CN118064861A - Pyroelectric film integrated with infrared absorption material and preparation method and application thereof - Google Patents
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
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- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 3
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to the field of functional film materials, in particular to a pyroelectric film integrated with an infrared absorption material, and a preparation method and application thereof. The method disclosed by the invention adopts a magnetron sputtering mode to realize the growth of the PZT pyroelectric film on the silicon-based substrate. The PZT pyroelectric film with higher pyroelectric number, low dielectric constant and dielectric loss is obtained by a method of proper process setting, component design and combined seed layer induced film oriented growth. The invention provides a preparation method of an infrared absorption material compatible with a PZT pyroelectric film preparation process, and the pyroelectric film of the integrated infrared absorption material is prepared, so that the integration of the PZT pyroelectric film and the infrared absorption material is realized.
Description
Technical Field
The invention relates to the field of functional film materials, in particular to a pyroelectric film integrated with an infrared absorption material, and a preparation method and application thereof.
Background
The pyroelectric infrared sensor has the characteristics of no need of refrigeration, high detection rate, quick response, wide working band, low cost and the like, and is widely applied to the fields of industrial and medical analysis instruments, flame detection and early warning, intelligent guidance at the tail end of the military industry, spectrum instruments and the like. The infrared radiation is absorbed by the infrared absorption functional material in the pyroelectric infrared sensor so that the temperature rises, light-heat conversion occurs, then based on the pyroelectric effect of the infrared absorption material, heat-electricity conversion occurs, and finally an infrared radiation signal is converted into an electric signal form to be output. In evaluating a pyroelectric infrared detector, the detection rate figure of merit F d is a very important parameter, while F d is closely related to the pyroelectric coefficient, dielectric constant and dielectric loss of the pyroelectric material, as shown in formula (1).
Wherein p is the pyroelectric coefficient, c is the volumetric heat capacity, ε r is the relative permittivity, ε 0 is the vacuum permittivity, and tan delta is the dielectric loss.
The PZT thin film is used as a typical perovskite type metal oxide ceramic material, has excellent ferroelectric and pyroelectric properties, and is one of hot materials for preparing pyroelectric infrared sensors. The pyroelectric performance of PZT thin film is closely related to the material composition ratio, crystal orientation, thin film thickness, etc., for titanium-rich PZT, i.e. when the Ti element content in the material is greater than the Zr element content, the crystal structure of PZT is tetragonal phase, and the spontaneous polarization direction of tetragonal phase PZT is [001]. Therefore, the pyroelectric performance of the material is best when tetragonal phase PZT is oriented in [001]. The crystal growth orientation of the PZT thin film can be controlled by a method of preparing a buffer layer. The invention patent (publication No. CN 112928200A) discloses a lead zirconate titanate piezoelectric film, a preparation method and application thereof, and adopts a buffer layer guiding mode to prepare a PZT52/48 film with (001) orientation on a silicon substrate, wherein the film obtains higher remnant polarization intensity (more than 40 mu C/cm 2), but the dielectric constant of the film is higher (more than 1000), and the dielectric loss of a high dielectric constant material is higher, so that the prepared device has larger noise and is unfavorable for the performance of a pyroelectric infrared detector. In addition, to further enhance the performance of the pyroelectric infrared detector, it is generally necessary to cover the surface of the device with a layer of functional material with high absorptivity to enhance the performance of the infrared detector. However, the absorption efficiency of electromagnetic waves in the middle infrared band is low, which is not beneficial to the improvement of the performance of the film type pyroelectric infrared detector, whether the PZT film material is itself or the metal electrode materials such as Au, ag, pt and the like are covered on the surface of the PZT material.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a pyroelectric film integrated with an infrared absorption material, a preparation method and application thereof, and the PZT pyroelectric film with high pyroelectric number, low dielectric constant and low dielectric loss is prepared and obtained by adopting a method of inducing film orientation growth by a seed layer through proper component design, meanwhile, the design realizes a medium-infrared electromagnetic wave absorption material compatible with the preparation process of the PZT film pyroelectric detector, solves the problem of low infrared electromagnetic wave absorption efficiency of the PZT film pyroelectric infrared detector, is beneficial to further improving the performance of the pyroelectric infrared detector, and meets the requirements of fields such as industrial medical analysis instruments, military intelligence guides, spectral instruments and the like on the high-performance infrared detector. The invention mainly comprises the following contents:
The first aspect of the present invention provides a method for preparing a pyroelectric film of an integrated infrared absorbing material, the pyroelectric film of the integrated infrared absorbing material comprising a substrate, a bottom electrode layer, a seed layer, a PZT pyroelectric layer, and an infrared absorbing layer, the method comprising the steps of:
s1, arranging a bottom electrode layer on a substrate;
S2, setting a seed layer on the bottom electrode layer;
S3, setting a PZT pyroelectric layer on the seed layer;
S4, arranging an infrared absorption layer on the PZT pyroelectric layer.
Preferably, in step S1: the material of the base is a (100) oriented silicon single crystal substrate or a SiO 2/Si (100) substrate; and/or the bottom electrode layer is a Pt/TiO 2 or Pt/Ti composite electrode layer, wherein the thickness of the Pt layer is 150 nm-250 nm, and the thickness of the TiO 2 or Ti layer is 15-nm-30 nm.
