EP4347929A1 - Procédé de fabrication d'absorbeurs à large bande à positionnement très précis pour surfaces 2d et 3d - Google Patents

Procédé de fabrication d'absorbeurs à large bande à positionnement très précis pour surfaces 2d et 3d

Info

Publication number
EP4347929A1
EP4347929A1 EP22734102.1A EP22734102A EP4347929A1 EP 4347929 A1 EP4347929 A1 EP 4347929A1 EP 22734102 A EP22734102 A EP 22734102A EP 4347929 A1 EP4347929 A1 EP 4347929A1
Authority
EP
European Patent Office
Prior art keywords
coated
cathode
electrolyte
broadband
anode
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP22734102.1A
Other languages
German (de)
English (en)
Inventor
Sarmiza-Elena Stanca
Andreas Ihring
Frank Hänschke
Gabriel Zieger
Heidemarie Schmidt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institut fuer Physikalische Hochtechnologie eV
Original Assignee
Institut fuer Physikalische Hochtechnologie eV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institut fuer Physikalische Hochtechnologie eV filed Critical Institut fuer Physikalische Hochtechnologie eV
Publication of EP4347929A1 publication Critical patent/EP4347929A1/fr
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/02—Heating or cooling
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/02—Electroplating of selected surface areas
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/623—Porosity of the layers
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Definitions

