WO2005070005A2 - Carbone de film mince pyrolyse - Google Patents

Carbone de film mince pyrolyse Download PDF

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Publication number
WO2005070005A2
WO2005070005A2 PCT/US2005/002254 US2005002254W WO2005070005A2 WO 2005070005 A2 WO2005070005 A2 WO 2005070005A2 US 2005002254 W US2005002254 W US 2005002254W WO 2005070005 A2 WO2005070005 A2 WO 2005070005A2
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Prior art keywords
parylene
hydrocarbon
carbon
thin film
substrate
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PCT/US2005/002254
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English (en)
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WO2005070005A3 (fr
Inventor
Yu-Chong Tai
Matthieu Liger
Theodore Harder
Satoshi Konishi
Scott Miserendino
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California Institute Of Technology
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Priority claimed from US10/973,938 external-priority patent/US7238941B2/en
Application filed by California Institute Of Technology filed Critical California Institute Of Technology
Publication of WO2005070005A2 publication Critical patent/WO2005070005A2/fr
Publication of WO2005070005A3 publication Critical patent/WO2005070005A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/12—Organic material
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment

Definitions

  • the present invention is generally directed to carbon thin films, methods of their deposition, and methods of their use in Nanoelectromechanical Systems (NEMS), Microelectromechanical Systems (MEMS) and other devices. More particularly, the invention provides methods of carbon thin film deposition and methods of making carbon containing patterned structures. The invention also provides methods of controlling physical properties of carbon thin films. Moreover, the invention provides methods of use of carbon thin films and carbon containing patterned structures in devices. In particular, the invention provides use of carbon thin films as electrochemical sensors in a high performance liquid chromatography device.
  • NEMS Nanoelectromechanical Systems
  • MEMS Microelectromechanical Systems
  • Polymers can also be used as precursors of pyrolyzed carbons. Recently, Ranganathan et. al. reported photoresist-derived carbon for MEMS and electrochemical applications (see, Ranganathan et al., J. Electrochemical Society, 147 (1), 277-282 (2000)). Parylene can be an attractive candidate for pyrolysis because of its benzene- rich chemical structure. The use of parylene as the precursor of the pyrolyzed carbon in MEMS provides a new material for MEMS, while utilizing certain advantages of parylene based MEMS. Hui et. al. reported limited examples of carbon thin films prepared from pyrolyzed parylene. However, Hui et. al.
  • the present invention provides well characterized and well controlled methods of carbon thin film deposition.
  • the invention also provides methods of controlling physical properties of carbon thin films.
  • the present invention provides methods of making carbon containing patterned structures. Further, the present invention provides methods of using carbon thin films and carbon containing patterned structures in NEMS, MEMS and other devices.
  • the invention provides a method and apparatus for sensing electromagnetic radiation in the infrared spectrum using a bolometer device.
  • the invention also provides a method and apparatus for sensing chemical species. But it would be recognized that the invention has a much broader range of applicability.
  • the invention can be applied to other wavelengths such as millimeter waves or visible light, biological materials, and other species and/or particles, and the like.
  • Detection devices range from motion sensors to those that detect certain frequencies of electromagnetic radiation and detectors for a variety of chemical species.
  • Motion sensors include, among others, mechanical, capacitive, inductive, and optical designs.
  • a specific type of motion sensor includes accelerometers and the like, which rely upon MEMS based technology.
  • Such detection devices also include, among others, infrared detectors, and imagers.
  • An example of an infrared detector is a bolometer.
  • Other types of detectors include chemical sensors, which rely upon sensing differences in voltage potentials while being coupled to an unknown chemical species.
  • the present invention is directed to carbon thin films, devices and articles comprising the carbon thin films, as well as methods of their deposition and methods of their use in Nanoelectromechanical Systems (NEMS), Microelectromechanical Systems (MEMS), and other devices. More particularly, the invention provides methods of carbon thin film deposition and methods of making carbon containing patterned structures. The invention also provides methods of controlling physical properties of carbon thin films. Moreover, the invention provides methods of use of carbon thin films and carbon containing patterned structures in NEMS, MEMS and other devices. Many benefits can be achieved by way of the present invention over conventional techniques.
  • NEMS Nanoelectromechanical Systems
  • MEMS Microelectromechanical Systems
  • Existing carbon deposition techniques generally limit the feature size of on-chip electrochemical electrodes to greater than 90 um and to thicknesses in excess of 5 um with only 12 um resolution in geometric feature definition according to a specific embodiment.
  • the present invention allows for reliable and repeatable fabrication of carbon electrodes with feature sizes as small as 2 microns, thicknesses as small as 50 nm, and geometric resolution as small as 2 microns according to alternative embodiments. Thin films with even smaller feature sizes, thickness, and geometric resolution are achievable. For example, the feature sizes could be as small as 10 nanometers.
  • This thin-film carbon has the additional benefit of having tunable mechanical and electrical properties. Depending upon the embodiment, one or more of these benefits may be achieved.
  • the present invention provides a method of carbon thin film deposition comprising depositing a catalyst on a substrate, depositing a hydrocarbon on the substrate in contact with the catalyst, and pyrolyzing the hydrocarbon.
  • the hydrocarbon can be, for example, parylene. Other examples include polyimide, photoresist, and other polymers.
  • the catalyst can be, for example, Ti/Pt or Cr/Au.
  • the catalyst also can comprise, for example, nickel, iron, cobalt, platinum, titanium, chrome, gold, ferrocene, or ferric nitrate.
  • the hydrocarbon can be pyrolyzed at a temperature ranging from, for example, about 500°C to about 900°C.
  • the pyrolyzing of the hydrocarbon can be performed in an atmosphere of, for example, argon, oxygen, or hydrogen. Alternatively, the pyrolyzing of the hydrocarbon can be performed in an atmosphere of nitrogen.
  • the present invention provides methods of making carbon containing patterned structures.