Preferably, the TiO 2 layer in the bottom electrode layer is prepared by radio frequency magnetron sputtering deposition, the sputtering power is 100W-150W, and the deposition atmosphere is Ar gas with the flow of 30sccm-50 sccm; and/or the Pt layer in the bottom electrode layer is prepared by direct-current magnetron sputtering deposition, the sputtering power is 80-120W, and the deposition atmosphere is Ar gas with the flow of 30sccm-50 sccm.
Preferably, the seed layer in the step S2 is a metal oxide ceramic material with an ABO 3 perovskite structure, and the thickness of the seed layer is 100nm-300nm.
Preferably, the metal oxide ceramic material with the ABO 3 perovskite structure is lanthanum nickelate LaNiO 3, which can reduce lattice mismatch between the PZT thin film and the bottom electrode and between the PZT thin film and the substrate, reduce interface defects, reduce interface stress and facilitate oriented growth of the thin film.
Preferably, the LaNiO 3 seed Layer (LNO) is prepared by direct current magnetron sputtering deposition, and the sputtering power is 100V-150V; the deposition atmosphere is Ar and O 2, wherein the Ar gas flow is 30sccm-60 sccm, and the O 2 gas flow is 5sccm-20 sccm; the deposition substrate temperature is 450 ℃ to 500 ℃.
Preferably, after the preparation of the LaNiO 3 seed layer by direct-current magnetron sputtering deposition is completed, annealing treatment is carried out, wherein the annealing temperature is 600-650 ℃, and the annealing time is 10min-15 min.
Preferably, in step S3: the PZT pyroelectric layer is a PZT thin film layer, wherein Zr/Ti (molar ratio) in the PZT thin film is 10/90-30/70, and/or the thickness of the PZT pyroelectric layer is 400 nm-1000 nm.
Preferably, in the step S3, the PZT pyroelectric layer is prepared by radio frequency magnetron sputtering deposition, and the sputtering power is 120W-160W; the deposition atmosphere is Ar and O 2, wherein the Ar gas flow is 50sccm-100 sccm, and the O 2 gas flow is 10sccm-30sccm; the deposition substrate temperature is 600 ℃ to 650 ℃.
Preferably, after the preparation of the PZT pyroelectric layer by radio frequency magnetron sputtering deposition is completed, annealing treatment is carried out, wherein the annealing temperature is 600-650 ℃, and the annealing time is 10-15 min.
Preferably, in the step S4, the infrared absorption layer is a multilayer composite film, and the multilayer composite film sequentially includes a first Si 3N4 layer, a Ti layer, a second Si 3N4 layer, and a Pt layer from top to bottom, where the thickness of the first Si 3N4 layer is 100nm-1000 nm, the thickness of the Ti layer is 10nm-100nm, the thickness of the second Si 3N4 layer is 100nm-1000 nm, and the thickness of the Pt layer is 50nm-200 nm. According to the invention, through reasonably adjusting the thicknesses of the first Si 3N4 layer, the Ti layer and the second Si 3N4 layer, impedance matching between the multilayer film and free space can be realized, so that the reflectivity of electromagnetic waves of infrared specific wave bands on the surface of a material is close to 0, the existence of the Pt layer is used for preventing transmission of the electromagnetic waves, so that the transmissivity is close to 0, and efficient absorption of the electromagnetic waves is realized based on the characteristics. In addition, the Pt layer can also be used as an upper electrode of the PZT pyroelectric film.
Preferably, in the multilayer composite film: the Pt layer is prepared by direct-current magnetron sputtering deposition, the sputtering power is 80W-120W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm-50sccm; and/or the first Si 3N4 layer and/or the second Si 3N4 layer are/is prepared by radio frequency magnetron sputtering deposition, the sputtering power is 100-150W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm-50sccm; and/or the Ti layer is prepared by direct current magnetron sputtering deposition, the irradiation power is 80W-120W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm-50sccm.
The invention also provides a pyroelectric film of the integrated infrared absorption material prepared by the preparation method.
The third aspect of the invention provides an application of the pyroelectric film integrated with the infrared absorption material in an infrared detector.
The invention has the beneficial effects that:
(1) The preparation method of the PZT pyroelectric film disclosed by the invention adopts a magnetron sputtering mode to realize the growth of the PZT pyroelectric film on a silicon-based substrate. The PZT pyroelectric film with higher pyroelectric number, low dielectric constant and dielectric loss is obtained by a method of proper process setting, component design and combined seed layer induced film oriented growth.
(2) The invention also provides a preparation method of the infrared absorption material compatible with the PZT pyroelectric film preparation process, and the pyroelectric film of the integrated infrared absorption material is prepared, so that the integration of the PZT pyroelectric film and the infrared absorption material is realized, and the performance of the pyroelectric infrared detector is further improved. The infrared absorption material can realize impedance matching between the multilayer film and free space by reasonably adjusting the thicknesses of the first Si 3N4 layer, the Ti layer and the second Si 3N4 layer in the infrared absorption layer, so that the reflectivity of electromagnetic waves of infrared specific wave bands on the surface of the material is close to 0, the existence of the Pt layer is used for preventing the transmission of the electromagnetic waves, so that the transmissivity is close to 0, and the efficient absorption of the electromagnetic waves is realized based on the reflection of the Pt layer, and in addition, the Pt layer can also be used as an upper electrode of the PZT pyroelectric film.
