WO2015194458A1 - 多層膜の製造方法および多層膜 - Google Patents
多層膜の製造方法および多層膜 Download PDFInfo
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- WO2015194458A1 WO2015194458A1 PCT/JP2015/066926 JP2015066926W WO2015194458A1 WO 2015194458 A1 WO2015194458 A1 WO 2015194458A1 JP 2015066926 W JP2015066926 W JP 2015066926W WO 2015194458 A1 WO2015194458 A1 WO 2015194458A1
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- Prior art keywords
- film
- substrate
- dielectric layer
- multilayer film
- layer
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 81
- 150000001875 compounds Chemical class 0.000 claims abstract description 25
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 13
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 13
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 12
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004544 sputter deposition Methods 0.000 claims description 41
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 24
- 239000010936 titanium Substances 0.000 claims description 19
- 238000002441 X-ray diffraction Methods 0.000 claims description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 25
- -1 strontium (Sr) Chemical class 0.000 abstract 1
- 239000010408 film Substances 0.000 description 130
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 48
- 238000000151 deposition Methods 0.000 description 22
- 230000008021 deposition Effects 0.000 description 22
- 239000007789 gas Substances 0.000 description 17
- 229910004121 SrRuO Inorganic materials 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 9
- 239000013078 crystal Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/541—Heating or cooling of the substrates
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- C01G25/00—Compounds of zirconium
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- C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
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- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
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- C01G55/002—Compounds containing, besides ruthenium, rhodium, palladium, osmium, iridium, or platinum, two or more other elements, with the exception of oxygen or hydrogen
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/568—Transferring the substrates through a series of coating stations
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/07—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base
- H10N30/074—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing
- H10N30/076—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing by vapour phase deposition
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- H—ELECTRICITY
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- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/07—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base
- H10N30/074—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing
- H10N30/079—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing using intermediate layers, e.g. for growth control
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/853—Ceramic compositions
- H10N30/8548—Lead-based oxides
- H10N30/8554—Lead-zirconium titanate [PZT] based
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/74—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by peak-intensities or a ratio thereof only
Definitions
- the present invention relates to a method for manufacturing a multilayer film including a dielectric layer having high crystallinity and a multilayer film.
- the crystal of the PZT film includes a pyrochlore phase having no piezoelectricity, which is a metastable phase, in addition to the target perovskite phase having piezoelectricity.
- crystals containing a pyrochlore phase were easily obtained, and it was extremely difficult to obtain a dielectric film having high crystallinity without containing a pyrochlore phase. Therefore, in order to improve the withstand voltage characteristics, development of a manufacturing method capable of stably forming a multilayer film including a dielectric film having a high crystallinity without including a pyrochlore phase has been expected.
- the present invention has been devised in view of such a conventional situation, and the first is to provide a method for producing a multilayer film including a dielectric layer having a high crystallinity and not including a pyrochlore phase. Objective. It is a second object of the present invention to provide a multilayer film including a dielectric layer having no crystallinity and containing no pyrochlore phase.
- a method for manufacturing a multilayer film includes forming a conductive layer on a substrate (step A), and adding strontium (Sr), ruthenium (Ru), and oxygen (O) by sputtering.
- a seed layer is formed so as to cover the conductive layer with a compound containing (Step B)
- a dielectric layer is formed so as to cover the seed layer (Step C)
- a substrate temperature when forming the dielectric layer Is defined as Td (dielectric), 560 ⁇ Td ⁇ 720 [° C.] is satisfied.
- the dielectric layer when forming the dielectric layer, includes lead (Pb) and zirconia (Zr).
- a compound containing titanium, titanium (Ti), and oxygen (O) may be formed by a sputtering method.
- the multilayer film has a conductive layer made of platinum (Pt), a seed layer, and a dielectric layer arranged at least in order on one main surface side of the substrate made of silicon.
- the seed layer is made of a compound containing strontium (Sr), ruthenium (Ru), and oxygen (O), and the dielectric layer is made of lead (Pb), zirconia (Zr), and titanium (Ti). And the compound that forms the dielectric layer does not include an X-ray diffraction peak due to the pyrochlore phase.
- the compound forming the dielectric layer is an X-ray diffraction peak due to (100) of Pb (Zr, Ti) O 3.
- the full width at half maximum (FWHM) may be 1 [degree] or less.
- Step B a compound containing strontium (Sr), ruthenium (Ru), and oxygen (O) is formed as the seed layer by a sputtering method.
- step C the substrate temperature Td (dielectric) at the time of forming the dielectric layer is set to a range of 560 [° C.] or more and 720 [° C.] or less, whereby the dielectric formed on the seed layer The film has high crystallinity.
- this invention can provide the manufacturing method of the multilayer film provided with the dielectric material layer which does not contain a pyrochlore phase and has high crystallinity.
