CN110832116A - Articles and methods of making the same - Google Patents
Articles and methods of making the same Download PDFInfo
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- CN110832116A CN110832116A CN201880042667.4A CN201880042667A CN110832116A CN 110832116 A CN110832116 A CN 110832116A CN 201880042667 A CN201880042667 A CN 201880042667A CN 110832116 A CN110832116 A CN 110832116A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
Abstract
A method includes exposing a particle coating disposed on a heat-softenable film to a modulated source of electromagnetic radiation. The particle coating comprises different particles that are not covalently bonded to each other and do not remain in the binder material other than the heat-softenable film. Articles made by the method are also disclosed.
Description
Technical Field
The present disclosure broadly relates to methods for improving the durability of particulate coatings on heat-softenable films, and articles that can be made therefrom.
Background
Coatings of certain particles (e.g., graphite) on substrates can be formed by rubbing a powder containing the particles against a substrate such as, for example, a thermoplastic film. Such powder coatings will be referred to herein as "powder friction coatings". Examples of powder friction coatings and methods of forming the same include those disclosed in U.S. patent 6,511,701B 1 (Divigalpitiaya et al). However, such films are often susceptible to damage by methods such as grinding and/or rinsing with solvents.
Disclosure of Invention
In a first aspect, the present disclosure provides a method comprising exposing a particle coating disposed on a heat-softenable film to a modulated source of electromagnetic radiation (e.g., a flash lamp), wherein the particle coating comprises loosely bound distinct particles that are not covalently bonded to each other and do not remain in a binder material other than the heat-softenable film.
By this technique, the durability of the powder coating is improved, while alternative heating methods are prone to damage (e.g., warping) the heat-softenable film.
Accordingly, in a second aspect, the present disclosure provides an article made according to the method of the first aspect of the present disclosure.
In a third aspect, the present disclosure provides an article comprising a heat-softenable film having a particulate coating disposed thereon, wherein the particulate coating comprises distinct particles that are not covalently bonded to one another and that are not retained in a binder material other than the heat-softenable film, and wherein at least a portion of the particulate coating corresponding to a predetermined pattern has a greater transmission of visible light than at least a portion of the particulate coating not disposed within the predetermined pattern.
In a fourth aspect, the present disclosure provides an article comprising a heat-softenable film having disposed thereon a particle coating, wherein the particle coating comprises distinct particles that are not chemically bonded to one another and that do not remain in a binder material other than the heat-softenable film, and wherein the change in transmission is up to 60% after grinding the particle coating according to ASTM D6279-15 "Standard Test Method for Rub abrasive wear resistance of High Gloss Coatings (Standard Test Method for Rub Abrasion resistance of High Gloss Coatings)", wherein a 25mm friction element is provided using a two inch square crock tester cloth soaked in isopropanol for three seconds.
As used herein:
the term "visible light" refers to electromagnetic radiation having a wavelength of 400 nanometers (nm) to 700 nanometers (nm).
The term "powder" refers to a free-flowing collection of fine particles.
The term "pulsed electromagnetic radiation" refers to electromagnetic radiation that is modulated as a series of discrete spikes of increasing intensity. The spike may be relative to a background level of negligible or zero electromagnetic radiation, or the background level may be at a higher level that is substantially ineffective to increase the adhesion of the particles to the film in the particle coating.
The term "heat softenable" means softenable when heated.
The term "particle coating" refers to a coating of small particles that may or may not be free-flowing.
The features and advantages of the present disclosure will be further understood upon consideration of the detailed description and appended claims.
Drawings
Fig. 1 is an enlarged schematic side view of an exemplary article 100 according to the present disclosure.
FIG. 2 is a digital photograph of the mask used in example 9 (EX-9).
Figure 3 is a digital photograph of a flash lamp treated graphite coated film in EX-9.
Fig. 4 is a digital photograph of a flash lamp treated graphite coated film in EX-9 after grinding of a solvent soaked wipe.
It should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the scope and spirit of the principles of this disclosure.
