WO2014126388A1 - Polycarbonate bloquant des rayons ultraviolets et présentant une dureté et une résistance à l'usure améliorées - Google Patents

Polycarbonate bloquant des rayons ultraviolets et présentant une dureté et une résistance à l'usure améliorées Download PDF

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WO2014126388A1
WO2014126388A1 PCT/KR2014/001161 KR2014001161W WO2014126388A1 WO 2014126388 A1 WO2014126388 A1 WO 2014126388A1 KR 2014001161 W KR2014001161 W KR 2014001161W WO 2014126388 A1 WO2014126388 A1 WO 2014126388A1
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silicon
aluminum
nitride film
polycarbonate
sputtering
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PCT/KR2014/001161
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English (en)
Korean (ko)
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김영우
김대철
유석재
한승희
문선우
김성민
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한국기초과학지원연구원
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Priority claimed from KR1020130014911A external-priority patent/KR20140102345A/ko
Priority claimed from KR20130109509A external-priority patent/KR20150030366A/ko
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Publication of WO2014126388A1 publication Critical patent/WO2014126388A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides

Definitions

  • the present invention relates to an aluminum-silicon-nitride deposition method and apparatus for improving the surface hardness and wear resistance of polycarbonate materials, and more particularly, aluminum and silicon sputtering in a magnetron sputtering deposition source that is used as a deposition source for thin film deposition Replacing the vehicle glass by mounting a target and simultaneously injecting argon, which is an inert gas, and nitrogen gas, which is a reactive gas, into the vacuum chamber and depositing an aluminum-silicon-nitride film, which is a high hardness transparent film, on the surface of the polycarbonate by reactive sputtering
  • the present invention relates to an aluminum-silicon nitride film deposition method and apparatus for improving the surface hardness and wear resistance of a polycarbonate material.
  • Polycarbonate has a high impact resistance and light weight can be used as a replacement for automotive glass, but low hardness, low wear resistance, deterioration and discoloration due to ultraviolet rays are a problem. Therefore, in order to improve hardness and wear resistance, deterioration due to ultraviolet rays and discoloration, it is necessary to form a transparent hard coating layer on the surface thereof.
  • a technique of forming a coating layer by attaching an adhesive sheet to the surface of the polycarbonate a technique of forming a coating layer made of an organic material on the surface of the polycarbonate using a coating method such as dip coating is widely used. .
  • the coating layer manufactured by the organic coating method has a limitation in improving hardness, wear resistance, and the like, a technique of forming an inorganic coating layer by deposition methods such as PVD and PECVD has recently been studied.
  • Patent Document 1 US Patent, 2007026235, Glazing system for behicle tops and windows
  • This technology is used to form a film for UV protection after the coating of other materials through a wet process, and then to deposit a wear resistant hard coating film by forming a silicon oxide film or aluminum oxide film of ⁇ 5 ⁇ m thickness on the surface by PECVD method have.
  • Patent Document 2 US Pat. No. 2008083186, Polycarbonate glazing system and method for making the same
  • this coating method is difficult to secure economic feasibility because many processes are required for the multilayer structure.
  • Non-Patent Document 1 Thin Solid Films 502 (2006) 270-274, Hard coatings by plasma CVD on polycarbonate for automotive and optical applications).
  • Patent Document 0001 Republic of Korea Patent Publication No. 10-0337483 (2002.05.08)
  • the present invention is designed to complement the low hardness and weak wear resistance of the polycarbonate material, polycarbonate material by depositing a multi-functional, high hardness transparent three-dimensional thin film of aluminum-silicon nitride film on the surface of the polycarbonate material SUMMARY OF THE INVENTION
  • An object of the present invention is to provide an aluminum-silicon-nitride film deposition method and apparatus for improving the surface hardness and wear resistance of a polycarbonate material which can increase the surface hardness and improve the wear resistance.