  • One method comprises depositing a hydrocarbon on a substrate, pyrolyzing the hydrocarbon to form a carbon thin film, and patterning the carbon thin film by, for example, an etching technique.
  • Another method comprises depositing a hydrocarbon on a substrate, patterning the hydrocarbon by, for example, an etching technique, and pyrolyzing the hydrocarbon.
  • the hydrocarbon can be, for example, parylene.
  • the patterning of the carbon thin film or of the hydrocarbon can be done, for example, by plasma etching.
  • the patterning can comprise the use of a metal or a photoresist mask.
  • the carbon containing patterned structure can have a geometric resolution from, for example, about 2 microns to about 10 nanometers.
  • the present invention provides a method of controlling the physical properties of carbon thin films. More specifically, a carbon thin film density can be controlled by a method comprising etching a cavity into a substrate, depositing a hydrocarbon into the cavity and pyrolyzing the hydrocarbon while in cavity to form a carbon thin film.
  • the hydrocarbon can be, for example, parylene.
  • the method can further comprise etching the carbon thin film by plasma etching.
  • the method can further comprise etching the substrate around the cavity.
  • the method can further comprise controlling a carbon thin film density by changing the volume of the cavity.
  • a method of carbon thin film formation to provide good adhesion between the carbon thin film and a substrate comprising: (i) depositing a parylene film on a substrate, wherein the substrate does not comprise a prior coating of gamma-methacryloxypropyltrimethoxy silane, also known as A174, and (ii) pyrolyzing the parylene film to form a carbon thin film adhered to the substrate.
  • the substrate can be silicon, quartz, glass or metal.
  • the step of pyrolyzing the parylene film can be performed in the presence of a catalyst.
  • the catalyst can be a metal.
  • the catalyst can be Ti/Pt or Cr/Au.
  • the catalyst can comprise, for example, nickel, iron, cobalt, platinum, ferrocene, titanium, chrome, gold, ferric nitrate, or a combination thereof.
  • the pyrolyzing the parylene film can be performed at a temperature ranging from, for example, about 500°C to about 900°C.
  • the step of pyrolyzing the parylene film can be performed in an atmosphere of argon, oxygen, or hydrogen. Alternatively, the pyrolyzing of the parylene film can be performed in an atmosphere of nitrogen.
  • the method can further comprise patterning the carbon thin film.
  • the patterning the carbon thin film can be done by plasma etching.
  • the parylene film can be a patterned parylene film.
  • a method for forming thin film carbon comprising the steps of (i) depositing a hydrocarbon on a substrate, and (ii) pyrolyzing the hydrocarbon on the substrate, wherein the pyrolyzing is carried out in the presence of a catalyst which lowers the pyrolysis time and temperature.
  • the hydrocarbon can be, for example, parylene.
  • the method can further comprise patterning the hydrocarbon before pyrolyzing it, or patterning the pyrolyzed hydrocarbon.
  • the method can further comprise use of the pyrolyzed hydrocarbon in HPLC detection.
  • the invention provides a use of carbon thin films and carbon containing patterned structures in MEMS, NEMS, and other devices.
  • the invention provides a method and apparatus for sensing electromagnetic radiation in the infrared spectrum using a bolometer device.
  • the invention also provides a method and apparatus for sensing chemical species. But it would be recognized that the invention has a much broader range of applicability.
  • the invention can be applied to other wavelengths such as millimeter waves or visible light, biological materials, and other species and/or particles.
  • the present invention provides an apparatus for sensing electromagnetic radiation (e.g., bolometer) using carbon based sensing materials, e.g., pyrolyzed parylene, amorphous carbon based material.
  • the apparatus has a substrate (e.g., silicon, silicon on insulator, other semiconductor materials, glass, quartz, metal and organic) comprising a surface region and an array of substantially carbon based material regions having a resistivity ranging within a predetermined range disposed overlying the surface.
  • the predetemiined range is from about 10 Ohms cm to about 10 " Ohms cm.
  • Each of the carbon based material regions comprises a portion being suspended over a region of the surface to thermally insulate the portion of the suspended carbon based material.
  • the insulating region also electrically insulates the portion of the suspended carbon based material.
  • An insulating region is formed between the region and the portion of the carbon based material.
  • the insulating region is an air gap or other like structure according to a specific embodiment.
  • the insulating region can also include multiple regions and/or layers, depending upon the embodiment.
  • Each of the carbon based material regions is a pixel element for a plurality of pixel regions according to a specific embodiment.
  • the apparatus has an interconnection coupled to each of the carbon based material regions.
  • the interconnection is made of a pyrolyzed carbon based material and/or metal based material, e.g., aluminum, copper, gold, silver, titanium, platinum, tungsten, and alloys, and/or any combination of these materials, and the like.
  • One or more nodes couples to the interconnection.
  • the one or more nodes is able to independently read a resistivity value associated with (e.g., directly connected, coupled) at least one or more of the carbon based material regions.
  • each of the carbon based regions may change in resistivity value upon receiving a dosage of electromagnetic radiation, e.g., 8-14 micron wavelength band, 3-5 micron band.
  • the carbon based region changes in temperature upon irradiation, which causes a resulting change in resistivity, which can be read out via interconnections and/or related reading devices.
  • the present invention provides a method for fabricating a sensing device, e.g., radiation. The method includes providing a substrate comprising a surface region.
  • the method includes forming an insulating material overlying the surface region and forming a film of carbon based material overlying the insulating material.
  • the method includes treating to the film of carbon based material to pyrolyzed the carbon based material to cause formation of a film of substantially carbon based material having a resistivity ranging within a predetermined range.
  • the predetermined range is from about 10 Ohms cm to about 10 " Ohms cm.
  • the method also forms a gap underlying a portion of pyrolyzed carbon based material.
  • the present invention provides an apparatus for chemical sensing using carbon based sensing materials.
  • the apparatus has a pyrolyzed parylene carbon based electrode structure having a resistivity ranging within a predetermined range.
