CN103219153B - A kind of high pressure resistant high density capacitors and preparation method thereof - Google Patents
A kind of high pressure resistant high density capacitors and preparation method thereof Download PDFInfo
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- 239000003990 capacitor Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000010408 film Substances 0.000 claims abstract description 45
- 239000010409 thin film Substances 0.000 claims abstract description 36
- 238000004544 sputter deposition Methods 0.000 claims abstract description 20
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 16
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 6
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 230000008021 deposition Effects 0.000 claims abstract description 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 6
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 6
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910010293 ceramic material Inorganic materials 0.000 claims description 6
- 238000004033 diameter control Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 241000877463 Lanio Species 0.000 claims 1
- 238000004146 energy storage Methods 0.000 description 15
- 239000007789 gas Substances 0.000 description 7
- 230000005684 electric field Effects 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000003989 dielectric material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910002340 LaNiO3 Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052454 barium strontium titanate Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002241 glass-ceramic Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- PACGUUNWTMTWCF-UHFFFAOYSA-N [Sr].[La] Chemical compound [Sr].[La] PACGUUNWTMTWCF-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
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- 239000000945 filler Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The present invention relates to a kind of high pressure resistant high density capacitors and preparation method thereof, including matrix, hearth electrode, dielectric layer, top electrode, with Si or SiO2/ Si is as matrix, and hearth electrode is metallic film, conductive oxide film or two kinds of combinations;Dielectric layer is by BaTiO3Ferroelectric thin film forms, and top electrode is metallic film point electrode.Using metallic target or/and conductive oxide target, single target at substrate deposit metallic film or conductive oxide film or first deposition metallic film redeposition conductive oxide film, uses pottery BaTiO in the way of radio frequency or magnetically controlled DC sputtering3Target, deposits BaTiO in the way of rf magnetron sputtering on hearth electrode3Layer, uses metallic target, deposits top electrode in rf magnetron sputtering mode.The thin film capacitor volume that the present invention prepares is little, high pressure resistant, its disruptive field intensity EbHigher than 1000kV/cm;Its actual discharge energy density is not less than 10J/cm3;Being lost low, when frequency and variations in temperature, dielectric properties keep stable.
Description
Technical field
The present invention relates to ferroelectric ceramic thin film capacitor and preparation method thereof.
Background technology
Compared with common batteries and electrochemical capacitor, conventional capacitor is light owing to having, efficiently, environmental friendliness, the characteristics such as specific power is high, but its specific energy is low.In recent years, due to development and the requirement of new opplication of new technique, high energy storage, miniaturization, lightweight, low cost, the high density capacitors of high reliability obtain studying the most widely.
More capacitor is applied at present mainly to have following three classes: 1) electrolysis condenser (Al, Ta).The capacitance of this capacitor is big, but under high-temperature high-frequency, electric capacity reduces, and leakage conductance electric current increases.2) polymer thin film capacitor.This capacitor breakdown field intensity is big, but dielectric constant is relatively low, and operating temperature < 150 DEG C, the most easily lost efficacy.3) ceramic capacitor.This capacitor has high dielectric constant but disruptive field intensity is little.First two material cannot meet the friendly sustainable development of environment, and ceramic material (lead-free ceramics) is good due to its environment friendly, it will is increasingly widely applied.The general character of these three capacitor is that energy storage density is low.Energy storage density and the first power of dielectric constant, the quadratic power of electric field intensity is directly proportional, and is inversely proportional to the volume of capacitor.So can be by improving dielectric constant and the breakdown field strength of dielectric layer, the volume reducing capacitor increases the energy storage density of capacitor.
For the problem of raising capacitor energy storage density, a lot of scholar is had to conduct in-depth research both at home and abroad.J.K.Yuan is respectively with PVDF and PANI as matrix with filler, the mixture dielectric material prepared, and dielectric constant reaches 385 at 1kHz, and breakdown electric field and energy storage density are respectively 10MV.m-1,6.1J.cm-3.B.J.Chu optimizes PVDF polymer, and the dielectric material obtained is at 575MV.m-1Time, energy storage density reaches 17J.cm-3.This kind of technology mainly improves its energy storage density by the dielectric constant of raising polymer;Barium strontium titanate (BST) glass ceramics prepared by E.P.Gorzkowski, dielectric constant and disruptive field intensity respectively reach 1000 and 800KV/cm, and energy storage density is 0.3 0.9J/cm3.The 15.4Na such as J.Luo2O-15.4PbO-23.1Nb2O5-46.2SiO2The glass ceramics of 850 DEG C of crystallizations makees dielectric layer, and energy storage density reaches 8J/cm3.Dong etc. are at Ba0.3Sr0.7TiO3Middle interpolation ZnO, has obtained the highdensity dielectric material of fine grained, and energy storage density reaches 3.9J/cm3.This kind of technology mainly improves its energy storage density by the breakdown electric field of raising ceramic material.Although these researchs improve the memory density of dielectric material, but there is following deficiency: 1) preparation method complexity 2) sintering temperature of pottery is high by 3) the capacitor volume relative thin membrane capacitance big 4 prepared) poor compatibility 5 integrated with quasiconductor) energy storage density is low.