- the dielectric layer is made of a compound containing lead (Pb), zirconia (Zr), titanium (Ti), and oxygen (O), and the dielectric
- the layered compound does not contain an X-ray diffraction peak due to the pyrochlore phase. Therefore, according to the present invention, a multilayer film provided with a dielectric layer having high crystallinity can be provided. Such a multilayer film has excellent characteristics having both high piezoelectricity and high pressure resistance.
- FIG. 1 It is sectional drawing which shows one structural example of the multilayer film which concerns on one Embodiment of this invention. It is a figure which shows typically the magnitude
- FIG. 3 is a diagram showing a diffraction peak showing a crystal structure of a PZT film formed with Sample 1.
- FIG. 5 is a diagram showing diffraction peaks indicating crystal structures for the PZT films of Sample 2 to Sample 4. It is a graph which shows the relationship between a substrate temperature and the peak intensity resulting from a pyrochlore phase. It is a figure which shows the crystallinity about the PZT film
- FIG. 1 is a cross-sectional view illustrating a configuration example of a multilayer film according to the present embodiment.
- a seed layer 4 and a dielectric layer 5 are arranged at least in order on one main surface side of a substrate 2 made of silicon.
- the seed layer 4 is made of a compound containing strontium (Sr), ruthenium (Ru), and oxygen (O). Examples of the seed layer 4 include SrRuO 3 (SRO).
- the dielectric layer 5 is disposed on the seed layer 4 containing strontium (Sr), ruthenium (Ru), and oxygen (O) described above.
- the dielectric layer 5 is not particularly limited.
- the compound forming the dielectric layer has high crystallinity. Specifically, the compound constituting the dielectric layer does not contain a pyrochlore phase because no peak due to the pyrochlore phase is observed in the X-ray diffraction method.
- the dielectric layer 5 disposed on the seed layer 4 has a perovskite structure that does not include a different phase.
- this multilayer film 1 has excellent characteristics such as high piezoelectricity and pressure resistance.
- Such a multilayer film 1 is suitably used for a piezoelectric element, for example.
- the compound forming the dielectric layer 5 has a full width at half maximum (FWHM) of the X-ray diffraction peak due to (100) of Pb (Zr x Ti 1-x ) O 3. 1 [degree] or less.
- FWHM full width at half maximum
- FIGS. 2A and 2B are diagrams schematically showing the size of the crystallite and the shape of the X-ray diffraction peak.
- FIG. 2A when the crystallite is well grown, a half-width is narrow and a sharp peak is observed.
- FIG. 2B when the crystallite is small, a half-value width is widened and a dull peak is observed.
- the compound forming the dielectric layer 5 constituting the multilayer film according to the present embodiment in which the half-value width of 1 [degree] or less is observed, the “crystallite grows greatly, It has a very high crystallinity ”.
- a dielectric film formed on the seed layer 4 containing strontium (Sr), ruthenium (Ru), and oxygen (O) by adopting the multilayer film manufacturing method according to the present embodiment as will be described later is obtained as follows. It does not contain a pyrochlore phase and has high crystallinity.
- the multilayer film 1 has excellent characteristics such as high piezoelectricity and pressure resistance. Such a multilayer film 1 is suitably used for a piezoelectric element, for example.
- FIG. 3A to 3C are schematic cross-sectional views illustrating the manufacturing process of the multilayer film according to the present embodiment.
- the multilayer film manufacturing method according to the present embodiment includes a step A [FIG. 3A] of forming the conductive layer 3 on the substrate 2, and a step B [FIG. 3B] of forming the seed layer 4 so as to cover the conductive layer 3. , Forming a dielectric layer 5 so as to cover the seed layer 4 (FIG. 3C).
- the method of manufacturing the multilayer film 1 includes at least a strontium (as a seed layer) in the step B.
- a compound containing strontium (Sr), ruthenium (Ru), and oxygen (O) is formed as the seed layer by sputtering
- step C 560 ⁇ Td ⁇ 720 [° C.], where Td (dielectric) is the substrate temperature when forming the dielectric layer.
- Td (dielectric) is the substrate temperature when forming the dielectric layer.
- the dielectric film formed on the seed layer does not contain a pyrochlore phase and has high crystallinity.
- Such a multilayer film has excellent characteristics such as high piezoelectricity and pressure resistance.
- a case where lead zirconate titanate [Pb (Zr x Ti 1-x ) O 3 : PZT] is used as the dielectric layer 5 will be described as an example. It is not limited.
- FIG. 4 is a schematic cross-sectional view showing an example of the internal configuration of the film forming apparatus 10.
- the film forming apparatus 10 includes a vacuum chamber 11, a target 21, a support unit (substrate holding table) 32, a temperature control unit 18, a sputtering power supply 13, a sputtering gas introduction unit 14, and a first deposition plate 34. And a second deposition preventing plate 35.