  • Aluminum-silicon-nitride film deposition method for improving the surface hardness and wear resistance of the polycarbonate material according to the present invention for achieving the above object (a) a conductive sample mount located inside the vacuum chamber for thin film deposition using magnetron sputtering Mounting a silicon wafer or polycarbonate substrate as a sample on the sample; (b) evacuating the vacuum in the vacuum chamber to a high vacuum region with a high vacuum turbopump and a low vacuum pump to assist the turbopump, and (c) magnetron deposition.
  • argon (Ar) which is an inert gas
  • nitrogen (N2) which is a reactive gas
  • RF power is applied to the RF antenna inside the vacuum chamber to form a plasma of the gas introduced in step (c), and (e) after the plasma formation, to a magnetron sputtering deposition source equipped with an aluminum metal target and a silicon target.
  • a pulsed DC power by a direct current or pulsed DC power supply to generate a plasma for thin film deposition.
  • Aluminum-silicon-nitride film deposition apparatus for improving the surface hardness and wear resistance of the polycarbonate material according to the present invention for achieving the above object is a vacuum chamber for thin film deposition using magnetron sputtering, aluminum mounted on the deposition source of magnetron sputtering Pulsed DC power supply for applying DC or pulsed DC power to the target and silicon sputtering target, plasma generated by the sputtering target mounted on the deposition source, RF antenna for entering gas into the vacuum chamber, and inside the vacuum chamber Conductive sample mount for mounting the sample deposited in the, RF power supply for supplying power to the RF antenna, high-vacuum turbopump for maintaining the high vacuum inside the vacuum chamber, vacuum gauge for measuring the degree of vacuum inside the vacuum chamber, And oils of argon (Ar) and nitrogen (N 2) gases used for plasma generation It characterized in that it comprises a gas flow rate adjusting unit for adjusting the amount.
  • Pulsed DC power supply for applying DC or pulsed DC power to the target and silicon s
  • the present inventors have recognized the above problems, and through the present invention, to provide a multi-functional thin film deposition technology for implementing a high hardness, wear resistance, UV protection properties with a double thin film.
  • the present invention is to deposit a hydrogenated silicon nitride film for blocking UV rays on the surface of the polycarbonate, for the purpose of compensating the polycarbonate material is low in hardness, high wear, deterioration and discoloration by ultraviolet light,
  • the present invention relates to a thin film deposition method and apparatus for depositing a high hardness transparent aluminum-silicon-nitride film to increase hardness and reduce wear.
  • the present invention the hydrogenated silicon nitride (SiN: H) deposited on one side or both sides in order to improve the high hardness, wear resistance and UV protection characteristics; And an aluminum-silicon nitride film deposited on the hydrogenated silicon nitride film.
  • the hydrogenated silicon nitride film improves UV blocking properties, and the aluminum-silicon nitride film improves hardness and wear resistance.
  • the hydrogenated silicon nitride film is formed by a reactive sputtering method by introducing an inert gas, nitrogen, and hydrogen in a plasma reactive magnetron sputtering thin film deposition apparatus including a silicon sputtering target.
  • the aluminum silicon nitride film is formed by a reactive sputtering method by introducing an inert gas and nitrogen in a plasma reactive magnetron sputtering thin film deposition apparatus including a silicon sputtering target and an aluminum sputtering target.
  • the pressure inside the deposition apparatus is characterized in that 0.5 mTorr to 20 mTorr.
  • the inert gas is characterized in that the argon.
  • the present invention provides a method of depositing nitride on a polycarbonate surface to improve high hardness, abrasion resistance and sun protection properties.
  • the method includes the steps of: mounting a polycarbonate substrate having a polycarbonate substrate or a silicon oxide film formed on a plasma reactive magnetron sputtering thin film deposition apparatus; Depositing a silicon hydride nitride film on the polycarbonate substrate by sputtering from a silicon sputtering target; And depositing an aluminum silicon nitride film on the hydrogenated silicon nitride film from the silicon sputtering target and the aluminum sputtering target.
  • the hydrogenated silicon nitride film improves UV blocking properties, and the aluminum-silicon nitride film improves hardness and wear resistance.
  • the hydrogenated silicon nitride film deposition is characterized by a reactive sputtering method by introducing an inert gas, nitrogen and hydrogen into the deposition apparatus.