Summary of the invention
The invention aims to solve capacitor energy storage density low, capacitor volume is big, environmental friendliness requirement and the problem with quasiconductor integrated technique poor compatibility, and provides a kind of high pressure resistant high density capacitors and preparation method thereof.
It is an object of the invention to be achieved through the following technical solutions:
A kind of high pressure resistant high density capacitors, including matrix, hearth electrode, dielectric layer, top electrode, with Si or SiO2/ Si is as matrix, and hearth electrode is metallic film, conductive oxide film or two kinds of combinations, and thickness is 100~1000nm;Dielectric layer is by BaTiO3Ferroelectric thin film forms, and thickness is 200nm~5 μm;Top electrode is the metallic film point electrode of diameter 20~500 μm.
Metallic film can be Ti, Pt etc.;Conductive oxide film can be strontium titanates, nickel acid lanthanum, cobalt acid lanthanum-strontium etc.;Metallic film point electrode is golden or silver-colored.
Hearth electrode is preferably metallic film and combines with conductive oxide film, and metallic film is Ti, Pt thin film, and conductive oxide film uses perovskite ABO3The conducting ceramic material of structure, such as LaNiO3。
The preparation method of above-mentioned high pressure resistant high density capacitors, comprises the following steps that
(1) matrix processes:
Select Si or SiO2/ Si, as the matrix of thin film capacitor, carries out ultrasonic cleaning with acetone and ethanol to it, dries up, be heated to 200~500 DEG C;
(2) at substrate deposit hearth electrode
Use metallic target or/and conductive oxide target, single target in the way of radio frequency or magnetically controlled DC sputtering at substrate deposit metallic film or conductive oxide film or first deposition metallic film redeposition conductive oxide film;During deposition metallic film, atmosphere is pure Ar gas, and gas flow optimized is 20~100sccm, and air pressure controls 0.3~3Pa, and target power density is 2-5W/cm2;During conductive oxide thin film, atmosphere is Ar and O2Mixed gas, Ar throughput controls at 20-100sccm, O2Flow-control is 10~40sccm, and air pressure controls 0.3~3Pa, and target power density is 2.5-10W/cm2, hearth electrode total film thickness is 100-1000nm.(3) dielectric layer on hearth electrode
Use pottery BaTiO3Target, deposits BaTiO in the way of rf magnetron sputtering on hearth electrode3Layer, sputtering atmosphere is Ar and O2Mixed gas, Ar throughput controls at 20-100sccm, O2Flow-control 10~40sccm, BaTiO3The power density of target is 2.5-10W/cm2, thickness is 200nm-5 μm.
(4) top electrode is deposited on the dielectric layer
Using metallic target, deposit in rf magnetron sputtering mode, sputtering atmosphere is air, and target power density is 2-5W/cm2, the diameter control of upper electrode is in 20-500 μm.
Rf magnetron sputtering is prepared thin film and is had the advantage that 1) sputtering yield is high by 2) the thin film consistency prepared is high by 3) good with integrated technique compatibility.Magnetron sputtering is sent out and is prepared the principle of thin film as shown in Figure 3: magnetron sputtering electronics, under the effect of electric field, collides with ar atmo so that it is ionize out Ar during flying to substrate+。Ar+Accelerating to fly to cathode target under electric field action, and bombard target surface with high-energy, make target sputter, in sputtering particle, neutral target atom or molecule are then deposited on substrate formation thin film.Multiple thin-film material can be prepared, such as metal material, ceramic material etc. by rf magnetron sputtering.There is several factors (such as gas flow, target power etc.) that the quality of magnetron sputtering gained thin film can be affected, so each technological parameter should be controlled in plated film practice process well to improve uniformity and the stability of performance of thin film.