  • the invention relates to a method for producing highly precisely localized broadband absorbers for structured 2D and 3D surfaces, e.g. as a miniaturized functional element in thermal sensors for aerospace and industry or as a functional element in broadband precision radiometers for radiation power measurements.
  • precious metal black [see publications Hedayati, MK, Faupel, F., Elbahri, M. 2014 Review of Plasmonic Nanocomposite Metamaterial Absorber, Materials. 7:1221-1248; Tan F et al. 2016 Rough gold films as broadband absorbers for plasmonic enhancement of Ti0 2 photocurrent over 400-800 nm. Sei Rep. 6: 33049 and Zhou, S., Wang, Z., Feng, Y. 2012 Optimal Design of Wideband Microwave Absorber Consisting of Resistive meta-surface layers. Journal of Electromagnetic Analysis and Applications, 4:187-191.] represents a valued optical absorber material that can be used as a thin film in optical sensors.
  • optical absorbers used in the wavelength range from 0.4 pm to 20 pm are based, for example, on silver black [see the publications Paussa, L., Guzman, L., Marin, E., Isomaki, N., Fedrizzi, L. 2011 Protection of silver surfaces against tamishing by means of alumina/titanium nanolayers. Surface & Coatings Technology 206: 976-980 and Nagiri, R., Kumar, K.J., Subrahmanyam, A. 2009 Physical properties of silver oxide thin films by pulsed laser deposition: effect of oxygen pressure during growth. J.Phys. D: appl. Phys. 42:135411.].
  • silver-black shows undesirable chemical reactivity to air components [see the publications Paussa, L., Guzman, L., Marin, E., Isomaki, N., Fedrizzi, L. 2011 Protection of silver surfaces against tamishing by means of alumina/titania - nanolayers. Surface & Coatings Technology 206: 976-980 and Nagiri, R., Kumar, K.J., Subrahmanyam, A. 2009 Physical properties of silver oxide thin films by pulsed laser deposition: effect of oxygen pressure during growth. J.Phys. D: appl. Phys. 42: 135411.], affecting its long-term stability in terms of structural and spectral properties, which is an important property for microelectronics technology.
  • Feltham and Spiro also studied the nucleation and growth of the porous platinum black on the cathode produced in aqueous media.
  • the object of the present invention is to provide a method for producing highly precisely localized broadband absorbers for 2D and 3D surfaces, e.g. in the form of thermal sensors for space travel and industry or for use in broadband precision radiometry, which overcomes the disadvantages of the Avoids the prior art and, in particular, leads to highly precisely localized, porous noble metal broadband absorber nanolayers with low reflectivity and high absorptivity for visible light and infrared radiation in the wavelength range with wave numbers from 25000 cm 1 to 600 cm 1 and beyond, and at the same time high scalability and reproducibility in their production.
  • the essence of the invention is that with the water-free electrochemical in-situ process, highly precisely localized, porous noble metal broadband absorber nanolayers can be produced using water-free microelectrochemistry in-situ on microstructured 2D and 3D metal multi-contact components (heterojunctions), in order to e.g. To equip 2D and 3D thermal sensors with highly effective and long-term stable broadband absorbers.
  • the highly precisely localized, porous noble metal broadband absorber nanolayers have a low reflectivity and a high absorptivity for infrared radiation, particularly in the wavelength range with wave numbers from 25,000 cm 1 to 600 cm 1 or parts of this range.
  • the process of electrochemical deposition is suitable for producing in-situ electrolytically composed noble metal black layers, for example platinum black, in isopropanol with layer thicknesses of the order of magnitude of and smaller than the wavelengths of visible light.
  • noble metal black layers for example platinum black
  • in isopropanol with layer thicknesses of the order of magnitude of and smaller than the wavelengths of visible light.
  • porous noble metals as optical absorber materials, e.g. in the form of Pt, Au, Pd, Ru, Rh, Os, Ir, Ti, in order to carry out the anhydrous process in situ and thereby achieve the following advantages 1 to 8 of the procedure to achieve:
  • the process results in a high localization of noble metal black broadband absorber nanolayers on electrically conductive multi- and multi-contact surfaces, in particular also on multi-layer thin-film structures, using non-aqueous microelectrochemistry.
  • the process of producing the porous noble metal nanosheets by electrolysis is carried out in an electrochemical cell.
  • the structure consists of an electrochemical cell including temperature control and controllable power supply, whereby voltage and current can be measured.
  • the electrochemical cell includes:
  • a tank for the electrochemical bath e.g. made of glass or plastic (with an optional lid), • an electrolyte inside, the temperature of which is stabilized by means of a thermostat or equivalent device,
  • a working electrode in the form of the cathode surfaces to be coated
  • a counter-electrode anode
  • the electrolyte is based on a solution of a precious metal salt in isopropanol, for platinum this is PtCl 4 .
  • concentration of the salt is usually between 0.05% and 3.00%, but is not limited to this range.
  • An additive is added to this solution and mixed thoroughly.
  • Pb(CH 3 COO) 2 can be used as an additive in each case.
  • concentration of the additive usually ranges between 0.001% and 0.050%, but larger or smaller amounts are also possible.
  • the cathode or cathodes are defined by the surfaces to be coated.
  • the object of which the cathode is or are an integral part is generally referred to as “the cathode” in the text. Its shape and structure can be freely selected and is usually specified by the application.
  • the prerequisite, however, is that the surfaces to be coated are electrically conductive (e.g. metallic, conductive oxides or polymers), are in direct contact with the electrolyte at the start of coating and can be electrically connected to the power source.
