KR20110059563A - Metal and electronic device coating process for marine use and other environments - Google Patents

Abstract

The present disclosure is in part directed to conformal coating compositions based on parylene having improved properties, such as improved heat transfer and durability properties, and methods and devices for coating objects with these compositions, and objects coated with these compositions. It is about. In some aspects, a coating composition comprising parylene and boron nitride is disclosed. The present disclosure also includes objects having conformal coatings (eg, electronic equipment, textiles, etc.) comprising parylene compounds and boron nitride.

Description

METAL AND ELECTRONIC DEVICE COATING PROCESS FOR MARINE USE AND OTHER ENVIRONMENTS}

Related application

The present invention is related in part to US Patent Application No. 12 / 104,080, filed April 16, 2008 and US Patent Application No. 12 / 104,152, filed April 16, 2008, the content of which is incorporated herein by reference. The entirety of which is incorporated herein by reference, the benefit of which is 35 USC It is claimed by this name under §120.

For example, conformal coatings with high electrical resistance and moisture resistance are used to protect components in commercial devices used in, for example, the consumer goods, automotive, military, medical and aerospace industries. Often used. There are various ways of applying such coatings. For example, chemical vapor deposition at low pressure can produce thin, uniform conformal (also called conformational) coatings on various surfaces. There is a need for improved methods of application for this to broaden the application of conformal coatings. In addition, there is also a need for new coating compositions having properties that improve the effectiveness in certain applications. For example, there is a particular need for coatings with better durability and heat transfer properties.

Summary of the Invention

Applicant has found, in part, an ultra-thin conformal polymer coating that resists water penetration, and a method and apparatus for applying the coating to an object. Ultra-thin conformal polymer coatings that resist moisture penetration can be applied directly to a wide range of objects, particularly including "off-the-shelf" electronic equipment. Accordingly, some aspects of the present disclosure include compositions, methods, and devices for coating an object. In another aspect, a conformal coating compound, such as a Parylene compound, is disclosed that can form an ultra-thin conformal coating on an object. In another aspect, an conformal coating compound capable of forming an ultra-thin conformal coating, and an additive that modifies any one of a number of properties of conformal coatings, including, for example, electrical resistance, thermal conductivity, light transmittance, hardness, and durability A coating composition is disclosed that includes (s) (eg, a thermally conductive material (eg, boron nitride)). In another aspect, the present disclosure includes "standardized" electronic equipment, such as cell phones and mp3 players, having an ultra-thin conformal coating (eg, a waterproof coating) that resists moisture penetration. Also disclosed are methods and apparatus useful for applying an ultra-thin conformal coating on the surface of an object by vapor deposition. In another aspect, a multistage heating apparatus for vapor deposition of an ultra thin conformal polymer coating is disclosed. Objects coated by the coating compositions and methods disclosed herein include electronic equipment such as mobile phones, radios, circuit boards, and speakers; Equipment used for offshore and space exploration; Hazardous waste transport equipment; Medical Equipment; Paper products; And fabrics. It can coat any solid surface of an object, including plastics, metals, wood, paper, and fabrics. Biomedical devices (e.g. hearing aids, cochlear ear implants, prostheses, etc.), automobiles, electromechanics, art (painting, wood, watercolors, chalk, ink, charcoal), military system components, ammunition, guns Inorganic and similar objects can be coated using the methods and coating compositions disclosed herein.

According to some aspects, a coating composition is provided comprising a conformal coating compound and a thermally conductive material. In some embodiments, the thermally conductive material is dispersed in the polymer of the conformal coating compound. In some embodiments, the coating composition is a solid (eg, conformal coating) having a hardness of about R80 to about R95. In some embodiments, the coating composition is a gaseous mixture comprising monomers of conformal coating compounds in a gaseous phase. In certain embodiments, this gaseous mixture comprises a thermally conductive material of solid particles.

In some embodiments, the conformal coating compound is a parylene compound optionally selected from the group consisting of parylene D, parylene C, parylene N, and parylene HT® compounds. In some embodiments, the coating composition comprises two or more different parylene compounds. In some embodiments, the coating composition comprises two or more parylene compounds that differ in purity level. In some embodiments, such coating compositions have a 5-10% greater thermal conductivity than the parylene compound alone. In some embodiments, the coating composition has a thermal conductivity greater than 10% greater than that of the parylene compound alone. In some embodiments, the coating composition has a thermal conductivity up to about 5% greater than that of the parylene compound alone.

In some embodiments, the thermally conductive material is ceramic. In some embodiments, the thermally conductive material is selected from the group consisting of aluminum nitride, aluminum oxide and boron nitride. In some embodiments, the thermally conductive material has a volume resistivity of greater than 10 ¹⁰ ohm * cm. In some embodiments, the mass of thermally conductive material in the coating composition is about 3% or less (or more) of the total mass of the conformal coating compound and thermally conductive material in the coating composition. In some embodiments, the mass of the thermally conductive material in the coating composition is about 1% or less of the total mass of the conformal coating compound and the thermally conductive material in the coating composition.

In some aspects, a conformal coating is provided that is present on at least a portion of the surface of the object. In some embodiments, the conformal coating comprises any of the above coating compositions.

In some embodiments, the conformal coating is present on at least a portion of the surface of the object, which is an electronic device. Electronic components include communications devices, speakers, mobile phones, audio players, cameras, video players, remote controls, satellite positioning systems, computer components, radar displays, depth finders, fish finders, and emergency position indicators. It may be arbitrarily selected from an indicating radio beacon (EPIRB), an emergency locator transmitter (ELT), and a personal locator beacon (PLB).

In some embodiments, the conformal coating is a paper product; Textile products; Art work; A circuit board; Offshore exploration devices; Space exploration devices; Hazardous waste transportation devices; Automotive devices; Electromechanical devices; Military system components; ammunition; gun; weapon; Medical Equipment; And a biomedical device optionally selected from the group consisting of hearing aids, cochlear implants and prostheses.

In some embodiments, the conformal coating is present on at least a portion of the surface of the object, where the surface is plastic, metal, wood, paper or fabric. In certain embodiments, the surface is the outer surface of the object. In another particular embodiment, the surface is the interior surface of the object.

In some aspects, an object is provided that includes a conformal coating on at least a portion of the surface. In some embodiments, the conformal coating on the surface of the object comprises any of the above coating compositions.

In some embodiments, the object may be a communication device, speaker, cell phone, audio player, camera, video player, remote control device, satellite positioning system, computer component, radar display, depth meter, fish finder, radio for emergency positioning. An electronic device selected arbitrarily from an EPIRB, an emergency location transmitter (ELT) and a personal location signal (PLB).

In some embodiments, the object is a paper product; Textile products; Art work; A circuit board; Offshore exploration devices; Space exploration devices; Hazardous waste transportation devices; Automotive devices; Electromechanical devices; Military system components; ammunition; gun; weapon; Medical Equipment; And a biomedical device optionally selected from the group consisting of hearing aids, cochlear implants and prostheses.

In some embodiments, the surface of the object is a plastic, metal, wood, paper or fabric. In certain embodiments, the object is coated on the outer surface. In another particular embodiment, the object is coated on the inner surface. In some embodiments, the surface is substantially covered with a conformal coating. The substantially coated surface may be a completely covered or sufficiently coated surface to protect the underlying surface of the object from contact with a substance (eg water) for which protection is desired.

In some aspects, a method of applying a conformal coating to an object is provided. In some embodiments, the method

A) heating the conformal coating compound to form a gaseous monomer of the conformal coating compound,

B) combining a thermally conductive material with the gaseous monomer to form a gaseous mixture and

C) applying the conformal coating to the object by contacting the object with the gaseous mixture under conditions such that a conformal coating comprising a conformal coating compound and a thermally conductive material is formed on at least a portion of the surface of the object.

It includes.

In some embodiments of this method, the conformal coating compound is any parylene compound selected from the group consisting of parylene D, parylene C, parylene N, and parylene HT® compounds.

In some embodiments of this method, the thermally conductive material is a ceramic. In other embodiments, the thermally conductive material is selected from the group consisting of aluminum nitride, aluminum oxide and boron nitride. In certain embodiments, the thermally conductive material is in the form of solid particles. In certain embodiments, the solid particles are about 1.8 micrometers to about 2.5 micrometers.

In some embodiments, the method

A) heating the parylene compound to a temperature of about 125 to about 200 ° C. to form a gaseous parylene compound, wherein heating of the parylene compound is carried out in at least two heating steps,

B) heating the gaseous parylene compound to a temperature of about 650 to about 700 ° C. to decompose the gaseous parylene compound to form a parylene monomer, and

C) applying the coating to the object by contacting the object with the parylene monomer under conditions such that a conformal coating comprising a parylene polymer is formed on at least a portion of the surface of the object

It includes.

In some embodiments of this method, step A comprises heating the parylene compound to a temperature of about 125 to about 180 ° C., and heating the parylene compound to a temperature of about 200 to about 220 ° C.

In some embodiments of this method, heating of the gaseous parylene compound is carried out in two or more steps. In some embodiments, step B comprises heating the gaseous parylene compound to a temperature of about 680 ° C., and heating the gaseous parylene compound to a temperature of about 700 ° C. or more.

In some embodiments, the parylene compound is selected from the group consisting of parylene D, parylene C, parylene N, and parylene HT® compounds.

In some embodiments, the method further comprises, prior to step C, contacting the object with gaseous silane under conditions that the silane activates the surface of the object. In some embodiments, the silane is one or more silanes selected from the group consisting of Silquest® A-174, Silquest® 111 and Silquest® A-174 (NT).

In some embodiments of the method, the object during step C is at a temperature of about 5 ° C to about 30 ° C. In some embodiments, the conformal coating applied to the surface is about 100 angstroms to about 3.0 millimeters. In some embodiments, the conformal coating applied to the surface is about 0.0025 mm to about 0.050 mm thick.

In some embodiments of the method, the object is a communication device, speaker, cell phone, audio player, camera, video player, remote control device, satellite positioning system, computer component, radar display, depth meter, fish finder, emergency position indication Electronic device selected arbitrarily from EPIRB, emergency location transmitter (ELT) and personal location signal (PLB).

In some embodiments of the method, the object is a paper product; Textile products; Art work; A circuit board; Offshore exploration devices; Space exploration devices; Hazardous waste transportation devices; Automotive devices; Electromechanical devices; Military system components; ammunition; gun; weapon; Medical Equipment; And a biomedical device optionally selected from the group consisting of hearing aids, cochlear implants and prostheses.

In some embodiments of the method, the surface is plastic, metal, wood, paper, and fabric.

In some aspects, an object is provided by which the coating is applied to at least a portion of a surface (outer or inner).