Drawings
FIG. 1 is a schematic view of a multilayer film structure obtained in an embodiment of the present invention;
FIG. 2 is an XRD pattern of a PZT pyroelectric film obtained in an embodiment of the present invention;
FIG. 3 is an SEM image of a PZT pyroelectric film obtained in an embodiment of the present invention;
FIG. 4 shows the result of pyroelectric coefficient test of PZT pyroelectric film obtained in the embodiment of the present invention;
FIG. 5 shows the dielectric constant and dielectric loss test results of the PZT pyroelectric film obtained in the embodiment of the present invention;
FIG. 6 is an absorption curve obtained by finite element simulation of the infrared absorption structure obtained in the examples of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following detailed description.
A method for preparing a pyroelectric film of an integrated infrared absorbing material, the pyroelectric film of the integrated infrared absorbing material comprising a substrate, a bottom electrode layer, a seed layer, a PZT pyroelectric layer, and an infrared absorbing layer, the method comprising the steps of:
S1, arranging a bottom electrode layer on a substrate; the material of the base is a (100) oriented silicon single crystal substrate or a SiO 2/Si (100) substrate, the bottom electrode layer is a Pt/TiO 2 or Pt/Ti composite electrode layer, wherein the thickness of the Pt layer is 150 nm-250 nm, and the thickness of the TiO 2 or Ti layer is 15 nm-30 nm; the TiO 2 layer is prepared by radio frequency magnetron sputtering deposition, the sputtering power is 100W-150W, and the deposition atmosphere is Ar gas with the flow of 30sccm-50 sccm; the Pt layer is prepared by direct current magnetron sputtering deposition, the sputtering power is 80-120W, and the deposition atmosphere is Ar gas with the flow of 30-50 sccm.
S2, setting a lanthanum nickelate LaNiO 3 seed layer with the thickness of 100-300 nm on the bottom electrode layer; the LaNiO 3 seed Layer (LNO) is prepared by direct current magnetron sputtering deposition, and the sputtering power is 100V-150V; the deposition atmosphere is Ar and O 2, wherein the Ar gas flow is 30sccm-60 sccm, and the O 2 gas flow is 5sccm-20 sccm; the deposition substrate temperature is 450 ℃ to 500 ℃. After the preparation of the LaNiO 3 seed layer is completed, annealing treatment is carried out, wherein the annealing temperature is 600-650 ℃, and the annealing time is 10min-15 min.
S3, setting a PZT pyroelectric layer on the seed layer; the PZT pyroelectric layer is a PZT thin film layer, wherein Zr/Ti (molar ratio) in the PZT thin film is 10/90-30/70, and the thickness of the PZT pyroelectric layer is 400 nm-1000 nm. The PZT pyroelectric layer is prepared by radio frequency magnetron sputtering deposition, and the sputtering power is 120W-160W; the deposition atmosphere is Ar and O 2, wherein the Ar gas flow is 50sccm-100 sccm, and the O 2 gas flow is 10sccm-30sccm; the deposition substrate temperature is 600 ℃ to 650 ℃. And after the PZT pyroelectric layer is prepared, annealing treatment is carried out, wherein the annealing temperature is 600-650 ℃, and the annealing time is 10-15 min.
S4, arranging an infrared absorption layer on the PZT pyroelectric layer. The infrared absorption layer is a multilayer composite film, and the multilayer composite film sequentially comprises a first Si 3N4 layer, a Ti layer, a second Si 3N4 layer and a Pt layer from top to bottom, wherein the thickness of the first Si 3N4 layer is 100nm-1000 nm, the thickness of the Ti layer is 10nm-100nm, the thickness of the second Si 3N4 layer is 100nm-1000 nm, and the thickness of the Pt layer is 50nm-200 nm. The Pt layer is prepared by direct-current magnetron sputtering deposition, the sputtering power is 80W-120W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm-50sccm; the first Si 3N4 layer and the second Si 3N4 layer are prepared through radio frequency magnetron sputtering deposition, the sputtering power is 100-150W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm-50sccm; the Ti layer is prepared by direct current magnetron sputtering deposition, the irradiation power is 80W-120W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm-50sccm.
The pyroelectric film of the integrated infrared absorption material prepared by the preparation method can be applied to an infrared detector, and the pyroelectric film of the integrated infrared absorption material prepared by the preparation method is beneficial to further improving the performance of the pyroelectric infrared detector.
The invention will now be described in detail with reference to figures 1-6 and the examples. The embodiments shown below do not limit the inventive content described in the claims in any way. The whole contents of the constitution shown in the following examples are not limited to the solution of the invention described in the claims.