- the target 21 is disposed in the vacuum chamber 11.
- the support part 32 is disposed at a position facing the target 21 and holds the substrate 31 (substrate 2).
- the temperature control unit 18 adjusts the substrate temperature by heating / cooling the substrate 31 held by the support unit 32.
- the sputtering power source 13 applies a voltage to the target 21.
- the sputtering gas introduction unit 14 introduces a sputtering gas into the vacuum chamber 11.
- the first deposition plate 34 and the second deposition plate 35 are arranged in the vacuum chamber 11 at positions where particles emitted from the target 21 are attached.
- a cathode electrode 22 is disposed on the upper wall surface of the vacuum chamber 11 via an insulating member 28, and the cathode electrode 22 and the vacuum chamber 11 are electrically insulated.
- the vacuum chamber 11 is at ground potential.
- One surface side of the cathode electrode 22 is locally exposed in the vacuum chamber 11.
- the target 21 is fixed in close contact with the central portion of the exposed region on one side of the cathode electrode 22, and the target 21 and the cathode electrode 22 are electrically connected.
- the sputtering power source 13 is disposed outside the vacuum chamber 11.
- the sputtering power source 13 is electrically connected to the cathode electrode 22 and can apply an AC voltage to the target 21 via the cathode electrode 22.
- a magnet device 29 is disposed on the opposite side of the cathode electrode 22 from the target 21, that is, on the other surface side of the cathode electrode 22.
- the magnet device 29 is configured to form magnetic lines of force on the surface of the target 21.
- the support portion 32 on which the substrate 31 is placed is made of, for example, silicon carbide (SiC).
- SiC silicon carbide
- the outer periphery of the support portion 32 is formed larger than the outer periphery of the substrate 31.
- the surface of the support portion 32 is arranged to face the surface of the target 21.
- a means for electrostatically attracting the substrate 31 is contained in the support portion 32.
- the back surface of the substrate 31 is brought into close contact with the center portion of the surface of the support portion 32, and the substrate 31 is thermally connected to the support portion 32.
- the first deposition preventing plate 34 is a ceramic such as quartz or alumina.
- the first deposition preventing plate 34 is formed in an annular shape in which the inner periphery of the first deposition preventing plate 34 is larger than the outer periphery of the substrate 31, and covers the outer edge portion that is the outside of the center portion of the surface of the support portion 32. Has been placed. Thereby, the particles emitted from the target 21 are prevented from adhering to the outer edge portion of the surface of the support portion 32.
- the back surface of the first deposition preventing plate 34 is in close contact with the outer edge portion of the surface of the support portion 32, and the first deposition preventing plate 34 is thermally connected to the support portion 32.
- the first deposition preventing plate 34 is disposed so as to surround the outer periphery of the substrate 31.
- the second adhesion-preventing plate 35 is a ceramic such as quartz or alumina.
- the second deposition preventing plate 35 is formed in a cylindrical shape in which the inner circumference of the second deposition preventing plate 35 is larger than the outer circumference of the target 21 and the outer circumference of the substrate 31.
- the second deposition preventing plate 35 is disposed between the support portion 32 and the cathode electrode 22 and is configured to surround the side of the space between the substrate 31 and the target 21. Thereby, the particles emitted from the target 21 are prevented from adhering to the wall surface of the vacuum chamber 11.
- the temperature control unit 18 includes a heat generating member 33 and a heating power source 17.
- SiC is used as the heat generating member 33.
- the heat generating member 33 is disposed at a position opposite to the substrate 31 with the support portion 32 interposed therebetween.
- the heating power source 17 is electrically connected to the heat generating member 33.
- the back surface of the substrate 31 is in close contact with the central portion of the surface of the support portion 32, and heat is evenly transferred from the central portion of the substrate 31 to the outer edge portion.
- a cooling unit 38 is disposed on the side of the heat generating member 33 opposite to the support unit 32.
- the cooling unit 38 is configured to circulate a temperature-controlled cooling medium therein, and prevents heating of the wall surface of the vacuum chamber 11 even when the heat generating member 33 generates heat.
- the sputter gas introducing unit 14 is connected to the inside of the vacuum chamber 11 and is configured so that the sputter gas can be introduced into the vacuum chamber 11.
- FIG. 4 illustrates the case where the film forming apparatus 10 has one vacuum chamber 11 for the sake of simplicity.
- the manufacturing method of the following steps A to C at least three vacuum chambers 11a, 11b, The description will be made on the assumption that the film forming apparatus 11c (11) communicates in the depth direction of the drawing via a partition valve (not shown) in FIG.
- the vacuum chamber 11a (11) is a vacuum chamber for forming a conductive layer.