In some aspects, an apparatus for applying a conformal coating to an object is provided. In some embodiments, an apparatus comprises a vaporization chamber comprising two or more temperature zones; A pyrolysis chamber operably connected to the vaporization chamber; And a vacuum chamber operably connected to the pyrolysis chamber. In some embodiments, the apparatus is operably connected to the pyrolysis chamber and the vacuum chamber, capable of transferring gas between the pyrolysis chamber and the vacuum chamber, and further comprising a connection comprising a T-port. . In some embodiments, the T-port is operably connected with means for injecting a thermally conductive material from the pyrolysis chamber into the gas delivered through the connection to the vacuum chamber. In some embodiments, the vacuum generated in the vacuum chamber leads the thermally conductive material into the connection comprising the gas through the T-port.

In some embodiments, the vacuum chamber includes a deposition chamber and a vacuum generating component operably connected to the pyrolysis chamber. In some embodiments, the vacuum generating component (vacuum means) comprises one or more vacuum pumps.

In some embodiments, the vaporization chamber has two temperature zones. In some embodiments, the vaporization chamber is a tubular furnace.

In some embodiments, the pyrolysis chamber has a plurality of temperature zones. In some embodiments, the pyrolysis chamber has two temperature zones. In some embodiments, the pyrolysis chamber is a tubular furnace.

Further advantages of the present invention may be understood with reference to the following description provided in conjunction with the accompanying drawings:
1A-1E are diagrams of the chemical structures of various parylenes and Silquest®. 1A is a view of parylene N. FIG. 1B is a view of parylene C. 1C is a view of parylene D. FIG. 1D is a view of Parylene HT®. 1E is a diagram of Silquest® A-174 silane (also known as Silquest® A-174 (NT)).
2A is a schematic diagram of one embodiment of an apparatus for chemical vapor deposition of parylene.
2B is a schematic diagram of one embodiment of an apparatus for applying a coating of parylene and powder.
3A-3C are schematic diagrams of parylene-coated objects of three embodiments. 3A shows an object coated with a separate layer of parylene and boron nitride, wherein the boron nitride layer is closer to the object. 3B shows an object coated with separate layers of parylene and boron nitride, in which the parylene layer is closer to the object. 3C shows an object coated with a layer of inter-dispersed parylene with boron nitride.

Detailed description of the invention

In some aspects, the present disclosure provides compositions, methods, and devices for coating an object with a conformal polymer. In some aspects, a conformal coating compound (eg parylene) is provided that can form an ultra thin conformal coating on an object. In another aspect, conformal coating compounds (eg parylene), and additives for modifying any one of a number of coating properties, including, for example, electrical resistance, thermal conductivity, light transmittance, hardness, and durability Additives), for example, a coating composition comprising a thermally conductive material is provided. In another aspect, an object, such as an electronic device, is provided that has an ultra-thin conformal coating (eg, a waterproof coating) that resists moisture penetration. Also provided are methods and apparatus useful for applying an ultra-thin conformal coating on at least a portion of an object surface by vapor deposition. In certain embodiments, a multistage heating apparatus is provided that is useful for vapor deposition of an ultra thin conformal polymer coating.

A particularly important finding disclosed herein is that conformal coatings can be applied directly to "pre-assembled" or "standardized" devices, such as consumer electronics devices. Thus, with the methods and compositions disclosed herein it is possible to apply conformal coatings to all or part of the outer surface of a "pre-assembled" or "standardized" device (eg, a hermetic seal) Or almost sealed seals), thereby protecting the internal components of the device from environmental damage such as moisture penetration and oxidation. Thus, using the methods disclosed herein, certain objects, such as electronic devices (facilities), can be coated in their "standardized" state without the need to disassemble, coat and then reassemble. The methods disclosed herein can, for example, apply a conformal coating comprising a parylene compound to both the outer surface of the electronic device as well as the internal circuit board of the electronic device (eg, in a one-step method). Thus, the method can be used particularly advantageously for "standardized" electronic equipment. In addition, the methods disclosed herein can be very useful for improving ease and efficiency by conformal coating of many other objects.

Suitable objects for conformal coatings using the compositions and methods disclosed herein include, but are not limited to, electronic equipment, cameras, circuit boards, computer chips, paper, textiles, batteries, speakers, solid fuels, medical devices, hazardous waste Transportation equipment, hazardous waste, medical equipment, equipment used for marine and space exploration, and space suits. In some embodiments, the object is a communication device, speaker, mobile phone, audio player, camera, video player, remote control device, satellite positioning system, computer component, radar display, depth finder, fish finder, radio beacon for emergency position indication. (EPIRB), emergency location information transmitter (ELT) and personal location signal device (PLB).

In some embodiments, the object is, but is not limited to, standardized electronic components such as laptop computers, cameras, radios, cell phones, paper, textiles, batteries, speakers, solid fuels, medical devices, paper, spacesuits, and Objects unsuitable for immersion, including other objects disclosed herein or known in the art. In other embodiments, the object may be an object of poor quality upon immersion, such as, but not limited to, metal screws and other hardware, paper products and fabrics. In other embodiments, the object may be an object, such as an audio speaker, that requires flexibility in operation. In further embodiments, the object may be a fuel cell, an inorganic cartridge, and an ammunition, including, but not limited to, objects that are preferably protected from oxygen. In further embodiments, the object may be an object to be isolated from the environment, such as hazardous waste. In further embodiments, the object may be an object requiring protection from chemical exposure, such as, but not limited to, a hazardous waste transport facility.

Coatings may be applied to objects having various surface materials, such as ceramics, polymers, plastics, metals, freezing liquids, and the like. In some embodiments, the object to be coated may be an object that generates or consumes heat, and / or an object that requires a bumpy coating. In some embodiments, the object can be a heat pack, such as a cold pack, freezing liquid and gas, and a heat pump capable of generating heat or absorbing heat. In some embodiments, an object can be expected to be subject to severe physical shocks during its lifetime. In some aspects, methods are provided in the present disclosure that can be used to coat such objects and surfaces.

The conformal coatings disclosed herein may be applied to a variety of devices used in household appliances, commercial vessels, recreational boats, military (aerospace and defense), industrial and medical industries, and also other devices. In some instances, conformal coatings are especially designed as "sealing" devices. Such coatings are useful for protecting, for example, devices commonly used in marine and hazardous environments from operational failures due to moisture, flooding, exposure to dust, strong winds and the effects of chemicals. Coatings can enhance the viability and sustainability of operating equipment and high yield products that are susceptible to corrosion and degradation.

In some embodiments, conformal coatings may be present on the interior and exterior surfaces of the object, in particular conformal coatings on the exterior of the object may be continuous with conformal coatings on the interior of the object.

In some instances where pretreatment with a compound, such as an organic compound, such as silane, is desired, any object having a solid surface that can be exposed to the pretreatment compound (eg, in their gas phase) is suitable. Thus, one embodiment provides an object coated with a silane, such as one or more conformal coating compounds pretreated with Silquest®, wherein the uncoated object may be unsuitable for immersion. Uncoated objects unsuitable for immersion may be objects that lose some or all of their function after immersion. In a preferred embodiment, the object can be an object, such as, but not limited to, a standardized electronic component such as a laptop computer, a radio and a mobile phone that will lose at least some function after immersion and subsequent drying if uncoated. .

An object coated with at least a conformal coating compound (and optionally pretreated with silane) may be applied to an object in which the conformal coating compound gas (optionally and / or silane gas) can enter the interior of the object if there is a gap on the exterior surface of the object. It can have a conformal coating on the inside of the object as well as outside. In a preferred embodiment, the outer conformal coating is continuous with the inner conformal coating.

The coated object may be particularly suitable for use in the harsh external conditions encountered in the military. In some embodiments, the coated object may meet the applicable requirements of military specification MIL PRF-38534, ie general performance requirements for hybrid microcircuits, multi-chip modules (MCMs), and similar devices. In some embodiments, the coated object may meet the applicable requirements of military specification MIL-PRF-38535, ie, general performance requirements for integrated or microcircuits. In some embodiments, the coated object may meet applicable requirements of both military standards MIL-PRF-38534 and MIL-PRF-38535.

Another embodiment includes objects coated with parylene and boron nitride compositions (eg, by the methods disclosed herein). Objects coated in this manner may have a solid surface capable of contacting gaseous parylene monomers and boron nitride under conditions suitable for forming conformal coatings comprising parylene polymer and boron nitride on at least a portion of the surface of the object. It includes any object having. Such objects include, but are not limited to, electronic equipment, circuit boards, paper, textiles, batteries, speakers, solid fuels, medical devices, hazardous waste transportation equipment, hazardous waste, equipment used for marine and space exploration, and space suits. , And other objects disclosed herein and / or known in the art. In some embodiments, the object may be an object that generates heat or consumes heat, such as, but not limited to, a computer, a drill installation for deep hole drilling, an electronic product exposed on an oil rig. In other embodiments, the object may be an object in particular requiring a bumpy coating.

Objects coated with one or more conformal coating compounds and thermally conductive materials, such as boron nitride, may be conformal coating compounds and thermally conductive materials (eg, boron nitride powder particles) in the presence of gaps on the outer surface of the object. The gaseous mixture, including may have a conformal coating on the interior of the object as well as the outside of the object capable of entering the interior of the object. In a preferred embodiment, the outer conformal coating is continuous with the inner conformal coating. For example, an electronic device, such as a cell phone, may have a conformal coating on its keyboard and screen, as well as on circuit boards and batteries inside the device.

In some embodiments, parylene and boron nitride may be inter-dispersed within the coating 8 'on the object 7' (FIG. 3C). In some embodiments, the co-dispersion of parylene and boron nitride can be at the molecular level. In some embodiments, the coating of inter-dispersed parylene and boron nitride can be about 0.0025 mm to about 0.050 mm. In other embodiments, the inter-dispersed parylene and boron nitride coating can be less than about 2.0 mm.

In other embodiments, one or more conformal coatings, such as parylene conformal coatings, and boron nitride are found in separate layers on the object. Conformal coatings of interest include, but are not limited to, polynaphthalene (1-4-naphthalene), diamine (O-tolidine), polytetrafluoroethylene (Teflon®), polyimide have. In a preferred embodiment, the polymer coating may be parylene C. In other embodiments, other forms of parylene may be used including, but not limited to, parylene N, parylene D, and parylene HT®. In a preferred embodiment, the thickness of the boron nitride and polymer coating layer may each be about 0.05 mm. In other preferred embodiments, each layer may contain essentially a polymer coating or may contain essentially boron nitride. In some embodiments, boron nitride layer 2 'may be closer to object 1' than parylene layer 3 '(Figure 3A). In other embodiments, parylene layer 5 'may be closer to object 4' than boron nitride 6 '(FIG. 3B).

