TW201431977A - Metal and electronic device coating process for marine use and other environments - Google Patents

Abstract

The present disclosure relates, in part, to Parylene based conformal coating compositions having improved properties, e.g. improved heat transfer and durability characteristics, as well as a methods and apparatus to coat objects with these compositions, and objects coated with these compositions. In some aspects, coating compositions comprising Parylene and boron nitride are disclosed. The disclosure also includes objects (e.g., electronic equipment, textiles, etc.) having a conformal coating comprising a Parylene compound and boron nitride.

Description

Metal and electronic component coating processes for marine use and other environments

The present invention is directed, in part, to conformal coating compositions having improved properties, for example, improved heat transfer characteristics and improved resistance characteristics, and methods and apparatus for coating articles using such compositions, And articles coated with the compositions, for example, electronic devices.

Conformal coatings (for example, coatings with high resistivity and moisture resistance) are often used to protect commercial components used in the consumer, automotive, military, medical, and aerospace industries. In the device. A variety of methods are currently available for coating such coatings. For example, low pressure chemical vapor deposition can produce a thin, uniform conformal (also known as conformate) coating on various surfaces. There is a need for improved methods for coating conformal coatings in order to expand their use. Furthermore, there is a need for new coating compositions whose characteristics will improve their effectiveness in a particular application. For example, in particular, coating layers with greater tolerance and greater heat transfer characteristics are sought.

Applicants have found ultra-thin, conformal polymer coatings that prevent moisture infiltration to some extent, and methods and apparatus for applying such coatings to articles. An ultra-thin, conformal polymer coating that prevents moisture from penetrating can be applied directly to a wide range of materials In particular, it includes "off-the-shelf" electronic devices. Accordingly, certain aspects of the invention include compositions, methods, and devices for coating articles. In other aspects, the present invention discloses conformal coating compounds capable of forming an ultra-thin, conformal coating on an article, such as a parylene compound. In other aspects, the present invention discloses a coating composition comprising: a conformal coating compound capable of forming an ultrathin, conformal coating layer; and one (or more) additives (eg, a thermally conductive material, for example, Boron nitride) is used to modify any of the properties of the conformal coating layer (for example, it includes resistivity, thermal conductivity, light transmission, hardness, and resistance). In other views, the present invention encompasses "off-the-shelf" electronic devices, such as mobile phones and mp3 players, having an ultra-thin, conformal coating (for example, a water-repellent coating) that prevents moisture from penetrating. The present invention also discloses a method and apparatus for applying an ultra-thin, conformal coating on the surface of an article by vapor deposition. In other aspects, the present invention discloses a multi-stage heating apparatus for vapor deposition of an ultrathin, conformal polymer coating. Articles disclosed herein to be coated by such coating compositions and methods include: electronic devices such as mobile phones, radios, circuit boards, and speakers; equipment for marine and space detection; hazardous waste transportation Equipment; medical equipment; paper products; and textiles. Any solid surface of an article can be coated, including plastic, metal, wood, paper, and textile materials. Biomedical components (for example, hearing aids, cochlear implants, prosthetic limbs, etc.), automatic vehicles, motor systems, art (painting, woodwork, watercolor, chalk, ink painting, charcoal painting), military system components, ammunition, guns Branches, weapons, and identical objects can be coated using the methods and coating compositions disclosed herein.

According to certain aspects, the coating composition provided by the present invention comprises a conformal coating compound and a thermally conductive material. In some embodiments, the thermally conductive material is interspersed among the polymers of the conformal coating compound. In some embodiments, the coating composition is a solid (for example, a conformal coating) having a hardness of from about R80 to about R95. In some embodiments, the coating composition is a gaseous mixture comprising a conformal coating compound monomer in the vapor phase. In a particular embodiment, the gaseous mixture comprises solid particles of the thermally conductive material.

In some embodiments, the conformal coating compound is a parylene compound, optionally selected from the group consisting of: a D-type poly-p-xylene compound, a C-type poly-p-xylene compound. , N-type poly-p-xylene compound and HT-type parylene compound®. In some embodiments, the coating composition includes two or more different parylene compounds. In some embodiments, the coating composition comprises two or more parylene compounds of different purities. In some embodiments, the coating composition has a thermal conductivity that is 5 to 10% higher than the parylene compound alone. In some embodiments, the coating composition has a thermal conductivity level that is 10% higher than the individual parylene compound alone. In some embodiments, the coating composition has a thermal conductivity that is up to about 5% higher than the parylene compound alone.

In some embodiments, the thermally conductive material is a 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 thermal conductivity of the thermally conductive material is greater than 1010 ohms*cm. In some embodiments, the amount of thermally conductive material in the coating composition is up to about 3% (or even higher) of the total mass of the conformal coating compound and the thermally conductive material in the coating composition. In some embodiments, the amount of thermally conductive material in the coating composition is up to about 1% of the total mass of the conformal coating compound and the thermally conductive material in the coating composition.

In some aspects, the conformal coating provided by the present invention is positioned over at least a portion of the surface of an article. In some embodiments, the conformal coating layer comprises any of the foregoing coating compositions.

In some embodiments, the conformal coating layer is over at least a portion of a surface of an article, wherein the article is an electronic component. Depending on the situation, the electronic component may be selected from the following: communication components, speakers, mobile phones, audio players, cameras, video players, remote controls, global positioning systems, computer devices, radar displays, depth detectors, Fish Detector, Emergency Positioning Radio Beacon (EPIRB), Emergency Positioning Signal Transmitter (ELT), and Personal Positioning Beacon (PLB).

In some embodiments, the conformal coating layer is positioned on at least a portion of a surface of an article, wherein the article is selected from the group consisting of: paper products, textile products, artwork, Circuit boards, marine detecting components, space detecting components, hazardous waste transporting components, automatic vehicle components, motor components, military system components, ammunition, firearms, weapons, medical instruments, and biomedical components, wherein the biomedical components are as appropriate The ground is chosen to be free among the following groups: hearing aids, cochlear implants, and prostheses.

In some embodiments, the conformal coating layer is on at least a portion of a surface of an article, wherein the surface is a plastic, metal, wood, paper, or textile material. In a particular embodiment, the surface is the outer surface of the article. In a particular embodiment, the surface is the inner surface of the article.

In some aspects, the invention provides an article comprising a conformal coating layer over at least a portion of a surface. In some embodiments, the conformal coating on the surface of the article comprises any of the foregoing coating compositions.

In some embodiments, the object is an electronic component that is optionally selected from the group consisting of: communication components, speakers, mobile phones, audio players, cameras, video players, remote controls, global Positioning systems, computer devices, radar displays, depth detectors, fish finder, emergency finger radio beacons (EPIRB), emergency location signal transmitters (ELTs), and personal location beacons (PLBs).

In some embodiments, the article is selected from the group consisting of: paper products, textile products, artwork, circuit boards, marine detecting components, space detecting components, hazardous waste transport components, automated vehicle components, Motor components, military system components, ammunition, guns, weapons, medical instruments, and biomedical components, wherein the biomedical components are optionally selected from the group consisting of hearing aids, cochlear implants, and prosthetic limbs.

In some embodiments, the surface of the article is plastic, metal, wood, paper, or textile material. In a particular embodiment, the article will be coated on an outer surface. In a particular embodiment, the article will be coated on an inner surface. In some embodiments, the surface is substantially covered by the conformal coating. A substantially covered surface may be a fully covered or fully covered surface to protect the underlying surface of the article from contact with the material (e.g., water) that the protection desires to isolate.

In some aspects, the invention provides a method of applying a conformal coating to an article. In some embodiments, the method comprises: A) heating a conformal coating compound to form a gaseous monomer of the conformal coating compound; B) combining a thermally conductive material with the gaseous monomer, thereby Forming a gaseous mixture; and C) allowing the article to contact the gaseous mixture under conditions in which the conformal coating layer comprising the conformal coating compound and the thermally conductive material is formed on at least a portion of the surface of the article A conformal coating is applied to the article.

In some embodiments of the methods, the conformal coating compound is optionally selected from the group consisting of polyparaxylene compounds in the group consisting of: a D-type poly-p-xylene compound, a C-type parylene. Compound, N-type parylene compound, and HT-type parylene compound®.

In some embodiments of the methods, 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 a particular embodiment, the thermally conductive material is in the form of solid particles. In a particular embodiment, the solid particles are from about 1.8 microns to about 2.5 microns.

In some embodiments, the method comprises: A) heating a parylene compound to a temperature of from about 125 ° C to about 200 ° C to form a gaseous parylene compound, wherein the poly pair Heating of the toluene compound can be carried out in two or more heating stages; B) heating the gaseous parylene compound to a temperature of from about 650 ° C to about 700 ° C for cracking the gaseous parylene compound to form a parylene monomer; C) comprising a poly-pair A conformal coating of the toluene polymer is formed on at least a portion of the surface of the article, the article being contacted with the parylene monomer to apply a coating to the article.

In certain embodiments of the methods, step A includes heating the parylene compound to a temperature of from about 125 ° C to about 180 ° C, and heating the parylene compound to between about 200 ° C and about 220 ° C. temperature.

In certain embodiments of the methods, the heating of the gaseous parylene compound can be carried out in two or more stages. In some embodiments, step B includes heating the gaseous parylene compound to a temperature of about 680 ° C and heating the gaseous parylene compound to a temperature of at least about 700 ° C.

In some embodiments, the parylene compound is selected from the group consisting of a D-type poly-p-xylene compound, a C-type poly-p-xylene compound, an N-type poly-p-xylene compound, and HT. Type of parylene compound®.

In some embodiments, the methods further comprise contacting the article with gaseous decane prior to step C under conditions in which the decane activates the surface of the article. In certain embodiments, the decane is selected from one or more of the following groups: silane coupling agent (Silquest)® A-174, decane coupling agent® 111, and decane coupling agent®. A-174 (NT).

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

In some specific examples of the foregoing method, the object is an electronic component, and the electronic component is selected from the following: a communication component, a speaker, a mobile phone, and a sound. Frequency players, cameras, video players, remote controls, global positioning systems, computer devices, radar displays, depth detectors, fish detectors, emergency finger radio beacons (EPIRB), emergency position transmitters (ELT), and Personal Location Beacon (PLB).

In some specific examples of the foregoing methods, the object is selected from the group consisting of: paper products, textile products, artwork, circuit boards, marine detecting elements, space detecting elements, hazardous waste transport elements, Automated vehicle components, motor components, military system components, ammunition, guns, weapons, medical instruments, and biomedical components, wherein the biomedical components are optionally selected from the following group: hearing aids, cochlear implants And prosthetic.

In some specific examples of the foregoing methods, the surface is plastic, metal, wood, paper, and textile materials.

In some aspects, the articles provided by the present invention will apply a coating to at least a portion of a surface (outer or interior) by any of the foregoing methods.

In some aspects, the present invention provides an apparatus for applying a conformal coating to an article. In some embodiments, the apparatus includes: a vaporization chamber including at least two temperature zones; a pyrolysis chamber operatively coupled to the vaporization chamber; and a vacuum chamber operatively linkable To the pyrolysis chamber. In some embodiments, the apparatus further includes a connector operatively coupled to the pyrolysis chamber and the vacuum chamber, wherein the connector is capable of transporting gas between the pyrolysis chamber and the vacuum chamber, And wherein the connector comprises a T port. In some embodiments, the T-port is operatively coupled to an injection member for injecting a thermally conductive material into a gas that is transferred from the pyrolysis chamber to the vacuum chamber via the connector. In some embodiments, the vacuum generated in the vacuum chamber draws the thermally conductive material into the connector containing the gas via the T-port.