- the vacuum chamber 11b (11) is a vacuum chamber for forming a seed layer.
- the vacuum chamber 11c (11) is a vacuum chamber for forming a dielectric layer.
- only the vacuum chambers are distinguished from each other, and the components associated with each vacuum chamber are not distinguished from each other.
- Step A Formation of Conductive Layer
- the conductive layer 3 made of platinum (Pt) is formed on one main surface side of the substrate 2 made of silicon (Si).
- Si silicon
- a conductive layer is formed directly on one main surface of the substrate.
- another film is provided on one main surface of the substrate 2 before forming the conductive layer. It does not matter.
- the internal space of the vacuum chamber 11a (11) in which the target made of Pt is installed is depressurized by the vacuum exhaust device 15.
- the internal space of the vacuum chamber 11a (11) is evacuated to a higher vacuum than the pressure atmosphere during film formation. Thereafter, evacuation is continued and the vacuum atmosphere in the vacuum chamber 11 is maintained.
- the substrate 31 to be deposited is carried into the internal space of the vacuum chamber 11 a (11) through an unillustrated entrance. Then, the substrate 31 is held at the center of the support portion 32 so that one main surface of the substrate 31 faces the sputtering surface of the target 21.
- a cooling medium whose temperature is controlled is circulated in the cooling unit 38.
- Ar gas is introduced as a sputtering gas from the sputtering gas introduction unit 14 into the vacuum chamber 11 while the substrate 31 is kept at the deposition temperature, and an AC voltage is applied from the sputtering power source 13 to the cathode electrode 22. Is applied to sputter the Pt target. Thereby, the Pt conductive layer 3 is formed on one main surface side of the substrate 31.
- Step B Formation of Seed Layer
- a seed layer 4 is formed so as to cover the conductive layer 3.
- an oxide made of a compound containing strontium (Sr), ruthenium (Ru), and oxygen (O) is formed by a sputtering method.
- the internal space of the vacuum chamber 11b (11) in which the SRO target made of an oxide containing Sr, Ru, and O is installed as the target 21 is depressurized in advance by the vacuum evacuation device 15, so that the pressure atmosphere during film formation Also, the vacuum atmosphere is evacuated to high vacuum.
- the substrate 31 provided with the Pt conductive layer 3 in advance is carried from the vacuum chamber 11a (11) to the internal space of the vacuum chamber 11b (11). Then, the substrate 31 is held at the center of the surface of the support portion 32 so that one main surface side of the substrate 31, that is, the Pt conductive layer 3 faces the sputtering surface of the SRO target 21.
- Ar gas and oxygen gas are introduced into the vacuum chamber 11 b (11) from the sputtering gas introduction unit 14 as sputtering gas, and AC voltage is applied from the sputtering power supply 13 to the cathode electrode 22. Is applied to sputter the SRO target.
- the seed layer 4 made of SRO is formed on the Pt conductive layer 3 on the one main surface side of the substrate 31.
- the substrate temperature within the film formation time is controlled by a predetermined temperature profile as necessary. It may be set so that a constant temperature is maintained from the start of film formation to the end of film formation. For example, the start of film formation may be set to be higher than the end of film formation.
- Step C Formation of Dielectric Layer
- a dielectric layer 5 is formed so as to cover the seed layer 4.
- a PZT film is formed as the dielectric layer 5 by sputtering.
- the substrate temperature Td when forming the dielectric layer 5 is set to 560 ⁇ Td ⁇ 720 [° C.].
- the internal space of the vacuum chamber 11c (11) in which the PZT target is installed is depressurized by the vacuum exhaust device 15 so that the vacuum atmosphere is evacuated to a higher vacuum than the pressure atmosphere during film formation.
- the substrate 31 provided with the Pt conductive layer 3 and the seed layer 4 in advance is carried from the vacuum chamber 11b (11) into the internal space of the vacuum chamber 11c (11). To do. Then, the substrate 31 is held at the center of the surface of the support portion 32 so that one main surface side of the substrate 31, that is, the seed layer 4 faces the sputtering surface of the PZT target 21.
- the dielectric layer 5 made of a PZT film having a perovskite structure is formed on the seed layer 4 on the one main surface side of the substrate 31.
- the substrate temperature Td when forming the dielectric layer 5 is set to a range of 560 ⁇ Td ⁇ 720 [° C.]. If the substrate temperature Td is lower than 560 [° C.], crystallite growth does not proceed sufficiently. When the substrate temperature Td is higher than 720 [° C.], it is difficult to suppress the generation of the pyrochlore phase. Therefore, by setting the substrate temperature Td in the range of 560 ⁇ Td ⁇ 720 [° C.], formation of the pyrochlore phase can be suppressed and the dielectric layer 5 having high crystallinity can be formed.