Conformal  Composition / Coating

According to some aspects, a coating composition is provided comprising a conformal coating compound and a thermally conductive material. As used herein, “an conformal coating compound” is a compound that can form an ultra-thin, pin-hole free polymeric coating on a surface depending on the shape of the surface (eg, some purified compounds, purified compounds, synthetics Compound, isolated natural compound). Such coatings are referred to herein as "conformal coatings". Conformal coating compounds may also be referred to equivalently as "morphological coating compounds". Conformal coating compounds may be applied as a coating to the surface of an object by various methods, including, for example, chemical vapor deposition. For example, the gaseous monomer of the conformal coating compound can be contacted with the surface of the object under conditions such that the monomers aggregate and are absorbed on the surface and simultaneously polymerized together to form a pin-hole free conformal coating on the surface. . The thickness of the coating may range from about 10 Angstroms up to 50 micrometers, or more, depending on the application. For example, the thickness of the coating can be 3 millimeters or less. In some embodiments, the thickness of the coating is about 0.0025 mm to about 0.050 mm. The conformal coating can be an electrical insulation (eg, volume resistivity greater than 10 ¹⁰ ohm * cm). Alternatively or additionally, the conformal polymer may have a hardness of about R70 to about R90 (Rockwell hardness scale). Conformal coatings may also be hydrophobic, depending on the application. Conformal coating compounds can exist in various forms, including monomer and polymer (eg dimer, multimeric) forms, and phase states (eg gaseous, solid).

Particularly useful conformal coating compounds are parylene compounds. Parylene is the common name for members of a unique series of compounds. The basic member of the series of parylenes, called parylene N, is poly-para-xylene and the compound is prepared from di-p-xylene ([2,2] paracyclophan). Parylene N is a completely linear high crystalline material. Parylene C, the second commercial member of the series of parylenes, is produced from the same monomer modified by only replacing one of the aromatic hydrogens with a chlorine atom. Parylene D, the third member of the series of parylenes, is produced from the same monomer modified by substituting two of the aromatic hydrogens with chlorine atoms. Parylene D has similar properties to parylene C, but additionally has the ability to withstand higher use temperatures. In some embodiments, parylene may be derived from poly-para-xylene by substitution of various chemical moieties. In a preferred embodiment, parylene may form a linear high crystalline material. In addition, other parylene molecules can be used, such as derivatives and analogs of the parylene. In some embodiments, parylene compounds provided by commercial sources such as Specialty Coating Systems (SCS), Inc. can be used.

In addition, examples of conformal coating compounds include, but are not limited to, polynaphthalene (1,4-naphthalene), diamine (O-tolidine), polytetrafluoroethylene (Teflon®), and polyimide. These polymers can be applied by standard techniques as is well known in the art.

Conformal coatings, including parylene, may be adiabatic and do not facilitate the release of coated objects into the environment. This property of parylene can cause problems for objects such as electronic equipment that generate heat, and can lead to early failure of the equipment if the heat is not dissipated. Some parylene-based conformal coatings disclosed herein include conductive materials that facilitate heat dissipation from the coated object. Compared with parylene-only coatings, these conformal coatings are useful for coating objects that require heat dissipation by heat release or heat absorption. Parylene-based conformal coating compositions disclosed herein can also have increased hardness compared to parylene-only coatings. Thus, parylene-based coating compositions may also be useful for coating objects that require a rugged protective coating, such as objects that will be subject to severe physical impacts over their lifetime.

Thus, in accordance with some aspects of the present disclosure, a conformal coating compound may be combined with other additive (s) to obtain a coating composition having one or more improved performance characteristics when compared to the conformal coating compound alone. For example, it is possible to produce coating compositions with improved heat transfer capabilities. As used herein, a “thermally conductive material” is a material that can be combined with a conformal coating compound to form a coating composition having a higher thermal conductivity than that of the conformal coating compound alone. The thermally conductive materials disclosed herein have higher thermal conductivity compared to conformal coating compounds themselves. Exemplary thermally conductive materials include at least 1 W / (m * K), at least 5 W / (m * K), at least 10 W / (m * K), at least 15 W / (m * K) or 20 W / ( m * K) or more. Those skilled in the art will appreciate that there are a variety of thermal conductivity measurement methods, including, for example, the test methods set forth in the following standards: IEEE Standard 98-2002, "Standard for the Preparation of Test Procedures for the Thermal Evaluation of Solid Electrical Insulating Materials", ISBN 0-7381-3277-2; ASTM standard D5470-06, "Standard Test Method for Thermal Transmission Properties of Thermally Conductive Electrical Insulation Materials"; ASTM standard E1225-04, "Standard Test Method for Thermal Conductivity of Solids by Means of the Guarded-Comparative-Longitudinal Heat Flow Technique"; ASTM standard D5930-01, "Standard Test Method for Thermal Conductivity of Plastics by Means of a Transient Line-Source Technique"; And ISO 22007-2: 2008 "Plastics-Determination of thermal conductivity and thermal diffusivity-Part 2: Transient plane heat source (hot disc) method". Exemplary thermally conductive materials include various ceramic materials such as silicon dioxide and silicon nitride. The thermally conductive material may also be selected from the group consisting of aluminum nitride, aluminum oxide and boron nitride. Other thermally conductive materials include, for example, titania (TiO ₂ ). Still other materials will be apparent to those skilled in the art. In some embodiments, the coating composition comprises a conformal coating compound and lanthanum hexaborate (LaB ₆ ). In some embodiments, the coating composition comprises a conformal coating compound and silica (SiO ₂ ).

In some aspects, a coating composition comprising a parylene compound and a thermally conductive material as a conformal coating compound has a greater thermal conductivity than the parylene compound alone, and in some cases about 10% greater thermal conductivity than the thermal conductivity of the parylene compound alone Has In some embodiments, the thermal conductivity of the coating composition is about 5-10% greater than that of the parylene compound alone. Alternatively or additionally, the coating composition may have a greater hardness than parylene alone, in particular about 10% greater than parylene alone.

An exemplary thermally conductive material is boron nitride. Boron nitride (BN) is a binary chemical compound composed of the same number of boron and nitrogen atoms. Therefore, its empirical formula is BN. Boron nitride is carbon and isoelectronics, and, like carbon, boron nitride exists in various polymorphic forms, one of which is analogous to diamond and the other to graphite. Diamond-like polymorphs are one of the highest hardness materials known and graphite-like polymorphs are useful lubricants. In addition, both of these polymorphs exhibit radar-absorbing properties (see Silverberg, Martin S. Chemistry: The Molecular Nature of Matter and Change, Fifth Edition. New York: McGraw-Hill, 2009. p. 483). Thus, in some aspects, the present disclosure provides a coating composition that may contain parylene compounds and boron nitride. In these compositions, the parylene compound and boron nitride can be inter-dispersed (eg, the boron nitride particles can be dispersed in the parylene polymer). Although any parylene compound can be used in these compositions, parylene D, parylene C, parylene N and parylene HT® compounds may be preferred, and parylene C compounds may be particularly preferred. In these compositions, the boron nitride may have a hexagonal plate structure. In some embodiments, the weight of boron nitride relative to the total weight of parylene compound and boron nitride may be less than about 80%. In some embodiments, the weight of boron nitride may be about 1% or less, about 2% or less, about 3% or less, about 5% or less, about 10% or less, or about 20% or less of the total weight of the parylene compound and boron nitride. have.

In some embodiments, the coating composition may consist essentially of parylene and boron nitride. In other embodiments, the coating composition consists of parylene and boron nitride. In some embodiments, parylene and boron nitride comprise at least about 50%, at least about 70%, at least about 90%, at least about 95%, at least about 99% or at least about 99.9% of the composition.

In some embodiments, when the coating on the object includes parylene and boron nitride, the boron nitride may be inter-dispersed in the parylene in the coating (dispersed in the polymer of the parylene compound). Although any parylene may be used for these objects, parylene C, parylene N, parylene D and parylene HT® may be preferred, and parylene C may be particularly preferred. In some embodiments, the coating can be about 0.0025 mm to about 0.050 mm thick.

In some embodiments such parylene-boron nitride coating compositions may contain parylene C, and in other embodiments may contain parylene D, parylene N or parylene HT® (FIGS. 1A, 1B, 1C). And 1d). In some embodiments, parylene may be derived from parylene N or poly-para-xylene by substitution of various chemical moieties. In a preferred embodiment, parylene forms a completely linear highly crystalline material. In some embodiments, the boron nitride may have a hexagonal plate structure. In some embodiments, parylene and boron nitride form separate layers in the parylene composition. In some embodiments, the parylene composition can have strong covalent bonds in the parylene and boron nitride layers. In other embodiments, the parylene composition may have a weak Van der Waals force between the parylene and the boron nitride layer.

In some embodiments, parylene compositions may have greater thermal conductivity than parylene alone (eg, measured in (cal / sec) / cm ² / C). In certain embodiments, parylene-boron nitride compositions may have a thermal conductivity greater than about 10%, greater than about 30%, or greater than about 50% than parylene alone. In other embodiments, the parylene composition may have a greater hardness than that of parylene alone, as defined by Rockwell hardness test (EL Tobolski & A. Fee, Macroindentation Hardness Testing ASM Handbook. Volume 8 : Mechanical Testing and Evaluation, 203-211 (ASM International, 2000). In certain embodiments, parylene-boron nitride compositions may have a hardness of greater than about 10%, greater than about 30%, greater than about 50%, or greater than about 90% than parylene alone. The relative amounts of parylene and boron nitride in the parylene-boron nitride composition can determine the thermal conductivity and hardness of the composition. In some embodiments, the weight of boron nitride relative to the total weight of parylene and boron nitride in the composition is less than about 5%, less than about 10%, less than about 20%, less than about 40%, less than about 60% or about 80% Will be less. In some embodiments, the weight of boron nitride relative to the total weight of parylene and boron nitride in the composition will be about 1% or less, about 2% or less, about 3% or less or about 4% or less.

In some cases, the object may require pretreatment, such as the application of silane, to make the surface of the object easier to attach to the conformal coating. The pretreatment method may involve impregnating the object in a solution comprising a suitable compound, including, for example, an organic compound such as silane, and then removing the object from the silane-solution and drying the object. Such pretreatment can improve the surface bonding of conformal coating compounds and improve (improve) the mechanical and electrical properties.

If an object, for example an electronic device, can be destroyed by immersion in a solution, other pretreatment methods can be used, including coating the object with silane. For example, the silane may be applied vapor phase to an object to be coated with a conformal coating comprising a parylene compound. This may allow some objects, for example objects not suitable for impregnation but requiring surface pretreatment with silane, to be coated with parylene.

In another aspect, the present disclosure includes an object having at least one coat of conformal coating compound and at least one coat of boron nitride. In some embodiments, the conformal coating compound may be polynaphthalene, diamine, polytetrafluoroethylene, polyimide, parylene C, parylene N, parylene D or parylene HT®, preferably parylene Cyl Can be. In some embodiments the boron nitride coat may be closer to the object than the polymer coat, while in other embodiments the polymer coat may be closer to the object than the boron nitride coat. In some embodiments, the coating of boron nitride and polymer may each be at least about 0.05 mm thick.