In some embodiments, the vacuum chamber includes a deposition chamber operatively coupled to the pyrolysis chamber and a vacuum generating device. In some embodiments, the vacuum generating device (vacuum member) includes one or more vacuum cylinders.

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.

1‧‧‧vaporization room

1’‧‧‧ objects

2‧‧‧Device

2'‧‧‧ Boron Nitride Layer

3‧‧‧ Pyrolysis Room

3'‧‧‧Polypylene compound layer

4‧‧‧ Valve

4’‧‧‧ objects

5‧‧‧Device

5'‧‧‧Polypylene compound layer

6‧‧‧Deposition room

6'‧‧‧ Boron Nitride

7‧‧‧Items to be coated

7’‧‧‧ objects

8‧‧‧Devices/Connectors

8'‧‧‧ Coating

9‧‧‧Vacuum components

10‧‧‧ Temperature zone

11‧‧‧ Temperature zone

12‧‧‧ Temperature zone

13‧‧‧temperature zone

14‧‧‧vacuum room/system

15‧‧‧vaporization room

16‧‧‧Devices

17‧‧‧ Pyrolysis Room

18‧‧‧ Valve

19‧‧‧Device

20‧‧‧T埠口

21‧‧‧Deposition room

22‧‧‧ Items to be coated

23‧‧‧Device

24‧‧‧Vacuum components

25‧‧‧vacuum room/system

Further advantages of the present invention will be apparent from the following description with reference to the accompanying drawings in which: FIG. 1A-E shows the chemical structure of various polyparaxylene compounds and decane coupling agent®. Figure 1A is a diagram of an N-type parylene compound. Figure 1B is a diagram of a C-type parylene compound. Figure 1C is a diagram of a D-type parylene compound. Figure 1D is a diagram of the HT-type parylene compound®. Figure 1E is a diagram of a decane coupling agent® A-174 decane (also known as decane coupling agent® A-174 (NT)).

Fig. 2A is a schematic view showing a specific example of a device for chemical vapor deposition of a parylene compound.

Fig. 2B is a schematic view showing a specific example of a device for coating a coating layer of a parylene compound and a powder.

3A to C are schematic diagrams showing three specific examples of articles coated with a parylene compound. Figure 3A depicts an article coated with a layer of separated parylene compound and a layer of boron nitride, wherein the layer of boron nitride is closest to the article. Figure 3B depicts an article coated with a layer of separated parylene compound and a layer of boron nitride, wherein the layer of parylene compound is closest to the article. Figure 3C depicts an article coated with a layer of parylene compound interleaved with boron nitride.

The present invention provides, in certain aspects, for coating articles with conformal polymers Compositions, methods, and devices. In some aspects, the present invention provides a conformal coating compound (e.g., a parylene compound) capable of forming an ultra-thin, conformal coating on an article. In another aspect, in other aspects, the coating composition provided by the present invention comprises a conformal coating compound (for example, a parylene compound) and one (or more) additives (for example, A thermally conductive material) for modifying any of a plurality of characteristics of the coating layer (for example, including resistivity, thermal conductivity, light transmittance, hardness, and resistance). In other aspects, the present invention provides articles, such as electronic components, having an ultra-thin, conformal coating (e.g., a water repellent coating) that prevents moisture from penetrating. The present invention also provides a method and apparatus for applying an ultra-thin, conformal coating layer on at least a portion of a surface of an article by vapor deposition. In a particular aspect, the present invention provides a multi-stage heating apparatus for vapor deposition of an ultrathin, conformal polymer coating.

A particularly important finding disclosed herein is that the conformal coating can be applied directly to "pre-assembled" or "off-the-shelf" components, such as consumer electronic components. Thus, the conformal coating can be applied to the outer surface of all or a portion of the "pre-assembled" or "off-the-shelf" component using the methods and compositions disclosed herein (for example, to create a closed or nearly closed seal) The seals) and thus the internal components of the components are protected from environmental damage (eg, moisture infiltration and oxidation). Accordingly, it is not necessary to disassemble, coat, and reassemble a particular article (for example, an electronic component (device)) using the methods disclosed herein, and conversely, in the "off-the-shelf" state, it can be coated. object. The method disclosed herein can apply a conformal coating layer (including, for example, a parylene compound) to a circuit board inside an electronic component and an outer surface of the electronic component (for example, in a single In the process). Therefore, these methods are particularly advantageous for use with "off-the-shelf" electronic devices. The methods disclosed herein are also well suited for improving the ease and efficiency of conformal coating of other articles.

Objects suitable for conformal coating using the compositions and methods disclosed herein include, but are not limited to, electronic devices, cameras, circuit boards, computer chips, paper, textiles, batteries, speakers, solid fuels, medical Components, hazardous waste transportation equipment, Waste, medical equipment, equipment for marine and space exploration, space equipment, etc. In some embodiments, the object is an electronic component. The electronic components are selected from the following: communication components, speakers, mobile phones, audio players, cameras, video players, remote control components, global positioning systems, computer devices, radar displays, depth detectors, fish schools Detector, Emergency Positioning Radio Beacon (EPIRB), Emergency Positioning Signal Transmitter (ELT), and Personal Positioning Beacon (PLB).

In some embodiments, the items are items that cannot be submerged, including, but not limited to, off-the-shelf electronics such as laptops, cameras, radios, mobile phones, paper, textiles, Batteries, speakers, solid fuels, medical components, paper, space equipment, and other items disclosed herein or known in the art. In other embodiments, the items may be items that are damaged by immersion in water, for example, but are not limited to metal screws and other hardware, paper products, and textiles. In other embodiments, the items may be items that require flexibility to function, such as a speaker. In further embodiments, the items may be items that need to be protected from oxygen damage, such as, but not limited to, fuel cells, weapons, cartridges, and ammunition. In further embodiments, the items may be items that must be isolated from the environment, such as hazardous waste products. In further embodiments, such items may be items that need to be protected from chemical exposure, for example, but are not limited to hazardous waste transport equipment.

The coatings can be applied to articles having a wide variety of surface materials including, for example, ceramics, polymers, plastics, metals, frozen liquids, and the like. In some embodiments, the article to be coated may be an article that will generate or consume heat and/or require a rough coating. In some embodiments, the article may generate heat or heat absorbing articles such as cold packs, chilled liquids and gases, and heated cartridges. In some embodiments, the article may be expected to experience severe physical shocks during its lifetime. In some aspects, the present invention provides methods for coating such articles and surfaces.

The conformal coatings disclosed herein can be applied to various components used in the consumer electronics, for-profit marine, recreational marine, military (aviation and defense), industrial and medical, and other industries. . In some cases, the conformal coatings are specifically designed to "seal" the components. For example, such coatings can be used to protect marine and hazardous components in the environment, avoiding operational malfunctions due to exposure to moisture, submerged water, dust, strong winds, and chemical action. These coatings enhance the viability and sustainability of operating equipment and high-priced specialty products that are susceptible to corrosion and damage.

In some embodiments, the conformal coating layer may be located on the inner and outer surfaces of the article, and in particular, the conformal coating on the outer side of the article may be located on the inside of the article. The conformal coating is coherent.

In some applications where a compound, such as an organic compound (e.g., decane), is pretreated, it is highly desirable to have the ability to be exposed to the pretreatment compound (for example, exposed to its gaseous state). Any object on a solid surface. Accordingly, one embodiment provides an article coated with at least one conformal coating compound that has been pretreated with decane (e.g., decane coupling agent®), wherein the uncoated article cannot be submerged. An uncoated item that cannot be submerged may be an item that will partially or completely lose its function after it has fallen into the water. In a preferred embodiment, the articles may be at least partially non-functional after being uncoated and then dried, and include, but are not limited to, off-the-shelf electronics. Devices such as laptops, radios, and mobile phones.

If there is a gap in the outer surface of the article coated with at least one conformal coating compound (and optionally pre-treated with decane), the conformal coating compound gas (as appropriate, and/or decane gas) enters the object. Internally, there may be a conformal coating on both the outside of the article and the inside of the article. In a preferred embodiment, the outer conformal coating layer will be continuous with the inner conformal coating layer.

These coated objects may be particularly suitable for the severe ring encountered by the military. In the context. In some embodiments, the coated article can meet the application requirements of the military specification MIL PRF-38534, which is a general performance requirement for hybrid microcircuits, multi-chip modules (MCMs), and similar components. In some embodiments, the coated article can meet the application requirements of the military specification MIL PRF-38535, which is a general performance requirement for an integrated circuit or microcircuit. In some embodiments, the coated article can simultaneously meet the application requirements of both military specifications MIL PRF-38534 and MIL PRF-38535.

Another specific example includes articles coated with a parylene compound and a boron nitride composition (for example, by the methods disclosed herein). An article to be coated by such a method comprises any article having a solid surface, wherein the solid surface is capable of forming a conformal coating layer (including a poly-pair) on at least a portion of the surface suitable for the article The gaseous polyparaxylene monomer and boron nitride are contacted under the conditions of xylene polymer and boron nitride. These items are, but are not limited to, electronic equipment, circuit boards, paper, textiles, batteries, speakers, solid fuels, medical components, hazardous waste transport equipment, hazardous waste, for marine and space exploration. Equipment, space equipment, and other items disclosed herein and/or known in the art. In some embodiments, the item may be an item that generates or consumes heat, such as, but not limited to, a computer, a drilling apparatus for deep hole drilling, and an externally exposed electronic component on a well. In other embodiments, the article may be an article that requires a particularly rough coating.

If there is a gap in the outer surface of the article coated with at least one conformal coating compound and a thermally conductive material (for example, boron nitride), including the conformal coating compound and the thermally conductive material (for example, nitriding) If the gaseous mixture of boron powder particles enters the interior of the article, then a conformal coating may be present on both the outside of the article and the inside of the article. In a preferred embodiment, the outer conformal coating layer will be continuous with the inner conformal coating layer. For example, an electronic component, such as a mobile phone, may have a conformal coating on the circuit board and battery inside the component and on the keyboard and screen of the mobile phone.

In some embodiments, the parylene compound and the boron nitride may be The interaction is interspersed within the coating layer 8 on the article 7 in Figure 3C. In some embodiments, the interdiffusion of the parylene compound with the boron nitride may be at a molecular level. In some embodiments, the inter-dispersed parylene compound and boron nitride coating layer may be from about 0.0025 mm to about 0.050 mm. In other embodiments, the inter-dispersed parylene compound and boron nitride coating layer may be less than about 2.0 mm.

In other embodiments, at least one conformal coating (e.g., a parylene conformal coating) and boron nitride are found in the separation layer on the article. Conformal coatings of interest to the present invention include, but are not limited to, polynaphthalene (1-4-naphthalene), diamine (toluidine), polytetrafluoroethylene (Teflon®), poly Amidoxime. In a preferred embodiment, the polymer coating may be a C-type parylene compound. In other embodiments, other forms of parylene compounds may be used, including, but not limited to, N-type parylene compounds, D-type parylene compounds, and HT-type poly-pairs. Toluene Compound®. In a preferred embodiment, the boron nitride coating layer and the polymer coating layer may each be about 0.05 mm thick. In other preferred embodiments, each layer may comprise substantially the polymer coating layer or substantially contain boron nitride. In some embodiments, the boron nitride layer 2 of FIG. 3A may be closer to the object 1 than the layer of the parylene compound 3. In other embodiments, the parylene compound layer 5 in FIG. 3B may be closer to the article 4 than the boron nitride 6.