The dielectric layer of thin film capacitor of the present invention is made up of the Ca-Ti ore type Lead-free ferroelectric ceramics barium titanate film prepared by the sputtering of middle low temperature magnetic control list target.Thin film capacitor prepared by the present invention is the most integrated with quasiconductor Si, and obtained capacitor has the dielectric constant higher than macromolecular material, the resistance to pressure higher than ceramic material and high energy storage density.At civilian and military aspect, such as the grid-connected power generation system such as solar energy, wind energy, directed energy weapon, electrified flat pad etc.;And in terms of the miniaturization of device, have the biggest application prospect.
The invention have the benefit that
(1) core-dielectric layer of this capacitor arrangement, its material have employed the Lead-free ferroelectric ceramics material-BaTiO of environmental protection3Thin film.
(2) its preparation method-middle low temperature magnetic sputtering, with quasiconductor integrated technique highly compatible, operation is simple, it is possible to achieve prepared by low cost, high efficiency.
(3) the thin film capacitor volume prepared is little, high pressure resistant, its disruptive field intensity EbHigher than 1000kV/cm;Its actual discharge energy density is not less than 10J/cm3;Being lost low, outside 1000kV/cm, loss tangent angle is less than 2% after the match, and within the temperature range of-100-200 DEG C, or in the frequency range of kHz-MHz, dielectric properties keep stable.
(4) tool perovskite ABO3The conductive oxide film of structure can optimize orientation and the electric property of thin film as cushion.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the capacitor arrangement that the present invention prepares.
Fig. 2 is preparation method principle schematic used by the present invention.
Fig. 3 is the structural representation of preparation method used by the present invention.
Fig. 4 is the capacitor shape appearance figure that the embodiment of the present invention 2 prepares.
Wherein 1-Si matrix, 2-hearth electrode, 3-BaTiO3Dielectric layer thin film, 4-Au top electrode, 5-chip bench, 6-stove silk, 7-
Substrate frame, 8-plasma, 9-target, 10-baffle plate, 11-air inlet.
Detailed description of the invention
Further illustrate below in conjunction with embodiment.
The major experimental equipment of the present invention is magnetic control sputtering device.The magnetron sputtering structural representation of this equipment is as it is shown on figure 3, mainly include stove silk, target, substrate frame.
The magnetron sputtering chamber mechanical pump of this equipment is bled and is realized coarse vacuum, then by molecular pump pumping high vacuum to less than 10-4pa。
Being passed through the Ar gas of 20-100sccm in chamber, regulation equipment plate valve makes chamber pressure be maintained at 0.3-3pa.
Embodiment 1
By heater strip, matrix being heated to 200-500 DEG C, adjusts revoluting motor and make substrate be in the position being right against Ti target, open the radio-frequency power supply of Ti target, adjusting Ti target power density is 2-5W/cm2, prepare Ti metal film that thickness is 20-100nm as the transition zone between electrode Pt and Si matrix.
Adjusting revoluting motor makes substrate be in the position being right against Pt target, opens the radio-frequency power supply of Pt target, and adjusting Pt target power density is 2-5W/cm2, prepare the Pt metal film that thickness is 80-500nm.
Being passed through, to chamber, the oxygen that flow is 10-40sccm again, regulation equipment plate valve makes chamber pressure be maintained at 0.3-3pa.Adjustment revoluting motor makes substrate be in and is right against BaTiO3The position of target, opens BaTiO3The radio-frequency power supply of target, adjusts BaTiO3The power density of target is 2.5-10W/cm2, prepare the BaTiO that thickness is 200nm-5 μm3Thin film is as the dielectric layer of this thin film capacitor.
With using native gold target, deposit top electrode in rf magnetron sputtering mode.Sputtering atmosphere is air, and the diameter control of top electrode is in 20-500 μm.
Embodiment 2
All thin film are all preparing (≤500 ° of C) under middle cryogenic conditions.
Use single target to carry out the coaxial sputtering of radio frequency magnetron successively, comprise the following steps:
() matrix processes:
Select Si or SiO2/ Si, as the matrix of thin film capacitor, carries out ultrasonic cleaning with acetone and ethanol to it, dries up.It is heated to 200~500 ° of C.
() is at substrate deposit metallic film:
Use metal Ti target and Pt target, complete in the way of rf magnetron sputtering.Sputtering atmosphere is pure Ar, and gas flow controls 20~100sccm, and air pressure is 0.3~3Pa, and target power density is 2-5W/cm2, total film thickness controls at 100-600nm.
() conductive oxide thin film:
Use perovskite LaNiO3Target, completes in the way of rf magnetron sputtering.Sputtering atmosphere is Ar and O2, Ar throughput controls at 20-100sccm, O2Flow-control is 10~40sccm, and target power density is 2.5-10W/cm2。LaNiO3Buffer layer thickness controls at 100-400nm.