  • the aluminum silicon nitride film deposition is characterized by the reactive sputtering method by introducing an inert gas and nitrogen in the plasma reactive magnetron sputtering thin film deposition apparatus including a silicon sputtering target and an aluminum sputtering target.
  • the pressure inside the deposition apparatus is characterized in that 0.5 mTorr to 20 mTorr.
  • the inert gas is characterized in that the argon.
  • Aluminum-silicon nitride film deposition method and apparatus for improving the surface hardness and wear resistance of the polycarbonate material according to the present invention is a multi-functional high hardness transparent aluminum-silicon-nitride film deposited by a reactive magnetron sputter deposition method on the surface of the polycarbonate material Thereby, there exists an effect which improves surface hardness and abrasion resistance.
  • the aluminum-silicon-nitride film deposition method for improving the surface hardness and wear resistance of the polycarbonate material according to the present invention and the polycarbonate material by the apparatus can be used as a windshield of a vehicle, and also has a light skylight, It can be used in various fields such as skylights for buildings, living rooms, factories, safety glass, roofs and windows of public facilities, bulletproof and soundproof walls, public telephone boxes, indoor partitions, indoor and outdoor sign boards.
  • polycarbonate by depositing a hydrogenated silicon nitride film on the surface of the polycarbonate substrate can be obtained the effect of improving the UV protection properties, and by depositing a high hardness transparent aluminum-silicon-nitride film thereon to improve the hardness and wear resistance You can get the effect.
  • polycarbonate as a vehicle's windshield, and also includes light skylights, skylights for buildings and living rooms, factories, safety glass, roofs and windows of public facilities, soundproof walls, public telephone boxes, and interior partitions. It can be used in various fields such as indoor and outdoor sign boards.
  • FIG. 1 is a block diagram of an aluminum-silicon-nitride film deposition apparatus for improving the surface hardness and wear resistance of the polycarbonate material according to the present invention
  • Figure 2 is an aluminum nitride film, a seal deposited on the silicon wafer of Example 1 of the present invention
  • Figure 3 (a) is also a wear test result of the sample of the aluminum-silicon nitride film deposited on the polycarbonate substrate material of Example 2 of the present invention
  • FIG. 5 is a flowchart illustrating a method of depositing an aluminum-silicon nitride film for improving surface hardness and wear resistance of a polycarbonate material according to the present invention.
  • FIG. 6 illustrates a plasma reactive magnetron sputtering thin film deposition apparatus for the deposition of the aluminum-silicon-nitride film and the hydrogenated silicon nitride film of the present invention.
  • Example 7 is a hardness measurement result of the sample deposited with a hydrogenated silicon nitride film on the silicon wafer of Example 4 of the present invention, the hardness measurement results of the sample deposited with an aluminum-silicon nitride film on the silicon wafer of Example 5 and Example 6
  • the hydrogenated silicon nitride film is deposited on the silicon wafer of, and the hardness measurement results of the sample on which the aluminum-silicon-nitride film is deposited are shown.
  • Example 8 is a light transmittance measurement result of a sample deposited with a hydrogenated silicon nitride film on the Eagle 2000 glass substrate of Example 4 of the present invention, the light transmittance of a sample deposited aluminum-silicon-nitride film on the Eagle 2000 glass substrate of Example 5
  • the measurement results and the light transmittance measurement results of the sample deposited with the hydrogenated silicon nitride film and the aluminum-silicon nitride film deposited on the Eagle 2000 glass substrate of Example 6 are shown.
  • Figure 9a is a result of measuring the light transmittance before and after the taber abrasion test of the polycarbonate substrate
  • Figure 9b is before and after the taber wear test of the sample deposited with a hydrogenated silicon nitride film on the polycarbonate substrate and deposited on the silicon-silicon nitride film It is the result of the light transmittance measurement later.
  • Aluminum-silicon-nitride deposition apparatus for improving the surface hardness and wear resistance of the polycarbonate material according to the present invention is a vacuum chamber (1), pulsed DC power supply (2), sputtering target (3), plasma (4), RF antenna (5), sample (6), sample mounting table (7), matching box (8), RF power supply (9), gas used (10), gas flow rate control unit (11), vacuum gauge (12) Common turbo pump 13 and low vacuum pump 14 are included.