- the substrate temperature within the film formation time is controlled by a predetermined temperature profile as necessary. It may be set so that a constant temperature is maintained from the start of film formation to the end of film formation. For example, the start of film formation may be set to be higher than the end of film formation.
- the voltage application from the sputtering power source 13 to the cathode electrode 22 is stopped, and the sputtering gas is introduced into the vacuum chamber 11c (11) from the sputtering gas introduction unit 14. Stop the installation.
- the current supply from the heating power supply 17 to the heat generating member 33 is stopped, the heat generating member 33 is cooled, and the substrate 31 is set to a temperature lower than the film forming temperature.
- the temperature of the heat generating member 33 is lowered to 400 ° C. or lower and the temperature is maintained.
- the film-formed substrate 31 on which a multilayer film formed by sequentially stacking three layers (conductive layer, seed layer, dielectric layer) is formed is placed outside the vacuum chamber 11. Then, it is carried out from a carrying outlet (not shown).
- a transfer robot (not shown) is suitable for the above-described substrate transfer, that is, transfer from outside to the vacuum chamber 11a (11), movement between the vacuum chambers, and transfer from the vacuum chamber 11c (11) to the outside. Used for.
- the multilayer film 1 having the configuration shown in FIG. 1 is manufactured.
- the dielectric layer 5 does not contain a pyrochlore phase and has high crystallinity.
- this multilayer film 1 has both excellent piezoelectricity and pressure resistance, for example, and has excellent characteristics.
- Such a multilayer film 1 is suitably used for a piezoelectric element, for example.
- a multilayer film is formed by sequentially laminating a conductive layer made of a Pt film, a seed layer made of a SrRuO 3 (SRO) film, and a dielectric layer made of a PZT film.
- a silicon (Si) wafer having a diameter of 8 inches was used as the substrate.
- a thermal oxide film (SiO 2 film), a Ti film (thickness 20 nm) functioning as an adhesion layer, and a Pt film (thickness 100 nm) functioning as a lower electrode layer are sequentially formed on one main surface of the Si wafer. A pre-layered one was used.
- a flat-plate magnetron type sputtering apparatus (SME-200) having a configuration as shown in FIG. 4 was used.
- a high frequency power source (frequency: 13.56 MHz) was used as the sputtering power source.
- the deposition conditions for the seed layer made of the SrRuO 3 film were set as follows.
- a SrRuO 3 target having a diameter of 300 mm and a thickness of 5 mm was used as the target.
- the sputtering power was 0.7 [kW]
- the sputtering pressure was 0.4 [Pa]
- the substrate temperature was 530 to 740 [° C.].
- the film thickness of the seed layer was 100 [nm].
- the conditions for forming the dielectric layer made of the PZT film were set as follows.
- a PZT target having a diameter of 300 mm and a thickness of 5 mm was used as the target.
- the sputtering power was 2.5 [kW]
- the sputtering pressure was 0.5 [Pa]
- the substrate temperature was 720 [° C.].
- the film thickness of the dielectric layer was 2.0 [ ⁇ m].
- Sample 1 The sample of Experimental Example 1 manufactured under the above-described conditions is referred to as Sample 1.
- Example 2 In this example, a multilayer film was formed by forming a PZT film on the Pt thin film of the substrate without providing a seed layer.
- the PZT film was formed with a substrate temperature condition of 585 [° C.].
- Other film formation conditions of the dielectric layer made of the PZT film are the same as those in Experimental Example 1.
- the sample of Experimental Example 2 manufactured under the conditions described above is referred to as Sample 2.
- Example 3 a multi-layer film was formed by forming a PZT film at a substrate temperature of 625 [° C.] on the Pt thin film of the Si substrate without forming a seed layer.
- Other deposition conditions for the PZT film are the same as those of the sample 1 described above.
- the sample of Experimental Example 3 manufactured under the conditions described above is referred to as Sample 3.
- Example 4 a multilayer film was formed by forming a PZT film at a substrate temperature of 665 [° C.] on the Pt thin film of the Si substrate without forming a seed layer.
- Other deposition conditions for the PZT film are the same as those of the sample 1 described above.
- the sample of Experimental Example 4 manufactured under the conditions described above is referred to as Sample 4.
- FIG. 5 is an X-ray chart of Sample 1 (seed layer: SrRuO 3 film).
- FIG. 6 is an X-ray chart of samples 2 to 4 (no seed layer).
- PZT films were formed by changing the substrate temperature during film formation in the range of 530 to 740 [° C.], and the crystal structure was analyzed for each PZT film formed at each substrate temperature.