Conformal composition/coating

According to certain aspects, the present invention provides a coating composition comprising a conformal coating compound and a thermally conductive material. As used herein, a "conformal coating compound" is an ultra-thin, pinhole-free, polymeric coating compound capable of forming a surface conforming to the geometry of the surface (for example, a partially purified compound, Purified compound, synthetic compound, isolated natural compound). Such coatings are also referred to herein as "conformal coatings." A conformal coating compound may also be equivalently referred to as a "shape-compatible coating compound". The conformal coating compound can be applied as a coating to the surface of an article by various methods (for example, chemical vapor deposition). for example, The vapor phase monomer of the conformal coating compound can contact the surface of the article under conditions in which the monomers are concentrated and adsorbed onto the surface of an article, and thus polymerized together to form a pinhole free surface on the surface. Conformal coating. The thickness of the coatings may range from about 10 angstroms up to 50 microns or even higher, depending on the application. For example, a coating layer may have a thickness of up to 3 mm. In some embodiments, the coating layer has a thickness of from about 0.0025 mm to about 0.050 mm. The conformal coating layer may be an electrical insulator (for example, a bulk resistance coefficient greater than 1010 ohms*cm). Alternatively, or even other than that, the conformal polymer may have a hardness of from about R70 to about R90 (Rockwell hardness value). The conformal coatings may also be hydrophobic, depending on the application. Conformal coating compounds may be present in a wide variety of forms, including monomeric and polymeric forms (e.g., dimeric, polymeric), as well as a wide variety of phases (for example, , gaseous, solid).

A particularly useful conformal coating compound is a parylene compound. The parylene compound is the common name for each member of a unique series of compounds. A basic member of this series (referred to as an N-type poly-p-xylene compound) is parylene, which is a compound made of p-xylene dimer ([2,2]-p-cycloalkane). The N-type parylene compound is a completely linear, highly crystalline material. a C-type parylene compound, which is a second commercially available member of the series, which is produced from the same monomer, which is corrected by replacing only one of the aromatic hydrogens with a chlorine atom. . A D-type parylene compound, which is a third member of the series, which is produced from the same monomer, is modified by replacing one of the aromatic hydrogens with a chlorine atom. The properties of the D-type parylene compound are similar to those of the C-type parylene compound, but increase the ability to withstand higher use temperatures. In some embodiments, the parylene compound may be derived from parylene by displacement of various chemical components. In a preferred embodiment, the parylene compound may be capable of forming a linear, highly crystalline material. Other polyparaxylene compound molecules can also be used, for example, the aforementioned derivatives and analogs. In some embodiments, a parylene compound provided by a commercial source (for example, Specialty Coating Systems (SCS), Inc.) can be used.

Conformal coating compounds may also include, but are not limited to, polynaphthalene (1,4-naphthalene), diamine (toluidine), polytetrafluoroethylene (Teflon®), and polyarylene amine. It will be readily apparent to those skilled in the art that the polymers can be applied by standard techniques.

The conformal coating layer comprising the parylene compound may be thermally insulating and does not readily allow the coated article to release heat to the environment. This feature of the parylene compound can be problematic for articles that generate heat, such as electronic devices, which, if not dissipated, can cause early failure of the device. Certain conformal coatings based on parylene compounds disclosed herein comprise a thermally conductive material that facilitates heat dissipation from the coated article. These conformal coating layers can be used to coat articles that require heat dissipation by releasing heat or absorbing heat as compared to coating layers of individual parylene compounds. The hardness of the conformal coating composition based on the parylene compound disclosed herein may also be higher than that of the coating layer of the individual parylene compound alone. Therefore, these coating compositions based on parylene compounds can also be used to coat articles that require a rough protective coating, such as articles that experience severe physical shock during their lifetime.

Thus, in accordance with certain aspects of the present invention, the conformal coating compound can be combined with other additive(s) to achieve a coating composition that has one or more improved performance characteristics compared to the conformal coating compound alone. For example, a coating composition having improved heat transfer capability can be produced. As used herein, "thermally conductive material" is a material that is capable of bonding a conformal coating compound to form a coating composition having a thermal conductivity greater than the thermal conductivity of the conformal coating compound alone. The thermal conductivity of the thermally conductive materials used herein will generally be higher than the conformal coating compound itself. The exemplary thermally conductive material has a thermal conductivity of 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 at least It is 20W/(m*K). Those skilled in the art will appreciate that there are a variety of methods for measuring the thermal conductivity, for example, which include the test methods set forth in the following standards: IEEE Standard 98-2002, "Thermal Electrical Insulation Material Heat 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) - Part 2; Transient plane heat source (hot disc) method )method)". Exemplary thermally conductive materials include various ceramic materials including, for example, hafnium oxide and tantalum nitride. Thermally conductive materials may also be selected from the group consisting of aluminum nitride, aluminum oxide, and boron nitride. For example, other thermally conductive materials include titanium dioxide (TiO2). Moreover, those skilled in the art will appreciate other thermally conductive materials. In some embodiments, the coating composition comprises a conformal coating compound and lanthanum hexaboride (LaB6). In some embodiments, the coating composition comprises a conformal coating compound and cerium oxide (SiO2).

In some aspects, the coating composition provided by the present invention comprises: a parylene compound as a conformal coating compound; and a thermally conductive material having a thermal conductivity greater than a thermal conductivity of the individual parylene compound, And in some cases, it is about 10% larger than the thermal conductivity of the parylene compound alone. In some embodiments, the thermal conductivity of such coating compositions can be about 5 to 10% greater than the parylene compound alone. Alternatively, or even otherwise, the hardness of the coating compositions may be about 10% greater than the hardness of the individual parylene compounds.

An exemplary thermally conductive material is boron nitride. Boron nitride (BN) is a binary chemical compound composed of an equal number of boron atoms and nitrogen atoms. Therefore, its experimental formula is BN. Boron nitride and carbon are isoelectronic and, like carbon, boron nitride has various polymorphic forms, one of which is analogous to diamond and one of which is analogous to graphite. The multi-configuration of diamond-like diamonds is one of the hardest materials known, while the multi-structure of graphite-like graphite is a useful lubricant. In addition, both of these multiple configurations exhibit radar absorption characteristics (see Silberberg, Martin S., McGraw-Hill, New York, 2009, Chemistry: The Molecular Nature of Matter and Change, fifteenth edition, Page 483). Accordingly, in certain aspects, the present invention provides a coating composition that may contain a parylene compound and boron nitride. In such compositions, the coating composition of the parylene compound and boron nitride may be interspersed (for example, boron nitride particles may be interspersed between the parylene polymers). Any of the parylene compounds may be used in the compositions; however, it is possible to use a D-type parylene compound, a C-type parylene compound, an N-type parylene compound, and an HT type poly pair. Xylene compound® is preferred, and particularly preferred is a C-type parylene compound. In these compositions, the boron nitride may have a hexagonal plate structure. In some embodiments, the weight ratio of boron nitride to the total weight of the parylene compound and boron nitride may be less than about 80%. In some embodiments, the weight of boron nitride may be up to about 1%, about 2%, about 3%, about 5%, about 10%, or about the total weight of the parylene compound and boron nitride. 20%.

In some embodiments, a coating composition may consist essentially of a parylene compound and boron nitride. In other embodiments, a coating composition consists of a parylene compound and boron nitride. In some embodiments, the parylene compound 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 of the composition. About 99.9%.

In some embodiments, the coating layer on an object includes a parylene compound and boron nitride, and the boron nitride may interdigitate the polyparaxylene compound dispersed in the coating layer. Among them (spread in a polymer of a parylene compound). Any of the parylene compounds may be used in the articles; however, it is possible to use a C-type parylene compound, an N-type poly-p-xylene compound, a D-type parylene compound, and an HT-type poly-pair. Toluene compound® is preferred, and particularly preferred is a C-type parylene compound. In some embodiments, the coating layer may be from about 0.0025 mm to about 0.050 mm thick.

In some embodiments, the parylene compound-boron nitride coating composition may contain a C-type parylene compound, although in other embodiments, it may also contain a D-type parylene. Compounds, N-type parylene compounds, or HT-type parylene compounds®, see Figures 1A, 1B, 1C, and 1D. In some embodiments, the parylene compound may be derived from an N-type parylene compound, or parylene, by displacement of various chemical components. In a preferred embodiment, the parylene compound forms a completely linear, highly crystalline material. In some embodiments, the boron nitride may have a hexagonal plate structure. In some embodiments, the parylene compound and boron nitride form a layer that separates within the parylene composition. In some embodiments, the parylene composition may have strong covalent bonds within the parylene layer and the boron nitride layer. In other embodiments, the parylene composition may have a weak van der Waals force between the parylene layer and the boron nitride layer.

In some embodiments, the thermal conductivity of the parylene composition may be greater than the parylene compound alone, for example, the unit of measurement is (cal/sec)/cm2/C. In a specific embodiment, the thermal conductivity of a parylene-boron nitride composition may be about 10% larger, about 30% larger, or about 50% larger than the parylene compound alone. . In other embodiments, such as the definition of Rockwell hardness test, the hardness of a parylene composition may be greater than that of a single parylene compound, see Macroindentation Hardness Testing ASM Handbook by EL Tobolski & A. Feee. Volume 8: Mechanical Testing and Evaluation, pp. 203-211 (ASM International, 2000). Specific In a specific example, the parylene-boron nitride composition may be about 10% larger than the parylene compound alone, about 30% larger, about 50% larger, or larger. About 90%. The relative amount of the parylene compound and boron nitride in the parylene-boron nitride composition may determine the thermal conductivity and hardness of the composition. In some embodiments, the weight ratio of boron nitride to the total weight ratio of parylene compound and boron nitride in the composition will be less than about 5%, less than about 10%, less than about 20%, and less than about 40. %, less than about 60%, or less than about 80%. In some embodiments, the weight of boron nitride can be up to about 1%, about 2%, about 3%, or about 4% by weight of the total weight of the parylene compound and boron nitride in the composition.

In some cases, the article may need to be pre-treated to allow the surface of the article to adhere more to a conformal coating, such as by coating a decane. The pretreatment method may require immersing the article in a solution containing a suitable compound (for example, which contains an organic compound such as decane), then removing the article from the decane solution, and drying the article. object. These pretreatments improve the surface adhesion of the conformal coating compound and enhance (improve) mechanical and electrical properties.

In the case of objects that may be damaged in the solution (for example, electronic components), an alternative pre-treatment method may be used which involves coating the article with decane. For example, decane can be applied to an article to be coated with a conformal coating comprising a parylene compound in the vapor phase. This allows certain items that cannot be submerged but require pre-treatment with decane to be coated with a parylene compound.

In another aspect, the invention comprises an article having at least one conformal coating compound coating layer and at least one boron nitride coating layer. In some embodiments, the conformal coating compound may be polynaphthalene, diamine, polytetrafluoroethylene, polyamidamine, C-type parylene compound, N-type poly-p-xylene compound, D-type poly The p-xylene compound or the HT-type parylene compound®, and preferably a C-type parylene compound. In some embodiments, the boron nitride coating layer may be closer to the object than the polymer coating layer; and other specific examples The polymer coating layer may be closer to the article than the boron nitride coating layer. In some embodiments, the boron nitride coating layer and the polymer coating layer may each be at least about 0.05 mm thick.