  • the vacuum chamber (1) is a vacuum chamber for thin film deposition using magnetron sputtering
  • the pulsed DC power supply (2) is a direct current or to the aluminum and silicon sputtering target (3) mounted on the magnetron sputtering deposition source It is a power supply device for applying pulsed DC power.
  • the plasma 4 represents a plasma generated by the sputtering target 3 mounted on the magnetron deposition source, and the RF antenna 5 is a radio frequency (RF) for plasmalizing the gas introduced into the vacuum chamber. ) Antenna.
  • RF radio frequency
  • the sample 6 represents a sample mounted on the conductive sample holder 7, and the matching box 8 is an RF power matching system generated by the RF power supply 9.
  • the gas flow rate adjusting unit 12 is a gas flow rate adjusting device for controlling the flow rate of the use gas 10 used for plasma generation.
  • the vacuum gauge 12 is a vacuum gauge for measuring the degree of vacuum
  • the high vacuum turbo pump 13 is a pump for maintaining a high vacuum of the vacuum chamber 1
  • the low vacuum pump 14 is a high vacuum pump It is a pump to help the operation.
  • a method of plasma magnetron aluminum-silicon-nitride film deposition by an aluminum-silicon-nitride film deposition apparatus for improving surface hardness and wear resistance of a polycarbonate material including the above-described configuration will be described with reference to FIG. 5.
  • FIG. 5 is a flowchart of a method of plasma magnetron aluminum-silicon-nitride film deposition according to the present invention.
  • argon (Ar) which is an inert gas
  • nitrogen (N2) which is a reactive gas
  • the pressure inside the vacuum chamber 1 it is preferable to adjust the pressure inside the vacuum chamber 1 to a pressure of 0.5 mTorr to 30 mTorr.
  • the flow rate ratio of the argon and nitrogen gas is preferably drawn to be about 10: 1 ⁇ 1: 1.
  • the nitride film may be deposited untransparently, and in the case of 1: 1 or more, the nitride speed may be faster than the sputtering speed of the silicon and aluminum sputtering target 3 so that the deposition rate may be lowered.
  • step S30 when the pressure inside the vacuum chamber 1 is stabilized, RF power is applied to the RF antenna 5 inside the vacuum chamber 1 to form a plasma of the introduced gas. Perform (S40).
  • the power applied in step S40 is preferably a value of 0 to 300 W, more preferably 50 W of power.
  • the nitride film may not be formed well, and the film may be opaquely raised. If the RF power is too high, the temperature of the sample may increase, causing cracks in the deposited thin film. It can be weakened to form a transparent, crack-free film.
  • generating plasma for thin film deposition by applying pulsed direct current power by a direct current or pulsed direct current power supply device 2 to a magnetron sputtering deposition source equipped with an aluminum metal target and a silicon target. Perform (S50).
  • Direct current or pulsed direct current power can be deposited with a voltage of -200 to -1000 V and a current value of 0 to 1.6 A. In this manner, the composite target or the two targets are simultaneously sputtered (co-sputtering) to deposit the ternary nitride film.
  • the average power density of the direct current or pulsed direct current used in the thin film deposition process preferably has a value of 1 W / cm 2 to 20 W / cm 2 .
  • step S10 the silicon wafer is mounted on the sample holder 7 in the vacuum chamber according to the method of the present invention, and in step S20, after evacuating the inside of the vacuum chamber to 10 -6 Torr, In step S30, 24 sccm of argon gas and 6 sccm of nitrogen gas are introduced to adjust the pressure of the vacuum chamber to 10 mTorr, and in step S40, 200 W power is supplied to the RF antenna to form a plasma inside the vacuum chamber. It was made.
  • the magnetron sputtering deposition source equipped with the silicon target in step S50 is supplied with pulsed DC power of -550 V, 0.064 A, pulse width 30 ⁇ s, and pulse frequency 600 Hz, and the magnetron sputtering deposition equipped with an aluminum metal target.