Detailed Description
Advantageously, the present disclosure provides an easy method of enhancing the durability of particle coatings (e.g., to solvent milling) on heat-softenable films using transient heating by exposure to a modulated electromagnetic radiation source.
Referring now to fig. 1, an exemplary article 100 includes a heat-softenable (e.g., thermoplastic) film 110 having a particulate coating 120 disposed thereon. The particle coating comprises different particles that are not covalently bonded to each other and do not remain in the binder material other than the heat-softenable film.
Particle coatings on heat-softenable films can be prepared by a variety of known methods including, for example, exposure to an atomized particle cloud, contact with a powder bed, coating with a solvent-based powder dispersion coating and then evaporating the solvent, and/or friction bonding of the powder using a rubbing process (rubbing dry particles against a substrate to form a powder rubbed coating). Examples of friction bonding methods can be found in U.S. Pat. Nos. 6,511,701B 1 (Divigalpitiaya et al), 6,025,014(Stango) and 4,741,918(Nagybaczon et al). The remaining methods are familiar to those of ordinary skill in the art.
Useful powders include small loosely bound particles capable of absorbing at least one wavelength of pulsed electromagnetic radiation, preferably corresponding to a majority of the energy of the pulsed electromagnetic radiation. Suitable powders are preferably at least substantially impervious to electromagnetic radiation, yet robust to strong absorbers thereof. It is desirable to maximize light (electromagnetic radiation) to thermal conversion yield without changing the chemical nature of the powder particles.
Suitable powders include powders comprising: graphite, clay, hexagonal boron nitride, pigments, inorganic oxides (e.g., alumina, calcium oxide, silica, ceria, zinc oxide, or titanium dioxide), metals, organic polymer particles (e.g., polytetrafluoroethylene, polyvinylidene fluoride), carbides (e.g., silicon carbide), flame retardants (e.g., aluminum trihydrate, aluminum hydroxide, magnesium hydroxide, sodium hexametaphosphate, organophosphonates, and phosphates and esters thereof), carbonates (e.g., calcium carbonate, magnesium carbonate, sodium carbonate), dried biological powders (e.g., spores, bacteria), and combinations thereof. Preferably, the powder particles have an average particle size of from 0.1 to 100 microns, more preferably from 1 to 50 microns, and more preferably from 1 to 25 microns, but this is not required. Graphite and hexagonal boron nitride are particularly preferred in many applications.
In some embodiments, the particulate coating may consist essentially of (i.e., at least 98 wt.%, preferably at least 99 wt.%) or even consist of powder particles (e.g., graphite particles) after application.
Prior to exposure to electromagnetic radiation, the particle coating comprises loosely bound distinct particles that are not covalently bonded to each other and that do not remain in the binder material other than the heat-softenable film itself.
The heat-softenable film may comprise one or more heat-softenable (e.g., lightly crosslinked and/or thermoplastic) polymers. Exemplary heat-softenable polymers that may be suitable for inclusion in the heat-softenable film include polycarbonates, polyesters, polyamides, polyimides, polyurethanes, Polyetherketones (PEK), Polyetheretherketones (PEEK), polyphenylene sulfides, polyacrylics (e.g., polymethyl methacrylate), polyolefins (e.g., polyethylene, polypropylene, biaxially oriented polypropylene), and combinations of such resins.
The pulsed electromagnetic radiation can be from any source capable of generating sufficient fluence and pulse duration to achieve sufficient heating of the heat-softenable film to more tightly bond the particle coating thereto. At least three types of sources may be effective for this purpose: flash lamps, lasers, and shutter lamps. The selection of an appropriate source will typically be influenced by the desired process conditions (e.g., line speed, line width, spectral output, and cost).
Preferably, the pulsed electromagnetic radiation is generated using a flash lamp. Of which xenon flash lamps and krypton flash lamps are the most common. Both provide a broad continuous output in the wavelength range of 200 to 1000 nanometers, however krypton flash lamps have a higher relative output intensity in the wavelength range of 750 to 900nm compared to xenon flash lamps which have more relative output in the wavelength range of 300 to 750 nm. Xenon flash lamps are generally preferred for most applications, especially those involving graphite powders. Many suitable xenon and krypton flashlamps are commercially available from suppliers such as the Eleutida Technologies Corp. of Waltham, Mass and Hewley, Heraeus of Hanau, Germany, Haxan, Germany.