Example 1
A preparation method of a PZT pyroelectric film integrated with an infrared absorption enhancement material comprises the following steps:
S1, preparing a 4-inch Si/SiO 2 composite sheet, and cleaning, wherein the thickness of the SiO 2 layer is 1 mu m. The radio frequency magnetron sputtering method is adopted, firstly, a 20 nm TiO 2 adhesive layer is sputtered and grown on a substrate, and the sputtering power is 100W. Then, a lower electrode of 150 nm Pt is grown by direct current magnetron sputtering, and the sputtering power is 100W. The process gas is pure Ar gas, and the Ar gas flow is 30 sccm.
S2, growing a 100 nm LNO film by direct-current magnetron sputtering, wherein the sputtering power is 120W. The process gas is Ar gas and O 2 gas, the Ar gas flow is 50 sccm, the O 2 gas flow is 10 sccm, the gas pressure in the chamber is maintained at 1.3 Pa in the sputtering process, and the substrate temperature is 450 ℃. The magnetron sputtering time was 30 min. And after sputtering, annealing in an O 2 atmosphere in an annealing furnace at 650 ℃ for 12 min.
And S3, growing a 400 nm PZT film by radio frequency magnetron sputtering, wherein the sputtering power is 160W. The process gas is Ar gas and O 2 gas, the Ar gas flow is 90 sccm, the O 2 gas flow is 10 sccm, the gas pressure in the chamber is maintained at 3.0 Pa in the sputtering process, and the substrate temperature is 600 ℃. The magnetron sputtering time was 4 h. And after sputtering, annealing in an O 2 atmosphere in an annealing furnace at 600 ℃ for 12 min. Preparing a mask on the surface of the PZT film by photoetching, etching the PZT film and the LNO seed layer by adopting an ion beam etching method by taking photoresist as the mask, and removing part of the PZT film to expose part of the Pt lower electrode below the LNO seed layer. And (5) cleaning the photoresist by using acetone after etching is finished.
And S4, sequentially growing 200 nm Pt and 500 nm Si 3N4、40 nm Ti、400 nm Si3N4 film layers through magnetron sputtering growth. Wherein, the Pt and Ti film layer grows by a direct current magnetron sputtering mode, and the sputtering power is 100W; the Si 3N4 film layer grows by a radio frequency magnetron sputtering mode, and the sputtering power is 100W. The process gas is pure Ar gas, and the Ar gas flow is 30 sccm.
The structure of the multilayer film obtained in this example is schematically shown in FIG. 1, the XRD pattern of the PZT thin film is shown in FIG. 2, the SEM pattern is shown in FIG. 3, the pyroelectric performance test result of the PZT thin film is shown in FIG. 4, the dielectric performance test result of the PZT thin film is shown in FIG. 5, and the infrared absorption spectrum of the infrared absorption material is shown in FIG. 6.
As can be seen from FIG. 2, the PZT thin film prepared in accordance with the present invention has good crystallinity, and the main orientations of the thin film are (001) and (100) orientations.
As can be seen from FIG. 3, the PZT thin film prepared by the method has uniform thickness and a typical columnar perovskite structure, which shows that the thin film crystal structure grows well, the columnar microstructure of the thin film is compact and dense, and the inside of the thin film has no pore structure.
As can be seen from fig. 4 and 5, the PZT thin film prepared according to the present invention has a high pyroelectric coefficient and a low dielectric constant. The pyroelectric coefficient of the PZT thin film at room temperature can reach 20 nC cm -2·K-1, and the dielectric constant and dielectric loss of the material measured at the frequency of 1kHz are 173 and 0.016 respectively. As can be seen from the test results, the PZT thin film prepared by the method has higher pyroelectric coefficient and lower dielectric constant, and shows that the PZT thin film has excellent pyroelectric performance.
As can be seen from the finite element simulation result in FIG. 6, the infrared absorption layer of Si 3N4-Ti-Si3N4 -Pt designed by the invention has the absorption efficiency of infrared light being basically more than 80% in the wave band of 3-6 mu m, thus realizing the efficient absorption of infrared light.
Example 2
A method for preparing a pyroelectric film of an integrated infrared absorbing material, the pyroelectric film of the integrated infrared absorbing material comprising a substrate, a bottom electrode layer, a seed layer, a PZT pyroelectric layer, and an infrared absorbing layer, the method comprising the steps of:
S1, arranging a bottom electrode layer on a substrate; the base material is a (100) oriented silicon single crystal substrate, the bottom electrode layer is a Pt/TiO 2 composite electrode layer, wherein the thickness of the Pt layer is 150 nm, and the thickness of the TiO 2 layer is 15 nm; the TiO 2 layer is prepared by radio frequency magnetron sputtering deposition, the sputtering power is 100W, and the deposition atmosphere is Ar gas with the flow of 30 sccm; the Pt layer was prepared by DC magnetron sputtering deposition with a sputtering power of 80W and a deposition atmosphere of Ar gas with a flow rate of 30 sccm.
S2, setting a lanthanum nickel oxide LaNiO 3 seed layer with the thickness of 100nm on the bottom electrode layer; the LaNiO 3 seed Layer (LNO) is prepared by direct current magnetron sputtering deposition, and the sputtering power is 100V; the deposition atmosphere is Ar and O 2, wherein the Ar gas flow is 30sccm, and the O 2 gas flow is 5sccm; the deposition substrate temperature was 450 ℃. After the preparation of the LaNiO 3 seed layer is completed, annealing treatment is carried out, wherein the annealing temperature is 600 ℃, and the annealing time is 10min.