  • the electrode has a first end coupled to a second end and a length defined between the first end and the second end.
  • An interconnect is coupled to at least one of the ends.
  • the invention provides a method for fabricating a sensing device. The method includes providing a substrate comprising a surface region and forming an insulating material overlying the surface region.
  • the method also includes forming a film of carbon based material overlying the insulating material and treating to the film of carbon based material to pyrolyzed the carbon based material to cause formation of a film of substantially carbon based material having a resistivity ranging within a predetermined range.
  • the predetermined range is from about 10 8 Ohms cm to about 10 "3 Ohms cm.
  • the method also provides at least a portion of the pyrolyzed carbon based material in a sensor application and uses the portion of the pyrolyzed carbon based material in the sensing application.
  • the sensing application is selected from chemical, humidity, mechanical strain, radiation or thermal.
  • the present technique provides an easy to use process that relies upon conventional technology.
  • the method provides higher device yields.
  • the method provides a process that is compatible with conventional process technology without substantial modifications to conventional equipment and processes.
  • the invention provides for a method and device that can provide for room temperature detection of certain iofrared frequencies according to a specific embodiment.
  • the present invention provides a sensing material that is generally easy to use, inert, light weight, and has . good detection characteristics, e.g., signal to noise ratio.
  • Parylene which, has been pyrolyzed, rather than conventional materials allows for improvements in performance due to its mechanical and thermal properties.
  • Figure 1 is a simplified process flow diagram illustrating a fabrication sequence for a sensing device according to an embodiment of the present invention
  • Figure 2 is a simplified diagram of parylene C chemical structure according to an embodiment of the present invention.
  • Figure 3-12 are simplified diagrams illustrating characteristics of parylene pyrolysis according to embodiments of the present invention.
  • Figure 13 is a simplified diagram of a chemical sensing device according to an embodiment of the present invention
  • Figure 14 is a simplified diagram illustrating a fabrication sequence for a chemical sensing device according to an embodiment of the present invention
  • Figures 15 through 18 are simplified diagrams illustrate experimental results of a chemical sensing device according to an embodiment of the present invention
  • Figure 19 is a simplified diagram of a bolometer device according to an embodiment of the present invention
  • Figures 20-22 are simplified diagrams illustrating experimental results of a bolometer device according to an embodiment of the present invention.
  • Figure 23 is a simplified diagram illustrating a fabrication sequence for a bolometer device according to an embodiment of the present invention.
  • Figure 24 is a simplified top-view illustration of a bolometer device according to an embodiment of the present invention.
  • Figures 25-26 are simplified diagrams illustrating bolometer characteristics according to embodiments of the present invention
  • Figure 27 illustrates a method of controlling carbon thin film density.
  • Figure 28 illustrates a carbon thin film based electrochemical sensor incorporated into a High Performance Liquid Chromatography column.
  • the invention provides methods of carbon thin film deposition and methods of making carbon containing patterned structures.
  • the invention also provides methods of controlling physical properties of carbon thin films.
  • the invention provides methods of use of carbon thin films and carbon containing patterned structures in NEMS, MEMS and other devices.
  • the present invention provides a method of carbon thin film deposition comprising depositing a catalyst on a substrate, depositing a hydrocarbon on the substrate in contact with the catalyst, and pyrolyzing the hydrocarbon.
  • the substrate can be silicon or other semiconductor material, glass, quartz, metal or organic material
  • the hydrocarbon can be parylene, PDMS, polyethylene, Teflon, or benzene; but most preferably parylene.
  • the catalyst can be Ti/Pt or Cr/Au.
  • the catalyst can also comprise at least one selected from the group consisting of nickel, iron, cobalt, platinum, ferrocene, titanium, chrome, gold, or ferric nitrate.
  • Pyrolyzing the hydrocarbon can be performed in an atmosphere of nitrogen, argon, oxygen or hydrogen. In the most preferred embodiment, pyrolyzing the hydrocarbon is performed in the presence of a nitrogen atmosphere. Most preferably, pyrolyzing the hydrocarbon is performed in the temperature range from about 500°C up to about 900°C. Pyrolyzing the hydrocarbon is achieved by raising the temperature of the hydrocarbon to a temperature where it decomposes and holding it there a specific amount of time to produce a carbon thin film. In an alternative specific embodiment, the present invention provides methods of making carbon containing patterned structures. One method comprises depositing a hydrocarbon on a substrate, pyrolyzing the hydrocarbon to form a carbon thin film, and patterning the carbon thin film by an etching technique.
  • the other method comprises depositing a hydrocarbon on a substrate, patterning the hydrocarbon by an etching technique, and pyrolyzing the hydrocarbon.
  • the etching technique to be used for patterning the carbon thin film or for patterning the hydrocarbon can be plasma etching, chemical etching or physical removal.
  • the present invention provides a method of controlling physical properties of carbon thin films. More specifically, a carbon thin film density is controlled by a method comprising etching a cavity into a substrate, depositing a hydrocarbon into the cavity and pyrolyzing the hydrocarbon while in cavity to form a carbon thin film (see, for example, Figure 27). Controlling the carbon thin film density can be achieved by changing the volume of the cavity.
  • the method of controlling the physical properties of carbon thin films can further comprise etching the carbon thin film or alternatively etching the substrate around the cavity.
  • the substrate can be flat.
  • the present invention provides methods of using carbon thin films to produce MEMS or NEMS and other useful devices and structures.
  • techniques directed to sensing devices and their processing are provided. More particularly, the invention provides a method and apparatus for sensing electromagnetic radiation in the infrared spectrum using a bolometer device. The invention also provides a method and apparatus for sensing chemical species. But it would be recognized that the invention has a much broader range of applicability. For example, the invention can be applied to other wavelengths such as millimeter waves or visible light, biological materials, and other species and/or particles.