Conformal coating device

The present invention also discloses an apparatus for applying an ultrathin, conformal coating layer by vapor deposition on the surface of an article. In other aspects, the present invention discloses a multi-stage heating apparatus for vapor deposition of an ultrathin, conformal polymer coating.

In some aspects, the present invention provides an apparatus for applying a conformal coating comprising a parylene compound, the apparatus comprising a vaporization chamber having a plurality of (two or more) temperature zones, The vaporization chamber is operatively coupled to a pyrolysis chamber that is operatively coupled to a vacuum chamber. In some embodiments, the vacuum chamber may include a deposition chamber operatively coupled to the pyrolysis chamber and a vacuum member, and the vacuum member may be one or more vacuum tubes. In some embodiments, the vaporization chamber may have a plurality of temperature zones, preferably a system, and two temperature zones. In other embodiments, the pyrolysis chamber may have a plurality of temperature zones, preferably a system, and two temperature zones. In some embodiments, the vaporization chamber and/or the pyrolysis chamber may be a tubular furnace.

Other means for vapor depositing a conformal coating compound on an article are known in the art. For example, see 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, 5,556,473. No. 5, 641, 358, No. 5, 709, 753, No. 6, 406, 544, No. 6, 737, 224, and No. 6, 406, 544, all of which are incorporated herein by reference.

In another aspect, the present invention provides an apparatus for applying a conformal coating comprising a conformal coating compound and a thermally conductive material, the apparatus possibly comprising a vaporization chamber operatively linkable To the pyrolysis chamber, the pyrolysis chamber is operatively coupled to a vacuum chamber, wherein a connector including a T-port is operatively coupled to the vacuum chamber. to In some embodiments, the connector that is operatively coupled to the pyrolysis chamber and the vacuum chamber may be a transfer member for transferring gas from the pyrolysis chamber to the vacuum chamber. In other embodiments, the T-port can be operatively coupled to an injection member for injecting solid particles (for example, powder) or another gas into the gas being delivered via the connector. In some embodiments, the vacuum chamber may contain a deposition chamber operatively coupled to the pyrolysis chamber and a vacuum member, wherein the vacuum member may be one or more vacuum tubes.

One specific example is a device for chemical vapor deposition of a parylene compound, which may include a modified vaporization chamber and/or pyrolysis chamber. Although this device may be particularly suitable for chemical vapor deposition of parylene compounds; however, it may also be used for vapor deposition of other conformal coating compounds, including, but not limited to, polynaphthalene (1, 4-naphthalene), diamine (di-toluidine), polytetrafluoroethylene (Teflon®), poly-liminamide, and other conformal coating compounds well known in the art. In some embodiments, the apparatus includes a vaporization chamber and/or a pyrolysis chamber having a plurality of temperature zones. Although the invention does not limit the mode of operation of the apparatus, the present invention contemplates that having different temperature set points in each chamber improves the heating rate of the parylene compound. The vaporization chamber and the pyrolysis chamber of the multiple temperature zones can uniformly cleave the parylene compound into a single monomer, and can more preferably control the final thickness of the parylene compound coating layer on the article. The parylene compound may remain in the deposition chamber for a longer period of time, allowing it to be better distributed throughout the deposition chamber.

A polyparaxylene compound coating apparatus shown in Fig. 2A. The vaporization chamber 1 may have two temperature zones 10 and 11. The pyrolysis chamber 3 may also have two temperature zones 12 and 13. The vaporization chamber 1 can be operatively coupled to the pyrolysis chamber 3 by means of a device 2 capable of transporting gas from the vaporization chamber 1 to the pyrolysis chamber 3. The pyrolysis chamber 3 is operatively coupled to a vacuum chamber 14, which may include a deposition chamber 6 and is operatively coupled to a vacuum member 9 by means of a device 8 capable of pumping the deposition chamber 6 Vacuum. A device 5 operatively connecting the pyrolysis chamber 3 to the vacuum chamber 14 is capable of transferring gas from the pyrolysis chamber 3 to the vacuum chamber 14, and It is also possible to include a valve 4 that is capable of regulating the flow of gas from the pyrolysis chamber 3 to the vacuum system 14.

The vaporization chamber 1 can be any furnace/heating system capable of heating solids to between about 150 ° C and about 200 ° C. In a preferred embodiment, the vaporization chamber is capable of heating the gas to 1200 °C. In some embodiments, vaporization chamber 1 may contain a gas. The vaporization chamber 1 may also be capable of producing regions of different temperatures in its heating chamber. Finally, the vaporization chamber 1 may be able to maintain an extremely high vacuum. In a preferred embodiment, the vaporization chamber can support a vacuum of at least about 0.1 Torr.

The vaporization chamber 1 is operatively coupled to the pyrolysis chamber 3 by a number of devices well known to those skilled in the art. In some embodiments, the operable connector between the vaporization chamber 1 and the pyrolysis chamber 3 may be a connector that transfers gas from the vaporization chamber 1 to the pyrolysis chamber 3. In some embodiments, the device 2 may be a glass tube, a curved bottle, or a metal tube. In other embodiments, those skilled in the art will appreciate that the device 2 may also include valves, temperature sensors, other sensors, and other conventional devices.

The pyrolysis chamber 3 can be any furnace/heating system capable of heating the gas to between about 650 ° C and about 700 ° C. In some embodiments, the pyrolysis chamber 3 may contain a gas. In some embodiments, the pyrolysis chamber 3 may be capable of producing regions of different temperatures within its heating chamber. Finally, in some embodiments, the pyrolysis chamber 3 may be capable of maintaining an extremely high vacuum. In a preferred embodiment, the vaporization chamber can support a vacuum of at least about 0.1 Torr.

Preferably, the vaporization chamber and the pyrolysis chamber may be furnaces capable of producing two or more temperature zones in their chambers. In a preferred embodiment, the furnace has two temperature zones. In some embodiments, the temperature zones are located in the furnace chamber such that a gas moves sequentially through the temperature zones prior to exiting the furnace. 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 of the specific examples of a dual temperature zone furnace suitable for the vaporization chamber and/or the pyrolysis chamber can be found in Example 2.

The pyrolysis chamber 3 is operatively coupled to the vacuum system 14 by a number of devices well known to those skilled in the art. In some embodiments, the operable connector between the pyrolysis chamber 3 and the vacuum system 14 may be a connector that transfers gas from the pyrolysis chamber 3 to the vacuum system 14. In some embodiments, the device 5 may be a glass tube, a curved bottle, or a metal tube. In other embodiments, those skilled in the art will appreciate that the device 5 may contain one or more valves 4 by which the gas flowing through the device 5 can be adjusted.

The vacuum system 14 may contain a deposition chamber 6 that is operatively connectable to a vacuum member 9. In some embodiments, the operable connector 8 may be capable of maintaining a vacuum of up to at least about 0.05 Torr and is operable at at least about 1 x 10-4 Torr. In other embodiments, the vacuum member 9 may be one or more vacuum cartridges capable of drawing a vacuum into the deposition chamber of at least about 0.05 Torr, and preferably, drawing at least about 1 x 10-4 Torr. Vacuum. In some embodiments, the deposition chamber 6 may be sized to receive the article 7 to be coated. In other embodiments, the deposition chamber 6 may be capable of maintaining a vacuum of up to at least about 0.05 Torr and is operable at a range of at least about 1 x 10-4 Torr.

Another specific example disclosed herein is a device for chemical vapor deposition of the parylene compound and a boron nitride composition, comprising an injection member for injecting a powder into the chemical vapor phase prior to deposition Among them. The coating device shown in Fig. 2B is a coating device according to one of the specific examples. The vaporization chamber 15 can be operatively coupled to the pyrolysis chamber 17 by means of a device 16 that is capable of transporting gas from the vaporization chamber 15 to the pyrolysis chamber 17. The pyrolysis chamber 17 is operatively coupled to a vacuum chamber 25, which may include a deposition chamber 21 and is operatively coupled to a vacuum member 24 by means of a device 23 capable of pumping the deposition chamber 21 Vacuum. A device 19 operatively coupling the pyrolysis chamber 17 to the vacuum chamber 25 can transfer gas from the pyrolysis chamber 17 to the vacuum chamber 25, and may also include a valve 18 that can be adjusted from The gas from the pyrolysis chamber 17 to the vacuum system 25 flows. Device 19 may also have a T port 20, It is also known as "tee joint". In some embodiments, the T-port is operatively coupled to an injection member for injecting powder into the gas being delivered via device 19. In some embodiments, the means for injecting powder comprises, but is not limited to, an oven, a power coating apparatus, and high pressure air. In a preferred embodiment, the means for injecting the powder comprises a powder container operatively coupled to an electronic valve operatively coupled to the T port.

The vaporization chamber 15 can be any furnace/heating system capable of heating solids to between about 150 ° C and about 200 ° C. In some embodiments, vaporization chamber 15 may contain a gas. Finally, the vaporization chamber 1 may be able to maintain an extremely high vacuum.

The vaporization chamber 15 is operatively coupled to the pyrolysis chamber 17 by a number of devices well known to those skilled in the art. In some embodiments, the operable connector between the vaporization chamber 15 and the pyrolysis chamber 17 may be a connector that transfers gas from the vaporization chamber 15 to the pyrolysis chamber 17. In some embodiments, the device 16 may be a glass tube, a curved bottle, or a metal tube. In other embodiments, those skilled in the art will appreciate that the device 16 may also include valves, temperature sensors, other sensors, and other conventional devices.

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

The pyrolysis chamber 17 is operatively coupled to the vacuum system 25 by a number of devices well known to those skilled in the art. In some embodiments, the operable connector between the pyrolysis chamber 17 and the vacuum system 25 may be a connector that can transfer gas from the pyrolysis chamber 17 to the vacuum system 25. In some embodiments, the device 19 may be a glass tube, a curved bottle, or a metal tube. In other specific examples, familiar with the technology It is well understood by those skilled in the art that this device 19 may contain valves, temperature sensors, other sensors, and other conventional devices. In a preferred embodiment, device 19 may contain one or more valves 4 by which the gas flowing through the device 19 can be adjusted.

Vacuum system 25 may contain a deposition chamber 21 that is operatively coupled to a vacuum member 24 by means of device 23. In some embodiments, the connector 23 may be capable of maintaining a vacuum of up to at least about 0.05 Torr. In other embodiments, the vacuum member 24 may be one or more vacuum cartridges capable of drawing a vacuum into the deposition chamber of at least about 0.05 Torr. In some embodiments, the deposition chamber 21 may be sized to receive the article 22 to be coated. In other embodiments, the deposition chamber 21 may be capable of maintaining a vacuum of at least about 0.05 Torr.

Conformal coating method

The present invention also discloses a method for applying an ultra-thin, conformal coating on the surface of an article by vapor deposition. In some aspects, the present invention discloses a multi-stage heating process for vapor deposition of ultra-thin, conformal coatings. In other aspects, the present invention discloses a method of vapor depositing an ultrathin, conformal coating comprising an additive.