S3, setting a PZT pyroelectric layer on the seed layer; the PZT pyroelectric layer is a PZT thin film layer, wherein Zr/Ti (molar ratio) =10/90 in the PZT thin film, and the thickness of the PZT pyroelectric layer is 400 nm. The PZT pyroelectric layer is prepared by radio frequency magnetron sputtering deposition, and the sputtering power is 120W; the deposition atmosphere was Ar and O 2, wherein the Ar gas flow rate was 50sccm and the O 2 gas flow rate was 10sccm; the deposition substrate temperature was 600 ℃. And after the PZT pyroelectric layer is prepared, annealing treatment is carried out, wherein the annealing temperature is 600 ℃, and the annealing time is 10min.
S4, arranging an infrared absorption layer on the PZT pyroelectric layer. The infrared absorption layer is a multilayer composite film, and the multilayer composite film sequentially comprises a first Si 3N4 layer, a Ti layer, a second Si 3N4 layer and a Pt layer from top to bottom, wherein the thickness of the first Si 3N4 layer is 100nm, the thickness of the Ti layer is 10nm, the thickness of the second Si 3N4 layer is 100nm, and the thickness of the Pt layer is 50nm. The Pt layer is prepared by direct-current magnetron sputtering deposition, the sputtering power is 80W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm; the first Si 3N4 layer and the second Si 3N4 layer are prepared through radio frequency magnetron sputtering deposition, the sputtering power is 100W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm; the Ti layer is prepared by direct current magnetron sputtering deposition, the irradiation power is 80W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm.
The PZT thin film prepared in this example has good crystallinity, and the main orientations of the thin film are (001) and (100) orientations, which are experimentally examined. The PZT thin film has uniform thickness and a typical columnar perovskite structure, which shows that the thin film crystal structure grows well, the columnar microstructure of the thin film is compact and dense, and the inside of the thin film has no pore structure. The PZT thin film has a high pyroelectric coefficient and a low dielectric constant. The pyroelectric coefficient of the PZT thin film at room temperature can reach 25 nC cm -2·K-1, and the dielectric constant and dielectric loss of the material measured at the frequency of 1kHz are 170 and 0.015 respectively. As can be seen from the test results, the PZT thin film prepared by the method has higher pyroelectric coefficient and lower dielectric constant, and shows that the PZT thin film has excellent pyroelectric performance. From the result of finite element simulation, it can be seen that the infrared absorption layer of Si 3N4-Ti-Si3N4 -Pt in the embodiment of the invention has an infrared absorption efficiency of more than 85% in the 3-6 μm band, and realizes the efficient absorption of infrared light.
Example 3
A method for preparing a pyroelectric film of an integrated infrared absorbing material, the pyroelectric film of the integrated infrared absorbing material comprising a substrate, a bottom electrode layer, a seed layer, a PZT pyroelectric layer, and an infrared absorbing layer, the method comprising the steps of:
S1, arranging a bottom electrode layer on a substrate; the base is made of a SiO 2/Si (100) substrate, the bottom electrode layer is a Pt/Ti composite electrode layer, wherein the thickness of the Pt layer is 250 nm, and the thickness of the Ti layer is 30 nm; the Pt layer is prepared by direct current magnetron sputtering deposition, the sputtering power is 120W, and the deposition atmosphere is Ar gas with the flow of 50 sccm.
S2, setting a lanthanum nickel oxide LaNiO 3 seed layer with the thickness of 300nm on the bottom electrode layer; the LaNiO 3 seed Layer (LNO) is prepared by direct current magnetron sputtering deposition, and the sputtering power is 150V; the deposition atmosphere was Ar and O 2, wherein the Ar gas flow rate was 60 sccm and the O 2 gas flow rate was 20 sccm; the deposition substrate temperature was 500 ℃. After the preparation of the LaNiO 3 seed layer is completed, annealing treatment is carried out, wherein the annealing temperature is 650 ℃, and the annealing time is 15 min.
S3, setting a PZT pyroelectric layer on the seed layer; the PZT pyroelectric layer is a PZT thin film layer, wherein Zr/Ti (molar ratio) in the PZT thin film is=30/70, and the thickness of the PZT pyroelectric layer is 1000 nm. The PZT pyroelectric layer is prepared by radio frequency magnetron sputtering deposition, and the sputtering power is 160W; the deposition atmosphere was Ar and O 2, wherein the Ar gas flow rate was 100 sccm and the O 2 gas flow rate was 30sccm; the deposition substrate temperature was 650 ℃. And after the PZT pyroelectric layer is prepared, annealing treatment is carried out, wherein the annealing temperature is 650 ℃, and the annealing time is 15min.