  • a method according to an embodiment of the present invention for fabricating a sensing device is briefly outlined below, which can also be referenced in the simplified flow diagram 100 of Figure 1. At least some of the following steps can be carried out:
  • a substrate e.g., silicon, glass, organic, metal
  • step 107) an insulating material (e.g., silicon nitride, silicon oxide) overlying the surface region;
  • an insulating material e.g., silicon nitride, silicon oxide
  • step 109 a film of carbon based material or hydrocarbon (e.g., Parylene) overlying the insulating material;
  • hydrocarbon e.g., Parylene
  • step 111 the film of carbon based material or hydrocarbon (e.g., parylene) to pyrolyze the carbon based material or hydrocarbon;
  • hydrocarbon e.g., parylene
  • step 115 Provide (step 115) at least a portion of the pyrolyzed carbon based material in a sensing application
  • step 117 Use (step 117) the portion of the pyrolyzed carbon based material in the sensing application; 10. Detect (step 119) a change in characteristic (e.g., resistance) of the pyrolyzed carbon based material from an application of electromagnetic radiation and/or chemical and/or biological species and/or other entities; and
  • step 121 Perform (step 121) other steps, as desired.
  • the above sequence of steps provides a method according to an embodiment of the present invention. As shown, the method uses a combination of steps including a way of forming a sensing device using a pyrolyzed parylene bearing material or the like. Other alternatives can also be provided where steps are added, one or more steps are removed, or one or more steps are provided in a different sequence without departing from the scope of the claims herein. Further details of the present method and structure can be found throughout the present specification and more particularly below. Before discussing specific sensor type applications, we have provided a brief description of a carbon based material and in particular parylene-pyrolyzed carbon according to an embodiment of the present invention as applied generally to MEMS applications.
  • the present invention provides methods and structures using carbon bearing materials including Parylene-pyrolyzed carbon for MEMS and NEMS applications. More particularly, such MEMS and NEMS applications includes sensing devices and the like. Carbons have been used as conductive materials with many promising chemical and thermal properties.
  • the present invention preferably uses parylene-pyrolyzed carbon to take advantages of its smooth surface deposition and benzene-rich chemical structure. The description of the parylene-pyrolyzed carbon was tried through evaluations of electrical and mechanical properties in terms of MEMS and NEMS applications as well as general features. Young's modulus and the resistivity of parylene-pyrolyzed carbon (800 ° C pyrolysis) becomes 70 GPa and 0.1 ⁇ cm, respectively. The relationship between these properties and density will be also described.
  • Parylene can be used as the precursor of the pyrolyzed carbon according to a specific embodiment.
  • Parylene, especially Parylene C has been used in MEMS to take advantages of its useful combination of electrical and mechanical properties and low permeability. See, X-Q Wang, Q. Lin, and Y-C Tai, "A Parylene Micro Check Valve", in DigestTech. Papers MEMS '99 Conference, 1999, pp. 177-182.
  • smooth coating of Parylene film on the surface with topographical variations, such as grooves, cavities, and trenches can be expected due to CVD deposition at room temperature in vapor phase.
  • the pyrolysis or carbonization makes it possible to change properties of the precursor material according to a specific embodiment.
  • dielectric polymers change into conductive carbons through pyrolysis. Therefore, pyrolysis of Parylene provide a novel material for MEMS with taking over several advantages of Parylene based MEMS. Benzene-rich chemical structure of Parylene is also attractive for carbonization. According, further details of the present method and system using Parylene-pyrolyzed carbon have been provided throughout the present specification and more particularly below.
  • Parylene C film is employed as a precursor of carbon among members of Parylene
  • Chemical structure of Parylene C is shown in Figure 2.
  • Parylene C is modified poly-paraxylylene by the substitution of chlorine atom for one of the aromatic hydrogens according to a specific embodiment.
  • TGA N 2 atmosphere, 10 ° C/min ramp rate from 20 to 1200 ° C
  • 4 ⁇ m-thick Parylene C films were prepared on various substrates according to a specific embodiment.
  • the thermal gravimetric analysis suggested that there were three phases (for purposes of this description) of the pyrolysis process of Parylene C from 20 to 1200 ° C .
  • the first phase up to 500 ° C , slight weight change was observed. It seems to be due to the loss of moisture and some volatiles. The drastic weight loss could be observed between 500 and 600 ° C (the second phase). The main degradation seems to occur in this phase.
  • the third phase gradual weight loss continued at elevated temperature.
  • weight [%] as Y-axis means a ratio of weight of pyrolyzed film against initial weight of Parylene C film.
  • the results show good agreements with the preceded TGA except the weight increase at higher temperature. It was found that after exposure to air (20 ° C, 47% in humidity), the weight of carbon film decreased by baking at 100 ° C or in vacuum. The weight then increased once exposed to air again. We believe the weight change is due to moisture absorption and desorption.
  • FIG. 4 shows measured results of thickness changes of Parylene C film according to pyrolysis temperature.
  • Thickness [%] as Y-axis means a ratio of thickness of pyrolyzed film against initial thickness of Parylene C film. Thickness of films was measured by a surface profiler.
  • Three phases can be recognized as suggested by preceded TGA. Shrinkage of film still continued in the third phase differently from results of weight change. Furthermore, the shrinkage ratio of the film on Si/Ti/Pt dipped from 15% for 800 ° C pyrolysis, while those of the film on Si and Si/Cr/Au were about 20% for 800 ° C pyrolysis.
  • Parylene C films were pyrolyzed at different temperatures in N 2 atmosphere up to 900.
  • the resistivity was calculated from measured sheet resistance and film thickness.
  • the ramp rate of elevated temperature were set at two values (10 ° C /min and 4.5 ° C/min) and compared in this experiment.
  • Parylene C films pyrolyzed at a low pyrolysis temperature exhibited high resistivity.
  • the resistivity became less than lxl0 10 ⁇ cm above 600 ° C and decreased to about l ⁇ lO "2 ⁇ cm at 900 ° C, which was close to 5> ⁇ 10 "3 ⁇ cm reported for glassy carbons obtained above 1000 ° C .