  • a circle was applied with a pulse power of ⁇ 311 V, 1.40 A, and a 40% occupancy rate and deposited for 90 minutes to form a 2800 kW aluminum-silicon-nitride film.
  • the aluminum nitride film was applied to the silicon sputtering target and the silicon nitride film was deposited on the silicon wafer with the same thickness, respectively.
  • step S10 a polycarbonate substrate material on which a SiO 2 film having a thickness of ⁇ 5 ⁇ m is deposited is mounted on a sample mounting table in the vacuum chamber, and after evacuating the inside of the vacuum chamber to 10 ⁇ 6 Torr in step S20, In step S30, 24 sccm of argon (Ar) gas and 3 sccm of nitrogen (N 2 ) gas are simultaneously introduced to adjust the process pressure to 10 mTorr, and in step S40, 50 W RF power is applied to the RF antenna. Was supplied to form a plasma inside the vacuum chamber.
  • Ar argon
  • N 2 nitrogen
  • the pulsed direct current power of -450 V, 0.26 A, and 80% occupancy of the magnetron sputtering deposition source equipped with the silicon target in the 'S50' step is -452 V, 1.50 A of the magnetron sputtering deposition source equipped with the aluminum metal target.
  • a pulsed direct current power of 20% occupancy was applied to deposit an aluminum-silicon nitride film for 45 minutes.
  • a pin-on-disk wear test was performed using a ruby ball having a diameter of 3 mm at a load of 15 gf.
  • the rotational speed of the sample was 100 rpm. After 1000 revolutions, the worn surface was observed using an alpha-step profilometer and an optical microscope.
  • step 'S10' five 0.5 mm thick glass substrates (Eagle 2000) having a transparent shape in a vacuum chamber are placed in a line between the silicon target mounted on the left side and the aluminum target mounted on the right side, respectively.
  • step S20 After evacuating the inside of the vacuum chamber to 10 -6 Torr in the step S20, 24 sccm of argon gas and 5 sccm of nitrogen (N 2 ) gas are introduced to 10 mTorr in the step S30.
  • the RF power of 200 W was supplied to the RF antenna in step S40 to form a plasma inside the vacuum chamber.
  • the magnetron sputtering deposition source equipped with the silicon target is pulsed power of -780 V, 0.315 A, pulse width 100 ⁇ s, frequency 400 Hz, and the magnetron sputtering deposition source equipped with the aluminum metal target.
  • An aluminum-silicon-nitride film was deposited for 60 minutes by applying pulsed direct current power of -410 V, 1.10 A, 40% occupancy.
  • the thickness of the fabricated aluminum-silicon-nitride film was measured as (a) 4850 ⁇ , (b) 5450 ⁇ , (c) 5650 ⁇ , (d) 6100 ⁇ and (e) 6700 ⁇ . Were measured as (a) 55:45, (b) 58:42, (c) 67:33, (d) 74:26 and (e) 83:17.
  • the deposited aluminum-silicon-nitride film samples were measured for light transmittance using a UV-VIS measuring apparatus, and as shown in FIG. 4, all samples showed excellent visible light transmittance of 88 to 90%.
  • FIGS. 6 to 9B a plasma reactive magnetron sputtering thin film deposition apparatus for depositing an aluminum-silicon-nitride film and a hydrogenated silicon nitride film of the present invention will be described with reference to FIGS. 6 to 9B.
  • the plasma reactive magnetron sputtering thin film deposition apparatus 61 has a vacuum inside and a power source for applying direct current, pulse direct current, or RF power to the silicon sputtering target 64 and the silicon sputtering target 64 mounted therein.
  • Device 62 an aluminum sputtering target 65 mounted inside the vacuum, a power supply 63 for applying direct current, RF or pulsed direct current power to the aluminum sputtering target 65, and a gas drawn into the vacuum chamber.
  • RF (Radio Frequency) antenna 67 for plasma RF power supply 611 for supplying RF power to the antenna 67, matching system for impedance matching of the RF power supply 611 ),
  • a sample mount 69 configured to mount the polycarbonate sample 68, a plasma use gas storage 612, and a gas flow rate from the plasma use gas storage 612.