Preferably, the conformal coating deposition process disclosed herein can be carried out in a closed system under negative pressure. For example, a parylene compound can be deposited from the vapor phase at a low pressure (for example, about 0.1 Torr) to form a conformal coating. In this embodiment, the first step vaporizes the solid parylene dimer at about 150 ° C in a vaporization chamber. The second step is the quantitative cleavage (pyrolysis) of the dimer at two methyl-methyl bonds at about 680 ° C in a pyrolysis chamber to produce a stable diradical para-xylene monomer. Finally, the monomer in gaseous form will enter the deposition chamber at room temperature where they will adsorb and polymerize on the article to be coated. Preferably, the closed system has separate chambers for vaporizing, pyrolyzing, and depositing the parylene compound, the chambers being connected by suitable tubing or tubular connectors.

The conformal coating compound can be used in various forms and purity in such methods in. In certain 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%, even up to about 100% purity. In some embodiments, the conformal coating compound is comprised of a plurality of conformal coating compounds from different sources and/or different purities (for example, the same type, for example, a C-type parylene compound) The composition of the composition. In some embodiments, the conformal coating compound is comprised of a plurality of types of conformal coating compounds (for example, a C-type poly-p-xylene compound, an N-type poly-p-xylene compound, a D-type parylene) A compound consisting of a compound, a HT-type parylene compound®).

According to other aspects, a method for applying a conformal coating layer on an article comprises: heating a parylene compound to a temperature of from about 125 ° C to about 200 ° C to form a gaseous parylene. a compound, wherein the heating of the parylene compound is carried out in two or more heating stages; heating the gaseous parylene compound to a temperature of from about 650 ° C to about 700 ° C for cracking the gaseous state a parylene compound to form a parylene monomer; and contacting the article with a conformal coating comprising a parylene polymer on at least a portion of a surface of an article The parylene monomer is equalized to apply a coating layer to the article. In some embodiments, the parylene compound is heated to a temperature of from about 125 ° C to about 180 ° C and then heated to a temperature of from about 200 ° C to about 220 ° C. In some embodiments, the gaseous parylene compound will be heated in two or more stages. For example, the gaseous parylene compound may be first heated to a temperature of about 680 ° C and then heated to a temperature of at least about 700 ° C.

In some cases, the methods can be used to apply a uniform, conformal coating layer comprising a parylene compound in a vacuum chamber at 25 ° C using standard chemical vapor deposited particles, and The coating can range from 0.01 mm to 3.0 mm, depending on the item to be coated. Once coated, the article is weather resistant and water resistant, and can withstand exposure to extreme weather conditions and exposure to most chemicals. Any solid state table The faces can be coated and include plastic, metal, wood, paper, and textile materials. Embodiment applications disclosed herein include, but are not limited to, electronic devices such as mobile phones, radios; circuit boards and speakers; devices for marine and space detection, or devices for drilling oil well operations; Waste transportation equipment; medical equipment; paper products; and textiles.

In some embodiments, the length of time that the article can contact the gaseous parylene monomer may be altered to control the final thickness of the parylene coating layer on the article. In various embodiments, the final thickness of the parylene compound coating layer may be between about 100 angstroms and about 3.0 millimeters. In some embodiments, the final thickness of the parylene compound coating layer may be between about 0.5 mm to about 3.0 mm. In some embodiments, the final thickness of the parylene compound coating layer may be between about 0.0025 mm to about 0.050 mm. Preferably, a deposition time of from about 2 hours to about 18 hours (for example, 5 hours) can be used to achieve a coating thickness of about 0.002 inches (0.050 mm) of the parylene compound. It depends on the temperature of the deposition chamber. The choice of the final thickness of the parylene compound coating layer may depend on the particular degree of the article to be coated and the end use of the article. Objects that require some sort of movement to function may wish to have a thinner final coating, such as a power button. Objects that are immersed in water may wish to have a thicker coating.

The effect of adsorbing a particular coating composition (for example, a coating composition comprising a parylene compound) onto various articles can be achieved by utilizing an organic compound (e.g., decane) prior to application of the conformal coating layer. The surface of the article to be coated is pretreated to be improved. The decane treatment forms free radicals on the surface of the article to which the parylene can be coupled. Vinyl trichloromethane in either xylene, isopropanol or Freon, and gamma-methacryloxypropyltrimethoxysilane in methanol-water solvent Two kinds of decane, such as decane coupling agent® A-174 decane or decane coupling agent® A-174(NT) decane, have been used for this purpose. However, electronic devices cannot withstand the electrical path created by direct contact with conductive liquids, nor can they be applied to Residual ions that are often left behind by the immersed water or liquid. Even if it does not grow out immediately, it is still possible to grow a tree conductor later due to the voltage relationship between the conductors on the electronic device. Short circuit circuits caused by conductor fluids and dendritic tumors can deplete the energy of the battery and can cause high currents to flow in unintended areas and cause unintended circuit operation or even failure. Most preferably, devices in an electronic device, such as a circuit board, typically must be coated with a mixture of decane and parylene, and then assembled into a finished product.

In certain aspects, the present invention provides a method of coating an article with a decane such as a decane coupling agent® decane. In some embodiments, the methods may include: (A) vaporizing it by heating the decane to its evaporation point to form a gaseous decane; and (B) contacting the gaseous decane of step A to be At least a portion of the surface of the coated article (for example, it is desirable to apply a conformal coating layer (for example, which includes a surface of a parylene compound)). In some embodiments, the decane coupling agent® may be a decane coupling agent® A-174, a decane coupling agent® 111, or a decane coupling agent® A-174 (NT), and preferably矽 偶联 coupling agent ® A-174. In some embodiments, in step A, the decane may be vaporized in an aqueous 50:50 solution. In some embodiments, in step A, the decane may be vaporized at 80 ° C for 2 hours.

In some aspects, the present invention provides a method of pre-treating with decane and applying a parylene-coated compound to at least a portion of the surface of an article. The methods may comprise: (A) vaporizing the parylene dimer by heating it to 150 to 200 ° C to form a gaseous parylene dimer; (B) by bringing the gaseous The parylene dimer is heated to 650 to 700 ° C to cleave the gaseous parylene dimer to a gaseous parylene monomer; (C) to vaporize the decane by heating it to its evaporation point To form a gaseous decane; (D) to contact the article to be coated with the parylene compound using the gaseous decane of step C; and (E) to contact the gaseous polyparaxylene monomer of step B for contact The article of the parylene compound is maintained for a sufficient period of time to deposit a coating layer of the parylene compound having a final thickness. For some In a specific example, the parylene compound may be selected from the group consisting of a D-type poly-p-xylene compound, a C-type poly-p-xylene compound, an N-type poly-p-xylene compound, and an HT-type poly pair. A xylene compound®, and a parylene compound derived from an N-type parylene compound, and preferably a C-type parylene compound. In some embodiments, the decane may be a decane coupling agent® A-174, a decane coupling agent® 111, or a decane coupling agent® A-174 (NT), and preferably a decane coupling Agent® A-174.

In some embodiments, in step A, the parylene dimer may be vaporized by heating in two or more stages, and preferably, at about 170 ° C and about Heating is carried out in two stages of from 200 ° C to about 220 ° C. In some embodiments, in step B, the parylene dimer may be cleaved by heating in two or more stages, and preferably, at about 680 ° C and greater than Heating is carried out in two stages of about 700 °C. In some embodiments, in step C, the decane may be vaporized in an aqueous 50:50 solution. In other embodiments, in step C, the decane may be vaporized at 80 ° C for 2 hours. In some embodiments, the final thickness of the parylene compound coating layer may range from about 100 angstroms to about 3.0 mm.

A method comprising pretreating an article with a decane compound may comprise the steps of: A. vaporizing the parylene dimer by heating to 150 to 200 ° C to form a gaseous parylene dimer; The gaseous parylene dimer is cleaved into a gaseous parylene monomer by heating the gaseous parylene dimer to a temperature of from about 650 ° C to about 700 ° C; C. by decane Heating to its evaporation point to vaporize it to form gaseous decane; D. using gaseous decane to contact the object to be coated; and E. using gaseous parylene monomer to contact the object to be coated ,dimension Hold a sufficient period of time to deposit a coating layer of the parylene compound having a final thickness. Those skilled in the art will readily appreciate that steps A, B, and E can be practiced in any manner currently employed to coat a parylene compound with an article. Further, any such steps can be implemented in a different order than those presented herein. For example, step D can be implemented prior to step A. Further, some steps may be performed simultaneously with other steps. For example, step D may be performed simultaneously with step A. In a preferred embodiment, a C-type parylene compound can be used, see Figure IB. In other embodiments, other types of parylene compounds may be used, including, but not limited to, N-type parylene compounds, D-type parylene compounds, and HT-type parylenes. Compound®, see Figures 1A, 1B, and 1D. In some embodiments, the parylene compound may be derived from an N-type parylene compound, or parylene, by displacement of various chemical components. In a preferred embodiment, the parylene compound may form a completely linear, highly crystalline material. How to implement the method in order to present one of the specific examples of the method will be explained in more detail in the paragraphs of the following examples.

In some embodiments, step A may be carried out in a furnace chamber to vaporize the parylene dimer to form a gaseous parylene dimer by heating to 150 to 200 °C. In a preferred embodiment, the parylene dimer will be heated to a desired 150 to 200 ° C in multiple stages. In some embodiments, the hierarchical heating of the parylene dimer is performed in a furnace chamber having a plurality of temperature zones that allow different temperature set points for different regions of the furnace chamber. Although the method of operation of the hierarchical heating procedure is not limited; however, the inventors believe that the method allows the parylene compound to be uniformly "cracked" into monomers and better control the final pairing on the article. The thickness of the coating layer of the xylene compound can be distributed throughout the deposition chamber because it takes a long time to hold the monomer in the deposition chamber. In some embodiments, the parylene dimer is vaporized by heating in two stages, three stages, four stages, or four or more stages. In some specific examples, The temperatures of the stages are about 170 ° C, and about 200 ° C to about 220 ° C. Although not limited to a particular theory; however, the inventors believe that vaporizing the parylene compound in the first stage of vaporization and preheating the vapor in the second stage as the vapor enters the pyrolysis chamber can be higher The rate is split into monomers.

In some embodiments, step B may be performed in a furnace chamber to cleave the gaseous parylene dimer to a gaseous state by heating the gaseous parylene dimer to 650 to 700 °C. Polyparaxylene monomer. In a preferred embodiment, the gaseous parylene dimer will be heated to a desired 650 to 700 ° C in multiple stages. In some embodiments, the hierarchical heating of the gaseous parylene dimer is carried out in a furnace chamber having a plurality of temperature zones that allow different temperature set points for different regions of the furnace chamber. In some embodiments, the parylene dimer is cleaved by heating in two stages, three stages, four stages, or four or more stages. In some embodiments, the temperatures of the stages are about 680 ° C and above about 700 ° C. Although no particular theory is limited; however, the inventors of the present invention believe that the gaseous polyparaxylene dimer is cleaved into monomers during the first stage of heating and the gaseous monomers are in the second heated state. Further heating to above about 700 °C is used to ensure that the gaseous monomers will remain in the deposition chamber for a longer period of time to more evenly fill the deposition chamber.

In one step utilized by such methods, gaseous decane (Fig. 1E) may contact the article to be coated (step D). This step is particularly advantageous to aid in the application of the parylene compound to the hydrophilic surface of the article. In some embodiments, a mixture of decane coupling agent® decane, decane coupling agent® A-174 (NT), or decane coupling agent® A-174 is used throughout the process. Xylene compound. In one embodiment, the article may contact the gaseous decane in a vacuum chamber.