  • S. Ranganathan, R. McCreery, S.M. Majji, and M. Madou "Photoresist-derived for microelectromechanical Systems and Electrochemical applications", Journal of The Electrochemical Society, 147(1), pp.277-282, 2000.
  • the pyrolysis with a lower ramp rate could provide a lower resistivity.
  • 3 ⁇ m-thick Parylene C membranes on Si frame structures as specimens were prepared as follows. 3 ⁇ m-thick Parylene C film was deposited on a 20 ⁇ m-thick Si diaphragm structure and released to form Parylene C membrane by BrF 3 etching of remaining 20 ⁇ m-thick Si layer.
  • Figure 10 shows calculated Young's modulus and the stress according to pyrolysis temperature. In the calculation, a Poisson's ratio was assumed to be 0.4.
  • Parylene-pyrolyzed carbon for MEMS applications has been provided. Young's modulus and resistivity of parylene-pyrolyzed carbon (800 ° C pyrolysis) showed 70GPa and 0.1 ⁇ cm, respectively. The relations between these properties and density were also discussed. Further details of the use of Parylene-pyrolyzed carbon for sensing devices according to embodiments of the present invention can be found throughout the present specification and more particularly below.
  • Electrochemical sensors can be used in a wide variety of applications including pH monitoring, gas monitoring, and ion detection. Electrochemical sensors are also used as a basic laboratory instrument to study the chemical behavior and kinetics of many reactive species. Electrochemical sensors experience enhanced performance when they have micron and submicron feature sizes and are composed of highly inert materials. This sensor combines both micron feature sizes with a novel inert thin-film carbon that is compatible with standard surface micromachining processes. The ability to deposit a thin-film carbon and pattern it using photolithography improves device performance and simplifies device manufacturing, compared to screen printed carbon which is the only other available method for on- chip carbon electrodes.
  • FIG. 13 shows an example of the concept of the thin-film carbon electrochemical sensor 1300 according to a specific embodiment.
  • This diagram is merely an example, which should not unduly limit the scope of the claims herein.
  • various electrode elements 1305, 1303, 1309 can be disposed on an insulating material 1301.
  • the insulating material can be, for example, silicon dioxide or other film or films of insulating characteristics.
  • the electrodes can include reference electrode 1303 and electrode 1309, which can be made respectively of, for example, platinum and silver.
  • Each of these electrodes can include conductive wiring 1307, which is coupled to a measuring device.
  • the sensor also can include carbon based electrode 1305 formed on the insulating material.
  • the carbon layer is constructed by first depositing a hydrocarbon or a carbon containing polymer.
  • a hydrocarbon or a carbon containing polymer include but are not limited to all varieties of photoresist, Parylene N, Parylene C, and Parylene D.
  • Photoresist can be spun on, while all three types of Parylene can be deposited by vapor deposition.
  • the polymer is then heated to temperatures in excess of 450°C in an inert atmosphere to force the polymer to undergo pyrolysis according to a specific embodiment.
  • pyrolysis temperature several material properties can be controlled such as the carbon's porosity, resistivity, density, thickness, thermal conductivity, grain structure, and other parameters.
  • the resulting layer of carbon can then be patterned using standard photolithographic and plasma etching techniques. Variations on this process include (i) the addition of a metal catalyzer (e.g., nickel, gold, platinum, titanium) above or below the polymer, and (ii) modification of the carbon's surface with ion selective membranes or other specialized polymers such as, e.g., Nafion. Additional metallization layers can be added to the carbon to construct counter and reference electrodes as well as on-chip wiring and bonding pads. These metallization layers can be patterned through standard metal lift-off techniques. Such metallization layers include, for example, aluminum, gold, platinum, copper, silver, and others.
  • a metal catalyzer e.g., nickel, gold, platinum, titanium
  • modification of the carbon's surface with ion selective membranes or other specialized polymers such as, e.g., Nafion.
  • Additional metallization layers can be added to the carbon to construct counter and reference electrodes as well as on
  • FIG. 14 is a simplified diagram illustrating a fabrication sequence for a chemical sensing device according to an embodiment of the present invention. This diagram is merely an example, which should not unduly limit the scope of the claims herein. One of ordinary skill in the art would recognize many variations, modifications, and alternatives. As shown, the process starts (step 1) with the oxidation of a silicon wafer or the use of a high-temperature quartz wafer or other suitable materials including inorganic materials.
  • the carbon containing polymer can be deposited either by spinning it on the wafer or by vapor deposition according to a specific embodiment. If a metal catalysis is being used, it can be deposited and patterned by thermal evaporation, sputtering, or e-beam evaporation prior to the deposition of the polymer.
  • a metal catalysis is being used, it can be deposited and patterned by thermal evaporation, sputtering, or e-beam evaporation prior to the deposition of the polymer.
  • An example of such metal catalyzer is nickel, but it can be others.
  • the wafer with the polymer is then heated to the desired pyrolysis temperature in an inert (e.g., argon or nitrogen) atmosphere or vacuum.
  • an inert e.g., argon or nitrogen
  • the carbon layer is patterned (step 3) using O 2 plasma etching with a photoresist mask.
  • the wafer is then prepared for metal liftoff by depositing and patterning a layer of photoresist. Alternatively, other types of etching techniques can be used depending upon the embodiment.
  • a gold metal layer is deposited (step 4) to form wires and bonding pads.
  • metals such as aluminum, platinum, and silver
  • metals such as aluminum, platinum, and silver
  • Two additional metal layers of platinum and silver are deposited and patterned (steps 5 and 6) in the same manner to form the counter and reference electrodes, respectfully. These additional layers are optional depending on the application.
  • An additional layer of Parylene is also optional. This additional layer, for example, can serve as a chemical barrier to isolate on-chip wires and to better control the geometry of the exposed electrode surface. This layer can be patterned using an O 2 plasma etching with a photoresist mask.
