Coating, method for preparing coating, and device

Abstract

Provided are a coating, a method for preparing a coating, and a device. The method for preparing a coating comprises: placing a substrate on a support in a plasma reaction chamber; introducing an activating gas, and starting first plasma discharge to pretreat the substrate; and introducing an organic silicon monomer into the plasma reaction chamber, starting second plasma discharge, and applying a bias voltage to the support to deposit and form a coating having a thickness of 400 nm to 2000 nm on at least part of the surface of the substrate. The coating has excellent light transmission performance, vulcanization resistance, and environmental aging resistance.

Description

Coatings, coating preparation methods, and devices

[0001] This application claims priority to Chinese Patent Application No. 202411956544.5, filed on December 27, 2024, entitled "Coating, Method for Preparing Coating, and Device", the entire contents of which are incorporated herein by reference. Technical Field

[0002] This disclosure relates to the field of chemical protective coatings, specifically to a coating, a method for preparing the coating, and a device. Background Technology

[0003] Light-emitting diodes (LEDs), as commonly used light-emitting devices, emit light by releasing energy through the recombination of electrons and holes, achieving efficient conversion between electrical and light energy. LEDs are widely used in various fields due to their advantages such as high efficiency, long lifespan, environmental friendliness, fast response, diverse colors, intelligent control, and decreasing costs with technological advancements. In the display field, LEDs are widely used in televisions, computers, mobile phones, and advertising screens; in the lighting field, LEDs are used in general lighting, automotive lighting, and decorative lighting; in the signaling system and information board field, LEDs are commonly used in traffic lights, emergency vehicle photos, and information display boards; in addition, LEDs are also used in specialized fields such as medical equipment, remote controls, and plant growth lights. However, during the production and use of LEDs, protection is necessary, especially avoiding contact with sulfide gases. Sulfide gases may react chemically with LEDs, leading to performance degradation, such as decreased luminous flux, color temperature drift, shortened lifespan, or even failure.

[0004] During the production and use of LED products, they are sometimes exposed to sulfurous gas environments. Common anti-sulfurization measures include selecting sulfur-resistant LED materials, optimizing product structure design to improve anti-sulfurization performance from a mechanical perspective, and improving product sealing to reduce the impact of sulfurous gases. However, in practice, these measures are difficult to completely isolate sulfurous gases and often present several problems. For example, using phenyl adhesives as encapsulation materials increases production costs; using organic gas barrier materials to protect LED chips can lead to degradation and cracking due to molecular fission under high temperatures. Summary of the Invention

[0005] To address the aforementioned problems, this disclosure provides a method for preparing a coating. The method includes: placing a substrate in a support within a plasma reaction chamber; introducing an activation gas and activating a first plasma discharge to pretreat the substrate; introducing an organosilicon monomer into the plasma reaction chamber, activating a second plasma discharge, and applying a bias voltage to the support to deposit a coating with a thickness of 400 nm to 2000 nm on at least a portion of the surface of the substrate.

[0006] In some embodiments, the bias voltage ranges from 100V to 800V.

[0007] In some embodiments, applying a bias voltage to the stent includes applying a bias voltage of different magnitudes to the stent during at least a first time period and a second time period.

[0008] In some embodiments, a bias voltage of 100V to 400V is applied to the bracket during the first time period, and the duration of the first time period is 10min to 60min; a bias voltage of 400V to 800V is applied to the bracket during the second time period, and the duration of the second time period is 5min to 30min.

[0009] In some embodiments, the second time period is located after the first time period.

[0010] In some embodiments, during the deposition process of the coating, the power of the second plasma discharge is 50W to 500W, and the deposition time is 8min to 90min.

[0011] In some embodiments, during the pretreatment, the power of the first plasma discharge is 100W to 600W, and the duration of the first plasma discharge is 5min to 30min.

[0012] In some embodiments, the first plasma discharge and / or the second plasma discharge is an ICP discharge.

[0013] In some embodiments, the first plasma discharge and / or the second plasma discharge are continuous discharges.

[0014] In some embodiments, introducing the organosilicon monomer into the plasma reaction chamber includes: introducing the organosilicon monomer and a reaction gas into the plasma reaction chamber, wherein the reaction gas includes one or more of oxygen, argon, helium and hydrogen, the flow rate of the organosilicon monomer is 10 μL / min to 500 μL / min, and the flow rate of the reaction gas is 50 sccm to 500 sccm.