() dielectric layer:
Use pottery BaTiO3Target, completes in the way of rf magnetron sputtering.Sputtering atmosphere is Ar and O2, Ar throughput controls at 20-100sccm, O2Flow-control 10~40sccm, BaTiO3The power density of target is 2.5-10W/cm2, BaTiO3Medium thickness controls in 200nm-5 μm.
() deposits top electrode on the dielectric layer.
Use native gold target or other metallic targets, complete in the way of photoetching or mask plate sputtering.Preparing electrode step by photolithographicallpatterned is: at film surface gluing, with mask plate, it is carried out photoetching, sample is put into chamber and carries out magnetron sputtering, then remove the glue of remnants.The step preparing electrode with mask plate sputtering is: covering above thin film by the mask plate with electrode shape and size, sputter directly sputters, and sputtering atmosphere is air.The diameter control of top electrode is in 20-500 μm.
Performance test
Under zero-bias, thin film capacitor being carried out dielectric and magnetic test, its loss tangent angle is less than 1%;
Thin film capacitor carries out dielectric temperature spectrum and spectrum measurement, and within the temperature range of-100-200 DEG C, or in the frequency range of kHz-MHz, dielectric properties keep stable.
Thin film capacitor is carried out C-V test, and outside 1000kV/cm, loss tangent angle is less than 2% after the match.
Under more than 10V voltage, thin film capacitor being carried out discharge and recharge by pulse charge and discharge system, its actual discharge energy density is not less than 10J/cm3, disruptive field intensity EbIt is not less than 1000kV/cm.
Claims (3)
1. a high pressure resistant high density capacitors, is characterized in that, including matrix, hearth electrode, dielectric layer, top electrode, with Si or SiO2/ Si is as matrix, and hearth electrode is that metallic film combines with conductive oxide film, first deposition metallic film redeposition conductive oxide film, and metallic film is Ti thin film or Pt thin film, and conductive oxide film uses perovskite ABO3The conducting ceramic material LaNiO of structure3, the thickness of hearth electrode is 100 ~ 1000nm;Dielectric layer is by BaTiO3Ferroelectric thin film forms, and thickness is 200nm ~ 5 μm;Top electrode is the metallic film point electrode of diameter 20 ~ 500 μm.
The high pressure resistant high density capacitors of one the most according to claim 1, is characterized in that, metallic film point electrode is golden or silver-colored.
3. a preparation method for high pressure resistant high density capacitors, is characterized in that, comprises the following steps that
(1) matrix processes:
Select Si or SiO2/ Si, as the matrix of thin film capacitor, carries out ultrasonic cleaning with acetone and ethanol to it, dries up, be heated to 200 ~ 500 DEG C;
(2) at substrate deposit hearth electrode
Use metallic target or/and conductive oxide target, single target in the way of radio frequency or magnetically controlled DC sputtering at substrate deposit metallic film or conductive oxide film or first deposition metallic film redeposition conductive oxide film;During deposition metallic film, atmosphere is pure Ar gas, and gas flow optimized is at 20 ~ 100sccm, and air pressure controls at 0.3 ~ 3Pa, and target power density is 2-5W/cm2;During conductive oxide thin film, atmosphere is Ar and O2Mixed gas, Ar throughput controls at 20-100sccm, O2Flow-control is at 10 ~ 40sccm, and air pressure controls at 0.3 ~ 3Pa, and target power density is 2.5-10W/cm2, hearth electrode total film thickness is 100-1000nm;
(3) dielectric layer on hearth electrode
Use pottery BaTiO3Target, deposits BaTiO in the way of rf magnetron sputtering on hearth electrode3Layer, sputtering atmosphere is Ar and O2Mixed gas, Ar throughput controls at 20-100sccm, O2Flow-control is at 10 ~ 40sccm, BaTiO3The power density of target is 2.5-10W/cm2, thickness is 200nm-5 μm;
(4) top electrode is deposited on the dielectric layer
Using metallic target, deposit in rf magnetron sputtering mode, sputtering atmosphere is air, and target power density is 2-5W/cm2, the diameter control of top electrode is in 20-500 μm.
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Effective date of registration: 20231113 Address after: 250061 Qianfo campus, Shandong University, 17923 Jingshi Road, Lixia District, Jinan City, Shandong Province Patentee after: OuYang Jun Patentee after: Qilu University of Technology (Shandong Academy of Sciences) Address before: 250061 Qianfo campus, Shandong University, 17923 Jingshi Road, Lixia District, Jinan City, Shandong Province Patentee before: OuYang Jun |