- FIG. 7 is a graph showing the relationship between the substrate temperature and the peak intensity due to the pyrochlore phase. From FIG. 7, in the sample 1 in which the seed layer made of the SrRuO 3 film was formed, when the substrate temperature was set to 740 [° C.], a pyrochlore phase as a different phase was confirmed in the PZT film. At other substrate temperatures (560 to 720 [° C.]), no pyrochlore phase was observed. That is, it was clarified that when a configuration using an SrRuO 3 film as a seed layer is adopted, a PZT film containing no pyrochlore phase can be obtained at 560 ⁇ Td ⁇ 720 [° C.].
- the SrRuO 3 film as a seed layer, there is no Pyrochlore phase that is a heterogeneous phase (extremely suppressed below the background in the X-ray chart), and a PZT film of a perovskite phase (a crystal structure mainly composed of).
- a PZT film of a perovskite phase a crystal structure mainly composed of.
- FIG. 8 is an X-ray chart showing the crystallinity of the PZT films of Sample 1 (solid line) and Sample 3 (dotted line). Although sample 1 is poly PZT, it has been confirmed that the (100) rocking curve has a half-value width of 0.55 degrees and has extremely high crystallinity compared to sample 3 (half-value width 4.05 degrees). It was.
- the full width at half maximum (FWHM) of the (100) rocking curve was measured at 9 points across the entire area of the 8-inch wafer. As a result, it was confirmed that the full width at half maximum (FWHM) at 9 points was in the range of 0.52 to 0.59.
- the compound forming the dielectric layer produced according to the production conditions of Sample 1 has a half-value width (FWHM) of the X-ray diffraction peak due to (100) of Pb (Zr, Ti) O 3 of 1 [degree]. It turned out that it can be set as follows.
- the present invention is widely applicable to a multilayer film manufacturing method and a multilayer film.
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Abstract
Description
本願は、2014年6月20日に日本国に出願された特願2014-127468号に基づき優先権を主張し、その内容をここに援用する。
本発明者らは、PZT膜の耐電圧特性を改善すべく、種々の研究に取り組んでいる。
従来は、パイロクロア相が含まれた結晶が得られ易く、パイロクロア相を含まず、高い結晶性を有する誘電体膜を得ることが極めて困難であった。したがって、耐電圧特性を向上させるために、パイロクロア相を含まず、高い結晶性を有する誘電体膜を備えた多層膜が、安定に形成できる製法の開発が期待されていた。
また、本発明は、パイロクロア相を含まず、高い結晶性を有する誘電体層を備えた多層膜を提供することを第二の目的とする。
本発明の第二の態様によれば、前記第一の態様に係る多層膜の製造方法において、前記誘電体層を形成する際に、前記誘電体層として、鉛(Pb)とジルコニア(Zr)とチタン(Ti)と酸素(O)とを含む化合物を、スパッタ法により形成してもよい。