[0015] In some embodiments, the thickness of the coating is 400 nm to 500 nm.

[0016] In some embodiments, the organosilicon monomer comprises at least one structure shown in formula (1) or (2).

[0017] In equation (1), R1, R2, and R3 are independently selected from hydrogen atoms, C1-C atoms, and C2-C3 atoms, respectively. 12 Substituted or unsubstituted alkyl groups, C1-C 12 Substituted or unsubstituted alkoxy groups, or C1-C 12 The substituted or unsubstituted alkylsiloxy group, wherein at least one of R1, R2 and R3 is not a hydrogen atom, and R4 is C1-C2. 12 Substituted or unsubstituted alkyl groups, or C1-C 12 The substituted or unsubstituted alkylsilyl group, where X is selected from oxygen atom, nitrogen atom or linking bond, and n is an integer from 1 to 100; or in (2), R5 and R6 are independently selected from hydrogen atom, C1-C1 bond, C2-C2 ... 12 Substituted or unsubstituted alkyl groups, C1-C 12 Substituted or unsubstituted alkoxy groups, or C1-C 12 The substituted or unsubstituted alkylsiloxy group, wherein at least one of R5 or R6 is not a hydrogen atom, Y is selected from oxygen or nitrogen atoms, and m is an integer from 3 to 10.

[0018] In some embodiments, R1, R2, and R3 are each independently selected from methyl, ethyl, trimethylsiloxy, triethylsiloxy, or hydrogen atoms; R4 is methyl, ethyl, trimethylsilyl, or triethylsilyl; X is selected from oxygen or nitrogen atoms; and n is an integer from 1 to 20. R5 and R6 are each independently selected from hydrogen atoms, methyl, or ethyl atoms; and m is an integer from 3 to 6.

[0019] In some embodiments, R5 and R6 are selected from methyl groups, Y is selected from oxygen atoms, and m is an integer from 3 to 5.

[0020] In some embodiments, the organosilicon monomer includes one or more of hexamethyldisilazane, hexamethyldisiloxane, polymethylhydrosiloxane, hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, and decamethylcyclopentasiloxane.

[0021] In some embodiments, the substrate includes a light-emitting device.

[0022] In some embodiments, the light-emitting device includes an LED substrate, which includes an LED lamp, an LED display screen, or an LED bracket.

[0023] This disclosure also provides a coating, which is a plasma-polymerized silicone coating with a thickness of 400 nm to 2000 nm. After the coating is exposed to 1.3 mg / mL sulfur powder and 85°C for 8 hours, the reduction in luminous flux of the coating is less than 3%.

[0024] In some embodiments, after the coating is exposed to 1.3 mg / mL sulfur powder and 85°C for 8 hours, the reduction in luminous flux of the coating is less than 2.5%.

[0025] In some embodiments, the thickness of the coating is 400 nm to 500 nm.

[0026] In some embodiments, the coating is prepared by any of the coating preparation methods described above.

[0027] This disclosure also provides a device in which at least a portion of the surface is formed with any of the coatings described above.

[0028] Compared with the prior art, the technical solutions of the embodiments of this disclosure have the following beneficial effects:

[0029] The coating preparation method of this embodiment involves introducing an activation gas, activating a first plasma discharge, not applying a bias voltage to the support on which the substrate is placed, and pretreating the substrate; introducing an organosilicon monomer into the plasma reaction chamber, activating a second plasma discharge, and applying a bias voltage to the support on which the substrate is placed, thereby depositing a coating with a thickness of 400 nm to 2000 nm on at least a portion of the surface of the substrate. The coating has excellent light transmittance, anti-sulfurization properties, and environmental aging resistance.

[0030] The coating of this embodiment is a plasma-polymerized silicone coating with a thickness of 400 nm to 2000 nm. After being exposed to 1.3 mg / mL sulfur powder and 85°C for 8 hours, the coating shows a reduction in light flux of less than 3%, indicating excellent anti-sulfurization performance. Detailed Implementation

[0031] The inventors have discovered that by preparing a plasma-polymerized coating of organosilicon through PECVD, the substrate is first pretreated by introducing an activation gas and starting plasma discharge without applying a bias voltage; then, organosilicon monomers are introduced, plasma discharge is started, and a bias voltage is applied to the support on which the substrate is placed to obtain the coating. This coating has excellent light transmittance, anti-sulfurization properties, and environmental aging resistance.