S4, arranging an infrared absorption layer on the PZT pyroelectric layer. The infrared absorption layer is a multilayer composite film, and the multilayer composite film sequentially comprises a first Si 3N4 layer, a Ti layer, a second Si 3N4 layer and a Pt layer from top to bottom, wherein the thickness of the first Si 3N4 layer is 1000 nm, the thickness of the Ti layer is 100nm, the thickness of the second Si 3N4 layer is 1000 nm, and the thickness of the Pt layer is 200 nm. The Pt layer is prepared by direct-current magnetron sputtering deposition, the sputtering power is 120W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 50sccm; the first Si 3N4 layer and the second Si 3N4 layer are prepared through radio frequency magnetron sputtering deposition, the sputtering power is 150W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 50sccm; the Ti layer is prepared by direct current magnetron sputtering deposition, the irradiation power is 120W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 50sccm.
The PZT thin film prepared in this example has good crystallinity, and the main orientations of the thin film are (001) and (100) orientations, which are experimentally examined. The PZT thin film has uniform thickness and a typical columnar perovskite structure, which shows that the thin film crystal structure grows well, the columnar microstructure of the thin film is compact and dense, and the inside of the thin film has no pore structure. The PZT thin film has a high pyroelectric coefficient and a low dielectric constant. The pyroelectric coefficient of the PZT thin film at room temperature can reach 26 nC cm -2·K-1, and the dielectric constant and dielectric loss of the material measured at the frequency of 1kHz are 172 and 0.016 respectively. As can be seen from the test results, the PZT thin film prepared by the method has higher pyroelectric coefficient and lower dielectric constant, and shows that the PZT thin film has excellent pyroelectric performance. From the result of finite element simulation, it can be seen that the infrared absorption layer of Si 3N4-Ti-Si3N4 -Pt in the embodiment of the invention has an infrared absorption efficiency of more than 82% in the 3-6 μm band, and realizes high-efficiency absorption of infrared light.
Example 4
A method for preparing a pyroelectric film of an integrated infrared absorbing material, the pyroelectric film of the integrated infrared absorbing material comprising a substrate, a bottom electrode layer, a seed layer, a PZT pyroelectric layer, and an infrared absorbing layer, the method comprising the steps of:
S1, arranging a bottom electrode layer on a substrate; the base is made of a SiO 2/Si (100) substrate, the bottom electrode layer is a Pt/TiO 2 composite electrode layer, wherein the thickness of the Pt layer is 190nm, and the thickness of the TiO 2 layer is 20 nm; the TiO 2 layer is prepared by radio frequency magnetron sputtering deposition, the sputtering power is 120W, and the deposition atmosphere is Ar gas with the flow of 40 sccm; the Pt layer was prepared by DC magnetron sputtering deposition with a sputtering power of 100W and a deposition atmosphere of Ar gas with a flow rate of 40 sccm.
S2, setting a lanthanum nickel oxide LaNiO 3 seed layer with the thickness of 200nm on the bottom electrode layer; the LaNiO 3 seed Layer (LNO) is prepared by direct current magnetron sputtering deposition, and the sputtering power is 120V; the deposition atmosphere is Ar and O 2, wherein the Ar gas flow rate is 40sccm, and the O 2 gas flow rate is 10sccm; the deposition substrate temperature was 480 ℃. After the preparation of the LaNiO 3 seed layer is completed, annealing treatment is carried out, wherein the annealing temperature is 620 ℃, and the annealing time is 12 min.
S3, setting a PZT pyroelectric layer on the seed layer; the PZT pyroelectric layer is a PZT thin film layer, wherein Zr/Ti (molar ratio) in the PZT thin film is 10/80, and the thickness of the PZT pyroelectric layer is 650 nm. The PZT pyroelectric layer is prepared by radio frequency magnetron sputtering deposition, and the sputtering power is 140W; the deposition atmosphere is Ar and O 2, wherein the Ar gas flow rate is 70 sccm, and the O 2 gas flow rate is 20sccm; the deposition substrate temperature was 620 ℃. And after the PZT pyroelectric layer is prepared, annealing treatment is carried out, wherein the annealing temperature is 620 ℃, and the annealing time is 12min.
S4, arranging an infrared absorption layer on the PZT pyroelectric layer. The infrared absorption layer is a multilayer composite film, and the multilayer composite film sequentially comprises a first Si 3N4 layer, a Ti layer, a second Si 3N4 layer and a Pt layer from top to bottom, wherein the thickness of the first Si 3N4 layer is 500nm, the thickness of the Ti layer is 50nm, the thickness of the second Si 3N4 layer is 500nm, and the thickness of the Pt layer is 100nm. The Pt layer is prepared by direct-current magnetron sputtering deposition, the sputtering power is 100W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 40sccm; the first Si 3N4 layer and the second Si 3N4 layer are prepared through radio frequency magnetron sputtering deposition, the sputtering power is 120W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 40sccm; the Ti layer is prepared by direct current magnetron sputtering deposition, the irradiation power is 100W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 45sccm.
The PZT thin film prepared in this example has good crystallinity, and the main orientations of the thin film are (001) and (100) orientations, which are experimentally examined. The PZT thin film has uniform thickness and a typical columnar perovskite structure, which shows that the thin film crystal structure grows well, the columnar microstructure of the thin film is compact and dense, and the inside of the thin film has no pore structure. The PZT thin film has a high pyroelectric coefficient and a low dielectric constant. The pyroelectric coefficient of the PZT thin film at room temperature can reach 24 nC cm -2·K-1, and the dielectric constant and dielectric loss of the material measured at 1kHz frequency are 169 and 0.0145 respectively. As can be seen from the test results, the PZT thin film prepared by the method has higher pyroelectric coefficient and lower dielectric constant, and shows that the PZT thin film has excellent pyroelectric performance. From the result of finite element simulation, it can be seen that the infrared absorption layer of Si 3N4-Ti-Si3N4 -Pt in the embodiment of the invention has an infrared absorption efficiency of more than 82% in the 3-6 μm band, and realizes high-efficiency absorption of infrared light.