  • the coatability is not limited to surfaces of certain roughness. 3.
  • the anode is made of precious metal or other conductive material coated with platinum. To ensure a homogeneous field distribution, the anode should be dimensioned in such a way that it protrudes by at least 5% in all directions over the area of the cathode to be coated or the area of the part of the cathode carrier that includes all cathodes. Smaller expansions are also possible, but reduce the homogeneity of the field, particularly in the area outside the cathode.
  • the anode can be designed as a plate, wire mesh, cylinder, partial spherical shell or other shape.
  • the electrodes are fixed accordingly and connected to the power source.
  • the orientation of the electrodes should be chosen in such a way that they fulfill the condition from 3.
  • the target value of the temperature control is set, the control is activated and the coating is waited until the temperature is stable.
  • the power source is activated, with the voltage being regulated to the target value during the deposition process. 8. Termination of the deposition process based on a termination criterion, e.g. the current
  • the process ends when the termination criterion is reached by interrupting the current flow.
  • the layer thickness achieved via an in-situ layer thickness measurement, the coating duration or the current can be used as a termination criterion.
  • the cathode can be cleaned in isopropanol without water, and air or drying gas can be used for subsequent drying.
  • a subsequent tempering step can be carried out.
  • temperatures of 1000°C and above are possible, but the properties of the cathode must be taken into account.
  • Fig. 1 a schematic representation of a first, second, third and fourth embodiment (I, II, III and IV) of the structure for
  • FIG. 2 a schematic overview of the method according to the invention
  • FIG. 3 schematic basic representation of different surface structures on planar substrates that can be coated with the method according to the invention (left: 2D and right: 3D),
  • Fig. 5 schematic representation of four multilayer structures with pronounced topography after coating with the method according to the invention
  • 1 shows the schematic representation of an embodiment of the structure for carrying out the method according to the invention in the form of an electrochemical bath in different structure variants I to VI:
  • the electrochemical cell includes: • a container for the electrochemical bath (8), eg made of glass or plastic [with optional lid (11)]
  • the current monitor (6) is designed, for example, as an ammeter.
  • the reference electrode (3) can be designed, for example, in the form of a platinum quasi-reference.
  • the current source (5) can be programmable, for example in the form of a programmable direct current source or a potentiostat.
  • the container (8) for the electrochemical bath can be made of glass or polymers, for example.
  • a cover (11) can also be provided in order to limit the evaporation of the electrochemical bath.
  • the method runs through a total of 11 method steps, with the 11th and thus last method step being optional, and with the method steps according to FIG. 2 proceeding in detail as follows:
  • the electrolyte is based on a solution of a precious metal salt in isopropanol, for platinum this is PtCl 4 .
  • concentration of the salt is usually between 0.05% and 3.00% in each case, but is not limited to this range.
  • An additive is added to this solution and mixed thoroughly.
  • Pb(CH COO) 2 can be used as an additive in each case.
  • concentration of the additive usually ranges between 0.001% and 0.05%, but larger or smaller amounts are also possible.
  • the cathode or cathodes are defined by the surfaces to be coated.
  • the object of which the cathode is or are an integral part is generally referred to as “the cathode” in the text. It can be freely selected in terms of shape and structure and is usually specified by the application.
  • the prerequisite, however, is that the surfaces to be coated are electrically conductive (e.g. metallic, conductive oxides or polymers), are in direct contact with the electrolyte at the start of coating and can be electrically connected to the power source.
  • the coatability is not limited to surfaces of certain roughness.
  • the anode is made of precious metal or other conductive material coated with platinum. To ensure a homogeneous field distribution, the anode should be dimensioned in such a way that it protrudes by at least 5% in all directions over the area of the cathode to be coated or the area of the part of the cathode carrier that includes all cathodes. Smaller expansions are also possible, but reduce the field homogeneity, especially in the outer area of the cathode.
  • the anode can be designed as a plate, wire mesh, cylinder, partial spherical shell or other shape.
  • the electrodes are fixed as shown in Figure 1 and connected to the power source.
  • the orientation of the electrodes should be chosen in such a way that they fulfill the condition from 3. 5.
  • the target value of the temperature control is set, the control is activated and the coating is waited until the temperature is stable.
  • the power source is activated, with the voltage dropping to the target value during the deposition process.
  • Figure 2 is regulated.
  • the process ends when the termination criterion is reached by interrupting the current flow.
  • the layer thickness achieved via an in-situ layer thickness measurement, the coating duration or the current can be used as a termination criterion. 9. Removal of the coated cathodes.
  • the cathode can be cleaned in isopropanol without water, and air or drying gas can be used for subsequent drying.
  • a subsequent tempering step can be carried out.
  • temperatures of 1000°C and above are possible, but the properties of the cathode must be taken into account.
  • the selection of suitable parameters for the respective separation process depending on the desired pore size must be observed.
  • the electrode size must match the thickness of the