[0032] This disclosure provides a method for preparing a coating, the method comprising: placing a substrate in a support within a plasma reaction chamber; introducing an activation gas, activating a first plasma discharge, and pretreating the substrate; introducing an organosilicon monomer into the plasma reaction chamber, activating a second plasma discharge, and applying a bias voltage to the support, thereby depositing a coating with a thickness of 400 nm to 2000 nm on at least a portion of the surface of the substrate.

[0033] The preparation method of this disclosure avoids insufficient protection due to an excessively thin coating, and avoids problems such as coating cracking due to stress and other factors due to an excessively thick coating. The thickness of the coating is 400nm to 2000nm. In some specific embodiments, the coating thickness is 400nm to 1500nm; in some specific embodiments, the coating thickness is 400nm to 1000nm; in some specific embodiments, the coating thickness is 400nm to 500nm, specifically, for example, 400nm, 410nm, 415nm, 425nm, 431nm, 450nm, 460nm, 470nm, 480nm, 490nm, or 500nm, etc.; in some specific embodiments, the coating thickness is 400nm to 450nm; in some specific embodiments, the coating thickness is 410nm to 440nm.

[0034] In the preparation method of the specific embodiments of this disclosure, in order to avoid damage to the substrate due to excessive bias voltage during the deposition of the coating, in some specific embodiments, the bias voltage applied to the support is 100V to 800V, specifically, it can be 200V, 250V, 300V, 350V, 400V, 450V, 500V, 550V, 600V, 650V, 700V, 750V or 800V, etc.

[0035] In some specific embodiments, an organosilicon monomer is introduced into the plasma reaction chamber, a second plasma discharge is initiated, and a bias voltage is applied to the support. The specific method of applying the bias voltage is as follows: different bias voltages are applied to the support during at least a first time period and a second time period. Since the power of the second plasma discharge remains constant during the coating deposition process, films with different microstructures are deposited under different bias voltages, thereby depositing at least two stacked films on at least a portion of the substrate surface. The void structure and density of the different films are different, and the voids in one film layer are misaligned with the voids in the adjacent film layers, making it more difficult for gas molecules or liquid molecules to penetrate the film layer, thus giving the coating a better overall protective performance.

[0036] In some specific embodiments, applying a bias voltage to the stent further includes: applying a bias voltage of 100V to 400V to the stent during a first time period, the duration of which is 10min to 60min; and applying a bias voltage of 400V to 800V to the stent during a second time period, the duration of which is 5min to 30min.

[0037] In some specific implementations, the first time period and the second time period are adjacent.

[0038] In some specific embodiments, the second time period immediately follows the first time period. In the first time period, a relatively small bias voltage is applied first. Under the small bias voltage, the ratio of carbon atoms to silicon atoms in the film layer is relatively high, the internal stress of the film layer is small, and it is not easy for cracks to occur, which would lead to the destruction of the film layer structure. In the second time period, a relatively large bias voltage is applied, which can increase the deposition rate of the coating. The ratio of carbon atoms to silicon atoms in the film layer is relatively low, and the film layer has good anti-sulfurization performance. Finally, a coating consisting of two film layers is formed. The film layer formed in the first time period has low internal stress and can transition and buffer the internal stress of the film layer formed in the second time period, making the overall structure of the coating more stable.

[0039] In some specific embodiments, applying a bias voltage to the stent includes applying a bias voltage of different magnitudes to the stent in three or more time periods. The bias voltage applied in each time period is different from the bias voltage applied in the adjacent time periods, thereby causing the voids in the adjacent membrane layers to be misaligned, improving the overall anti-permeation effect of the coating. In some specific embodiments, the stent is first biased in a first time period, then biased in a second time period, and finally biased in a third time period. The bias voltage applied in the second time period is different from the bias voltage applied in the first and third time periods, and the bias voltage applied in the first and third time periods can be the same or different.

[0040] In some specific embodiments of the preparation method disclosed herein, the support is a rotatable rotating frame. During the deposition of the coating, the support can rotate, which is beneficial to improving the uniformity of the coating deposited on the substrate. In some specific embodiments, the support is adapted to rotate around its center. Furthermore, the support can be a planetary rotating frame, so that the substrate is displaced relative to the support while following the support to rotate around the center of the support, which is beneficial to improving the uniformity of the deposited coating.