  • a low flow rate pump 616 which operates a flow rate adjusting device 613, a vacuum gauge 614 for measuring an internal vacuum degree, a high vacuum pump 615 for maintaining an internal high vacuum, and a pump of the high vacuum pump 615. It includes.
  • Gas is supplied from the plasma use gas storage unit 612 into the thin film deposition apparatus 61, and the plasma use gas is converted into plasma by an electromagnetic field induced by the antenna 67.
  • the plasmalized gas is sputtered by the silicon sputtering target 64 and the aluminum sputtering target 65 and deposited on the surface of the polycarbonate sample 68.
  • reference numeral 66 denotes a plasma generated by the sputtering targets 64 and 65.
  • the vacuum degree inside the deposition apparatus 61 is exhausted to a high vacuum region using the vacuum pump 615.
  • argon gas is introduced from the plasma use gas storage unit 612 containing argon (Ar) gas, which is an inert gas, to generate a plasma, through the gas flow control device 613, so that the pressure inside the deposition apparatus 61 is reduced. Is adjusted to a pressure of 0.5 mTorr to 20 mTorr. For this reason, plasma generation is difficult at low pressures below 0.5 mTorr, while at higher pressures above 20 mTorr, the plasma density increases during deposition, increasing the sputtering rate, but also increasing the degree of sputtered atoms being scattered by high pressure. This is because the deposition rate is reduced.
  • Ar argon
  • RF power is applied to the RF antenna 67 inside the vacuum chamber to form a plasma of the introduced gas.
  • the RF power used is from 0 to 300W, which is mainly 50W. If the RF power is not applied, the nitride film may not be formed well, the film may be opaquely raised, and if the RF power is too high, the temperature of the sample may be increased to cause cracks in the deposited thin film.
  • plasma for thin film deposition is generated.
  • pulsed DC power a voltage ratio of -300 to -600 V is applied to allow the deposition to be performed at a duty ratio of 20, 40, 60, or 80%.
  • nitrogen (N 2 ) gas and hydrogen (H 2 ) gas are introduced to deposit hydrogenated silicon nitride film.
  • Hydrogen gas is suitable to draw 6 ⁇ 9 sccm. In the case of 6 sccm or less, it is difficult to obtain the UV blocking property of the deposited film, and in the case of 9 sccm or more, an arc may occur in the silicon sputtering target 64.
  • Hydrogenated silicon nitride film is deposited on the surface of the polycarbonate sample 68 located on the sample holder 69 inside the vacuum chamber by the material sputtered from the deposition source and nitrogen and hydrogen gas introduced into the vacuum chamber.
  • the vacuum degree inside the deposition apparatus 61 is measured using the vacuum pump 615. Exhaust to high vacuum area.
  • an argon (Ar) gas 612 which is an inert gas, is introduced through the gas flow controller 613 to generate a plasma to adjust the pressure inside the vacuum chamber to a pressure of 0.5 mTorr to 20 mTorr.
  • RF power is applied to the RF antenna 67 inside the deposition apparatus to form a plasma of the introduced gas.
  • the RF power used is from 0 to 300W, which is mainly 50W.
  • nitrogen (N 2 ) gas is introduced for aluminum-silicon-nitride deposition.
  • Nitrogen gas is suitable to draw 3 to 6 sccm. Because less than 3 sccm, the nitride film may be deposited untransparent, and if more than 6 sccm, the nitriding speed is faster than the sputtering speed of the silicon and aluminum sputtering targets 64 and 65, so that the deposition rate may be significantly lower. to be.
  • Nitrogen gas introduced into the deposition apparatus and the material sputtered from the deposition source causes the aluminum-silicon-nitride film to be deposited on the uppermost layer of the polycarbonate sample 68 positioned on the sample mount 69 in the deposition apparatus.
  • the nitride film is deposited according to the above method and has an excellent effect.