In step C, the decane can be vaporized by heating it to its evaporation point. In a preferred embodiment, this step can be performed before the object to be pretreated contacts the gaseous decane First implemented. In one embodiment, by placing the decane in a crucible, inserting the crucible into a 1 inch thermocouple on the heating chamber in the vacuum chamber containing the article to be coated, Implement this step. The amount of decane that is poured into the crucible may depend on the number and size of the objects in the vacuum chamber. In various embodiments, the amount of vaporized decane may range from about 10 ml to about 100 ml, or in some cases, the amount may be more. In one embodiment, the heating plate can heat the decane to its evaporation point. In other embodiments, it will be apparent to those skilled in the art that other methods can be used to heat the decane to its point of evaporation. In another embodiment, a mixture of decane containing distilled water may be vaporized. In one embodiment, a 50/50 mixture of decane and distilled water is heated until the decane is vaporized, which may last for about 2 hours at about 80 °C.

Although in some embodiments, the article may be pre-treated with decane in the same vacuum chamber and then coated with the parylene compound; however, in other embodiments, the two coatings It can also be applied in different chambers and/or at different times. In a preferred embodiment, once the article is exposed to the decane to be evaporated, the chamber can be placed under vacuum and the parylene can be started immediately upon reaching a suitable vacuum. Compound deposition. Preferably, the decane vapor in the chamber is completely discharged prior to introduction of the gaseous parylene compound monomers. In various embodiments, the time period between application of the decane pretreatment and coating of the parylene compound coating layer may range from about 0 minutes to about 120 minutes. The temperature at the evaporation point of decane was about 80 °C. Although not limiting the mechanism of action of decane; however, the inventors believe that the vaporized decane will pretreat the article, thereby increasing the surface by having the surface have free radicals that will bond the parylene monomers. The ability to accept the parylene monomer gas.

In step D, the article to be coated may be exposed to gaseous decane. In a preferred embodiment, this contact can be accomplished in the same deposition chamber that is later used to contact the gaseous parylene monomer to the article. In some embodiments, the object will contact the gas The decane lasted for about 2 hours.

In step E, a gaseous parylene monomer may be utilized to contact the article to be coated for a sufficient period of time to deposit the parylene compound coating. In a preferred embodiment, this step can be carried out in a deposition chamber, and a particularly preferred system is carried out in the same deposition chamber where the article contacts decane. In other preferred embodiments, the deposition chamber and the articles to be coated may be at room temperature. In some embodiments, the deposition temperature may range from about 5 ° C to about 30 ° C, preferably from about 20 ° C to about 25 ° C. In some embodiments, the deposition chamber can be frozen to speed up the deposition process.

Another embodiment provides a method of treating an article using decane. The method comprises the steps of: A. vaporizing it by heating the decane to its evaporation point to form a gaseous decane; and B. contacting the article to be coated with gaseous decane.

In step A, the decane may be vaporized by being heated to its evaporation point. In some embodiments, decane coupling agent®, decane coupling agent® A-174, decane coupling agent® 111, or decane coupling agent® A-174 (NT) is the decane used throughout the process. In a preferred embodiment, this step may be performed prior to contacting the article to be coated with gaseous decane. In one embodiment, by placing the decane in a crucible, inserting the crucible into a 2 inch thermocouple on the heating chamber in the vacuum chamber containing the article to be coated, In carrying out this step, the amount of decane that is poured into the crucible may depend on the number and size of the items in the vacuum chamber. In various embodiments, the amount of vaporized decane may range from about 10 ml to about 100 ml, or in some cases, the amount may be more. In one embodiment, the heating plate can heat the decane to its evaporation point. In other embodiments, it will be apparent to those skilled in the art that other methods can be used to heat the decane to its point of evaporation. In another embodiment, a mixture of decane containing distilled water may be vaporized. In one specific example, A 50/50 mixture of decane and distilled water may be heated until the decane is vaporized, which may last for about 2 hours at about 80 °C.

In step B, gaseous decane is used to contact the article to be coated. In some embodiments, the article will contact the gaseous decane for a period of about 2 hours.

The present invention also provides a method for applying a coating comprising a conformal coating compound and a thermally conductive material. In some embodiments, the method comprises: heating a conformal coating compound to form a gaseous monomer of the conformal coating compound; combining a thermally conductive material with the gaseous monomers to form a gaseous mixture And coating the conformal coating with a conformal coating comprising the conformal coating compound and the thermally conductive material on at least a portion of a surface of an article to coat the gaseous mixture Apply a layer to the article.

As used herein, a "gaseous mixture" is a mixture comprising at least one gas phase (gaseous) component and possibly at least one other component of the gas phase or possibly the non-gas phase. For example, a gaseous mixture may include a gas phase conformal coating compound and a solid phase compound (for example, powder particles) suspended in the vapor of the conformal coating compound. Similarly, a gaseous mixture may also include a vapor phase conformal coating compound and a liquid phase compound (e.g., an atomized liquid) suspended in the vapor of the conformal coating compound. In addition, a gaseous mixture may also include a plurality of gas phase components (for example, a plurality of different gas phase conformal coating compounds). It should be understood that the gaseous mixture may comprise any number of combinations of the same and/or different phase components. In some embodiments, the gaseous mixture includes at least one vapor phase conformal coating compound (for example, a parylene compound) and at least one thermally conductive material. In some embodiments, the thermally conductive material in a gaseous mixture is a solid phase (for example, powder particles). In some embodiments, the thermally conductive material in a gaseous mixture is in the liquid phase. Also, in other embodiments, the thermally conductive material in a gaseous mixture is in the vapor phase.

The coating methods disclosed herein can be used in for-profit marine, recreational yachting, military (aviation and defense), industrial and medical, and as disclosed herein and known in the art. It is used in products used in the industry. In some cases, the coating process may be specially designed to "seal" the component. Therefore, the coating methods can be used to protect components commonly used in the marine and harmful environments, and to avoid operational malfunction due to exposure to moisture, submerged water, dust, strong winds, and chemical action. The coating layer enhances the viability and sustainability of operating equipment and high-priced specialty products that are susceptible to corrosion and damage.

In another aspect, the present invention provides a method for applying a conformal coating layer comprising a parylene compound and boron nitride to at least a portion of a surface of an article, the method having The following steps: (A) vaporizing the parylene dimers by heating them to a temperature of from about 150 ° C to about 200 ° C to form a gaseous parylene dimer; (B) by means of a gaseous state The parylene dimer is heated to about 650 ° C to about 700 ° C to cleave the gaseous parylene dimer into a gaseous parylene monomer; (C) the boron nitride is injected into the gaseous state of step B Among the parylene monomers; and (D) using the gaseous polyparaxylene monomer of step C and boron nitride to contact the article to be coated with the parylene compound for a sufficient period of time for deposition to have a final A thickness of the parylene compound and a boron nitride coating layer. Although any parylene compound can be used in this method; however, it is possible to use a D-type parylene compound, a C-type parylene compound, an N-type parylene compound, and an HT-type parylene compound. ® is preferred, while the best one may be a C-type parylene compound. In certain preferred embodiments, the boron nitride may be injected into the gaseous parylene monomer in powder form (preferably between about 18 microns and about 25 microns). . In other embodiments, step D may occur between about 5 ° C and about 30 ° C. In some embodiments, the final thickness of the coating layer may be between about 100 angstroms and about 3.0 millimeters. In some embodiments, the method may have an additional step E in which the article to be coated may contact a decane composition until the article is coated with decane.

In some embodiments, the method uses standard chemical vapor deposited particles to coat a solution comprising a parylene compound and boron nitride in a vacuum chamber at 25 ° C. A uniform, conformal coating of a thin layer ranging in thickness from 0.01 mm to 3.0 mm, depending on the article to be coated. Once coated, the article is weather resistant and water resistant, and can withstand exposure to extreme weather conditions and exposure to most chemicals. Any solid surface can be coated, including plastic, metal, wood, paper, and textile materials. Embodiment applications include, but are not limited to, electronic devices such as mobile phones, radios, circuit boards, and speakers; equipment for marine and space detection; hazardous waste transport equipment; medical instruments; paper products; textile.

Therefore, the method of coating an article using a composition composed of a parylene compound and boron nitride may include the following steps: A. vaporizing the parylene dimer by heating to 150 to 200 ° C, Used to form a gaseous parylene dimer; B. The gaseous parylene dimer is cleaved into a gaseous poly pair by heating the gaseous parylene dimer to 650 to 700 °C. a xylene monomer; C. injecting boron nitride into the gaseous parylene monomer of step B; and D. contacting the object to be coated with gaseous parylene monomer and boron nitride, maintaining A sufficient period of time is required to deposit a coating layer of the parylene compound having a final thickness.

Those skilled in the art will readily appreciate that steps A and B of the method of coating articles using a parylene compound and boron nitride can be used to vaporize any of the articles on the article. Way to implement. Further, the steps may also be performed in a different order than those presented herein. In a preferred embodiment, a C-type parylene compound is used. In other embodiments, other types of parylene compounds may be used, including, but not limited to, N-type parylene compounds, D-type parylene compounds, and HT-type parylenes. Compound®. In some embodiments, the parylene compound may be derived from an N-type parylene compound, or parylene, by displacement of various chemical components. In a preferred embodiment, the parylene compound forms a completely linear, highly crystalline material. How to implement the method in order to present one of the specific examples of the method will be explained in more detail in the paragraphs of the following examples.

In some embodiments, step A, vaporizing the parylene dimer to form a gaseous parylene dimer by heating to 150 to 200 ° C may be carried out in a furnace chamber. In some embodiments, step B, the gaseous parylene dimer is cleaved into gaseous parylene monomer by heating the gaseous parylene dimer to 650 to 700 ° C. Will be implemented in a furnace room. In some embodiments, step C, injecting boron nitride into the gaseous parylene monomer of step B may be performed after step B. In some embodiments, the boron nitride may be injected into the gaseous parylene monomer in the form of a powder. One specific example of this step will be described in the examples section. In some embodiments, the boron nitride powder may be at least about 500 particles. In some embodiments, the boron nitride powder is between about 1.8 microns and about 2.5 microns.

In step D, the article to be coated may contact the gaseous parylene monomer and boron nitride for a sufficient period of time to deposit a parylene compound coating on the article. In some embodiments, this step may be performed in a deposition chamber. In other embodiments, the deposition chamber and the articles to be coated may be at room temperature, from about 5 ° C to about 30 ° C, or more preferably from about 20 ° C to about 25 ° C. In some embodiments, the length of time that the article can contact the gaseous parylene monomer and the boron nitride may be varied to control the parylene compound-boron nitride coating layer on the article. Final thickness. In various embodiments, the final thickness of the parylene compound-boron nitride coating layer may be between about 100 angstroms and about 3.0 millimeters. In some embodiments, the parylene compound is deposited for from about 8 hours to about 18 hours to achieve a coating thickness of about 0.05 mm. In some embodiments, the parylene compound is deposited for from about 5 hours to about 18 hours to achieve a coating thickness of about 0.05 mm. In a preferred embodiment, the final thickness of the parylene compound coating layer may be between about 0.5 mm and about 3.0 mm. The choice of the final thickness of the parylene coating layer will depend on the particular degree of the article to be coated and the end use of the article. Objects that need to be moved to function may want to have the thinnest The final coating, such as a power button. Objects that are immersed in water may wish to have a thicker coating.