[0041] In some specific embodiments of the preparation method disclosed herein, during the deposition of organosilicon monomers to form a coating, the discharge mode of the second plasma discharge is continuous discharge or pulsed discharge.

[0042] In some specific embodiments, during the process of introducing organosilicon monomers to deposit and form a coating, the second plasma discharge is an ICP (inductively coupled plasma) discharge.

[0043] In some specific embodiments, during the deposition of the organosilicon monomer to form the coating, the second plasma discharge method adopts continuous discharge, and the power of the second plasma discharge is 50W to 500W, specifically, for example, 50W, 80W, 100W, 120W, 140W, 160W, 180W, 200W, 220W, 240W, 260W, 280W, 300W, 320W, 340W, 360W, 380W, 400W, 420W, 440W, 460W, 480W, or 500W; the deposition time is 8min to 90min, specifically, for example, 8min, 10min, 15min, 20min, 25min, 28min, 30min, 35min, 40min, 45min, 50min, 55min, 60min, 65min, 70min, 75min, 80min, 85min, or 90min, etc.

[0044] The preparation method of this disclosure, in some specific embodiments, involves depositing an organosilicon monomer into a plasma reaction chamber to form a coating, including: evacuating the plasma reaction chamber to a pressure of 0.5 to 5 Pa, introducing the organosilicon monomer and the reaction gas into the plasma reaction chamber, activating the second plasma discharge, and applying a bias voltage to the support.

[0045] In some specific embodiments, the reactant gas includes one or more of oxygen, argon, helium, and hydrogen.

[0046] In some specific embodiments, the flow rate of the organosilicon monomer is 10 μL / min to 500 μL / min, and the flow rate of the reaction gas is 50 sccm to 500 sccm.

[0047] In some specific embodiments of the preparation method disclosed herein, when pretreating the substrate, the pressure in the plasma reaction chamber is evacuated to 0.5-5 Pa, and an activation gas is introduced at a flow rate of 20-200 sccm to initiate the first plasma discharge, thereby activating the substrate by bombarding it with plasma. This is beneficial for improving the adhesion between the subsequently formed coating and the substrate.

[0048] In some specific embodiments, the activating gas includes one or a mixture of several of He, Ar, and O2.

[0049] The preparation method of this disclosure, in the pretreatment stage, can use continuous discharge or pulsed discharge. In some specific embodiments, in the pretreatment stage, the first plasma discharge is a continuous discharge with a discharge power of 100-600W, specifically, for example, 100W, 120W, 140W, 160W, 180W, 190W, 200W, 210W, 220W, 230W, 240W, 250W, 260W, 270W, 280W, 290W, 300W, 400W, 500W, or 600W, etc.; the discharge duration is 5min-30min, specifically, for example, 5min, 10min, 15min, 20min, 25min, or 30min, etc.

[0050] In some specific implementations, during the pretreatment stage, the first plasma discharge is an ICP discharge.

[0051] It should be noted that the first plasma discharge and the second plasma discharge can be provided by the same or different power sources, such as the same ICP source. In some specific embodiments, the power of the first plasma discharge and the power of the second plasma discharge can be the same or different.

[0052] The preparation method of this disclosure, in some specific embodiments, further includes post-processing, which includes: depositing a coating on at least a portion of the surface of the substrate, then introducing clean compressed air or an inert gas until the plasma reaction chamber returns to atmospheric pressure, opening the plasma reaction chamber, and removing the substrate. In some specific embodiments, an inert gas is introduced, and the flow rate of the inert gas is 5–300 sccm.

[0053] In some specific embodiments of the preparation method disclosed herein, the organosilicon monomer includes at least one structure shown in formula (1) or (2).

[0054] In equation (1), R1, R2, and R3 are independently selected from hydrogen atoms, C1-C atoms, and C2-C3 atoms, respectively. 12 Substituted or unsubstituted alkyl groups, C1-C 12 Substituted or unsubstituted alkoxy groups, or C1-C 12 The substituted or unsubstituted alkylsiloxy group, where at least one of R1, R2, and R3 is not a hydrogen atom, and R4 is C1-C2. 12 Substituted or unsubstituted alkyl groups, or C1-C 12 The substituted or unsubstituted alkylsilyl group, where X is selected from oxygen atom, nitrogen atom or linking bond, and n is an integer from 1 to 100;

[0055] In (2), R5 and R6 are independently selected from hydrogen atoms and C1-C atoms, respectively. 12Substituted or unsubstituted alkyl groups, C1-C 12 Substituted or unsubstituted alkoxy groups, or C1-C 12 The substituted or unsubstituted alkylsiloxy group, at least one of R5 or R6 is not a hydrogen atom, Y is selected from oxygen or nitrogen atoms, and m is an integer from 3 to 10.