  • O 2 plasma etching with a photoresist mask.
  • metals used as counter and reference electrodes and for bonding pads and wiring can be varied (e.g., shorting reference and counter electrodes or using an electrode as a preconcentrator (electrochemical stripping) according to other embodiments.
  • Different carbon polymers may be used as the carbon source according to a specific embodiment. Such carbon polymers can include, among others, photoresist and other types of parylene.
  • a metal catalysis e.g., nickel or gold
  • a variety of ion selective membranes e.g., Nafion may be used to coat the carbon electrode to increase electrochemical sensitivity and selectivity for particular analytes in yet other embodiments.
  • such coatings can include Nafion or polypyrrole.
  • Mechanical structures can be added near the electrodes to aid in fluid containment and transport in further embodiments.
  • such structures can be micro-fluidic channels.
  • a coating or other type of insulation e.g., Parylene may be added to isolate parts of the chip from the chemical solution in alternative embodiments.
  • HPLC EMBODIMENT In a specific embodiment, the thin film of carbon can serve as an electrochemical sensor in a liquid chromatographic device, including an HPLC device.
  • the micromachining fabrication process used to make the present invention also can be used to fabricate an HPLC device.
  • HPLC devices and methods of making and using them, are described, for example, in the following US patent applications: (1) "Design of an IC-Processed Polymer Nano-Liquid Chromatography Systems On-a-Chip and Method of Making It” serial number 10/917,257, filed on August 11, 2004 (CalTech Ref. No.: CIT-3936); (2) "On-Chip Temperature Controlled Liquid Chromatography Methods and Devices” serial number 60/545,727, filed on February 17, 2004 (CalTech Ref. No.: CIT-4046P), both of which are hereby incorporated by reference in their entirety.
  • Figure 28(a) and (b) illustrates an example of an HPLC device.
  • Figure 28(a) illustrates a side view of the device comprising an inlet, a parylene layer defining a chromatographic media comprising, for example, beads, a filter, one more of thin film carbon (TFC) sensing electrodes, anchors, and an outlet.
  • Figure 28(b) illustrates a top view, showing the inlet, the column, the filter, the TFC sensing electrodes, and the outlet.
  • thin-film carbon microelectrodes were fabricated for integration into a variety of chemical and biochemical sensors.
  • the carbon films were compatible with standard MEMS processing, most importantly photolithography, and still maintained many if not all the electrochemical benefits of carbon.
  • Pyrolyzed parylene-C not only meets these desired requirements, but it is also conformal over high aspect ratio structures.
  • Conformal carbon coating could be used to make high effective surface area electrodes by coating high aspect ratio structures (See, for example, Figure 15).
  • a free standing film of parylene-C (15.8mg) was examined by simultaneous thermal analysis, which provides thermo gravimetric analysis and differential scanning calorimetry.
  • the sample was heated to 1500 Degrees Celsius with a heating rate of 5 Degrees Celsius /min in flowing Ar (lOOmL/min).
  • the material undergoes an endothermic phase transition, presumably melting, at 296 Degrees Celsius.
  • An exothermic event peaks near 480 Degrees Celsius, and is accompanied by a weight loss of 66%. Total weight loss to 1500 Degrees Celsius is 70.1%.
  • FIG. 18 shows cyclic voltammograms of 5 mM in 0.1 M KC1 for various processing parameters of the pyrolyzed parylene as well as a scan using a Pt electrode for comparison. Improvements in electrode kinetics, evident by a reduction in peak-to-peak separation, can be observed as carbonization temperature and film thickness are increased.
  • the present invention provides a method and apparatus for a bolometer design. More particularly, the invention provides a method and system for an uncooled, room-temperature, all parylene bolometer device.
  • the device includes two layers of pyrolyzed (or "carbonized") parylene and a metal layer for interconnections according to a specific embodiment.
  • Other embodiments may include a single layer of pyrolyzed parylene.
  • high responsivity can be achieved by tailoring the electrical conductivity and the temperature coefficient of resistance (TCR) using different pyrolysis conditions for each parylene layer. Further details of the present device and methods of manufacture can be found throughout the present specification and more particularly below.
  • FIG. 19 is a simplified diagram of a bolometer sensing device 1900 according to an embodiment of the present invention.
  • the sensing device is a resistive uncooled bolometer.
  • the device has a free-standing temperature-sensitive element that is linked to a substrate by low thermal conductance legs.
  • ⁇ is the TCR of the sensing element.
  • R is the bolometer resistance
  • G is the pixel-to-substrate thermal conductance
  • ⁇ is the bolometer absorptance.
  • C is the thermal capacitance.
  • a desirable parameters to obtain good responsivity are: high pixel-TCR and low pixel to-substrate thermal conductance.
  • vanadium oxide see P.E. Howard et al Proc. SPIE Vol. 3698 131 (1999)
  • amorphous silicon see Tissot JL, Infrared Physics & Technology 43 (3-5) 223-228 Jun-Oct 2002] as temperature-sensitive material, reaching a TCR of about 1.5% to 3%.
  • YBaCuO Another possible material is YBaCuO [see A Semiconductor YBaCuO Microbolometer for Room Temperature IR Imaging," A. Jahanzeb,C. M. Travers, Z. Celik-Butler, D. P. Butler, and S. Tan, IEEE Transactions on Electron Devices,yol. 44, pp. 1795-1801, 1997] .
  • the suspension legs are usually made of silicon nitride or polysilicon. In the case of silicon nitride legs, it is necessary to have another layer for electrical conduction.
  • a bolometer is proposed using pyrolyzed parylene both for the temperature-sensing element and for the suspension legs according to a specific embodiment. Certain properties of pyrolyzed parylene are described.
  • TCR temperature coefficient of resistance
  • the TCR of pyrolyzed parylene increases with resistivity.
  • Figure 22 shows the TCR of various films having different resistivities (obtained by pyrolysis at different temperatures).