Conformal  Coating device

Also disclosed is an apparatus useful for applying an ultra-thin conformal coating to the surface of an object by vapor deposition. In another aspect, a multistage heating apparatus for vapor deposition of an ultra thin conformal polymer coating is disclosed.

In some aspects, the present disclosure applies a conformal coating comprising parylene, comprising a vaporization chamber having a plurality of (two or more) temperature zones operably connected to a pyrolysis chamber operably connected to a vacuum chamber. It provides a device for. In some embodiments, the vacuum chamber may comprise a pyrolysis chamber and a deposition chamber operatively connected to the vacuum means, wherein the vacuum means may be one or more vacuum pumps. In some embodiments, the vaporization chamber may have a plurality of temperature zones, preferably two temperature zones. In other embodiments, the pyrolysis chamber may have a plurality of temperature zones, preferably two temperature zones. In some embodiments, the vaporization chamber and / or pyrolysis chamber may be tubular.

Other devices are known in the art for chemical vapor deposition of conformal coating compounds onto objects. For example, U.S. Patent Nos. 4,945,856, 5,078,091, 5,268,033, 5,488,833, 5,534,068, 5,536,319, 5,536,321, 5,536,322, 5,538,758, See 5,556,473, 5,641,358, 5,709,753, 6,406,544, 6,737,224, and 6,406,544, all of which are incorporated herein by reference.

In another aspect, the present disclosure includes a vaporization chamber operably connected to a pyrolysis chamber operably connected to a vacuum chamber, wherein the connection comprising a T-port operably connects the pyrolysis chamber to the vacuum chamber. A device is provided for applying a conformal coating comprising a conformal coating compound and a thermally conductive material. In some embodiments, the connection that operably connects the pyrolysis chamber and the vacuum chamber can be a means for delivering gas from the pyrolysis chamber to the vacuum chamber. In other embodiments, the T-port may be operably connected to means for injecting solid particles (eg, powder) or another gas into the gas delivered through the connection. In some embodiments, the vacuum chamber may contain a pyrolysis chamber and a deposition chamber operably connected to a vacuum means, where the vacuum means may be one or more vacuum pumps.

One embodiment is an apparatus for chemical vapor deposition of parylene, which may include an improved vaporization chamber and / or pyrolysis chamber. Such devices may be particularly useful for chemical vapor deposition of parylene, but also other conformal coating compounds such as polynaphthalene (1,4-naphthalene), diamine (O-tolidine), polytetrafluoroethylene (Teflon®) , Polyimide, and other compounds well known to those skilled in the art may be used for vapor deposition. In some embodiments, the apparatus includes a vaporization chamber and / or a pyrolysis chamber having a plurality of temperature zones. Without limiting the operation of the device, it is believed that the heating rate of parylene is improved by allowing different temperature set points in each chamber. Multi-zone vaporization and pyrolysis chambers allow parylene to be uniformly cut into monomers and better control the final thickness of the parylene coat on the object. Parylene may remain as monomer in the deposition chamber for a longer time so that it can spread better throughout the deposition chamber.

2a shows a parylene coating apparatus. The vaporization chamber 1 may have two temperature zones 10 and 11. In addition, the pyrolysis chamber 3 may also have two temperature zones 12 and 13. The vaporization chamber 1 can be operably connected to the pyrolysis chamber 3 by a component 2 capable of transferring gas from the vaporization chamber 1 to the pyrolysis chamber 3. The pyrolysis chamber 3 can comprise a deposition chamber 6 and a vacuum chamber which can be operatively connected to the vacuum means 9 by means of a component 8 capable of vacuuming on the deposition chamber 6. And operatively connected to (14). A component 5 operatively connecting the pyrolysis chamber 3 to the vacuum chamber 14 can transfer gas from the pyrolysis chamber 3 to the vacuum chamber 14, and also vacuums from the pyrolysis chamber 3. It may include a valve (4) capable of regulating the flow of gas into the system (14).

The vaporization chamber 1 can be any furnace / heating system capable of heating the solid to about 150 ° C to about 200 ° C. In a preferred embodiment, the vaporization chamber can heat the gas to 1200 ° C. In some embodiments, vaporization chamber 1 may contain a gas. The vaporization chamber 1 can also create zones at different temperatures in its heating chamber. Finally, the vaporization chamber 1 can maintain a high vacuum. In a preferred embodiment, the vaporization chamber can maintain a vacuum of at least about 0.1 Torr.

The vaporization chamber 1 may be operably connected to the pyrolysis chamber 3 by a number of components well known to those skilled in the art. In some embodiments, the operable connection between the vaporization chamber 1 and the pyrolysis chamber 3 is a connection that allows gas to pass from the vaporization chamber 1 to the pyrolysis chamber. In some embodiments, this component (2) may in particular be a glass tube, retort, or metal tube. In other embodiments, these components (2) may also contain valves, temperature sensors, other sensors, and other conventional components well known to those skilled in the art.

The pyrolysis chamber 3 may be any furnace / heating system capable of heating the gas to about 650 ° C to about 700 ° C. In some embodiments, pyrolysis chamber 3 may contain a gas. In some embodiments, the pyrolysis chamber 3 can create zones at different temperatures in its heating chamber. Finally, in some embodiments, the pyrolysis chamber 3 can maintain a high vacuum. In a preferred embodiment, the pyrolysis chamber can maintain a vacuum of at least about 0.1 Torr.

The vaporization chamber and the pyrolysis chamber may preferably be a furnace capable of creating two or more temperature zones in its chamber. In a preferred embodiment, the furnace has two temperature zones. In some embodiments, the temperature zone is located in the furnace chamber such that the gas leaves the furnace after the gas moves sequentially through the temperature zone. Preferably, the furnace may have a maximum temperature of 1200 ° C. In a preferred embodiment, the furnace is a tubular furnace. In other embodiments, the furnace may have a glass retort. Specific parameters of one embodiment of two zone furnaces suitable for use as vaporization chambers and / or pyrolysis chambers can be found in Example 2.

The pyrolysis chamber 3 may be operably connected to the vacuum system 14 by a number of components well known to those skilled in the art. In some embodiments, the operable connection between pyrolysis chamber 3 and vacuum system 14 is a connection that passes gas from pyrolysis chamber 3 to vacuum system 14. In some embodiments, this component 5 may in particular be a glass tube, a retort, or a metal tube. In other embodiments, these components 5 may also contain valves, temperature sensors, other sensors, and other conventional components well known to those skilled in the art. In a preferred embodiment, component 5 may contain one or more valves 4 capable of regulating the flow of gas through component 5.

The vacuum system 14 can contain a deposition chamber 6 in which 8 can be operatively connected to the vacuum means 9. In some embodiments, the operable connection 8 can maintain a vacuum of at least about 0.05 Torr, preferably at least about 1 × 10 ⁻⁴ Torr. In other embodiments, the vacuum means 9 may be one or more vacuum pumps capable of applying a vacuum of at least about 0.05 Torr, preferably at least about 1 × 10 ⁻⁴ Torr, onto the deposition chamber. In some embodiments, the deposition chamber 6 may be large enough to contain the object 7 to be coated. In other embodiments, the deposition chamber 6 may maintain a vacuum in the range of at least about 0.05 Torr, preferably at least about 1 × 10 ⁻⁴ Torr.

Another embodiment disclosed herein is an apparatus useful for chemical vapor deposition of parylene and boron nitride compositions, containing means for injecting the powder into the chemical vapor phase prior to deposition. 2B shows a coating apparatus according to one embodiment. The vaporization chamber 15 may be operably connected to the pyrolysis chamber 17 by a component 16 capable of delivering gas from the vaporization chamber 15 to the pyrolysis chamber 17. The pyrolysis chamber 17 can be operably connected to a vacuum chamber 25, which can include a deposition chamber 21 and by means of a component 23 which can vacuum the deposition chamber 21. It can be operatively connected to the vacuum means 24. A component 19 operatively connecting the pyrolysis chamber 17 to the vacuum chamber 25 can transfer gas from the pyrolysis chamber 17 to the vacuum chamber 25, and also from the pyrolysis chamber 17 a vacuum system. And a valve 18 that can regulate the flow of gas to 25. Component 19 may also have a T-port 20 also referred to as a “tee nipple”. In some embodiments, the T-port may be operably connected to a means for injecting powder into the gas delivered through component 19. In some embodiments, the means for injecting power includes, but is not limited to, an oven, a power coat apparatus, and compressed air. In a preferred embodiment, the means for injecting power comprises a power container operably connected to the solenoid valve, which is operably connected to the T-port.

The vaporization chamber 15 may be any furnace / heating system capable of heating the solid to about 150 ° C. to about 200 ° C. In some embodiments, the vaporization chamber 15 may contain a gas. Finally, the vaporization chamber 15 can maintain a high vacuum.

The vaporization chamber 15 may be operably connected to the pyrolysis chamber 17 by many components well known to those skilled in the art. In some embodiments, the operable connection between the vaporization chamber 15 and the pyrolysis chamber 17 may be a connection capable of passing gas from the vaporization chamber 15 to the pyrolysis chamber. In some embodiments, the component 16 may in particular be a glass tube, retort or metal tube. In other embodiments, the component 16 may also contain valves, temperature sensors, other sensors, and other conventional components that are well known to those skilled in the art.

The pyrolysis chamber 17 may be any furnace / heating system capable of heating the gas to about 650 ° C. to about 700 ° C. In some embodiments, the pyrolysis chamber 17 may contain a gas. Finally, in some embodiments, the pyrolysis chamber 17 can maintain a high vacuum, preferably at least 0.1 Torr.

The pyrolysis chamber 17 may be operably connected to the vacuum system 25 by many components well known to those skilled in the art. In some embodiments, the operable connection between pyrolysis chamber 17 and vacuum system 25 may be a connection capable of passing gas from pyrolysis chamber 17 to vacuum system 25. In some embodiments, the component 19 may in particular be a glass tube, retort or metal tube. In other embodiments, the component 19 may contain valves, temperature sensors, other sensors, and other conventional components that are well known to those skilled in the art. In a preferred embodiment, component 19 may contain one or more valves 4 capable of regulating the flow of gas through component 19.

The vacuum system 25 may contain a deposition chamber 21, which may be operatively connected to the vacuum means 24 by a component 23. In some embodiments, the connection 8 can maintain a vacuum to at least about 0.05 Torr. In other embodiments, the vacuum means 24 may be one or more vacuum pumps, which may bring the deposition chamber to a vacuum of at least about 0.05 Torr. In some embodiments, the deposition chamber 21 may be large enough to contain the object 22 to be coated. In other embodiments, the deposition chamber 21 may maintain a vacuum of at least about 0.05 Torr.

Conformal  Coating method

Also disclosed is a method of applying an ultra-thin conformal coating to the surface of an object by vapor deposition. In some aspects, a multi-stage heating method for vapor deposition of ultra thin conformal coatings is disclosed. In another aspect, a method for vapor deposition of an ultra thin conformal coating comprising an additive, such as a thermally conductive material, is disclosed.