[0056] In some specific embodiments, in formula (1), R1, R2 and R3 are independently selected from hydrogen atoms, substituted or unsubstituted alkyl groups of C1-C6, substituted or unsubstituted alkoxy groups of C1-C6, or substituted or unsubstituted alkylsiloxy groups of C1-C6; R4 is a substituted or unsubstituted alkyl group of C1-C6, or a substituted or unsubstituted alkylsilyl group of C1-C6; furthermore, R1, R2 and R3 are independently selected from hydrogen atoms, C1-C6 alkyl groups, C1-C6 alkoxy groups, or C1-C6 alkylsiloxy groups; R4 is a C1-C6 alkyl group or a C1-C6 alkylsilyl group.

[0057] In some specific embodiments, in formula (1), R1, R2 and R3 are independently selected from methyl, ethyl, trimethylsiloxy, triethylsiloxy or hydrogen atoms, R4 is methyl, ethyl, trimethylsilyl or triethylsilyl, X is selected from oxygen atom or nitrogen atom, and n is an integer from 1 to 20.

[0058] In some specific embodiments, in formula (2), R5 and R6 are independently selected from hydrogen atoms, substituted or unsubstituted alkyl groups of C1-C6, substituted or unsubstituted alkoxy groups of C1-C6, or substituted or unsubstituted alkylsiloxy groups of C1-C6; further, R5 and R6 are independently selected from hydrogen atoms, C1-C4 alkyl groups, C1-C4 alkoxy groups, or C1-C4 alkylsiloxy groups.

[0059] In some specific embodiments, in formula (2), R5 and R6 are independently selected from hydrogen atoms, methyl or ethyl atoms, and m is an integer from 3 to 6; in some specific embodiments, R5 and R6 are selected from methyl atoms, Y is selected from oxygen atoms, and m is an integer from 3 to 5.

[0060] In some specific embodiments, the organosilicon monomer includes one or more of the following: hexamethyldisilazane, hexamethyldisiloxane, polymethylhydrosiloxane, hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, and decamethylcyclopentasiloxane.

[0061] In some specific embodiments, the organosilicon monomer includes one or more of hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, and decamethylcyclopentasiloxane.

[0062] The preparation method of this disclosure includes, in some specific embodiments, a light-emitting device as the substrate. In some specific embodiments, the light-emitting device includes an LED substrate, which comprises LED lights, LED displays, or LED brackets, etc., representing both light-emitting and non-light-emitting parts of the LED. The LED lights can be plate-shaped, such as an LED light board, or spherical, such as LED beads, or other shapes. In some specific embodiments, the light-emitting device can also be an OLED device, a micro LED device, etc.

[0063] The coating prepared by the method of this disclosure, after being exposed to 1.3 mg / mL sulfur powder and 85°C for 8 hours, shows no discoloration, cracking, or detachment from the substrate. The reduction in luminous flux of the coating is less than 3%, and in some specific embodiments, the reduction is less than 2.5%; further, less than 2%; further, less than 1.5%; further, less than 1%. The prepared coating has excellent anti-sulfurization performance and provides good protection for the substrate in a sulfur gas environment. Especially for light-emitting device substrates, the coating does not affect the luminous flux of the substrate itself after formation, and the reduction in luminous flux in a sulfur environment is low.

[0064] This disclosure also provides a coating, which is a plasma-polymerized silicone coating with a thickness of 400 nm to 2000 nm. After the coating is exposed to 1.3 mg / mL sulfur powder and 85°C for 8 hours, the reduction in luminous flux of the coating is less than 3%.

[0065] In some specific embodiments, after the coating is exposed to 1.3 mg / mL sulfur powder and 85°C for 8 hours, the reduction in luminous flux of the coating is less than 2.5%; further, less than 2%; further, less than 1.5%; further, less than 1%.