In another embodiment, the pulsed electromagnetic radiation may be generated using a pulsed laser. Suitable lasers may include, for example, excimer lasers (e.g., XeF (351nm), XeCl (308nm), and KrF (248nm)), solid-state lasers (e.g., ruby (694nm)), and nitrogen lasers (337.1 nm).
In yet another embodiment, the pulsed electromagnetic radiation is generated using a continuous light source and a shutter (preferably a rotating aperture/shutter to reduce overheating of the shutter). Suitable light sources may include high pressure mercury lamps, xenon lamps, and metal halide lamps.
To achieve maximum efficiency, the electromagnetic radiation spectrum is preferably most intense at wavelengths that are strongly absorbed by the powder particles, but this is not a requirement. Also, in the case of reflective particles, the electromagnetic radiation spectrum is preferably most intense in the region of the spectrum where the powder is least reflective, but this is not a requirement.
Preferably, the pulsed electromagnetic radiation source is capable of generating a high fluence (energy density) with a high intensity (high power/unit area), but this is not a requirement. These conditions ensure that sufficient heat is absorbed to achieve increased adhesion of the powder particles to the film. However, the combination of intensity and fluence should not be too large/high to cause ablation, excessive degradation, or volatilization of the heat-softenable film. The selection of suitable conditions is within the ability of one of ordinary skill in the art.
In order to minimize heating of the inner part of the heat-softenable film that cannot interact with the powder particles, the pulse duration is preferably short; for example, less than 10 milliseconds, less than 1 millisecond, less than 100 microseconds, less than 10 microseconds, or even less than 1 microsecond, although this is not a requirement.
To achieve high line speeds in a continuous manufacturing process, not only should the pulsed electromagnetic radiation be preferably strong, but the exposure area is preferably large, and the pulse repetition rate is preferably fast (e.g., 100Hz to 500 Hz).
Advantageously, the modulated electromagnetic radiation may be directed through a mask having transmissive and non-transmissive regions according to a predetermined pattern (see, e.g., fig. 2). Thus, the exposed areas of the particle coating may become more transparent to visible light than the unexposed areas of the particle coating (see fig. 3). After an optional development step (e.g., light milling of the solvent soaked wipe), the particle coating remains in the exposed areas according to a predetermined pattern while substantially or completely removing the particle coating in the unexposed (i.e., masked) areas (see fig. 4).
Selected embodiments of the present disclosure
In a first embodiment, the present disclosure provides a method comprising exposing a particle coating disposed on a heat-softenable film to a modulated source of electromagnetic radiation, wherein the particle coating comprises loosely bound distinct particles that are not covalently bonded to each other and that are not retained in a binder material other than the heat-softenable film.
In a second embodiment, the present disclosure provides the method according to the first embodiment, wherein the particulate coating comprises at least one of graphite or hexagonal boron nitride.
In a third embodiment, the present disclosure provides the method according to the first or second embodiment, wherein the particle coating consists essentially of graphite.
In a fourth embodiment, the present disclosure provides the method according to any one of the first to third embodiments, wherein the modulated electromagnetic radiation source comprises a flash lamp.
In a fifth embodiment, the present disclosure provides the method according to any one of the first to third embodiments, wherein the modulated electromagnetic radiation source comprises a pulsed laser.
In a sixth embodiment, the present disclosure provides the method according to any one of the first to third embodiments, wherein the particulate coating comprises a powder friction coating.
In a seventh embodiment, the present disclosure provides the method according to any one of the first to sixth embodiments, wherein the particle coating is exposed to pulsed electromagnetic radiation according to a predetermined pattern.
In an eighth embodiment, the present disclosure provides an article made according to the method of any one of the first to seventh embodiments.