  • the Eagle 2000 glass substrate and the silicon wafer were placed in the deposition apparatus according to the method specified in the present invention, and after exhausting the inside of the deposition apparatus to 10 -6 Torr, 8 sccm of argon (Ar) gas was introduced, and the opening ratio of the vacuum pump was adjusted. After adjusting the process pressure to 5 mTorr, 50 W power was supplied to the RF antenna to form a plasma inside the deposition apparatus.
  • Ar argon
  • the Eagle 2000 glass substrate and silicon wafer were placed in the deposition apparatus, the inside of the deposition apparatus was evacuated to 10 -6 Torr, and 8 sccm of argon (Ar) gas was introduced, and the process pressure was adjusted to 3 mTorr by adjusting the vacuum pump opening ratio. Then, 50 W of power was supplied to the RF antenna to form a plasma inside the deposition apparatus. Subsequently, 406 V, 0.26 A, 80% pulsed DC power was applied to the magnetron sputtering device equipped with silicon deposition source, and 331 V, 1.43 A, 60% pulse rate was applied to the magnetron sputtering device equipped with aluminum metal deposition source. A DC film was applied, 5 sccm of nitrogen (N 2 ) gas was introduced to form a nitride film, and an aluminum-silicon nitride film was deposited for 60 minutes to form a film of 4000 kV.
  • N 2 nitrogen
  • 31 GPa was shown as an average value of 6 Knoop hardness tests of 10 g load, and the light transmittance of 86% was confirmed in the visible light range of 400 nm to 700 nm.
  • the Eagle 2000 glass substrate and silicon wafer were placed in the deposition apparatus, the inside of the deposition apparatus was evacuated to 10 -6 Torr, and 8 sccm of argon (Ar) gas was introduced, and the process pressure was adjusted to 5 mTorr by adjusting the vacuum pump opening ratio. Then, 50 W of power was supplied to the RF antenna to form a plasma inside the deposition apparatus.
  • Ar argon
  • the process pressure was adjusted to 3 mTorr by adjusting the vacuum pump aperture ratio, and then a magnetron sputtering device equipped with a silicon deposition source had a 406 V, 0.26 A, 80% occupancy ratio.
  • Pulsed DC power was applied, and a magnetron sputtering device equipped with an aluminum metal deposition source was applied with pulsed DC power of 331 V, 1.43 A, and 60% of the occupancy rate.
  • Nitrogen (N 2 ) gas was introduced into 5 sccm to form a nitride film.
  • An aluminum-silicon-nitride film was deposited for 60 minutes to form a film of 4000 kPa.
  • 29 GPa was shown as an average value of Knob hardness test 6 times at 10 g load, and a light transmittance of 78% was observed in the visible light range of 400 nm to 700 nm, and 300 nm. At the ultraviolet wavelength, the light transmittance was measured at 3%. In this way, it was confirmed that a high hardness two-layer thin film having high visible light transmittance and UV blocking effect could be formed.
  • the process pressure was adjusted to 3 mTorr by adjusting the vacuum pump opening ratio, and a magnetron sputtering device equipped with a silicon deposition source had a pulsed direct current power of 406 V, 0.26 A, and 80% occupancy, and a magnetron equipped with an aluminum metal deposition source.
  • a pulsed direct current power of 331 V, 1.43 A, and 60% occupancy was applied to the sputtering apparatus, and 5 sccm of nitrogen (N 2 ) gas was introduced to form a nitride film.
  • N 2 nitrogen
  • the sample was loaded with 43 g of hydrogen nitride on top of polycarbonate and a two-layer film of aluminum-silicon-nitride. was rotated at a speed of 100 RPM around the lower axis of rotation to perform a Taber wear experiment to rotate 2000 times. The light transmittance was measured after the Taber wear test.
  • the light transmittance was 87% in the wavelength range of 400 nm to 700 nm before performing the Taber wear test, but after the Taber wear test was performed Scratch generation due to low hardness reduced the light transmittance to 42%.