Example 5
A method for preparing a pyroelectric film of an integrated infrared absorbing material, the pyroelectric film of the integrated infrared absorbing material comprising a substrate, a bottom electrode layer, a seed layer, a PZT pyroelectric layer, and an infrared absorbing layer, the method comprising the steps of:
S1, arranging a bottom electrode layer on a substrate; the base is made of a (100) oriented silicon single crystal substrate, the bottom electrode layer is a Pt/TiO 2 composite electrode layer, wherein the thickness of the Pt layer is 210 nm, and the thickness of the TiO 2 or Ti layer is 26nm; the TiO 2 layer is prepared by radio frequency magnetron sputtering deposition, the sputtering power is 135W, and the deposition atmosphere is Ar gas with the flow of 45 sccm; the Pt layer is prepared by direct current magnetron sputtering deposition, the sputtering power is 110W, and the deposition atmosphere is Ar gas with the flow of 40 sccm.
S2, setting a lanthanum nickel oxide LaNiO 3 seed layer with the thickness of 220nm on the bottom electrode layer; the LaNiO 3 seed Layer (LNO) is prepared by direct current magnetron sputtering deposition, and the sputtering power is 135V; the deposition atmosphere was Ar and O 2, wherein the Ar gas flow rate was 50 sccm and the O 2 gas flow rate was 18 sccm; the deposition substrate temperature was 490 ℃. After the preparation of the LaNiO 3 seed layer, annealing treatment is carried out, wherein the annealing temperature is 635 ℃, and the annealing time is 14 min.
S3, setting a PZT pyroelectric layer on the seed layer; the PZT pyroelectric layer is a PZT thin film layer, wherein Zr/Ti (molar ratio) =20/70 in the PZT thin film, and the thickness of the PZT pyroelectric layer is 800 nm. The PZT pyroelectric layer is prepared by radio frequency magnetron sputtering deposition, and the sputtering power is 150W; the deposition atmosphere was Ar and O 2, wherein the Ar gas flow was 90 sccm and the O 2 gas flow was 25sccm; the deposition substrate temperature was 640 ℃. And after the PZT pyroelectric layer is prepared, annealing treatment is carried out, wherein the annealing temperature is 640 ℃, and the annealing time is 13min.
S4, arranging an infrared absorption layer on the PZT pyroelectric layer. The infrared absorption layer is a multilayer composite film, and the multilayer composite film sequentially comprises a first Si 3N4 layer, a Ti layer, a second Si 3N4 layer and a Pt layer from top to bottom, wherein the thickness of the first Si 3N4 layer is 800nm, the thickness of the Ti layer is 80nm, the thickness of the second Si 3N4 layer is 800nm, and the thickness of the Pt layer is 150 nm. The Pt layer is prepared by direct-current magnetron sputtering deposition, the sputtering power is 110W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 45sccm; the first Si 3N4 layer and the second Si 3N4 layer are prepared through radio frequency magnetron sputtering deposition, the sputtering power is 135W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 45sccm; the Ti layer is prepared by direct current magnetron sputtering deposition, the irradiation power is 110W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 45sccm.
The PZT thin film prepared in this example has good crystallinity, and the main orientations of the thin film are (001) and (100) orientations, which are experimentally examined. The PZT thin film has uniform thickness and a typical columnar perovskite structure, which shows that the thin film crystal structure grows well, the columnar microstructure of the thin film is compact and dense, and the inside of the thin film has no pore structure. The PZT thin film has a high pyroelectric coefficient and a low dielectric constant. The pyroelectric coefficient of the PZT thin film at room temperature can reach 27nC cm -2·K-1, and the dielectric constant and dielectric loss of the material measured at the frequency of 1kHz are 168 and 0.0142 respectively. As can be seen from the test results, the PZT thin film prepared by the method has higher pyroelectric coefficient and lower dielectric constant, and shows that the PZT thin film has excellent pyroelectric performance. From the result of finite element simulation, it can be seen that the infrared absorption layer of Si 3N4-Ti-Si3N4 -Pt in the embodiment of the invention has an infrared absorption efficiency of more than 83% in the 3-6 μm band, and realizes high-efficiency absorption of infrared light.
In the description of the present application, it should be noted that the azimuth or positional relationship indicated by the terms "upper", "lower", etc. are based on the azimuth or positional relationship shown in the drawings, and are merely for convenience of describing the present application and simplifying the description, and are not indicative or implying that the apparatus or element in question must have a specific azimuth, be constructed and operated in a specific azimuth, and thus should not be construed as limiting the present application. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (14)
1. The preparation method of the pyroelectric film of the integrated infrared absorption material is characterized in that the pyroelectric film of the integrated infrared absorption material comprises a substrate, a bottom electrode layer, a seed layer, a PZT pyroelectric layer and an infrared absorption layer, and comprises the following steps:
s1, arranging a bottom electrode layer on a substrate;
S2, setting a seed layer on the bottom electrode layer;
S3, setting a PZT pyroelectric layer on the seed layer;
S4, arranging an infrared absorption layer on the PZT pyroelectric layer.