本発明の第三の態様によれば、多層膜は、シリコンからなる基板の一主面側に、白金(Pt)からなる導電層と、シード層と、誘電体層と、を少なくとも順に配してなり、前記シード層は、ストロンチウム(Sr)とルテニウム(Ru)と酸素(O)とを含む化合物から構成され、前記誘電体層は、鉛(Pb)とジルコニア(Zr)とチタン(Ti)と酸素(O)とを含む化合物から構成され、前記誘電体層をなす化合物は、パイロクロア相に起因するX線回折ピークを含まない。
本発明の第四の態様によれば、前記第三の態様に係る多層膜において、前記誘電体層をなす化合物は、Pb(Zr,Ti)O3 の(100)に起因するX線回折ピークの半値幅(FWHM)が1[度]以下であってもよい。
また、上記各態様に係る多層膜においては、前記誘電体層が、鉛(Pb)とジルコニア(Zr)とチタン(Ti)と酸素(O)とを含む化合物から構成されており、前記誘電体層をなす化合物は、パイロクロア相に起因するX線回折ピークを含まない。したがって、本発明によれば、高い結晶性を有する誘電体層を備えた多層膜を提供することができる。このような多層膜は、高い圧電性と高い耐圧性とを兼ね備えた、優れた特性を有する。
この多層膜1は、シリコンからなる基板2の一主面側に、白金(Pt)からなる導電層3、シード層4、誘電体層5が、少なくとも順に配されている。
前記シード層4は、ストロンチウム(Sr)とルテニウム(Ru)と酸素(O)とを含む化合物から構成されている。シード層4としては、例えば、SrRuO3 (SRO)が挙げられる。
誘電体層5は、特に限定されるものではないが、例えば、チタン酸ジルコン酸鉛[Pb(ZrxTi1-x)O3 :PZT]、PbTiO3 、BaTiO3 、PMM-PZT、PNN-PZT、PMN-PZT、PNN-PT、PLZT、PZTN、NBT、KNN等の強誘電体からなる。
この評価法に照らし合わせると、上述した1[度]以下の半値幅が観測された、本実施形態に係る多層膜を構成する誘電体層5をなす化合物は、「結晶子が大きく成長し、極めて高い結晶性を有している」ことが分かる。
この多層膜1は、例えば高い圧電性と耐圧性のように、優れた特性を有する。このような多層膜1は、例えば圧電素子等に好適に用いられる。
図3Aから図3Cは、本実施形態に係る多層膜の製造工程を示す模式的な断面図である。
本実施形態に係る多層膜の製造方法は、基板2に導電層3を形成する工程A[図3A]と、前記導電層3を覆うようにシード層4を形成する工程B[図3B]と、前記シード層4を覆うように誘電体層5を形成する工程C[図3C]と、を少なくとも備えた多層膜1の製造方法であって、前記工程Bにおいて、前記シード層として、ストロンチウム(Sr)とルテニウム(Ru)と酸素(O)とを含む化合物を、スパッタ法により形成し、前記工程Cにおいて、前記誘電体層を形成する際の基板温度をTd(dielectric)、としたとき、560≦Td≦720[℃]である。
なお、以下の説明では、誘電体層5としてチタン酸ジルコン酸鉛[Pb(ZrxTi1-x)O3 :PZT]を用いた場合を例に挙げて説明するが、本発明はこれに限定されるものではない。
以下では、本実施形態に係る多層膜の製造方法を実施するために好適な成膜装置の構造について説明する。
図4は、成膜装置10の内部構成の一例を示す模式的な断面図である。
カソード電極22の一面側は局部的に真空槽11内に露出されている。ターゲット21はカソード電極22の一面側のうち露出された領域の中央部に密着して固定され、ターゲット21とカソード電極22とは電気的に接続されている。
カソード電極22のターゲット21とは反対側、すなわちカソード電極22の他面側には磁石装置29が配置されている。磁石装置29はターゲット21の表面に磁力線を形成するように構成されている。
支持部32の表面の中央部に基板31を載置した際に、第一の防着板34は基板31の外周より外側を取り囲むように配されている。
発熱部材33としては例えばSiCが用いられる。発熱部材33は、支持部32を挟んで基板31とは反対側の位置に配されている。加熱用電源17は発熱部材33と電気的に接続されている。加熱用電源17から発熱部材33に直流電流が供給されると、発熱部材33が発する熱が、支持部32を通して、支持部32上の基板31と第一の防着板34へ伝わる。これにより、基板31と第一の防着板34が一緒に加熱される。
発熱部材33の支持部32とは反対側には冷却部38が配置されている。冷却部38は内部に温度管理された冷却媒体を循環できるように構成され、発熱部材33が発熱しても真空槽11の壁面の加熱を防止する。
以下では、多層膜の成膜方法について説明する。
図3Aから図3Cは、本実施形態に係る多層膜の製造工程を示す断面図である。このような製造工程を実施する際に、前述した図4に示す成膜装置を用いた。
図4には、説明を簡略とするため、成膜装置10が1つの真空槽11を有する場合を例示したが、以下の工程A~Cの製造方法では、少なくとも3つの真空槽11a、11b、11c(11)が、図4で言うと紙面奥行き方向に、不図示の仕切りバルブを介して連通して成る構成の成膜装置を使用した場合を前提として説明する。ここで、真空槽11a(11)は導電層形成用の真空槽である。真空槽11b(11)はシード層形成用の真空槽である。真空槽11c(11)は誘電体層形成用の真空槽である。以下では、真空槽のみ符号を区別し、各真空槽に付随する構成の符号は区別せず説明する。
図3Aに示すように、シリコン(Si)からなる基板2の一主面側に、白金(Pt)からなる導電層3を形成する。以下では、基板の一主面に直接、導電層を形成するものとして説明するが、必要に応じて、基板2の一主面に対して、導電層の形成前に、他の被膜を設ける構成としても構わない。
冷却部38に温度管理された冷却媒体を循環させておく。
図3Bに示すように、前記導電層3を覆うようにシード層4を形成する。