In some embodiments, the method may have an additional step E for contacting the article to be coated with a decane composition until the decane is pretreated to the article. In a preferred embodiment, this step may be performed prior to step D. In some embodiments, when the article contacts the decane, the decane composition may be in solution. In other embodiments, the decane composition may be a gas when the article contacts the decane. In some embodiments, the decane composition may be a decane coupling agent® A-174 decane (Fig. 1E). This step is particularly advantageous to aid in the application of the parylene compound to the hydrophilic surface of the article.

Example

Example 1: Method and apparatus for coating articles with parylene compounds

This specific example uses a C-type parylene compound.

Coating process

The device consists of two sections: (1) a furnace/heating section; and (2) a vacuum section. The furnace section is composed of two furnaces which are connected by a glass tube called a retort. The furnace sections and vacuum sections are connected by valves that allow gas flow between the furnace sections and the vacuum section.

Mellen Furnace Co. (Concord, New Hampshire, USA) has manufactured the furnace section of the equipment, see Example 2. Laco Technologies Inc. (Salt Lake City, Utah, USA) has created a vacuum section.

The process for coating articles using a parylene compound is as follows:

(1) First furnace chamber. A C-type parylene compound in an amount sufficient to coat the dimeric form (bimolar form) of the article is placed in the furnace chamber. The articles are coated to a thickness ranging from 0.01 to 3.0 mm. The C-type parylene compound is placed in a stainless steel "boat" (standard container made of metal or glass) through which the tube is A vacuum fixed opening is inserted into the furnace (the boat is pushed into the furnace by a rod). After the C-type parylene compound is placed, the opening is sealed. Next, the furnace is heated to 150 to 200 ° C to create an environment that will cause the solid C-type parylene compound to become a gas. The gas is retained in the first furnace chamber before the two valves are opened. The first of the two valves does not open until the cold trap in the vacuum section is filled with liquid nitrogen (LN2) and the cold traps are "cold". LN2 is purchased from local suppliers. LN2 is placed in a one gallon container at the supplier. LN2 will be poured into the "cold trap" from the container. The second valve is variable and opens when the gas is withdrawn from the first furnace due to vacuum.

(2) The second furnace chamber. The C-type parylene compound gas is moved to the second furnace at a temperature of 650 to 700 °C. The heat in the furnace separates the C-type parylene compound gas into individual molecules (monomers). The monomeric form of the gas is then fed into the deposition chamber by vacuum.

(3) Vacuum chamber. The vacuum section of the machine consists of a deposition chamber with two vacuum cylinders. The first vacuum cylinder is a "rough" cartridge that is drawn into an initial vacuum. This initial pressure is in the range of 1 x 10-3 Torr. The second stage cylinder is then pumped to a final pressure in the range of 1x10-4 Torr. The vacuum cylinders are protected by a liquid nitrogen cold trap that protects the cylinders from condensation of the monomer gas by condensing the gas on the surface of the cold trap.

The item to be coated is placed on the scaffolding in the deposition chamber before the coating process begins. The areas above and inside the elements to be coated that are to be coated are masked (using well-known methods). This masking operation is performed in an area where electrical or mechanical connection must be maintained. The material will be applied to the article at room temperature (75 degrees Fahrenheit).

Inside the vacuum chamber there will be a cesium coupling agent® A-174 decane (available from Momentive Performance Materials Inc., Wilton, Conn.). Oh, the decane will be poured into a ceramic crucible. The crucible is inserted into a 2 inch thermocouple on a hot plate in the vacuum chamber. The amount of decane coupling agent® A-174 decane that is poured will depend on the amount of the item in the chamber, but will range from 10 to 100 ml. The plate will heat the decane coupling agent® A-174 decane to the point of evaporation, which will coat the entire area of the interior containing any items within the chamber.

Once the decane coupling agent vapor is withdrawn from the deposition chamber, the monomer gas is withdrawn due to the lower vacuum in the vacuum chamber. When the gas is fed into the chamber, it changes direction so that it will spray over the entire area of the chamber. The items are applied as the monomer gas cools. The gas will cool from 600 ° C to 25 ° C and will solidify on the components in the chamber. During the cooling process, the monomers are deposited on the surface of the article to be coated, resulting in a uniform and pinhole-free polymer three-dimensional chain. The deposition apparatus controls the coating rate and final thickness. The necessary thickness of the parylene compound coating layer depends on the time of exposure to the monomer gas. This thickness may range from hundreds of angstroms to several millimeters.

Example 2: Multi-temperature zone furnace for coating a parylene compound coating layer in the apparatus

Mellen Company, Inc. (Concord, New Hampshire, USA) has manufactured this furnace assembly. One of them is the Mellen model TV 12-3x32-1/2Z.

A solid tubular furnace in a single temperature zone or a dual temperature zone is capable of operating in air at temperatures up to 1200 °C. The furnace utilizes a 12V heating element from the Mellen standard series (exposed Fe-Cr-Al coils in a specially designed bracket). The furnace has an energy-saving ceramic fiber insulation package with a plurality of 2 inch long connecting tracks. The thermocouples are placed in the center of each temperature zone. A ten-foot power cable is provided in each temperature zone to help connect to the power source. A furnace will be designed for horizontal or vertical operation and has the following specifications:

Mellen Series PS205 Power Supply / Temperature Controller

One (1) Mellen model PS205-208-(2)25-S, two temperature zones, digital temperature controller and solid state relay. The Mellen series PS205 consists of the following:

a) Two (2) digital temperature controllers corrected for "S" type thermocouples featuring 126 sections and 31 programs.

b) One (1) solid state relay.

c) One (1) General Electric or Equivalent Circuit Breaker, Bipolar, which has a suitable size and a suitable rated amperage.

d) A (1) Mellen housing to accommodate the above components.

e) Two (2) "S" type thermocouples, each of which contains 10 compensated thermocouple extensions, terminal boards, etc.

f) All necessary wires, terminal boards, interconnects, etc. used to make a complete workable system.

Over temperature protection of power supply / temperature controller

A (1) over temperature (O.T.) alerter that uses a separate digit to indicate the digital setpoint "high limit alert" controller. The OT warning package is equipped with a suitable thermocouple, TIC extension cable, and enough (several) mechanical power contactors to interrupt the delivery to the furnace when an overtemperature condition occurs at the location of the overtemperature sensor. electric power. The O.T. warning option will be placed in the main temperature control enclosure.

Stem bottle model: RTA-2.5x32-OBE

The furnace described above will use a (1) Mellen model RTA-2.5-32-OBE, a round, high-purity aluminum (the actual system has a quartz retort). The retort has a working diameter of approximately 2.5 inches and an inner diameter of 32 inches. The retort has an outer diameter of approximately 2.75 inches and a length of 48 inches and contains the necessary stainless steel flange/seal fittings for airtight operation and thermal barriers. A feedthrough line is provided in the cover of the curved bottle for gas in/out and temperature measurement. The retort can be operated with different types of atmospheres.

Example 3: Method and apparatus for coating articles using polyparaxylene compounds and boron nitride

This specific example uses a C-type parylene compound.

Coating process

The device consists of two sections: (1) a furnace/heating section; and (2) a vacuum section. The furnace section is composed of two furnaces which are connected by a glass tube called a retort. The furnace sections and the vacuum section are connected by valves, the valves The door allows gas flow between the furnace sections and the vacuum section.

Mellen Furnace Co. (Concord, New Hampshire, USA) has manufactured the furnace section of the equipment. Laco Technologies Inc. (Salt Lake City, Utah, USA) has created a vacuum section.

The process for coating articles using polyparaxylene compounds and boron nitride is as follows:

(1) First furnace chamber. A C-type parylene compound in an amount sufficient to coat the dimeric form (bimolar form) of the article is placed in the furnace chamber. The articles are coated to a thickness ranging from 0.01 to 3.0 mm. The C-type parylene compound is placed in a stainless steel "boat" (standard container made of metal or glass) which is inserted into the furnace through the vacuum fixed opening of the tube ( The boat will be pushed into the furnace by a rod. After the C-type parylene compound is placed, the opening is sealed. Next, the furnace is heated to 150 to 200 ° C to create an environment that will cause the solid C-type parylene compound to become a gas. The gas is retained in the first furnace chamber before the two valves are opened. The first of the two valves does not open until the cold trap in the vacuum section is filled with liquid nitrogen (LN2) and the cold traps are "cold". LN2 is purchased from local suppliers. LN2 is placed in a one gallon container at the supplier. LN2 will be poured into the "cold trap" from the container. The second valve is variable and opens when the gas is withdrawn from the first furnace due to vacuum.

(2) The second furnace chamber. The C-type parylene compound gas is moved to the second furnace at a temperature of 650 to 700 °C. The heat in the furnace separates the C-type parylene compound gas into individual molecules (monomers). The monomeric form of the gas is then fed into the deposition chamber by vacuum.

The boron nitride in powder form is placed in a KF16 tube that is connected to a KF connecting tube having a "T" KF16 port. This K1716 tube is partially filled with the "charge" of boron nitride powder (minimum 500 particles). The KF16 body will be covered. For the coating After the coating process is initiated, boron is injected into the coating "flow". The boron will flow in the form of a powder and will be trapped as the coating process is deposited.

The K1716 body will be attached to the retort perpendicular to the flow of the monomer gas before it is about to enter the deposition chamber. There will be an open valve that allows boron nitride to flow into the gas. The gas will blend with the monomer and will be deposited on the item to be coated. This process is similar to powder coating. The process can be repeated to increase the amount of boron nitride in the coating applied to the article. Although not limiting the characteristics of the boron nitride/parylene compound coating layer; however, the inventors believe that boron nitride will improve the hardness of the coating layer and provide a better way to allow heat to leave the coated article. , for example, electronic components. Boron nitride is placed in the form of dust into the parylene compound.

(3) Vacuum chamber. The vacuum section of the machine consists of a deposition chamber with two vacuum cylinders. The first vacuum cylinder is a "rough" cartridge that is drawn into an initial vacuum. The initial vacuum is in the range of 1 x 10-3 Torr. The second stage cylinder is then pumped to a final vacuum in the 1x10-4 Torr range. The vacuum cylinders are protected by a liquid nitrogen cold trap that protects the cylinders from condensation of the monomer gas by condensing the gas on the surface of the cold trap.

The item to be coated is placed on the scaffolding in the deposition chamber before the coating process begins. The areas above and inside the elements to be coated that are to be coated are masked (using well-known methods). This masking operation is performed in an area where electrical or mechanical connection must be maintained. The material will be applied to the article at room temperature (75 degrees Fahrenheit).

Inside the vacuum chamber there is a helium filled with decane coupling agent® A-174 decane which is poured into a ceramic crucible. The crucible is inserted into a 2 inch thermocouple on a hot plate in the vacuum chamber. The amount of decane coupling agent® A-174 decane that is poured will depend on the amount of the item in the chamber, for example between 10 and 100 ml. The plate will heat the decane coupling agent® A-174 decane to the evaporation point, which will coat the entire area of the chamber. A domain that contains any objects in the room.

The monomer gas is withdrawn due to the lower vacuum in the vacuum chamber. When the gas is fed into the chamber, it changes direction so that it will spray over the entire area of the chamber. The items are applied as the monomer gas cools. The gas will cool from 600 ° C to 25 ° C and will solidify on the components in the chamber. During the cooling process, the monomers are deposited on the surface of the article to be coated, resulting in a uniform and pinhole-free polymer three-dimensional chain. The deposition apparatus controls the coating rate and final thickness. The necessary thickness of the parylene compound coating layer depends on the time of exposure to the monomer gas. This thickness may range from hundreds of angstroms to several millimeters.