  • Diffusion layer d exceed according to V & where D is the diffusion coefficient and t is the deposition time. A value from 5°C ⁇ T ⁇ 35°C is selected and fixed as the working temperature T, with 22°C being the preferred value. The resulting pore size is set by the potential difference between the reference electrode (3) and the working electrode (1).
  • a 100 mm silicon wafer with a highly structured surface is coated using the procedure described above.
  • conductive and non-conductive areas alternate on the surface, the structure sizes of which can be in the micrometer range or less (millielectrodes, microelectrodes and nanoelectrodes).
  • the conductive areas are coated with smooth platinum. These are connected to the contact with high conductivity (cf. Fig. 1 and Fig. 3).
  • a 2000 ml bath with a platinized surface defines the anode according to (I) in FIG. 1.
  • the surface to be coated is at a distance of at least 10 mm from the bath.
  • the temperature of the electrolyte is stabilized at (22.0 ⁇ 0.2)°C.
  • the electrodes are fixed according to (I) in Fig. 1 and connected to the deactivated power source.
  • the power source uses an automatic control based on an external voltage measurement that is tapped between the cathode and reference electrode. Before activation, the regulation of the voltage values according to FIG. 2 is programmed to match the desired pore size.
  • the power source is activated, with the voltage being regulated to the target value during the deposition process. After the desired deposition time of 90 s has been reached, the deposition process is terminated by switching off the power source in order to achieve a layer thickness of approx. 100 nm.
  • a three-dimensionally structured silicon chip with an edge length of 10 mm is coated with black platinum.
  • the surfaces to be coated are coated with smooth silver and alternate with non-conductive areas whose structure sizes vary between nanometers, a few micrometers and millimeters.
  • the silver plated areas are connected to the contact (see Figure 4).
  • a 40 ml bath corresponding to (II) in Fig. 1 is used, in which a planar platinum anode is installed.
  • the electrodes are fixed according to (I) in Fig. 1 and connected to the deactivated power source.
  • the surface to be coated is 10 mm from the anode.
  • 30 ml of a 0.5% PtCl 4 solution in isopropanol are used as the electrolyte and mixed with 0.01% Pb(CH COO) 2 until the color changes to yellow-greenish.
  • the electrolyte is filled into the bath.
  • the power source uses a computer-assisted control based on an external voltage measurement that is tapped between the cathode and reference electrode. Before activation, the control is programmed with the voltage value according to FIG. 2 to match the desired pore size.
  • the power source is activated, with the voltage being regulated to the target value during the deposition process. After the desired deposition time of 27 s has been reached, the deposition process is terminated by switching off the power source in order to achieve a layer thickness of approx. 200 nm.
  • the coated object is removed from the bath, rinsed in isopropanol and dried in a dry atmosphere.
  • Rh a 15 mM RhCl 2 solution
  • the temperature of the electrolyte is stabilized at (22.0 ⁇ 0.2)°C.
  • the power source uses automatic regulation based on an external voltage measurement between the cathode and
  • Reference electrode is tapped. Before activation, the control of the voltage value according to FIG. 2 is programmed to match the desired pore size. The power source is activated, with the voltage being regulated to the target value during the deposition process.
  • the deposition process is ended by switching off the power source in order to achieve a layer thickness of approx. 100 nm.
  • the coated substrates are removed from the baths in
  • a highly localized platinum black nanolayer is deposited on microstructured thermal sensor components with structure widths varying from a few microns to millimeters (see Fig. 6). To minimize agglomeration of the porous metal at the edges of the cathode faces:
  • the current density distribution and the diffusion field are optimized by magnetic stirring.
  • a square silicon chip with an edge length of 15mm and a periodically arranged grid of thermal sensors on free-standing Si 3 N 4 membranes is used as the cathode.
  • the surfaces to be coated are covered with a 50 nm thick silver layer, which is electrically connected between the sensors with conductor tracks in such a way that these are severed when the sensors are separated.
  • the conductor tracks are covered with Si 3 N 4 , as a result of which a coating is avoided there.
  • a 500 ml bath is equipped with a magnetic stirrer as shown in FIG.
  • a planar platinum anode is installed in the bath, which protrudes 50% beyond the cathode on all sides.
  • the electrodes are fixed as shown and connected to the deactivated power source.
  • the surface to be coated is 15mm from the anode.
  • the temperature of the electrolyte is stabilized at (22.0+0.1)°C.
  • the magnetic stirrer is activated at 100 rpm. The speed is adjusted accordingly until an even, smooth flow of liquid is established.
  • the power source uses an automatic control based on an external voltage measurement that is tapped between the cathode and reference electrode. Before activation, the control is programmed with the voltage value according to FIG. 2 to match the desired pore size.
  • the power source is activated, with the voltage being regulated to the target value during the deposition process. After the desired deposition time of 27 s has been reached, the deposition process is terminated by switching off the power source in order to achieve a layer thickness of approx. 200 nm.
  • the coated article is removed from the bath, rinsed in isopropanol and dried in a dry nitrogen atmosphere.
  • the proposed micro-electrochemical design (see “Design” above) meets the criteria for small area/volume conditions and the passage of current does not significantly alter the bulk concentrations of electroactive species.
  • the microelectrodes provide charge confinement.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