本工程Bでは、シード層4として、ストロンチウム(Sr)とルテニウム(Ru)と酸素(O)とを含む化合物からなる酸化物を、スパッタ法により形成する。
図3Cに示すように、前記シード層4を覆うように誘電体層5を形成する。
本工程Cでは、誘電体層5として、PZT膜を、スパッタ法により形成する。ここで、本工程Cにおいて、誘電体層5を形成する際の基板温度Tdを、560≦Td≦720[℃]とする。
なお、上述した基板の搬送、すなわち、外部から真空槽11a(11)への搬入、各真空槽間の移動、真空槽11c(11)から外部への搬出には、不図示の搬送ロボットが好適に用いられる。
この多層膜1では、誘電体層5は、パイロクロア相を含まず、高い結晶性を有する。これにより、この多層膜1は、例えば高い圧電性と耐圧性とを両立し、優れた特性を有する。このような多層膜1は、例えば圧電素子等に好適に用いられる。
以下では、上述した本発明の効果を確認するために行った実験例について説明する。
シード層の有無を変えてPZT膜(誘電体層)を成膜し、その特性について評価した。
本例では、Pt膜からなる導電層、SrRuO3 (SRO)膜からなるシード層、PZT膜からなる誘電体層を順に積層して成る多層膜を形成した。
基板としては、直径8インチのシリコン(Si)ウェハを用いた。ここでは、Siウェハの一主面に、熱酸化膜(SiO2 膜)、密着層として機能するTi膜(厚さ20nm)、及び、下部電極層として機能するPt膜(厚さ100nm)が順に、予め積層されたものを使用した。
ターゲットには、300mm径、厚さ5mmのSrRuO3 ターゲットを用いた。
スパッタパワーは0.7[kW]、スパッタ圧は0.4[Pa]、基板温度は530~740[℃]とした。
シード層の膜厚は、100[nm]とした。
ターゲットには、300mm径、厚さ5mmのPZTターゲットを用いた。
スパッタパワーは2.5[kW]、スパッタ圧は0.5[Pa]、基板温度は720[℃]とした。
誘電体層の膜厚は、2.0[μm]とした。
上述した条件により作製した実験例1の試料を、サンプル1と呼ぶ。
本例では、シード層を設けることなく、基板のPt薄膜上にPZT膜を成膜することにより多層膜を形成した。PZT膜は、基板温度の条件を585[℃]として形成した。
PZT膜からなる誘電体層の他の成膜条件は、実験例1と同様である。
上述した条件により作製した実験例2の試料を、サンプル2と呼ぶ。
本例では、シード層を形成せず、Si基板のPt薄膜上に、基板温度を625[℃]としてPZT膜を成膜することにより多層膜を形成した。PZT膜の他の成膜条件は、上述したサンプル1と同様である。
上述した条件により作製した実験例3の試料を、サンプル3と呼ぶ。
本例では、シード層を形成せず、Si基板のPt薄膜上に、基板温度を665[℃]としてPZT膜を成膜することにより多層膜を形成した。PZT膜の他の成膜条件は、上述したサンプル1と同様である。
上述した条件により作製した実験例4の試料を、サンプル4と呼ぶ。
図5はサンプル1(シード層:SrRuO3 膜)のX線チャートである。また、図6は、サンプル2~4(シード層無し)のX線チャートである。
サンプル1については、成膜時の基板温度を530~740[℃]の範囲で変えてPZT膜の成膜を行い、各基板温度で形成されたPZT膜ごとに結晶構造を解析した。
2 基板
3 導電層
4 シード層
5 誘電体層
10 成膜装置
11 真空槽
13 スパッタ電源
14 スパッタガス導入部
18 温度制御部
21 ターゲット
31 基板
32 支持部
34 防着板(第一の防着板)
Claims (4)
- 基板に導電層を形成し、
スパッタ法により、ストロンチウム(Sr)とルテニウム(Ru)と酸素(O)とを含む化合物で、前記導電層を覆うようにシード層を形成し、
前記シード層を覆うように誘電体層を形成し、前記誘電体層を形成する際の基板温度をTd(dielectric)と定義したとき、560≦Td≦720[℃]を満たす
多層膜の製造方法。 - 前記誘電体層を形成する際に、前記誘電体層として、鉛(Pb)とジルコニア(Zr)とチタン(Ti)と酸素(O)とを含む化合物を、スパッタ法により形成する
請求項1に記載の多層膜の製造方法。 - シリコンからなる基板の一主面側に、白金(Pt)からなる導電層と、シード層と、誘電体層と、を少なくとも順に配してなり、
前記シード層は、ストロンチウム(Sr)とルテニウム(Ru)と酸素(O)とを含む化合物から構成され、
前記誘電体層は、鉛(Pb)とジルコニア(Zr)とチタン(Ti)と酸素(O)とを含む化合物から構成され、
前記誘電体層をなす化合物は、パイロクロア相に起因するX線回折ピークを含まない
多層膜。 - 前記誘電体層をなす化合物は、Pb(Zr,Ti)O3 の(100)に起因するX線回折ピークの半値幅(FWHM)が1[度]以下である
請求項3に記載の多層膜。
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WO2020250591A1 (ja) * | 2019-06-12 | 2020-12-17 | 富士フイルム株式会社 | 圧電素子 |
JP2020202327A (ja) * | 2019-06-12 | 2020-12-17 | 富士フイルム株式会社 | 圧電素子 |
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JP7539474B2 (ja) | 2020-07-28 | 2024-08-23 | 富士フイルム株式会社 | 圧電膜付き基板、圧電素子、及び圧電膜付き基板の作製方法 |
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