In a ninth embodiment, the present disclosure provides an article comprising a heat-softenable film having a particulate coating disposed thereon, wherein the particulate coating comprises distinct particles that are not covalently bonded to one another and that do not remain in a binder material other than the heat-softenable film, and wherein at least a portion of the particulate coating corresponding to a predetermined pattern has a greater transmission of visible light than at least a portion of the particulate coating not disposed within the predetermined pattern.
In a tenth embodiment, the present disclosure provides an article according to the ninth embodiment, wherein the particulate coating comprises at least one of graphite or hexagonal boron nitride.
In an eleventh embodiment, the present disclosure provides an article according to the ninth or tenth embodiment, wherein the particulate coating consists essentially of graphite.
In a twelfth embodiment, the present disclosure provides the article of any one of the ninth to eleventh embodiments, wherein the heat-softenable film comprises polyethylene terephthalate.
In a twelfth embodiment, the present disclosure provides the article of any one of the ninth to eleventh embodiments, wherein the heat-softenable film comprises polyethylene terephthalate.
In a thirteenth embodiment, the present disclosure provides an article according to any one of the ninth to twelfth embodiments, wherein the predetermined pattern comprises circuit traces.
In a fourteenth embodiment, the present disclosure provides an article according to any one of the ninth to thirteenth embodiments, wherein at least a portion of the particulate coating not disposed within the predetermined pattern comprises a powder friction coating.
In a fifteenth embodiment, the present disclosure provides an article comprising a heat-softenable film having disposed thereon a particle coating, wherein the particle coating comprises distinct particles that are not chemically bonded to one another and that do not remain in a binder material other than the heat-softenable film, and wherein the change in transmission is up to 60% after grinding the particle coating according to ASTM D6279-15, "standard test method for friction abrasive wear resistance of high gloss coatings," wherein a 25mm friction element is provided using a two inch square crock tester cloth soaked in isopropanol for three seconds.
In a sixteenth embodiment, the present disclosure provides an article according to the fifteenth embodiment, wherein the particulate coating comprises a powder friction coating.
In a seventeenth embodiment, the present disclosure provides the article of the fifteenth or sixteenth embodiment, wherein at least a portion of the particulate coating corresponding to the predetermined pattern has a greater transmission of visible light than at least a portion of the particulate coating not disposed within the predetermined pattern.
Objects and advantages of this disclosure are further illustrated by the following non-limiting examples, but the particular materials and amounts thereof recited in these examples, as well as other conditions and details, should not be construed to unduly limit this disclosure.
Examples
Unless otherwise indicated, all parts, percentages, ratios, and the like in the examples and the remainder of the specification are by weight. All reagents used in the examples were obtained or purchased from general chemical suppliers, such as Sigma-Aldrich Company of st Louis, Missouri, or may be synthesized by conventional methods.
Materials used in the examples
General Process for coating graphite on a substrate
To prepare the examples and comparative examples described below, a graphite coating was applied to the PET film by placing a small amount of MICRO850 on the PET film. Graphite was then rubbed against the membrane using a WEN 10PMC 10 inch (25.8-cm) random orbital wax coater/polisher (WEN Products, Elgin, Illinois) equipped with a wool buffing cap. The relative amount of graphite coating deposited on the PET film was determined by measuring the surface resistivity using a four-point probe and/or light transmittance.
Visible light transmission was measured for examples EX-1 to EX-12 and comparative examples CEX-A to CEX-C using a HAZE-GARD PLUS HAZE meter from BYK Additives and Instruments, Wesel, Germany, of DE Coverzel.
For examples EX-6 to EX-8, the surface resistivity was measured using an RC 2175R-CHEK surface resistivity meter from EDTM, Inc (Toledo, Ohio), Toledo, Ohio.
For comparative examples CEX-D to CEX-L, light transmittance was measured using a Flame-T-XR1-ES spectrophotometer from ocean optics, Inc. (Oceanoptics, Dunnedin, Florida), but Neniten, Florida. These transmission measurements were recorded over a wavelength range of 325nm to 1000nm and averaged.
If a thicker coating is desired, more graphite is applied and the coating step is repeated.