The conformal coating deposition method disclosed herein may be carried out in a closed system, preferably under negative pressure. For example, parylene compounds are deposited from the gas phase at low pressure, for example about 0.1 Torr, to form conformal coatings. In this example, the first step is the vaporization of the solid parylene dimer in a vaporization chamber at about 150 ° C. The second step is quantitative decomposition (pyrolysis) at two methylene-methylene bonds of the dimer in a pyrolysis chamber, for example at about 680 ° C., to obtain para-xylylene, which is a stable monomeric diradical. Finally, the gaseous monomer enters the room temperature deposition chamber, where it is absorbed and polymerized onto the object to be coated. The closed system preferably has separate chambers for vaporization, pyrolysis and deposition of parylene, which chambers are connected with suitable tubing or tubular connections.

Conformal coating compounds can be provided in various forms and purity for use in the method. In some embodiments, the conformal coating compound has a purity of about 90%, about 92.5%, about 95%, about 96%, about 97%, about 98%, about 98.5%, about 99%, about 99.5%, about 99.9% Levels, or up to about 100% purity. In some embodiments, conformal coating compounds are provided as blends of conformal coating compounds (eg, compounds of the same type, eg parylene C) of different sources and / or of different purity. In some embodiments, the conformal coating compound is provided as a blend of multiple forms of conformal coating compound (eg, parylene C, parylene N, parylene D, parylene HT®).

According to another aspect, a method of applying a conformal coating to an object comprises heating a parylene compound to a temperature of about 125 to about 200 ° C. to form a gaseous parylene compound, wherein the heating of the parylene compound is at least two. Performing a heating step, heating the gaseous parylene compound to a temperature of about 650 to about 700 ° C. to decompose the gaseous parylene compound to form a parylene monomer, and an conformal coating comprising a parylene polymer Applying the coating to the object by contacting the object with the parylene monomer under conditions in which water is formed on at least a portion of the surface of the object. In some embodiments, the parylene compound is heated to a temperature of about 125 to about 180 ° C and then to a temperature of about 200 to about 220 ° C. In some embodiments, the gaseous parylene compound is heated in two or more stages. For example, the gaseous parylene compound may be heated to a temperature of about 680 ° C. and then to a temperature of about 700 ° C. or more.

In some cases, the method may be useful for applying a uniform thin layer of conformal coating comprising parylene in a vacuum chamber at 25 ° C. using standard chemical vapor deposition, for example 0.01 depending on the article being coated. To 3.0 mm thick. Once coated the article can be weather and water resistant and can withstand exposure to extreme climatic conditions and exposure to most chemicals. Any solid surface can be coated, including plastics, metals, wood, paper, and fabrics. Sample articles disclosed herein include electronic devices such as mobile phones, radios; Circuit boards and speakers; Devices used for offshore and space exploration, or oil rig operations; Hazardous waste transportation devices; Medical Equipment; Paper products; And woven fabrics, but are not limited to these.

In some embodiments, the length of time an object can be in contact with the gaseous parylene monomer can vary to control the final thickness of the parylene coat on the object. In various embodiments, the final thickness of the parylene coating can be from about 100 angstroms to about 3.0 millimeters. In some embodiments, the final thickness of the parylene coating may be between about 0.5 millimeters and about 3.0 millimeters. In some embodiments, the final thickness of the parylene coating may be between about 0.0025 millimeters and about 0.050 millimeters. Preferably, depending on the temperature of the deposition chamber, a deposition time of about 2 hours to about 18 hours (eg, 5 hours) may be used to achieve a parylene coat thickness of about 0.002 inches (0.050 mm). The choice of the final thickness of the parylene coating can depend on the degree to which the object is coated and the end use of the object. Thinner final coats may be desirable for objects that require some movement to be activated, such as a power button. Thicker coatings may be desirable for the object to be submerged.

The adhesion to various objects of a particular coating composition, for example a composition comprising a parylene compound, can be improved by precoating the surface of the object to be coated with an organic compound, such as silane, before applying the conformal coating. The silane treatment forms radicals on the surface of the object to which parylene can bind. Vinyl trichlorosilane in xylene, isopropanyl alcohol, or freon, and gamma-methacryloxypropyltrimethoxy silane (silquest®) A-174 silane or silquest® A-174 (NT) in methanol-water solvent Two silanes) are used for this purpose. However, electronic components cannot allow the electrical paths generated by direct contact with liquids that allow the conduction of electricity, or they cannot also be combined with iron residues that often remain after evaporation of the immersed liquid or water. Even if there is no immediate growth, the dendritic conductor can grow later due to the voltage between the conductors on the electronic component. These short circuits caused by conductive fluids and dendrites can drain the battery and cause high current to flow in unintended areas, resulting in unintended circuit operation or failure. Often, parts of electronic equipment, such as circuit boards, must be individually coated with silane and parylene and then assembled into the final product.

In some aspects, the disclosure provides a method of coating an object with silane, such as Silquest® Saline. In some embodiments, the method comprises (A.) vaporizing the silane by heating the silane to its evaporation point to form a gaseous silane; And (B.) contacting at least a portion of the surface of the object to be coated (eg, the surface to be coated with the conformal coating comprising parylene) with the gaseous silane of step A. In some embodiments, the silane may be Silquest® A-174, Silquest® 111 or Silquest® A-174 (NT), preferably Silquest® A-174. In some embodiments, in step A, the silane may be vaporized in a 50:50 solution with water. In some embodiments, in step A, the silane may be vaporized at 80 ° C. for about 2 hours.

In some aspects, the present disclosure provides a method of applying a pretreatment with a silane and parylene coating compound to at least a portion of the surface of an object. The method comprises the steps of (A.) vaporizing the parylene dimer by heating to 150 ° C. to 200 ° C. to form a gaseous parylene dimer; (B.) decomposing the gaseous parylene dimer into a gaseous parylene monomer by heating the gaseous parylene dimer to 650 ° C. to 700 ° C .; (C.) vaporizing the silane by heating it to its evaporation point to form a gaseous silane; (D.) contacting the object coated with parylene with the gaseous silane of step C; And (E.) contacting the object coated with parylene with the gaseous parylene monomer of step B for a sufficient time to deposit a parylene coat of final thickness. In some embodiments, the parylene may be selected from the group consisting of parylene D, parylene C, parylene N, parylene HT, and parylene derived from parylene N, preferably be parylene C have. In some embodiments, the silane may be Silquest®, Silquest® A-174, Silquest® 111 or Silquest® A-174 (NT), preferably Silquest® A-174.

In some embodiments, in step A, parylene dimers can be vaporized by heating in two or more steps, preferably at about 170 ° C. and at about 200 ° C. to about 220 ° C. In some embodiments, in step B, parylene dimers can be decomposed by heating in two or more stages, preferably in two stages above about 680 ° C. and above about 700 ° C. In some embodiments, in step C, the silane may be vaporized in a 50:50 solution with water. In another embodiment, in step C, the silane may be vaporized at 80 ° C. for about 2 hours. In some embodiments, the final thickness of the parylene coat may be between about 100 angstroms and about 3.0 mm.

A method comprising pretreating an object with a silane compound

A. vaporizing the parylene dimer form by heating to 150 ° C. to 200 ° C. to form a gaseous parylene dimer;

B. decomposing the gaseous parylene dimer into a gaseous parylene monomer by heating the gaseous parylene dimer to about 650 ° C. to about 700 ° C .;

C. vaporizing the silane by heating it to its evaporation point to form a gaseous silane;

D. contacting the object to be coated with gaseous silane; And

E. contacting the object to be coated with the gaseous parylene monomer for a sufficient time to deposit a parylene coat of final thickness. Steps A, B and E can be carried out by any method currently used for coating by parylene of an object well known to those skilled in the art. In addition, any of the steps may be performed in a different order than that presented. For example, step D may be performed before step A. Also, some steps may be performed concurrently with other steps, eg, step D may be performed simultaneously with step A. In a preferred embodiment, parylene C can be used (see FIG. 1B). In other embodiments, other forms of parylene may be used, including but not limited to Parylene N, Parylene D, and Parylene HT® (see FIGS. 1A, 1B, and 1D). In some embodiments, parylene may be derived from substitution of various chemical moieties from parylene N, or poly-para-xylylene. In a preferred embodiment, parylene can form a material that is completely linear and highly crystalline. In the Examples section, embodiments of the method are described along with a more detailed description of how the method can be performed.

In some embodiments, step A of vaporizing the parylene dimer form by heating to 150 ° C. to 200 ° C. to form a gaseous parylene dimer can be performed in a furnace chamber. In a preferred embodiment, the parylene dimer is heated stepwise to the desired 150 ° C to 200 ° C. In some embodiments, the staged heating of the parylene dimer occurs in a multi-zoned furnace chamber where different temperature set points are allowed in different zones of the furnace chamber. Without being limited to the method of carrying out the stepwise heating procedure, it is believed that the method allows parylene to be “cracked” uniformly with monomers and allows better control of the thickness of the final parylene coating on the object, which is This is because the monomer may remain in the deposition chamber longer and may spread throughout the deposition chamber. In some embodiments, parylene dimers can be vaporized by heating in two, three, four, or more than four steps. In some embodiments, the temperature of the step is about 170 ° C, and about 200 to about 220 ° C. Without being bound to a particular theory, the inventors believe that parylene will be vaporized in the first stage of vaporization, and preheated and decomposed into monomers at higher rates until this vapor enters the pyrolysis chamber in the second stage. Be aware.

In certain embodiments, step B of decomposing the gaseous parylene dimer into gaseous parylene monomers by heating to 650 to 700 ° C. may be performed in a furnace chamber. In a preferred embodiment, the gaseous parylene dimer is heated stepwise to the desired 650 to 700 ° C. In certain embodiments, the staged heating of the gaseous parylene dimer occurs in a multicompartmented furnace chamber that allows different temperature set points in different zones of the furnace chamber. In certain embodiments, parylene dimers are broken down into monomers by heating in two, three, four, or more than four steps. In certain embodiments, the temperature of said step is above about 680 ° C, and about 700 ° C. Without being limited to a particular theory, the gaseous parylene dimer will decompose into monomers in the first heating step and the gaseous monomers are further heated above about 700 ° C. in the second heating step so that the gaseous monomers are deposited in the deposition chamber. It is believed that it will stay longer in, so that it can be filled more evenly.

The method may utilize a step (step D) that allows the gaseous silane (FIG. 1E) to be contacted with the object being coated. This step is particularly advantageous for creating a parylene-coated hydrophilic surface of the object. In certain embodiments, Silquest® silane, Silquest® A-174 (NT) silane or Silquest® A-174 silane are used throughout the method to coat the object with a parylene compound. In one embodiment, the object may be contacted with a gas silane in a vacuum chamber.