  • the TCR of pyrolyzed-parylene does show a logarithmic dependence on the resistivity.
  • the measured TCR was - 4%/K for films having ⁇ 10 8 ⁇ .cm resistivity down to -0.3%/K for films having ⁇ 10 " 2 ⁇ .cm resistivity.
  • the corresponding activation energies are 0.023eV and 0.3 leV respectively. Because higher bolometer resistance leads to higher thermal noise, there is a trade-off between high responsivity (given by high TCR) and signal-to-noise ratio (given by low resistance).
  • FIG. 22 shows the resistance drop of a pyrolyzed-parylene film when exposed to air after being stabilized in vacuum. This resistance change is reversible. However, this sensitivity to moisture is not a problem for our application since uncooled bolometers operate in vacuum (for thermal insulation purposes).
  • the bolometer design is similar to that shown on Figure 19.
  • the pixel size was chosen to be 50x50 ⁇ m2, a standard size allowing acceptable resolution with a chip-sized array.
  • the target TCR was set around -2%, which according to Figure 21 would be obtained for a resistivity in the order of 10 ⁇ ' cm.
  • the width of the suspensions legs was designed to be 5 ⁇ m and their lengths varied from 50 ⁇ m to 170 ⁇ m, corresponding to a number of resistor squares varying from 10 to 34. Therefore, for the total bolometer resistance to be dominated by the pixel resistance, the resistivity of the suspension legs should be on the order of 10 "1 to 10 "2 ⁇ cm (if the thicknesses are comparable).
  • a method of fabricating a bolometer sensing device according to an embodiment of the present invention can be provided below.
  • a substrate e.g., silicon wafer
  • a surface region e.g., silicon wafer
  • the above sequence of steps provides a method according to an embodiment of the present invention. As shown, the method uses a combination of steps including a way of forming a bolometer sensing device using a pyrolyzed parylene bearing material or the like. Other alternatives can also be provided where steps are added, one or more steps are removed, or one or more steps are provided in a different sequence without departing from the scope of the claims herein. Further details of the present method and structure can be found throughout the present specification and more particularly below.
  • One device process, Figure 23 begins with a 5000 A oxide growth and patterning.
  • a 3 ⁇ m-thick parylene-C layer is then deposited and pyrolyzed in a nitrogen atmosphere.
  • the temperature is raised to 800°C at 10°C/min then cooled down to room temperature at 2°C/min.
  • the resulting film is patterned to define the suspension legs.
  • the pyrolyzed-parylene etching is done in a Technics PEII plasma etcher with 400W, 200mT of 02 using a photoresist mask.
  • the etching rate of pyrolyzed-parylene was found to be comparable to that of parylene ( ⁇ 180 ⁇ A/min) for these same settings.
  • a second layer of parylene (0.8 ⁇ m) is deposited, and then pyrolyzed at 660°C (with the same ramping parameters as previously). For better repeatability, the samples are being kept at the pyrolysis temperature for 2 hours.
  • the second layer of pyrolyzed parylene is patterned define the pixel area.
  • the pyrolyzed parylene sensing element is deposited on a sacrificial layer, which is subsequently etched away to form a free standing portion of the pyrolyzed parylene sensing element.
  • the sacrificial layer can be made of a suitable material such as amorphous silicon, polysilicon, metal, organic material, or other materials, or combination of materials depending upon the specific application.
  • a Ti/Au interconnection layer (6 ⁇ A/200 ⁇ A) is evaporated and patterned.
  • the bolometers are released by XeF gas-phase etching.
  • Figure 24 shows a fabricated free-standing device.
  • parylene depositions involve a prior coating of Al 74 for adhesion promotion [see Product Specifications, A- 174 Silane Promotion, Specialty Coating Systems, Inc., Indianapolis, IN, Phone: (800) 356-8260.].
  • the contact between the pyrolyzed parylene layers and Ti/Au was found to be ohmic with a specific contact resistance of 3.5xl0 "3 ⁇ ' cm 2 for first layer and 3.5 ⁇ cm for the second layer.
  • the contact between the first and the second layer of pyrolyzed parylene was also ohmic with a specific contact resistance of 1.57 ⁇ ' cm 2 .
  • the TCR of the second parylene layer around room temperature was measured to be - 1.63%/K.
  • Table (1) shows different characteristics of interest for the two pyrolyzed- parylene layers.
  • the ratio between the sheet resistance of the first and the second layer is 8.7x10 . Therefore, for the chosen geometries, the total resistance of the bolometers is indeed dominated by the temperature-sensing element obtained from the second layer of pyrolyzed parylene.
  • FIG. 25 shows the IV curve for a 50x50 ⁇ m bolometer with two 5 ⁇ mxl70 ⁇ m suspensions beams. The upward curvature seen on this figure indicates self-heating (the TCR of pyrolyzed-parylene being negative). Unreleased bridges do not exhibit this self-heating.
  • Figure 26 shows the resistance and temperature rise as a function of input power.
  • the temperature rise is calculated from the resistance change and TCR.
  • the corresponding thermal conductance is 5.43x10 " W'K " .
  • Knowing the dimensions of the legs, we can estimate the thermal conductivity of the first layer of pyrolyzed parylene to be ⁇ pp 1.5 W'm "1 . K-l.
  • Similar calculations on other bolometers having different geometries (smaller suspensions legs) lead to lower thermal conductivities 1.5 W m "1, K "1 ⁇ K pp ⁇ l.l W'm '1 ! "1 .
  • This is comparable to values reported for PECVD silicon nitride [See, M. Von Arx, O. Paul and H. Baltes, JMEMS Vol.
  • the bolometer design can have certain other features according to the present invention. That is, the bolometer has a substrate as noted above that is free from any cooling element, which is associated with drawing off heat from electron hole interactions.
  • the increase in temperature on each of the carbon based regions is from radiation influence.
  • the interconnection of the bolometer acts as a heat sink.