General method for determining durability
The durability (restoring force of coating layer) of the samples prepared according to the examples and comparative examples described below was tested.
Durability of the graphite coated film samples was evaluated using a model 5750 linear grinder from Taber Industries, north tonawanda, New York, north tonanda, n.y. For CEX-A, CEX-B, EX-1 to EX-9 and CEX-D to CEX-L, the 25mm flat head on the linear grinder was covered with an L40 WYPALL universal wipe from Kimberly-Clark and saturated with isopropanol. The film was then subjected to 60 cycles/min of abrasion for a total of one minute using a 5750 linear abrasion machine with a total mass load on the head of 350 g. The durability of CEX-C and EX10 to EX12 was evaluated according to ASTM D6279-15, "standard test method for abrasion wear resistance of friction abrasives for high gloss coatings" (ASTM International, West consisocken, Pennsylvania), wherein a 25mm friction element was provided using a two inch (5.1cm) square crock tester cloth soaked in isopropanol for three seconds. Crock tester cloth is available from Testfabrics, inc. West Pittson, Pennsylvania. The crock cloth conforms to the specifications of ASTM D3690-02(2009) "Standard Performance Specification for Vinyl-Coated and Urethane-Coated Upholstery Fabrics-interior Standard Performance specifications for Vinyl-Coated and Urethane-Coated Fabrics-indicators. The transmittance of the graphite coated film samples was measured before and after the durability test. All transmittance measurements represent the average of at least 3 measurements.
All reported percent changes in transmission are calculated by the following equation:
wherein T isFilmIs the transmittance, T, of the underlying polymer filmCIs the transmittance of the same film after coating and treatment have been applied, and TGrindingIs the transmittance of the coating after being subjected to the desired number of grinding cycles. The transmission value of the film is typically about 92 ± 5%, depending on the quality of the substrate used. A smaller change in transmission (Δ T,%) indicates a higher retention of the total fraction of carbon on the original film.
Examples EX-1 to EX-12 and comparative examples CEX-A to CEX-C
CEX-a to CEX-C and EX-1 to EX-12 were prepared by subjecting the graphite-coated PET substrate film prepared as described above to Intense Pulsed Light (IPL) irradiation. In all cases of IPL, the source used was a SINTERON S-2100 Xe flash lamp equipped with a type C bulb from Xenon Corporation, Wilmington, Massachusetts, Wilmington, Mass.
For CEX-A and EX-1, the substrate was Bare PET. EX-1 was placed under a flash lamp with the graphite-coated surface facing up and at a pulse rate of 1Hz and 0.4J/cm2Ten times.
CEX-B was prepared in the same manner as CEX-A except that the substrate was Melinex PET.
EX-2 was prepared in the same manner as EX-1, except that the substrate was Melinex PET and the pulse rate was 1Hz and 0.3J/cm2The energy density of (3) was treated 5 times.
EX-3 and EX-4 were prepared in the same manner as EX-2, except that the pulse rate was 1Hz and 0.5J/cm2(EX-3) and 1.0J/cm2(EX-4) energy Density treatment of the film 1 time.
EX-5 was prepared similarly to EX-4, except that the film was flipped so that the graphite coated surface faced away from the flash lamp bulb.
Table 1 below reports the effect of IPL on barrel PET and Melinex PET.
TABLE 1
| Examples | IPL pulse | Energy density/pulse, J/cm2 | ΔT，％ |
| CEX-A | 0 | 0 | 100.0 |
| EX-1 | 10 | 0.4 | 13.3 |
| CEX-B | 0 | 0 | 98.3 |
| EX-2 | 5 | 0.3 | 29.9 |
| EX-3 | 1 | 0.5 | 20.9 |
| EX-4 | 1 | 1.0 | 10.5 |
| EX-5 | 1 | 1.0 | 5.4 |
EX-6 to EX-8 were prepared by coating three separate Bare PET sheets with different amounts of graphite to obtain different surface resistivity values for each example. EX-6 to EX-8 were placed under a flash lamp with the graphite-coated surface facing upwards and at a pulse rate of 1Hz and 0.4J/cm2Ten times. Table 2 below reports the change in transmission Δ T in%.