2. The method for preparing a pyroelectric film integrated with infrared absorbing material according to claim 1, wherein in step S1:
The material of the base is a (100) oriented silicon single crystal substrate or a SiO 2/Si (100) substrate; and/or the number of the groups of groups,
The bottom electrode layer is a Pt/TiO 2 or Pt/Ti composite electrode layer, wherein the thickness of the Pt layer is 150 nm-250 nm, and the thickness of the TiO 2 or Ti layer is 15 nm-30 nm.
3. The method for preparing a pyroelectric film integrated with infrared absorbing material as recited in claim 2, wherein,
The TiO 2 layer in the bottom electrode layer is prepared by radio frequency magnetron sputtering deposition, the sputtering power is 100W-150W, and the deposition atmosphere is Ar gas with the flow of 30sccm-50 sccm; and/or the number of the groups of groups,
The Pt layer in the bottom electrode layer is prepared by direct-current magnetron sputtering deposition, the sputtering power is 80-120W, and the deposition atmosphere is Ar gas with the flow of 30sccm-50 sccm.
4. The method for preparing a pyroelectric film integrated with an infrared absorbing material according to claim 1, wherein the seed layer in step S2 is a metal oxide ceramic material with ABO 3 perovskite structure, and the thickness of the seed layer is 100nm-300nm.
5. The method of claim 4, wherein the ABO 3 perovskite-structured metal oxide ceramic material is lanthanum nickelate LaNiO 3.
6. The method for preparing the pyroelectric film integrated with the infrared absorbing material as recited in claim 5, wherein said LaNiO 3 seed layer is prepared by direct current magnetron sputtering deposition with sputtering power of 100V-150V; the deposition atmosphere is Ar and O 2, wherein the Ar gas flow is 30sccm-60 sccm, and the O 2 gas flow is 5sccm-20 sccm; the deposition substrate temperature is 450 ℃ to 500 ℃.
7. The method for preparing a pyroelectric film of an integrated infrared absorbing material according to claim 6, wherein after the preparation of the LaNiO 3 seed layer by direct current magnetron sputtering deposition, annealing treatment is performed, the annealing temperature is 600-650 ℃, and the annealing time is 10min-15 min.
8. The method for preparing a pyroelectric film integrated with infrared absorbing material according to claim 1, wherein in step S3:
The PZT pyroelectric layer is a PZT thin film layer, the molar ratio of Zr/Ti in the PZT thin film=10/90 to 30/70, and/or,
The thickness of the PZT pyroelectric layer is 400 nm-1000 nm.
9. The method for preparing a pyroelectric film of an integrated infrared absorbing material according to claim 1, wherein said PZT pyroelectric layer in step S3 is prepared by rf magnetron sputtering deposition with a sputtering power of 120W-160W; the deposition atmosphere is Ar and O 2, wherein the Ar gas flow is 50sccm-100 sccm, and the O 2 gas flow is 10sccm-30sccm; the deposition substrate temperature is 600 ℃ to 650 ℃.
10. The method for preparing a pyroelectric film of an integrated infrared absorbing material according to claim 9, wherein after the preparation of the PZT pyroelectric layer by radio frequency magnetron sputtering deposition is completed, annealing treatment is performed, the annealing temperature is 600-650 ℃, and the annealing time is 10-15 min.
11. The method for preparing a pyroelectric film of an integrated infrared absorbing material according to any one of claims 1 to 10, wherein in step S4, said infrared absorbing layer is a multilayer composite film comprising, from top to bottom, a first Si 3N4 layer, a Ti layer, a second Si 3N4 layer, and a Pt layer, wherein the first Si 3N4 layer has a thickness of 100nm to 1000 nm, the Ti layer has a thickness of 10nm to 100nm, the second Si 3N4 layer has a thickness of 100nm to 1000 nm, and the Pt layer has a thickness of 50nm to 200 nm.
12. The method for preparing a pyroelectric film integrated with infrared absorbing material as recited in claim 11, wherein said multilayered composite film comprises:
The Pt layer is prepared by direct-current magnetron sputtering deposition, the sputtering power is 80W-120W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm-50sccm; and/or the number of the groups of groups,
The first Si 3N4 layer and/or the second Si 3N4 layer are/is prepared through radio frequency magnetron sputtering deposition, the sputtering power is 100-150W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm-50sccm; and/or the number of the groups of groups,
The Ti layer is prepared by direct current magnetron sputtering deposition, the irradiation power is 80W-120W, the deposition atmosphere is pure Ar gas, and the Ar gas flow is 30 sccm-50sccm.
13. A pyroelectric film of an integrated infrared absorbing material prepared by the method of any one of claims 1-12.
14. Use of the pyroelectric film of the integrated infrared absorbing material of claim 13 in an infrared detector.
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