode, piezoelectric film and upper electrode, it is characterized in that, utilizes and makes according to the manufacture method of each described piezoelectric/electrostrictive film element of claim 1～4.
7. a piezoelectric/electrostrictive device is characterized in that, has heavy section and have on the substrate that is made of pottery of thin-walled diaphragm portion at periphery to possess piezoelectric/electrostrictive film element according to claim 6.
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| JP2005189326 | 2005-06-29 | ||
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| CN100555697C CN100555697C (en) | 2009-10-28 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102468423A (en) * | 2010-11-11 | 2012-05-23 | 日本碍子株式会社 | Method for manufacturing piezoelectric element |
| CN106004047A (en) * | 2015-03-27 | 2016-10-12 | 精工爱普生株式会社 | Liquid discharge apparatus and control method thereof |
| CN113043582A (en) * | 2019-12-26 | 2021-06-29 | 中国科学技术大学 | Method for improving piezoelectric response of polymer material |
-
2006
- 2006-06-29 CN CN 200680023734 patent/CN100555697C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102468423A (en) * | 2010-11-11 | 2012-05-23 | 日本碍子株式会社 | Method for manufacturing piezoelectric element |
| CN102468423B (en) * | 2010-11-11 | 2015-09-30 | 日本碍子株式会社 | The manufacture method of piezoelectric element |
| US9246081B2 (en) | 2010-11-11 | 2016-01-26 | Ngk Insulators, Ltd. | Method for manufacturing piezoelectric element |
| CN106004047A (en) * | 2015-03-27 | 2016-10-12 | 精工爱普生株式会社 | Liquid discharge apparatus and control method thereof |
| CN106004047B (en) * | 2015-03-27 | 2018-04-13 | 精工爱普生株式会社 | Liquid ejection apparatus and its control method |
| CN113043582A (en) * | 2019-12-26 | 2021-06-29 | 中国科学技术大学 | Method for improving piezoelectric response of polymer material |
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| CN100555697C (en) | 2009-10-28 |
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