  • certain colors are desired in the sensor regions, e.g., carbon based regions. That is, the carbon based material regions comprises a substantially black color to increase a radiation influence.
  • the array of substantially carbon based regions is packaged and maintained in a vacuum.
  • the vacuum is less than 20 millitorr but can be at other vacuums or partial vacuums.
  • Other packaging designs also provide that the substantially carbon based regions is free from any coatings such as antireflection coating.
  • the bolometer may also include a transparent member overlying the array of substantially carbon based material regions, which is maintained in the vacuum.
  • the transparent member comprises a germanium, sapphire, calcium fluoride, zinc zelenide, zinc sulfide, AMTIR, or other alloy to allow infrared radiation according to specific embodiments.
  • the predetermined range is from about 10 8 Ohms-cm to about 10 "3 Ohms-cm, other ranges can also exist, which are within our outside of the predetermined range.
  • each of the carbon based regions in the bolometer design may have a dimension of less than 100 ⁇ m and an area of less than 10 "2 cm 2 , although other dimensions can also exist according to other embodiments.
  • Apparatus for sensing electromagnetic radiation using carbon based sensing materials comprising: a substrate comprising a surface region; an array of substantially carbon based material regions having a resistivity ranging within a predetermined range disposed overlying the surface, each of the carbon based material regions comprising a portion being suspended over a region of the surface to thermally insulate the portion of the suspended carbon based material; an insulating region formed between the region and the portion of the carbon based material; and an interconnection to coupled to each of the carbon based material regions; one or more nodes coupled to the interconnection, the one or more nodes being able to independently read a resistivity value associated at least one or more of the carbon based material regions.
  • the predetermined range is from about 10 Ohms cm to about 10 " Ohms cm.
  • the carbon based material comprises pyrolyzed parylene, polyimide, photoresist, or other polymers.
  • the interconnection comprises a metal layer.
  • each of the carbon based material regions is a pixel element for a plurality of pixel regions.
  • the insulating region is at least 2.5 ⁇ m in dimension from the surface of the region to the portion of the carbon based material. 10. The apparatus of embodiment 1 wherein the insulating region comprises an air gap.
  • each of the carbon based regions has a dimension of less than 100 ⁇ m.
  • the substrate is selected from silicon, silicon on insulator, other semiconductor materials, glass, quartz, metal or organic materials.
  • each of the carbon based regions is characterized by a thickness and surface area.
  • each of the carbon based regions may change in resistivity value upon receiving a dosage of electromagnetic radiation.
  • the sensor is uncooled.
  • the transparent member comprises a germanium, sapphire, calcium fluoride, zinc zelenide, zinc sulfide, AMTIR, or other alloy to allow infrared radiation.
  • inventions further comprising a substantially carbon based interconnect coupled to each of the regions, the substantially based interconnect being characterized by a first resistivity value and each of the regions being characterized by a second resistivity value.
  • a method for fabricating a sensing device comprising: providing a substrate comprising a surface region; forming an insulating material overlying the surface region; forming a film of carbon based material overlying the insulating material; and treating to the film of carbon based material to pyrolyzed the carbon based material to cause formation of a film of substantially carbon based material having a resistivity ranging within a predetermined range; and forming a gap underlying a portion of pyrolyzed carbon based material.
  • pyrolyzed carbon based material comprises Pyrolyzed Parylene, photoresist, or other polymer.
  • the substrate comprises silicon bearing material.
  • each of the regions is a pixel element, each of the pixel elements being characterized by a size of is 50 microns and less.
  • 51. Apparatus for chemical sensing using carbon based sensing materials, the apparatus comprising: a pyrolyzed parylene carbon based electrode structure having a resistivity ranging within a predetermined range, the electrode having a first end coupled to a second end and a length defined between the first end and the second end; an interconnect coupled to at least one of the ends.
  • the apparatus of embodiment 51 wherein the interconnection comprises a metal layer.
  • the pyrolyzed parylene carbon based electrode structure may change in an electrical characteristic upon exposure of one or more chemical species.
  • the apparatus of embodiment 51 further comprising a reference electrode coupled to the pyrolyzed parylene carbon based electrode structure.
  • a reference electrode coupled to the pyrolyzed parylene carbon based electrode structure.
  • a method for fabricating a sensing device comprising: providing a substrate comprising a surface region; forming an insulating material overlying the surface region; forming a film of carbon based material overlying the insulating material; and treating to the film of carbon based material to pyrolyzed the carbon based material to cause formation of a film of substantially carbon based material having a resistivity ranging within a predetermined range; providing at least a portion of the pyrolyzed carbon based material in a sensor application; using the portion of the pyrolyzed carbon based material in the sensing application. 1. The method of embodiment 60 wherein the sensing application chemical, humidity, mechanical strain or temperature.

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Abstract

L'invention concerne un procédé de fabrication de films minces de carbone consistant à déposer un catalyseur sur un substrat, à déposer un hydrocarbure en contact avec le catalyseur et à réaliser une pyrolyse de l'hydrocarbure. L'invention concerne également un procédé de commande de la densité du film mince de carbone consistant à graver une cavité dans un substrat, à déposer un hydrocarbure dans la cavité et à réaliser une pyrolyse de l'hydrocarbure quand il se trouve dans la cavité, aux fins de formation d'un film mince de carbone. La commande de la densité du film mince de carbone est obtenue par changement du volume de la cavité. L'invention concerne en outre des procédés de fabrication de structures à motifs renfermant du carbone. Les films minces de carbone et les structures à motifs renfermant du carbone peuvent être utilisés dans des NEMS, des MEMS, la chromatographie liquide et des dispositifs à capteurs.
PCT/US2005/002254 2004-01-23 2005-01-24 Carbone de film mince pyrolyse WO2005070005A2 (fr)

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US10/973,938 US7238941B2 (en) 2003-10-27 2004-10-25 Pyrolyzed-parylene based sensors and method of manufacture
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