In step C, the silane can be vaporized by heating to its evaporation point. In a preferred embodiment, this step can be followed by contacting the pretreated object with said gaseous silane. In one embodiment, the step can be performed by placing the silane into a crucible and placing the crucible into a T 'thermocouple on a hot place in a vacuum chamber containing the object to be coated. The amount of silane poured into the crucible can vary depending on the number and size of objects in the vacuum chamber. In various embodiments, the amount of vaporized silane may range from about 10 to about 100 ml, or in some cases more. In one embodiment, the hot plate may heat the silane to its evaporation point. In other embodiments, other methods of heating the silane to its evaporation point can be used, as is well known to those skilled in the art. In another embodiment, the mixture of silane and distilled water may be vaporized. In one embodiment, a mixture of 50/50 of silane and distilled water is heated until the silane is vaporized (which may be at about 80 ° C. for about 2 hours).

In certain embodiments, the object is pretreated with silane and then pretreated with parylene in the same vacuum chamber, while in other embodiments, the two coatings may be applied at different chambers and / or at different times. In a preferred embodiment, once the exposure of the object to the evaporated silane is complete, the chamber can be placed under vacuum to initiate deposition of parylene as soon as a suitable vacuum is reached. It is desirable to completely consume the silane vapor from the chamber before introducing the gaseous parylene monomer. The period of time between silane pretreatment and application of the parylene coating can be from about 0 minutes to about 120 minutes in various embodiments. The temperature of the silane evaporation point is about 80 ° C. Although the mechanism of action of the silane is not limited, it is believed that pretreatment of the object with vaporized silane causes its surface to have free radical sites to which the parylene monomers can bind, thereby improving its ability to receive parylene monomer gas.

In step D, the object to be coated may be contacted with a gas silane. In a preferred embodiment, the contacting can be done in the same deposition chamber that is later used to contact the gaseous parylene monomer to the object. In certain embodiments, the object is in contact with the gas silane for about 2 hours.

In step E, the object to be coated can be contacted with a gaseous parylene monomer for a sufficient time to deposit the parylene coat. In a preferred embodiment, this step can be carried out in a deposition chamber, particularly preferably in a deposition chamber in which the object is in contact with the silane. In other preferred embodiments, the deposition chamber and the object to be coated may be at room temperature. In certain embodiments, the deposition temperature may be about 5 to about 30 ° C, preferably about 20 to about 25 ° C. In certain embodiments, the deposition chamber may be cooled to speed up the deposition process.

Another embodiment provides a method of treating an object with silane. This method

A. heating the silane to its evaporation point to vaporize to form a gas silane; And

B. contacting the object to be coated with the gaseous silane.

In step A, the silane can be vaporized by heating to its evaporation point. In certain embodiments, Silquest®, Silquest® A-174, Silquest® 111 or Silquest® 174 (NT) are silanes used throughout the method. In a preferred embodiment, this step can be followed by contacting the pretreated object with said gaseous silane. In one embodiment, the step can be performed by placing the silane into a crucible and placing the crucible into a 2 "thermocouple on a hot place in a vacuum chamber containing the object to be coated. The amount of silane poured into the crucible is the vacuum chamber Depending on the number and size of objects in. In various embodiments, the amount of vaporized silane may range from about 10 to about 100 ml, or in some cases more. The silane can be heated to its evaporation point In other embodiments, other methods of heating the silane to its evaporation point can be used, as is well known to those skilled in the art In another embodiment, the silane and distilled water In one embodiment, a mixture of 50/50 of silane and distilled water is evaporated until the silane is vaporized (at about 80 ° C. May be for 2 hours).

In step B, the object to be coated may be contacted with a gas silane. In some embodiments, the object is in contact with the gas silane for about 2 hours.

Also provided is a method of applying a coating comprising a conformal coating compound and a thermally conductive material. In certain embodiments, the method comprises heating the conformal coating compound to form a gaseous monomer of the conformal coating compound; Combining a thermally conductive material with the gaseous monomer to form a gaseous mixture; And applying an conformal coating to the object by contacting the object with the gaseous mixture under conditions such that a conformal coating comprising a conformal coating compound and a thermally conductive material is formed on at least a portion of the surface of the object. .

As used herein, a "gas mixture" is a mixture comprising one or more components of the gas phase (gas phase), and one or more other components present or absent in the gas phase. For example, the gaseous mixture may comprise a gaseous conformal coating compound, and a solid compound (eg, powder particles) suspended in the conformal coating compound vapor. Similarly, the gaseous mixture may comprise a gaseous conformal coating compound and a liquid compound (eg, spray liquid) suspended in the conformal coating compound vapor. In addition, the gaseous mixture may comprise multiple gas phase components (eg, a plurality of different vapor conformal coating compounds). It is understood that the gaseous mixture may comprise any number of components of the same and / or different phases. In certain embodiments, the gaseous mixture comprises one or more vapor conformal coating compounds (eg parylene) and one or more thermally conductive materials. In certain embodiments, the thermally conductive material in the gaseous mixture is a solid phase (eg, powder particles). In certain embodiments, the thermally conductive material in the gaseous mixture is liquid. In another embodiment, the thermally conductive material in the gaseous mixture is gaseous.

The coating methods disclosed herein can be used in commercial marine, leisure boat, military (aerospace and defense), industrial and medical industries, as well as other uses disclosed herein and products known in the art. In certain cases, the coating process can be specifically designed to "seal" the device. Thus, the coating method may be useful for protecting devices commonly used in the ocean and in hazardous environments against exposure to moisture, flooding, dust, strong wind action, and malfunctions during operation caused by chemicals. Can be. The coating can improve the viability and sustainability of operating equipment and high value specialty products that are sensitive to corrosion and degradation.

In another aspect, the present disclosure provides a method of forming a gaseous parylene dimer, comprising: (A.) heating parylene dimer to about 150 to about 200 ° C. to vaporize it; (B.) heating the gaseous parylene dimer to about 650 to about 700 ° C. to decompose it into gaseous parylene monomers; (C.) injecting boron nitride into the gaseous parylene monomer of step B; And (D.) contacting the object coated with parylene with the gaseous parylene monomer and boron nitride of step C for a sufficient time to deposit a coat of parylene and boron nitride of final thickness. Provided is a method of applying a conformal coating comprising a len compound and boron nitride to at least a portion of the surface of an object. Although any parylene may be used in the process, parylene D, parylene C, parylene N and parylene HT® may be preferred, and parylene C may be particularly preferred. In certain preferred embodiments, boron nitride may be injected into the gaseous parylene monomer as a powder, preferably from about 18 micrometers to about 25 micrometers. In other embodiments, step D may occur at about 5 ° C to about 30 ° C. In certain embodiments, the final thickness of the coat may be between about 100 angstroms and about 3.0 millimeters. In certain embodiments, the method can have an additional step E that can contact the coated object with the silane composition until the object is coated with silane.

In certain embodiments, the method comprises a uniform thin layer of conformal coating comprising parylene compound and boron nitride at a thickness of 0.01-3.0 mm depending on the article coated using standard chemical vapor deposition in a vacuum chamber at 25 ° C. Apply with Once coated the article is weather and water resistant and can withstand exposure to extreme weather conditions and exposure to most chemicals. Any solid surface can be coated, including plastics, metals, wood, paper, and fabrics. Sample articles include electronic devices such as mobile phones, radios, circuit boards, and speakers; Equipment used for offshore and space exploration; Hazardous waste transportation devices; Medical Equipment; Paper products; And woven fabrics, but are not limited to these.

Thus, the method of coating an object with a composition of parylene and boron nitride may comprise several steps: A. Parylene dimer is heated to 150 to 200 ° C. to vaporize to form a gaseous parylene dimer. Making; B. heating the gaseous parylene dimer to 650-700 ° C. to decompose it into gaseous parylene monomers; C. injecting boron nitride into the gaseous parylene monomer of step B; And contacting the object to be coated with the gaseous parylene monomer and boron nitride for a sufficient time to deposit a parylene coat of final thickness.

Steps A and B of the method of coating the object with parylene and boron nitride may be carried out in any manner currently used for vapor coating of the object with parylene and will therefore be well known to those skilled in the art. In addition, the steps may be performed in a different order than the one currently being performed. In a preferred embodiment, parylene C is used. In other embodiments, other forms of parylene may be used, including but not limited to parylene N, parylene D, and parylene HT®. In certain embodiments, parylene may be derived from substitution of various chemical moieties, from parylene N, or poly-para-xylylene. In a preferred embodiment, parylene forms a material that is completely linear and highly crystalline. In the Examples section, embodiments of the method are described along with a more detailed description of how the method can be performed.

In certain embodiments, step A, wherein the parylene dimer form is vaporized by heating to 150-200 ° C. to form a gaseous parylene dimer, can be performed in a furnace chamber. In certain embodiments, step B, wherein the gaseous parylene dimer is heated to 650 to 700 ° C. to decompose it into gaseous parylene monomers, can be performed in a furnace chamber. In certain embodiments, step C of injecting boron nitride into the gaseous parylene monomer of step B may be performed after step B. In certain embodiments, boron nitride may be injected as a powder into the gaseous parylene monomer. One embodiment of this step is described in the Examples. In certain embodiments, the boron nitride powder may be at least about 500 grit. In certain embodiments, the boron nitrite powder is about 1.8 micrometers to about 2.5 micrometers.

In step D, the object to be coated may be contacted with gaseous parylene monomer and boron nitride for a sufficient time to deposit a coat of parylene and boron nitride on the object. In certain embodiments, the step can be performed in a deposition chamber. In other embodiments, the deposition chamber and the object to be coated may be present at room temperature, from about 5 ° C to about 30 ° C, or most preferably from about 20 ° C to about 25 ° C. In certain embodiments, the final thickness of the parylene-boron nitride coat on the object can be adjusted by modifying the length of time that the object can be contacted with the gaseous parylene monomer and boron nitride. In various embodiments, the final thickness of the parylene-boron nitride coating can be about 100 angstroms to about 3.0 millimeters. In certain embodiments, parylene is deposited from about 8 hours to about 18 hours to obtain a coating thickness of about 0.05 mm. In certain embodiments, parylene is deposited from about 5 hours to about 18 hours to obtain a coating thickness of about 0.05 mm. In a preferred embodiment, the final thickness of the parylene coating can be about 0.5 mm to about 3.0 mm. The choice of the final thickness of the parylene coating depends to some extent on the object being coated and the end use of the object. Thinner final coats may be desirable for objects that require some mobility to be functional, such as a power button. Thicker coatings may be desirable for the object to be submerged.

In certain embodiments, the method may have an additional step E of contacting the coated object with the silane composition until the object is pretreated with silane. In a preferred embodiment, said step can be carried out before step D. In certain embodiments, the silane composition may be in a dissolved state when contacting an object therewith. In other embodiments, the silane composition may be present as a gas when the object is in contact with it. In certain embodiments, the silane composition may be Silquest® A-174 silane (FIG. 1E). This step is particularly advantageous for creating a parylene-coated hydrophilic surface of the object.