L'invention concerne un procédé de fabrication d'absorbeurs à large bande à positionnement très précis pour des surfaces structurées 2D et 3D. L'objectif de la présente invention est de proposer un procédé de fabrication d'absorbeurs à large bande à positionnement très précis pour des surfaces 2D et 3D, ce qui donne lieu à des nanocouches d'absorbeur à large bande en métal précieux poreux, à positionnement très précis, présentant une faible réflectivité et une capacité d'absorption élevée pour la lumière visible et le rayonnement infrarouge dans la plage de longueurs d'onde ayant des nombres d'ondes de 25000 cm-1 à 600 cm-1 et plus, et permet en même temps une extensibilité et une reproductibilité élevées dans leur production. L'objectif est atteint en ce que des nanocouches d'absorbeur à large bande en métal précieux poreux sont déposées in situ sur des composants métalliques à multiples contacts 2D et 3D microstructurés par micro-électrochimie en milieu anhydre dans une cellule électrochimique.
EP22734102.1A 2021-05-31 2022-05-31 Procédé de fabrication d'absorbeurs à large bande à positionnement très précis pour surfaces 2d et 3d Pending EP4347929A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102021113985.6A DE102021113985A1 (de) 2021-05-31 2021-05-31 Verfahren zur herstellung hochgenau lokalisierter breitbandabsorber für 2d- und 3d-oberflächen
PCT/DE2022/100407 WO2022253385A1 (fr) 2021-05-31 2022-05-31 Procédé de fabrication d'absorbeurs à large bande à positionnement très précis pour surfaces 2d et 3d

Publications (1)

Publication Number Publication Date
EP4347929A1 true EP4347929A1 (fr) 2024-04-10

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP22734102.1A Pending EP4347929A1 (fr) 2021-05-31 2022-05-31 Procédé de fabrication d'absorbeurs à large bande à positionnement très précis pour surfaces 2d et 3d

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Country Link
EP (1) EP4347929A1 (fr)
DE (1) DE102021113985A1 (fr)
WO (1) WO2022253385A1 (fr)

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220415710A1 (en) * 2019-11-21 2022-12-29 Lam Research Corporation Interconnect structure with selective electroplated via fill

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DE102021113985A1 (de) 2022-12-01
WO2022253385A1 (fr) 2022-12-08

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