[0066] In some specific embodiments, the coating thickness is 400 nm to 500 nm.

[0067] In some specific embodiments, the coating is prepared by the preparation method of any of the above specific embodiments.

[0068] In some embodiments of the coating disclosed herein, the coating comprises at least two film layers, each film layer being formed sequentially under different bias voltages applied to the support; in some embodiments, the coating composed of at least two film layers, after being exposed to an environment of 1.3 mg / mL sulfur powder and 85°C for 8 hours, exhibits no discoloration, cracking, or substrate detachment, and the reduction in luminous flux of the coating is less than 1%.

[0069] The coating of this disclosure exhibits the following characteristics: In some embodiments, after being placed in an environment of 85°C and 85% RH for 1000 hours, the coating surface shows no defects; in other embodiments, the light-emitting device with the coating formed on its surface emits light after being placed in an environment of 85°C and 85% RH for 1000 hours, without problems such as missing colors or dead lights (unable to light up). The surface coating demonstrates excellent resistance to environmental aging.

[0070] This disclosure also provides a device in which at least a portion of the surface of the device is formed with a coating of any of the above embodiments.

[0071] In some specific embodiments, the device is a light-emitting device, such as an LED device. The coating formed on at least part of the surface of the light-emitting device has excellent light transmittance. After the coating is formed, it does not affect the light flux of the device itself. Moreover, the coating has excellent anti-sulfurization performance and environmental aging resistance. It provides good protection for the device in sulfur gas environment and high temperature and high humidity environment. The reduction value of light flux in sulfur environment is low and does not affect the light emission and use of the device.

[0072] The present disclosure will be further illustrated by specific embodiments below.

[0073] Example

[0074] Test Method Description

[0075] Thickness: Measured using a Filmetrics F20-UV thin film thickness meter (USA);

[0076] Anti-sulfurization test: (1) After 8 hours in an environment with sulfur powder of 1.3 mg / mL and a temperature of 85℃, observe whether the LED substrate has blackening, adhesive cracking, peeling and other phenomena; The specific process includes: take 0.26 g of sulfur powder and place it in a 25 mL beaker, put the 25 mL beaker into a 200 mL beaker, put the coated LED substrate into the 200 mL beaker, seal the 200 mL beaker, put the beaker into an oven at 85℃ for 8 hours, and observe whether the substrate has blackening, coating adhesive cracking, coating peeling and other phenomena; (2) Before and after (1), test the luminous flux of the LED substrate and calculate the reduction value of luminous flux after the anti-sulfurization test.

[0077] High temperature and high humidity test: The test was conducted using Zhenghang's ZH-CTH-225D constant temperature and humidity chamber. The test conditions were 85℃ and 85%RH. After 1000 hours, the LED substrate was lit up and the problem of dead LEDs or missing colors was observed. If there were no problems, the test result was recorded as qualified; otherwise, it was unqualified.

[0078] Example 1

[0079] (1) Substrate cleaning: Wipe the substrate LED light board with a lint-free cloth soaked in anhydrous ethanol to remove surface stains, and then put it in a drying cabinet for more than 1 hour to remove the moisture adsorbed by the substrate.

[0080] (2) Substrate activation: After the cleaned substrate is dried, it is loaded onto the rotating rack in the vacuum chamber. The vacuum chamber is evacuated to a vacuum level of less than 1 Pa. Oxygen is introduced at a flow rate of 200 sccm to maintain a vacuum level of 8 Pa. ICP plasma discharge is turned on with a discharge power of 600 W. The substrate is activated by plasma bombardment for 10 minutes.

[0081] (3) Coating preparation: Evacuate the vacuum chamber to a vacuum level below 1 Pa, introduce argon at a flow rate of 50 sccm, oxygen at a flow rate of 50 sccm, and octamethylcyclotetrasiloxane (D4) at a flow rate of 250 μL / min, turn on ICP plasma discharge with a discharge power of 400 W, turn on the bias power supply to apply a bias voltage of 450 V to the rotating frame, and the deposition time is 10 minutes;

[0082] (4) After the coating is completed, the coated substrate is taken out for thickness testing, anti-sulfurization testing, calculation of the reduction in luminous flux after the anti-sulfurization test, and high temperature and high humidity testing. The test results are recorded in Table 1.