Example

Example 1 A method and apparatus used to coat an object with parylene.

This embodiment used Parylene C.

Coating process

The apparatus consisted of two parts ((1) furnace / heating part; and (2) vacuum part). The furnace section consisted of two furnaces connected by glass tubes called retort. The furnace and vacuum portion were connected by a valve that allowed gas to flow between the furnace and the vacuum portion.

The furnace part of the device was made by Mellen Furnace Co. (Concord, New Hampshire, USA). See Example 2. The vacuum portion was made by Laco Technologies Inc., Salt Lake City, Utah.

The process for coating the article with parylene is as follows:

(1) First furnace chamber. Parylene C in dimer form (two molecule form) in sufficient quantity to coat the article was placed in the furnace chamber. The article was coated to a thickness ranging from 0.01 to 3.0 mm. Parylene C was placed in a stainless steel "boat" (standard vessel made of metal or glass), which was inserted into the furnace through a vacuum secured opening in the tube (the boat used the rod to load the furnace). Push). The hole was sealed after inserting Parylene C. The furnace was then brought to 150-200 ° C. to create an environment in which solid parylene C became a gas. Gas was maintained in the first furnace chamber until the two valves were opened. The first of the two valves was not opened until the cold trap in the vacuum portion was filled with liquid nitrogen (LN2) and the trap was "cooled". LN2 was purchased from local suppliers. LN2 was placed in a 1 gallon container of the feeder. LN2 was injected from the vessel into the "trap". The second valve was variable and opened when the gas was drawn out of the first furnace by vacuum.

(2) a second furnace chamber. Parylene C gas was transferred to a second furnace at a temperature of 650 to 700 ° C. The heat of the furnace caused the parylene C gas to separate into individual molecules (monomers). The gas in monomeric form was then drawn out into the deposition chamber by vacuum.

(3) vacuum chamber. The vacuum portion of the machine consisted of a deposition chamber with two vacuum pumps. The first vacuum pump was a "roughing" pump that produced an initial vacuum. Initial pressure was in the range of 1 × 10 ⁻³ Torr. The second stage pump then produced a final pressure in the range of 1 × 10 ⁻⁴ Torr. The vacuum pump was protected using a liquid nitrogen trap that protects the pump from solidification of the monomer gas by condensing the gas on the cold trap surface.

The article to be coated was placed on a shelf in the deposition chamber before starting the coating process. The devices to be coated were masked (by one of ordinary skill in the art) in the areas above and within the devices that would not be coated. Shielding was performed in areas where electrical or mechanical connections should remain. The material was coated on the article at room temperature (75 ° F.).

Inside the vacuum chamber was a crucible of Silquest® A-174 silane (Momentive Performance Materials Inc., Wilton, Conn.) Injected into a ceramic crucible. The crucible was inserted into a 2 inch thermocouple on a hot plate in a vacuum chamber. The amount of Silquest® A-174 silane injected was 10-100 ml, depending on the amount of article in the chamber. The Silquest® A-174 silane was heated to the evaporation point with a plate such that Silquest® A-174 silane coated the entire area inside the chamber, including any article inside the chamber.

Once the Silquest vapors were withdrawn from the deposition chamber, the monomer gas was drawn off by the lower vacuum in the vacuum chamber. When the gas was drawn into the chamber it deflected and was injected into the entire area of the chamber. The article was coated as the monomer gas cooled. The gas was cooled at 600 ° C. to 25 ° C. and cured on the device in the chamber. During the cooling process, monomer was deposited on the surface of the article to be coated to produce a homogeneous, pinhole free polymer three dimensional chain. The deposition rate and final thickness were controlled by the deposition apparatus. The desired thickness of the parylene coating was determined by the time it was exposed to the monomer gas. The thickness can range from several hundred angstroms to several millimeters.

Example 2: Zoned furnaces usable in apparatus for applying parylene coatings.

The furnace assembly was manufactured by Mellen Company, Inc. (Concord, New Hampshire, USA). Melen Model TV12.

Single zone or two zoned-solid tubular furnaces could be operated at temperatures below 1200 ° C. in air. The furnace used a Mellen standard Series 12V heating element (exposed Fe-Cr-Al windings in a specially designed holder). The furnace has an energy-efficient ceramic fiber insulation package with a 2 "single length connection path. The thermocouple is located at the center of each zone. Provides a 10 foot long power cable for each zone to connect to the power supply. The furnace is designed for horizontal or vertical operation and the detailed specifications are as follows.

Melene  series PS205  Power supply / temperature controller

One Melen model PS205-208- (2) 25-S, two zones, digital thermostat and solid state relay. Melen series PS205

a.) Two digital temperature controllers, calibrated for type "S" thermocouples, featuring 126 segments & 31 programs

b.) one solid state relay,

c.) one two-pole General Electric breaker or equal circuit breaker, with an appropriately rated amperage rating,

d.) one melen cabinet for containing said ingredients,

e.) two type "S" thermocouples, including 10 compensating thermocouple extension wires per area, end boards, etc.,

f.) all necessary wiring, end boards, interconnects, etc. to create a fully operational system;

Was done.

Over temperature for power supply / temperature controller ( over - temperature ) protect

One over temperature (O.T.) alarm with independent digitally specified digital setpoint "hi-limit alarm" regulator. O.T. The alarm package was provided with appropriate thermocouples, TIC extension wires, and sufficient mechanical power contactor (s) to shut off power to the furnace when an over temperature condition occurred at the location of the over temperature sensor. O.T. Alarm options are located in the central thermostat details.

Retort Model: RTA  -2.5 x32- OBE

One melen model RTA-2.5-32-OBE, round, Hi-Purity Alumina retort used with the furnace described above (actual system has quartz retort). The retort working diameter is approximately 2.5 inches l.D. X 32 inches. The retort included a stainless steel flange / steel assembly and a heat shield that were approximately 2.75 "inches long by O.D., 48" inches long, and required for hermetic operation. Feedthroughs were provided to the retort's cover plate for gas injection / exhaust and temperature measurement. The retort could operate in different types of atmospheres.

Example  3: Parylene  And With boron nitride  A method and apparatus used to coat an object.

This embodiment used Parylene C.

Coating process

The apparatus consisted of two parts ((1) furnace / heating part and (2) vacuum part). The furnace section consisted of two furnaces connected by glass tubes called retort. The furnace and vacuum sections were connected by valves that allowed gas to flow between the furnace and vacuum sections.

The furnace part of the device was manufactured by Melen Furnace Company (Concord, New Hampshire, USA). The vacuum part is Laco Technologies Inc. (Salt Lake City, Utah, USA).

The process for coating the article with parylene and boron nitride is as follows.

(1) First furnace chamber. Parylene C in dimer form (two molecule form) in sufficient quantity to coat the article was placed in the furnace chamber. The article was coated to a thickness ranging from 0.01 to 3.0 mm. Parylene C was placed in a stainless steel "boat" (standard vessel made of metal or glass), which is inserted into the furnace through the vacuum sealing hole of the tube (the boat is pushed into the furnace using a rod). The hole was sealed after inserting Parylene C. The furnace was then brought to 150-200 ° C. to create an environment in which solid parylene C became a gas. Gas was maintained in the first furnace chamber until the two valves were opened. The first of the two valves was not opened until the cold trap in the vacuum portion was filled with liquid nitrogen (LN2) and the trap was "cooled". LN2 was purchased from local suppliers. LN2 was placed in a 1 gallon container of the feeder. LN2 was injected from the vessel into the "trap". The second valve was variable and opened when the gas was drawn out of the first furnace by vacuum.

(2) a second furnace chamber. Parylene C gas was transferred to a second furnace at a temperature of 650 to 700 ° C. The heat of the furnace caused the parylene C gas to separate into individual molecules (monomers). The gas in monomeric form was then drawn out into the deposition chamber by vacuum.

Boron nitride in powder form was placed in a KF 16 tube connected to a KF connector with a “T” KF 16 port. The K1716 tube was partially filled with a "fill" of boron nitride powder (minimum 500 grit). KF 16 tubes were capped. After the coating process began, boron was injected into the coating "stream". Boron flowed into the powder and was captured by the deposition of the coating process.

The K1716 tube was attached to a retort perpendicular to the flow of monomer gas just before the monomer gas entered the deposition chamber. There was an open valve to allow boron nitride to flow into the gas. The gas was deposited with the monomer and deposited on the article to be coated. The process was similar to powder coating. The process could be repeated to increase the amount of boron nitride inserted into the coating on the article. Without limiting the properties of the boron nitride / parylene coating, it is believed that boron nitride provides a method for improving the hardness of the coating and for better escape of heat from coated articles, such as electronic devices. Boron nitride was inserted into parylene as dust.

(3) vacuum chamber. The vacuum portion of the machine consisted of a deposition chamber with two vacuum pumps. The first vacuum pump was a "roughing" pump that produced an initial vacuum. Initial pressure was in the range of 1 × 10 ⁻³ Torr. The second stage pump then produced a final vacuum in the range of 1 × 10 ⁻⁴ Torr. The vacuum pump was protected using a liquid nitrogen trap that protects the pump from solidification of the monomer gas by condensing the gas on the cold trap surface.

The article to be coated was placed on top of the deposition chamber before starting the coating process. The devices to be coated were shielded (by the skilled person's method) in the areas above and in the areas that would not be coated. Shielding was performed in areas where electrical or mechanical connections should remain. The material was coated on the article at room temperature (75 ° F.).

Inside the vacuum chamber was a crucible of Silquest® A-174 silane which was injected into a ceramic crucible. The crucible was inserted into a 2 inch thermocouple on a hot plate in a vacuum chamber. The amount of Silquest® A-174 silane injected was dependent on the amount of article in the chamber, for example 10 to 100 ml. The Silquest® A-174 silane was heated to the evaporation point with a plate such that Silquest® A-174 silane coated the entire area inside the chamber, including any article inside the chamber.

The monomer gas was drawn off by the lower vacuum in the vacuum chamber. As gas was drawn into the chamber it was deflected and injected into the entire area of the chamber. The article was coated as the monomer gas cooled. The gas was cooled from 600 ° C. to 25 ° C. and cured on the device in the chamber. During the cooling process, monomer was deposited on the surface of the article to be coated to produce a homogeneous, pinhole free polymer three dimensional chain. The deposition rate and final thickness were controlled by the deposition apparatus. The desired thickness of the parylene coating was determined by the time it was exposed to the monomer gas. The thickness could range from several hundred angstroms to several millimeters.

While some aspects and embodiments of the invention have been described, it will be apparent that various modifications, changes and adjustments to these embodiments may be made by those skilled in the art while obtaining some or all of the advantages of the invention. For example, in some embodiments of the invention disclosed herein, a single component can be replaced by a multiple component, and the multiple component can be replaced by a single component to perform a certain function or functions. Except where such substitutions are not used to practice embodiments of the invention, such substitutions are within the scope of the present invention. Accordingly, the disclosed embodiments are intended to embrace all such alterations, modifications and adjustments without departing from the scope and spirit of the invention as defined by the appended claims. Preferred features of each of the aspects and embodiments of the invention are each of the other aspects and embodiments, with only minor modifications necessary.