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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

La présente invention concerne un appareil de dépôt de film de nitrure d'aluminium-silicium destiné à améliorer la dureté superficielle et la résistance à l'usure d'un matériau à base de polycarbonate, qui comprend un bain sous vide destiné à déposer un film mince à l'aide d'une pulvérisation par magnétron ; une alimentation en courant continu pulsé destinée à appliquer un courant continu ou un courant continu pulsé à des cibles de pulvérisation d'aluminium et de silicium montées sur une source de dépôt de pulvérisation par magnétron ; un plasma engendré par les cibles de pulvérisation montées sur la source de dépôt ; une antenne RF insérée à l'intérieur du bain sous vide de façon à plasmifier un gaz ; une plaque de montage d'échantillon conductrice destinée à monter un échantillon qui est déposé sur l'intérieur du bain sous vide ; une alimentation RF destinée à alimenter en courant l'antenne RF ; une turbopompe à vide secondaire destinée à maintenir un vide secondaire sur l'intérieur du bain sous vide ; un manomètre à vide destiné à mesurer le degré de vide sur l'intérieur du bain sous vide ; et une unité de régulation de débit de gaz destinée à réguler les débits de gaz argon (Ar) et azote (N2) utilisés afin d'engendrer le plasma ; ainsi, l'appareil a pour effet d'améliorer la dureté superficielle et la résistance à l'usure.
PCT/KR2014/001161 2013-02-12 2014-02-12 Polycarbonate bloquant des rayons ultraviolets et présentant une dureté et une résistance à l'usure améliorées WO2014126388A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR10-2013-0014911 2013-02-12
KR1020130014911A KR20140102345A (ko) 2013-02-12 2013-02-12 폴리카보네이트 소재의 표면 경도 및 내마모성 향상을 위한 알루미늄-실리콘-질화막 증착방법 및 그 장치
KR20130109509A KR20150030366A (ko) 2013-09-12 2013-09-12 폴리카보네이트의 내마모성 및 자외선에 대한 내후성 향상을 위한 코팅막 증착 방법 및 이 방법에 의한 코팅막이 증착된 폴리카보네이트
KR10-2013-0109509 2013-09-12

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WO2014126388A1 true WO2014126388A1 (fr) 2014-08-21

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022016283A1 (fr) * 2020-07-22 2022-01-27 National Research Council Of Canada Substrats revêtus et procédés pour la préparation de ceux-ci

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KR20020078618A (ko) * 2001-04-06 2002-10-19 이정중 다중 코일 방식의 유도 결합 플라즈마 마그네트론스퍼터링 시스템 및 그 방법
KR100977330B1 (ko) * 2007-03-29 2010-08-20 어플라이드 머티어리얼스, 인코포레이티드 태양 전지를 위한 반사방지층 또는 패시베이션층을 제조하기 위한 방법
WO2011007543A1 (fr) * 2009-07-17 2011-01-20 三井化学株式会社 Stratifié et procédé pour sa production
KR101117261B1 (ko) * 2010-09-03 2012-02-24 한국과학기술연구원 절연체 박막 내에 반도체 물질 양자점들을 형성하는 장치 및 방법

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Publication number Priority date Publication date Assignee Title
KR20020078618A (ko) * 2001-04-06 2002-10-19 이정중 다중 코일 방식의 유도 결합 플라즈마 마그네트론스퍼터링 시스템 및 그 방법
KR100977330B1 (ko) * 2007-03-29 2010-08-20 어플라이드 머티어리얼스, 인코포레이티드 태양 전지를 위한 반사방지층 또는 패시베이션층을 제조하기 위한 방법
WO2011007543A1 (fr) * 2009-07-17 2011-01-20 三井化学株式会社 Stratifié et procédé pour sa production
KR101117261B1 (ko) * 2010-09-03 2012-02-24 한국과학기술연구원 절연체 박막 내에 반도체 물질 양자점들을 형성하는 장치 및 방법

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022016283A1 (fr) * 2020-07-22 2022-01-27 National Research Council Of Canada Substrats revêtus et procédés pour la préparation de ceux-ci
EP4185732A4 (fr) * 2020-07-22 2024-07-31 Nat Res Council Canada Substrats revêtus et procédés pour la préparation de ceux-ci

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