[0083] Example 2

[0084] Compared to Example 1, the other processes remain the same, except that in step (3), the bias voltage applied to the rotating frame is set to 200V and the deposition time is 25 minutes.

[0085] Example 3

[0086] Compared to Example 1, the other processes remain the same, except that in step (3), a bias voltage of 200V is first applied to the rotating frame and the deposition time is 20 minutes; then the bias voltage applied to the rotating frame is changed to 450V and the deposition time is 8 minutes.

[0087] Example 4

[0088] Compared to Example 1, the other processes remain unchanged, except that in step (3), a bias voltage of 450V is first applied to the rotating frame, and the deposition time is 8 minutes; then the bias voltage applied to the rotating frame is changed to 200V, and the deposition time is 20 minutes.

[0089] Comparative Example 1

[0090] Thickness testing, sulfur resistance testing, calculation of luminous flux reduction after sulfur resistance testing, and high temperature and humidity testing were performed on the uncoated LED light panels. The test results are recorded in Table 1.

[0091] Comparative Example 2

[0092] Compared to Example 1, the other processes remain the same, except that in step (2), the bias power supply is turned on to apply a 400V bias to the rotating frame.

[0093] Comparative Example 3

[0094] Compared to Example 1, the other processes remain the same, except that in step (3), no bias is applied to the rotating frame, and the deposition time is 40 minutes.

[0095] Comparative Example 4

[0096] Compared to Example 1, the other processes remain unchanged, except that the coating time in step 3) is set to 6 minutes.

[0097] Table 1 Test Results

[0098] According to the test results in Table 1, the coatings prepared in Examples 1-3 exhibit excellent light transmittance, anti-sulfurization performance, and environmental aging resistance without affecting the performance of the LED light panel itself. In Example 3, the coating consists of two film layers formed under different bias voltages at two different time periods, with a smaller bias voltage applied first and a larger bias voltage applied later. Compared to Examples 1-2 and Example 4, it has a better protective effect, and the reduction in luminous flux after the anti-sulfurization test is smaller. This may be because the carbon atom content in the first film layer is relatively high, resulting in lower internal stress. This lower stress can help transition and buffer the internal stress of the film layer formed in the later time period, making the overall coating structure more stable. Furthermore, the carbon atom content in the film layer formed in the later time period is relatively low, resulting in good anti-sulfurization performance.

[0099] As shown in Comparative Example 1, LED light panels without surface coating are easily sulfided, and after high temperature and high humidity testing, they exhibit dead LEDs and color loss.

[0100] Comparative Example 2 shows that the activation step applied a bias voltage to the rotating frame, which improved the ion bombardment capability. However, it also affected the coating or product, causing damage to the coating or product, significantly impacting the light flux, and resulting in poor anti-sulfurization effect and poor environmental aging resistance.

[0101] Comparative Example 3 shows that the lack of bias voltage applied to the rotating frame during coating resulted in poor anti-sulfurization performance and environmental aging resistance of the prepared coating.

[0102] Comparative Example 4 shows that the coating thickness formed by reducing the coating time is relatively thin, and the anti-sulfurization effect of the coating is poor.

[0103] The above description is merely an exemplary embodiment used to illustrate the principles of this disclosure and is not intended to limit the scope of protection of this disclosure. Various modifications and improvements can be made by those skilled in the art without departing from the spirit and substance of this disclosure, and these modifications and improvements are also within the scope of protection of this disclosure.

Claims

1. A method for the production of a coating, characterized in that include: A support for placing the substrate within the plasma reaction chamber; An activation gas is introduced, and the first plasma discharge is initiated to pretreat the substrate. The organosilicon monomer is introduced into the plasma reaction chamber, the second plasma discharge is activated, and a bias voltage is applied to the support to deposit a coating with a thickness of 400 nm to 2000 nm on at least a portion of the surface of the substrate.

2. The production method according to claim 1, characterized by, The bias voltage ranges from 100V to 800V.

3. The preparation method according to claim 1, characterized in that, The bias voltage applied to the bracket includes: Different bias voltages are applied to the support during at least two time periods, the first time period and the second time period.

4. The production method according to claim 3, characterized by, A bias voltage of 100V to 400V is applied to the bracket during the first time period, which lasts from 10 minutes to 60 minutes. During the second time period, a bias voltage of 400V to 800V is applied to the bracket, and the duration of the second time period is 5min to 30min.