TABLE 2
| Examples | Initial surface resistivity, Ω/square | ΔT，％ |
| EX-6 | 250 | 14.5 |
| EX-7 | 564 | 22.3 |
| EX-8 | 975 | 23.4 |
For EX-9, the graphite coated substrate was Bare PET. A chrome/glass patterned photomask (shown in fig. 2) was positioned between the flash lamp and graphite prior to exposure to the IPL. The area directly adjacent to the mask is denoted as unmasked area, while the area below the mask is masked to avoid suffering from IPL and is denoted as masked area. In addition, the photomask includes a linear shaped opening in the chromium layer having a width of approximately about 250 microns or having a width of approximately about 500 microns. This demonstrates the ability of these coatings to be patterned, with the open portions of the mask representing the desired pattern for improved particle retention. Table 3 reports the effect of IPL on particle retention of masked and unmasked (patterned) graphite coated PET.
Fig. 3 shows the resulting pattern having portions located below the openings and masked portions. Fig. 4 shows the resulting pattern after being subjected to grinding as described above, wherein the portions located below the openings remain coated with carbon and the masked portions are devoid of carbon due to grinding.
TABLE 3
| EX-9 | ΔT，％ |
| Masking | 99.3 |
| Is not masked | 15.0 |
For CEX-C to EX-10,the substrate was Bare PET. EX-10 was placed under a flash lamp with the graphite-coated surface facing up and at a pulse rate of 1Hz and 0.4J/cm2Ten times.
EX-11 was prepared in the same manner as EX-10, except that the film was coated with varying amounts of graphite to obtain higher surface resistivity values than EX-10.
EX-12 was prepared in the same manner as EX-10, except that the substrate was Melinex PET, and at a pulse rate of 1Hz and 0.3J/cm2The energy density of (3) was treated 5 times.
Table 4 below reports the change in transmission Δ T in%.
TABLE 4
| Examples | IPL pulse | Energy density/pulse, J/cm2 | ΔT，％ |
| CEX-C | 0 | 0 | 79.4 |
| EX-10 | 10 | 0.4 | 5.9 |
| EX-11 | 10 | 0.4 | 11.1 |
| EX-12 | 5 | 0.3 | 8.2 |
Comparative examples CEX-D to CEX-L
For CEX-D to CEX-L, several barrel PET sheets were coated with graphite as described above and subjected to several different methods to induce particle retention.
For CEX-D to CEX-F, graphite coated Bare PET films were subjected to heat blowing by a temperature controlled heat gun (sternel America inc., Bloomington, Minnesota, sternline electron heat gun model HL 2010E, model 3482, available from sternline America inc. With the heat gun set at stage II, one end of the nozzle was located 2 inches (about 5cm) above and perpendicular to the film surface, which was secured to the desktop with tape at each end, and heat was applied to the film for a given amount of time.
For CEX-G through CEX-J, the graphite coated barrel PET film was subjected to electron beam irradiation using an electron beam system (model CB-300 electron beam system from Energy Sciences, inc., Wilmington, Massachusetts), a model CB-300 electron beam system from Wilmington, Massachusetts. The coated PET samples were glued onto a moving PET web and conveyed through an electron beam processor at a voltage of 110 keV. The web speed and electron beam current applied to the cathode were varied to ensure that the target dose was delivered.
For CEX-K to CEX-L, the graphite coated Bare PET film was subjected to biaxial strain using a laboratory stretcher (Br ü cknerMaschinenbau, obtained from sn gesdov, Germany (Br ü ckner Maschinenbau GmbH & co. kg, Siegsdorf, Germany) Br ü ckner Maschinenbau, model Karo IV biaxial stretcher the oven of the machine was set to 150 ℃ and the sample was placed in the oven for 5 minutes and then biaxially stretched at a constant rate of 1%/second.