While the invention has been described with respect to the embodiments of the present invention, it will be understood by those skilled in the art Or all advantages. For example, in some embodiments of the invention disclosed herein, a single device may be replaced by multiple devices, and multiple devices may be replaced by a single device for performing a given function or functions. This alternative is also intended to be encompassed within the scope of the present invention, except that this alternative is not made to the actual embodiments of the invention. Therefore, the specific examples disclosed herein are intended to embrace all such modifications, changes, and modifications, and the scope and spirit of the invention as defined by the appended claims. The preferred features of each of the aspects and specific examples of the present invention are susceptible to modification and other features.

The drawings and description of the present invention have been simplified to explain the related elements in order to clearly understand the present invention; at the same time, other elements have been omitted for clarity, for example, conventional conformal coating methods Or device device. For example, a particular conformal coating system may also include additional components not described herein, such as deposition chambers, valves, vacuum cylinders. However, those skilled in the art will appreciate that such and other components may be required in a typical conformal coating system. However, because such elements are well known in the art and because they do not help to better understand the present invention, such elements are not discussed herein.

In addition, any element that is represented by a component used to implement a specified function is intended to cover any means of performing the function, for example, a combination of components that perform the function. . Furthermore, in the invention defined by the patent application described in the "means plus function", the functions provided by the various described components are actually combined and defined by the scope of the attached patent application. The way is combined. Therefore, any component capable of providing such functionality can be considered equivalent to the components shown herein.

Unless otherwise indicated, all numbers that are used in this specification to indicate the quantity, time, temperature, coating thickness, and other characteristics or parameters used for the purposes of this specification will be It is decorated with the word "about". Accordingly, unless otherwise indicated, the numerical parameters set forth in the foregoing specification and the appended claims are intended to At the very least, and without any limitation of the scope of application of the equivalents of the subject matter of the invention, the numerical parameters should be understood in accordance with the numerical values of the important figures presented herein and the common rounding techniques.

In addition, as the above discussion, although the numerical ranges and parameters are set forth in the broad scope of the invention, the numerical values are set forth as much as possible. However, it should be understood that such values inherently contain specific errors due to measurement equipment and/or measurement techniques.

Any patents, publications, or other disclosures that are hereby incorporated by reference in their entirety, in their entirety, in their entirety, inso Or other disclosures. In this regard, and to the extent necessary, the disclosure explicitly set forth herein supersedes any content that is incorporated herein by reference. Any material that is incorporated herein by reference but that is contrary to the present definition, narrative, or other disclosures set forth herein, or a part thereof, is not incorporated herein by reference. The incorporation of the material and the existing disclosure material creates a violation.

1‧‧‧vaporization room

2‧‧‧Device

3‧‧‧ Pyrolysis Room

4‧‧‧ Valve

5‧‧‧Device

6‧‧‧Deposition room

7‧‧‧Items to be coated

8‧‧‧Devices/Connectors

9‧‧‧Vacuum components

10‧‧‧ Temperature zone

11‧‧‧ Temperature zone

12‧‧‧ Temperature zone

13‧‧‧temperature zone

14‧‧‧vacuum room/system

15‧‧‧vaporization room

16‧‧‧Devices

17‧‧‧ Pyrolysis Room

18‧‧‧ Valve

19‧‧‧Device

20‧‧‧T埠口

21‧‧‧Deposition room

22‧‧‧ Items to be coated

23‧‧‧Device

24‧‧‧Vacuum components

25‧‧‧vacuum room/system

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, which is optionally selected from the group consisting of: a D-type parylene compound , a C-type poly-p-xylene compound, an N-type poly-p-xylene compound, and an HT-type parylene compound®. A coating composition according to claim 2, which comprises two or more different parylene compounds. A coating composition according to claim 2 or 3, which comprises two or more parylene compounds of different purities. The coating composition of any one of claims 1 to 3, wherein the thermally conductive material is a ceramic. The coating composition of any one of claims 1 to 3, wherein the thermally conductive material is selected from the group consisting of aluminum nitride, aluminum oxide, and boron nitride. The coating composition according to any one of claims 1 to 3, wherein the heat conductive material has a body resistance coefficient greater than 10 ¹⁰ ohms * cm. The coating composition of any one of claims 1 to 3, wherein the thermally conductive material has a mass of up to about 3% of the total mass of the conformal coating compound and the thermally conductive material. The coating composition of any one of claims 1 to 3, wherein the thermally conductive material has a mass of up to about 1% of the total mass of the conformal coating compound and the thermally conductive material. The coating composition of claim 2 or 3 has a thermal conductivity higher than that of the individual parylene compound by 5 to 10%. The coating composition according to any one of claims 1 to 3, which has a hardness of from about R80 to about R95. The coating composition of any one of claims 1 to 3, wherein the thermally conductive material is dispersed in the polymer of the conformal coating compound. The coating composition according to any one of claims 1 to 3, wherein the coating composition is a gaseous mixture comprising a conformal coating compound monomer in a gas phase. The coating composition of claim 13, wherein the gaseous mixture comprises solid particles of the thermally conductive material. A conformal coating layer on at least a portion of a surface of an article comprising a coating composition according to any one of claims 1 to 14. The conformal coating of claim 15 wherein the object is an electronic component selected from the group consisting of: a communication component, a speaker, a mobile phone, an audio player, a camera , video players, remote control components, global positioning systems, computer devices, radar displays, depth detectors, fish detectors, emergency finger radio beacons (EPIRB), emergency positioning signal transmitters (ELTs), and personal positioning beacons ( PLB). The conformal coating layer of claim 15 wherein the object is selected from the group consisting of: paper products, textile products, artwork, circuit boards, marine detecting elements, space detecting elements, Harmful waste A waste transporting component, an automatic vehicle component, a motor component, a military system component, an ammunition, a firearm, a weapon, a medical instrument, and a biomedical component, wherein the biomedical component is optionally selected from the group consisting of: a hearing aid , cochlear implants and prosthetic limbs. The conformal coating of any one of claims 15 to 17, wherein the surface is a plastic, metal, wood, paper or textile material. The conformal coating of any one of clauses 15 to 17, wherein the surface is an outer surface of the article. The conformal coating of claim 18, wherein the surface is an outer surface of the article. An article comprising a conformal coating layer on at least a portion of a surface, wherein the conformal coating layer is comprised of the coating composition of any one of claims 1 to 14. An object as claimed in claim 21, wherein the object is an electronic component, the electronic component being selected from the following: a communication component, a speaker, a mobile phone, an audio player, a camera, a video player, Remote control components, global positioning systems, computer devices, radar displays, depth detectors, fish detectors, emergency finger radio beacons (EPIRB), emergency location signal transmitters (ELTs), and personal positioning beacons (PLBs). For example, the object of claim 21, wherein the object is selected from the group consisting of: paper products, textile products, art, circuit boards, marine detecting elements, space detecting elements, hazardous waste transportation Components, automatic vehicle components, motor components, military system components, ammunition, guns, weapons, medical instruments, and biomedical components, wherein the biomedical components Choose from the group consisting of the following: Hearing aids, cochlear implants, and prostheses. The article of any one of claims 21 to 23, wherein the surface is plastic, metal, wood, paper or textile material. The article of any one of claims 21 to 23, wherein the surface is an outer surface. An article of claim 24, wherein the surface is an outer surface. The article of any one of claims 21 to 23, wherein the surface is substantially covered by the conformal coating layer. An article of claim 24, wherein the surface is substantially covered by the conformal coating. The article of claim 25, wherein the surface is substantially covered by the conformal coating. The article of claim 26, wherein the surface is substantially covered by the conformal coating. A method for applying a conformal coating to an article comprising: A) heating a conformal coating compound to form a gaseous monomer of the conformal coating compound; B) incorporating a thermally conductive material And the gaseous monomer to form a gaseous mixture; and C) the conformal coating comprising the conformal coating compound and the thermally conductive material is formed on at least a portion of a surface of the article Contacting the article with the gaseous mixture to apply a conformal coating to the object. The method of claim 31, wherein the conformal coating compound is selected from the group consisting of polyparaxylene compounds in the group consisting of: D-type poly-p-xylene compound, C-type poly-pair Toluene compound, N-type poly-p-xylene compound, and HT-type parylene compound®. The method of claim 31, wherein the thermally conductive material is ceramic. The method of claim 31, wherein the thermally conductive material is selected from the group consisting of aluminum nitride, aluminum oxide, and boron nitride. The method of claim 31, wherein the thermally conductive material is in the form of solid particles. The method of claim 35, wherein the solid particles are from about 1.8 microns to about 2.5 microns. The method of claim 31, wherein the method further comprises contacting the article with gaseous decane prior to step C, under conditions in which the decane activates the surface of the article. The method of claim 37, wherein the decane is selected from the group consisting of one or more of decane: a silane coupling agent (Silquest)® A-174, a decane coupling agent® 111, and Hydrane coupling agent® A-174 (NT). The method of claim 31, wherein the article is at a temperature of from about 5 ° C to about 30 ° C during step C. The method of claim 31, wherein the conformal coating layer is from about 100 angstroms to about 3.0 millimeters. The method of claim 31, wherein the conformal coating layer has a thickness of from about 0.0025 mm to about 0.050 mm. The method of claim 31, wherein the object is an electronic component selected from the group consisting of: a communication component, a speaker, a mobile phone, an audio player, a camera, a video. Players, remote control components, global positioning systems, computer devices, radar displays, depth detectors, fish detectors, emergency finger radio beacons (EPIRB), emergency positioning signal transmitters (ELT), and personal positioning beacons (PLB) . The method of claim 31, wherein the object is selected from the group consisting of: paper products, textile products, artwork, circuit boards, marine detecting elements, space detecting elements, hazardous waste. Object transport components, automatic vehicle components, motor components, military system components, ammunition, firearms, weapons, medical instruments, and biomedical components, wherein the biomedical components are optionally selected from the group consisting of: hearing aids, Cochlear implants and prostheses. The method of claim 31, wherein the surface is plastic, metal, wood, paper or textile material. An article having a coating applied to at least a portion of a surface by a method according to any one of claims 31 to 44 of the patent application. An article of claim 45, wherein the surface is an outer surface. An apparatus for applying a conformal coating to an article, comprising: a vaporization chamber comprising at least two temperature zones; a pyrolysis chamber operatively coupled to the vaporization chamber; and a vacuum chamber operatively coupled to the pyrolysis chamber. The device of claim 47, further comprising a connector operatively coupled to the pyrolysis chamber and the vacuum chamber, wherein the connector is capable of transporting gas between the pyrolysis chamber and the vacuum chamber And wherein the connector comprises a T port. The device of claim 47, wherein the T-port is operatively coupled to an injection member for injecting a thermally conductive material from the pyrolysis chamber to the vacuum chamber via the connector. Among the gases. The apparatus of claim 47 or 48, wherein the vacuum chamber includes a deposition chamber operatively coupled to the pyrolysis chamber and a vacuum generating device. The device of claim 50, wherein the vacuum generating device comprises one or more vacuum cylinders. The apparatus of claim 47 or 48, wherein the vaporization chamber has two temperature zones. The apparatus of claim 47 or 48, wherein the vaporization chamber is a tubular furnace. The apparatus of claim 47 or 48, wherein the pyrolysis chamber has a plurality of temperature zones. A device according to claim 47 or 48, wherein the pyrolysis chamber has two temperature zones. A device according to claim 47 or 48, wherein the pyrolysis chamber is a tubular furnace.