5. The preparation method according to claim 4, characterized in that, The second time period is located after the first time period.

6. The method of claim 1, wherein, During the deposition process to form the coating, the power of the second plasma discharge is 50W to 500W, and the deposition time is 8min to 90min.

7. The preparation method according to claim 1, characterized in that, In the pretreatment, the power of the first plasma discharge is 100W to 600W, and the duration of the first plasma discharge is 5min to 30min.

8. The method of claim 1, wherein, The first plasma discharge and / or the second plasma discharge are ICP discharges.

9. The method of claim 1, wherein, The first plasma discharge and / or the second plasma discharge are continuous discharges.

10. The method of claim 1, wherein, The step of introducing the organosilicon monomer into the plasma reaction chamber includes: The organosilicon monomer and the reactant gas are introduced into the plasma reaction chamber. The reactant gas includes one or more of oxygen, argon, helium and hydrogen. The flow rate of the organosilicon monomer is 10 μL / min to 500 μL / min, and the flow rate of the reactant gas is 50 sccm to 500 sccm.

11. The production method according to any one of claims 1 to 10, characterized by, The thickness of the coating is 400nm to 500nm.

12. The production method according to any one of claims 1 to 10, characterized by, The organic silicon monomer includes at least one of the structures represented by the following formula (1) or (2), In equation (1), R1, R2, and R3 are independently selected from hydrogen atoms, C1-C atoms, and C2-C3 atoms, respectively. 12 Substituted or unsubstituted alkyl groups, C1-C 12 Substituted or unsubstituted alkoxy groups, or C1-C 12 The substituted or unsubstituted alkylsiloxy group, wherein at least one of R1, R2 and R3 is not a hydrogen atom, and R4 is C1-C2. 12 Substituted or unsubstituted alkyl groups, or C1-C 12 The substituted or unsubstituted alkylsilyl group, where X is selected from oxygen atom, nitrogen atom or linking bond, and n is an integer from 1 to 100; or (2) R5and R6are each independently selected from the group consisting of hydrogen atom, C1-C 12 substituted or unsubstituted alkyl group, C1-C 12 substituted or unsubstituted alkoxy group, or C1-C 12 substituted or unsubstituted alkylsiloxy group, at least one of R5or R6not being hydrogen atom, Y is selected from the group consisting of oxygen atom or nitrogen atom, and m is an integer of 3 to 10.

13. The method of claim 12, wherein, R1, R2, and R3 are each independently selected from methyl, ethyl, trimethylsiloxy, triethylsiloxy, or hydrogen atoms; R4 is methyl, ethyl, trimethylsilyl, or triethylsilyl; X is selected from oxygen or nitrogen atoms; and n is an integer from 1 to 20. R5 and R6 are each independently selected from hydrogen atoms, methyl or ethyl atoms, and m is an integer from 3 to 6.

14. The method of claim 13, wherein, R5 and R6 are selected from methyl groups, Y is selected from oxygen atoms, and m is an integer from 3 to 5.

15. The preparation method according to claim 12, characterized in that, The organosilicon monomers include one or more of the following: hexamethyldisilazane, hexamethyldisiloxane, polymethylhydrosiloxane, hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, and decamethylcyclopentasiloxane.

16. The production method according to any one of claims 1 to 10, characterized by, The substrate includes a light-emitting device.

17. The method of claim 16, wherein the method further comprises, The light-emitting device includes an LED substrate, which includes an LED lamp, an LED display screen, or an LED bracket.

18. A coating, characterized in that, The coating is a plasma polymerized coating of organosilicon, the thickness of the coating is between 400 nm and 2000 nm, the decrease in luminous flux of the coating is below 3% after 8 hours in an environment of 1.3 mg / mL of sulfur powder and a temperature of 85°C.

19. The coating of claim 18, wherein, The coating is a plasma polymerized coating of organosilicon, the thickness of the coating is between 400 nm and 2000 nm, the decrease in luminous flux of the coating is below 2.5% after 8 hours in an environment of 1.3 mg / mL of sulfur powder and a temperature of 85°C.

20. The coating of claim 18, wherein, The thickness of the coating is between 400 nm and 500 nm.

21. The coating of claim 18, wherein, The coating is obtained by the production method according to any one of claims 1 to 17.

22. A device, comprising: At least part of the surface of the device is formed with a coating according to any one of claims 18 to 21.

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