Tables 5 to 7 summarize the effect of heat gun (table 5), electron beam (table 6) and biaxial stretching (table 7) exposure on particle retention (Δ T,%, change in average normalized transmission). For the heat gun, an output of greater than 232 ℃ and/or an output lasting longer than 10 minutes was also applied, but this was found to lead to two cases: excessive thermal degradation of the polymer or unrealistic processing conditions for manufacturing. For biaxial stretching, more than 5% stretching was also applied, but this was found to result in excessive tension of the polymer causing film breakage.
TABLE 5
| Examples | Temperature, C | Duration of time in minutes | ΔT，％ |
| CEX-D | 232 | 1 | 90.4 |
| CEX-E | 232 | 5 | 89.1 |
| CEX-F | 232 | 10 | 81.3 |
TABLE 6
| Examples | Dose, MRad | ΔT，％ |
| CEX-G | 2.5 | 90.0 |
| CEX-H | 5 | 88.9 |
| CEX-I | 10 | 91.3 |
| CEX-J | 20 | 90.4 |
TABLE 7
| Examples | Temperature, C | % elongation | ΔT，％ |
| CEX-K | 150 | 0 | 92 |
| CEX-L | 150 | 5 | 93.8 |
Claims (17)
1. A method of making an article, the method comprising exposing a particle coating disposed on a heat-softenable film to a modulated source of electromagnetic radiation, wherein the particle coating comprises loosely bound distinct particles that are not covalently bonded to each other and that do not remain in a binder material other than the heat-softenable film.
2. The method of claim 1, wherein the particulate coating comprises at least one of graphite or hexagonal boron nitride.
3. The method of claim 1 or 2, wherein the particle coating consists essentially of graphite.
4. The method of any one of claims 1 to 3, wherein the modulated electromagnetic radiation source comprises a flash lamp.
5. The method of any one of claims 1 to 3, wherein the modulated electromagnetic radiation source comprises a pulsed laser.
6. The method of any one of claims 1 to 3, wherein the particulate coating comprises a powder friction coating.
7. The method according to any one of claims 1 to 6, wherein the particle coating is exposed to pulsed electromagnetic radiation according to a predetermined pattern.
8. An article prepared according to the method of any one of claims 1 to 7.
9. An article comprising a heat-softenable film having a particulate coating disposed thereon, wherein the particulate coating comprises distinct particles that are not covalently bonded to one another and that are not retained in a binder material other than the heat-softenable film, and wherein at least a portion of the particulate coating corresponding to a predetermined pattern has a greater transmission of visible light than at least a portion of the particulate coating not disposed within the predetermined pattern.
10. The article of claim 9, wherein the particulate coating comprises at least one of graphite or hexagonal boron nitride.
11. The article of claim 9 or 10, wherein the particulate coating consists essentially of graphite.
12. The article of any one of claims 9 to 11, wherein the heat-softenable film comprises polyethylene terephthalate.
13. The article of any of claims 9 to 12, wherein the predetermined pattern comprises circuit traces.
14. The article of any one of claims 9 to 13, wherein the at least a portion of the particulate coating not disposed within the predetermined pattern comprises a powder friction coating.
15. An article comprising a heat-softenable film having disposed thereon a particulate coating, wherein the particulate coating comprises distinct particles that are not chemically bonded to one another and that do not remain in a binder material other than the heat-softenable film, and wherein the change in transmission is up to 60% after grinding the particulate coating according to ASTM D6279-15 "standard test method for friction grind abrasion resistance for high gloss coatings", wherein a 25mm friction element is provided using a two inch square crock tester cloth soaked in isopropanol for three seconds.