It is also to be understood that the figures and detailed description of the present disclosure have been simplified to illustrate elements associated with a clear understanding of the present disclosure, while excluding elements of clarity and other elements, such as conventional conformal coating methods or devices. . For example, certain conformal coating systems may include additional components not described herein, such as deposition chambers, valves, and vacuum pumps. However, those skilled in the art will appreciate that these and other elements may be required for a typical conformal coating system. However, as such elements are well known in the art and do not better understand the present disclosure, discussion of such elements is not provided herein.

Furthermore, in the claims appended hereto, any element described as a means for performing a particular function is to include any method of performing the function, including, for example, a combination of elements that perform the function. . Furthermore, the invention described in the method and functional claims is based on the fact that the functionality provided by the incorporation of the various cited means is combined and combined in a manner as defined by the appended claims. Thus, any means capable of providing such functionality may be considered equivalent to the means disclosed herein.

For purposes of this specification, unless stated otherwise, all numbers expressing quantities of components, time, temperature, thickness of coatings, and other properties or variables used in the specification are modified by the term "about" in all examples. It should be understood that. Accordingly, unless indicated to the contrary, the numerical variables set forth in the following description and appended claims should be understood to be approximations. At the very least, without attempting to limit the application of the equivalence principle to the scope of the claims, the numerical variable should be construed in light of the number of reported significant digits and the application of ordinary skill in the art.

In addition, while the numerical ranges and variables setting forth the broad scope of the invention are approximations as discussed above, the numerical values set forth in the Examples section have been described as precisely as possible. However, it should be understood that such numerical values inherently include some error arising from the measurement device and / or measurement technique.

The entirety or part of any patent, publication, or other disclosed material incorporated herein by reference is cited herein only to the extent that the referenced material does not conflict with existing definitions, statements, or other disclosed materials described in this disclosure. Accordingly, and to the extent necessary, the disclosure expressly described herein supersedes any conflicting content incorporated herein by reference. While incorporated herein by reference, any material, or portion thereof, that conflicts with existing definitions, statements, or other disclosures described herein will be cited such that there is no conflict between the cited material and the previously disclosed material.

Claims (56)

A coating composition comprising a conformal coating compound and a thermally conductive material. The coating composition of claim 1, wherein the conformal coating compound is a parylene compound optionally selected from the group consisting of Parylene D, Parylene C, Parylene N, and Parylene HT® compounds. The coating composition of claim 2 comprising at least two different parylene compounds. The coating composition of claim 2 or 3 comprising at least two parylene compounds having different purity levels. The coating composition of claim 1 wherein the thermally conductive material is a ceramic. The coating composition of claim 1, wherein the thermally conductive material is selected from the group consisting of aluminum nitride, aluminum oxide and boron nitride. The coating composition of claim 1, wherein the thermally conductive material has a volume resistivity of greater than 10 ¹⁰ ohm * cm. The coating composition of claim 1, wherein the mass of the thermally conductive material is about 3% or less of the total mass of the conformal coating compound and the thermally conductive material. The coating composition of claim 1, wherein the mass of the thermally conductive material is about 1% or less of the total mass of the conformal coating compound and the thermally conductive material. 10. The coating composition of claim 2 having a thermal conductivity of 5-10% greater than the thermal conductivity of the parylene compound alone. The coating composition of claim 1 having a hardness of about R80 to about R95. The coating composition of claim 1, wherein the thermally conductive material is dispersed in a polymer of the conformal coating compound. A conformal coating on at least a portion of the surface of an object, comprising the coating composition of claim 1. The radio of claim 13, wherein the object is a communication device, a speaker, a mobile phone, an audio player, a camera, a video player, a remote control device, a satellite positioning system, a computer component, a radar display, a depth finder, a fish finder, an emergency positioning radio. Conformal coating, which is an electronic device selected arbitrarily from an indicator position-indicating radio beacon (EPIRB), an emergency locator transmitter (ELT) and a personal locator beacon (PLB). The method of claim 13, wherein the object is a paper product; Textile products; Art work; A circuit board; Offshore exploration devices; Space exploration devices; Hazardous waste transportation devices; Automotive devices; Electromechanical devices; Military system components; ammunition; gun; weapon; Medical Equipment; And a biomedical device optionally selected from the group consisting of hearing aids, cochlear ear implants, and prostheses. The conformal coating according to claim 13, wherein the surface is plastic, metal, wood, paper or fabric. The conformal coating of claim 13, wherein the surface is an exterior surface of the object. The coating composition according to claim 1, which is a gaseous mixture comprising monomers of conformal coating compounds in a gaseous phase. The coating composition of claim 18, wherein the gaseous mixture comprises a thermally conductive material of solid particles. An object comprising a conformal coating composed of the coating composition of claim 1 on at least a portion of the surface. 21. A radio beacon according to claim 20, comprising a communication device, a speaker, a mobile phone, an audio player, a camera, a video player, a remote control device, a satellite positioning system, a computer component, a radar display, a depth finder, a fish finder, an emergency position indicator An electronic element arbitrarily selected from an EPIRB), an emergency location transmitter (ELT) and a personal location signal (PLB). 21. The article of claim 20, further comprising: paper products; Textile products; Art work; A circuit board; Offshore exploration devices; Space exploration devices; Hazardous waste transportation devices; Automotive devices; Electromechanical devices; Military system components; ammunition; gun; weapon; Medical Equipment; And a biomedical device optionally selected from the group consisting of hearing aids, cochlear implants and prostheses. The object of claim 20, wherein the surface is plastic, metal, wood, paper or fabric. The object of claim 20, wherein the surface is an outer surface. The object of claim 20, wherein the surface is coated with a substantially conformal coating. A) heating the conformal coating compound to form a gaseous monomer of the conformal coating compound,
B) combining a thermally conductive material with the gaseous monomer to form a gaseous mixture and
C) applying the conformal coating to the object by contacting the object with the gaseous mixture under conditions such that a conformal coating comprising a conformal coating compound and a thermally conductive material is formed on at least a portion of the surface of the object.
Comprising a conformal coating on the object. 27. The method of claim 26, wherein the conformal coating compound is a parylene compound optionally selected from the group consisting of parylene D, parylene C, parylene N, and parylene HT® compounds. 28. The method of claim 26 or 27, wherein the thermally conductive material is a ceramic. 28. The method of claim 26 or 27, wherein the thermally conductive material is selected from the group consisting of aluminum nitride, aluminum oxide and boron nitride. 30. The method of any one of claims 26-29, wherein the thermally conductive material is in the form of solid particles. The method of claim 30, wherein the solid particles are about 1.8 micrometers to about 2.5 micrometers. A) heating the parylene compound to a temperature of about 125 to about 200 ° C. to form a gaseous parylene compound, wherein heating of the parylene compound is carried out in at least two heating steps,
B) heating the gaseous parylene compound to a temperature of about 650 to about 700 ° C. to decompose the gaseous parylene compound to form a parylene monomer, and
C) applying the coating to the object by contacting the object with the parylene monomer under conditions such that a conformal coating comprising a parylene polymer is formed on at least a portion of the surface of the object
Comprising a conformal coating on the object. 33. The method of claim 32, wherein step A comprises heating the parylene compound to a temperature of about 125 to about 180 ° C and heating the parylene compound to a temperature of about 200 to about 220 ° C. 34. The method of claim 32 or 33, wherein the heating of the gaseous parylene compound is carried out in two or more stages. 35. The method of any of claims 32-34, wherein step B comprises heating the gaseous parylene compound to a temperature of about 680 ° C and heating the gaseous parylene compound to a temperature of about 700 ° C or more. Which method. 36. The method of any one of claims 32-35, wherein the parylene compound is selected from the group consisting of parylene D, parylene C, parylene N, and parylene HT® compounds. 37. The method of any one of claims 26 to 36, further comprising, prior to step C, contacting the object with gaseous silane under conditions that the silane activates the surface of the object. 38. The method of claim 37, wherein the silane is at least one silane selected from the group consisting of Silquest® A-174, Silquest® 111, and Silquest® A-174 (NT). The method of claim 26, wherein the object is at a temperature of about 5 ° C. to about 30 ° C. during Step C. 40. 40. The method of any one of claims 26-39, wherein the conformal coating is from about 100 angstroms to about 3.0 millimeters. 41. The method of any one of claims 26-40, wherein the conformal coating is about 0.0025 mm to about 0.050 mm thick. 42. The apparatus of any of claims 26 to 41, wherein the object is a communication device, speaker, cell phone, audio player, camera, video player, remote control device, satellite positioning system, computer component, radar display, depth meter, And an electronic device arbitrarily selected from a fish finder, an emergency position indication radio beacon (EPIRB), an emergency position information transmitter (ELT) and a personal position signal (PLB). 42. The method of claim 26, wherein the object is a paper product; Textile products; Art work; A circuit board; Offshore exploration devices; Space exploration devices; Hazardous waste transportation devices; Automotive devices; Electromechanical devices; Military system components; ammunition; gun; weapon; Medical Equipment; And a biomedical device optionally selected from the group consisting of hearing aids, cochlear implants and prostheses. 44. The method of any one of claims 26 to 43, wherein the surface is plastic, metal, wood, paper or fabric. An object wherein a coating is applied to at least a portion of a surface by the method of any one of claims 26 to 41. 46. The object of claim 45, wherein the surface is an outer surface. A vaporization chamber comprising two or more temperature zones;
A pyrolysis chamber operably connected to the vaporization chamber; And
A vacuum chamber operatively connected to the pyrolysis chamber
Apparatus for applying a conformal coating to the object, comprising. 48. The apparatus of claim 47, further comprising a connection operatively connecting the pyrolysis chamber and the vacuum chamber, capable of transferring gas between the pyrolysis chamber and the vacuum chamber, and comprising a T-port. 49. The device of claim 47 or 48, wherein the T-port is operably connected with means for injecting a thermally conductive material into the gas transferred from the pyrolysis chamber through the connection to the vacuum chamber. 50. The apparatus of claim 47, wherein the vacuum chamber comprises a deposition chamber and a vacuum generating component operably connected to the pyrolysis chamber. 51. The apparatus of claim 50, wherein the vacuum generating component comprises one or more vacuum pumps. 52. The device of any of claims 47-51, wherein the vaporization chamber has two temperature zones. 53. The apparatus of any one of claims 47-52, wherein the vaporization chamber is a tubular furnace. 54. The apparatus of any of claims 47-53, wherein the pyrolysis chamber has a plurality of temperature zones. 55. The apparatus of any of claims 47-54, wherein the pyrolysis chamber has two temperature zones. The apparatus of claim 47, wherein the pyrolysis chamber is a tubular furnace.

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