16. The article of claim 15, wherein the particulate coating comprises a powder friction coating.
17. The article of claim 15 or 16, wherein at least a portion of the particulate coating corresponding to a predetermined pattern has a greater transmission of visible light than at least a portion of the particulate coating not disposed within the predetermined pattern.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11241711B2 (en) | 2017-03-22 | 2022-02-08 | 3M Innovative Properties Company | Buff-coated article and method of making the same |
| CN110785684B (en) | 2017-06-29 | 2022-06-03 | 3M创新有限公司 | Article and method of making the same |
| KR102461992B1 (en) * | 2020-12-30 | 2022-11-03 | 마이크로컴퍼지트 주식회사 | Coating method of coating solution comprising hexagonal boron nitride particles and heat dissipation member manufactured thereby |
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| US5925402A (en) * | 1998-07-15 | 1999-07-20 | Morton International, Inc. | Method of forming a hidden identification using powder coating |
| JP2002069607A (en) * | 2000-06-16 | 2002-03-08 | Mitsubishi Heavy Ind Ltd | Coating material for shielding heat, its production method, gas-turbine member applied with the same material, and gas turbine |
| US6511701B1 (en) * | 2000-05-09 | 2003-01-28 | 3M Innovative Properties Company | Coatings and methods |
| TW200301319A (en) * | 2001-12-27 | 2003-07-01 | Ebara Corp | Substrate processing apparatus and method |
| US20050147767A1 (en) * | 2001-11-28 | 2005-07-07 | Peter Choi | Method for coating a support with a material |
| GB0523280D0 (en) * | 2004-12-07 | 2005-12-21 | 3D Systems Inc | Controlled densification of fusible powders in laser sintering |
| CN104066573A (en) * | 2011-12-22 | 2014-09-24 | 3M创新有限公司 | Carbon coated articles and methods for making the same |
| US20150344712A1 (en) * | 2014-05-27 | 2015-12-03 | Paul W. Harrison | High contrast surface marking using nanoparticle materials |
| US20170145554A1 (en) * | 2014-06-26 | 2017-05-25 | Shell Oil Company | Coating method and coated substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5827368A (en) | 1997-06-02 | 1998-10-27 | Marquette University | Device for depositing a layer of material on a surface |
| JP2009124029A (en) | 2007-11-16 | 2009-06-04 | Shinshu Univ | Method of manufacturing electronic circuit board using ink jetting |
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2018
- 2018-06-27 US US16/626,238 patent/US20200115804A1/en not_active Abandoned
- 2018-06-27 CN CN201880042667.4A patent/CN110832116B/en active Active
- 2018-06-27 JP JP2019572188A patent/JP7170677B2/en active Active
- 2018-06-27 WO PCT/IB2018/054772 patent/WO2019003153A1/en unknown
- 2018-06-27 EP EP18755304.5A patent/EP3645769A1/en active Pending
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|---|---|---|---|---|
| US4741918A (en) * | 1984-01-24 | 1988-05-03 | Tribohesion Limited | Coating process |
| US5925402A (en) * | 1998-07-15 | 1999-07-20 | Morton International, Inc. | Method of forming a hidden identification using powder coating |
| US6511701B1 (en) * | 2000-05-09 | 2003-01-28 | 3M Innovative Properties Company | Coatings and methods |
| JP2002069607A (en) * | 2000-06-16 | 2002-03-08 | Mitsubishi Heavy Ind Ltd | Coating material for shielding heat, its production method, gas-turbine member applied with the same material, and gas turbine |
| US20050147767A1 (en) * | 2001-11-28 | 2005-07-07 | Peter Choi | Method for coating a support with a material |
| TW200301319A (en) * | 2001-12-27 | 2003-07-01 | Ebara Corp | Substrate processing apparatus and method |
| GB0523280D0 (en) * | 2004-12-07 | 2005-12-21 | 3D Systems Inc | Controlled densification of fusible powders in laser sintering |
| CN104066573A (en) * | 2011-12-22 | 2014-09-24 | 3M创新有限公司 | Carbon coated articles and methods for making the same |
| US20150344712A1 (en) * | 2014-05-27 | 2015-12-03 | Paul W. Harrison | High contrast surface marking using nanoparticle materials |
| US20170145554A1 (en) * | 2014-06-26 | 2017-05-25 | Shell Oil Company | Coating method and coated substrate |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2019003153A1 (en) | 2019-01-03 |
| JP2020525271A (en) | 2020-08-27 |
| US20200115804A1 (en) | 2020-04-16 |
| JP7170677B2 (en) | 2022-11-14 |
| EP3645769A1 (en) | 2020-05-06 |
| CN110832116B (en) | 2023-01-13 |
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