CN111893435A - Light irradiation-resistant high-reflectivity film and preparation method thereof - Google Patents

Light irradiation-resistant high-reflectivity film and preparation method thereof Download PDF

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CN111893435A
CN111893435A CN202010661775.9A CN202010661775A CN111893435A CN 111893435 A CN111893435 A CN 111893435A CN 202010661775 A CN202010661775 A CN 202010661775A CN 111893435 A CN111893435 A CN 111893435A
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layer
sputtering
substrate
light irradiation
reflectivity
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CN111893435B (en
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李忠盛
董玲抒
吴护林
孙彩云
黄安畏
舒露
吴永鹏
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No 59 Research Institute of China Ordnance Industry
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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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic 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
    • C23C14/10—Glass or silica
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic 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
    • C23C14/22—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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • Optical Elements Other Than Lenses (AREA)

Abstract

The invention provides a light irradiation-resistant high-reflectivity film and a preparation method thereof, wherein the light irradiation-resistant high-reflectivity film sequentially comprises a protective layer (4), a high-reflectivity layer (3), a transition layer (2), a base layer (1), the transition layer (2), the high-reflectivity layer (3) and the protective layer (4) from inside to outside; wherein the substrate layer (1) adopts a polyimide film; the transition layer (2) is made of metal copper; the high-reflection layer (3) is made of low-cobalt stainless steel; the protective layer (4) is made of silicon oxide. The film has lower surface density and high reflectivity; meanwhile, the film has good thermal stability, high oxidation resistance and long service life, and effectively meets the requirements of light weight and high heat preservation performance.

Description

Light irradiation-resistant high-reflectivity film and preparation method thereof
Technical Field
The invention relates to the technical field of functional materials, in particular to a light irradiation-resistant high-reflectivity film and a preparation method thereof.
Background
Under the normal operation condition of a nuclear power plant, a large difference value needs to exist between the temperature of various devices or pipelines and the temperature of the external environment; for example, where the average temperature inside the pipe is above 310 ℃, an outside ambient temperature of less than 50 ℃ is generally required. Therefore, in order to reduce the heat loss of equipment and pipes in a nuclear power plant under normal operating conditions, the outer walls of the equipment and pipes are usually covered with an insulating layer. Compared with a non-metal heat-insulating layer, the metal heat-insulating layer has the characteristics of unobvious aging phenomenon, excellent high-temperature resistance and irradiation resistance and the like; and the fragments generated after the metal heat-insulating layer break accident have small influence on downstream physics and chemistry, so that the fragments are widely applied to nuclear power plant equipment and pipelines.
The metal heat-insulating layer mainly utilizes the reflection characteristic of the reflecting layers to enable radiant heat to be reflected for many times in the gaps so as to reduce radiant heat transfer, and the gaps among the reflecting layers are utilized to cause obstruction to heat convection so as to play a heat-insulating role, so that the metal heat-insulating layer has good thermal resistivity.
At present, the adopted traditional reflecting layer is stainless steel foil, the thickness of the commonly used stainless steel foil is 0.03mm, and the surface density is 237g/m2The surface is easy to oxidize at high temperature, the reflectivity is reduced along with the increase of the oxidation degree and is usually 0.60-0.75, the heat radiation efficiency is low, and the requirements of the market on light weight and high heat insulation performance of a new generation of products are difficult to meet.
Disclosure of Invention
In view of the problems of the prior art, the present invention aims to provide a light irradiation-resistant high-reflectivity film, which has low surface density and high reflectivity; meanwhile, the film has good thermal stability, high oxidation resistance and long service life, and effectively meets the requirements of light weight and high heat preservation performance.
The invention also aims to provide a preparation method of the light irradiation-resistant high-reflectivity film.
The purpose of the invention is realized by the following technical scheme:
a light irradiation-resistant high-reflectivity film is used for coating the surface of equipment or a pipeline and is characterized in that: the light-emitting diode comprises a substrate layer, a transition layer, a high-reflection layer and a protective layer, wherein the protective layer, the high-reflection layer, the transition layer, the substrate layer, the transition layer, the high-reflection layer and the protective layer are sequentially arranged from inside to outside;
wherein the substrate layer is a polyimide film; the transition layer adopts metal copper; the high-reflection layer is made of low-cobalt stainless steel; the protective layer is made of silicon oxide.
The polyimide film has low surface density, excellent thermal stability, flame retardance and mechanical properties, and the light weight of the whole film is ensured by adopting the polyimide; the reflection characteristic of the low-cobalt stainless steel is adopted for reflecting radiant heat and reducing radiant heat transfer; the silicon oxide layer is adopted to prevent the low-cobalt stainless steel from being oxidized and ensure the reflection characteristic of the low-cobalt stainless steel.
Due to the thermal expansion coefficient of 2 multiplied by 10 of the polyimide film-5The thermal expansion coefficient of the/K, low-cobalt stainless steel is 1.44 multiplied by 10-5The thermal expansion coefficients of the polyimide film substrate and the low-cobalt stainless steel have large difference and the thermal deformation temperature is close, so that the polyimide film substrate and the low-cobalt stainless steel can be simultaneously subjected to thermal deformation and have large difference in deformation under the condition of continuous high temperature, and the integral reflection effect of the film is influenced due to the fact that the high-reflection layer is uneven, and even the phenomenon that the high-reflection layer partially or integrally falls off from the substrate layer due to deformation occurs. The invention introduces the thermal expansion coefficient of 1.65 multiplied by 10-5The metal copper of/K is used as a transition layer, the thermal stability of the whole film structure is increased by utilizing the step-type reduction of the thermal expansion coefficient (from the base layer to the protective layer), and the high-reflection layer of the low-cobalt stainless steel is prevented from generating thermal deformation along with the polyimide film substrate, so that the conditions of reflectivity reduction, uneven heat resistance or falling-off of the reflection layer are avoided; at the same time, the transition layer is also in a certain rangeThe radiation heat is reflected to a certain extent, so that the temperature transferred to the high reflection layer or the substrate layer is reduced, the heat deformation amount of the high reflection layer or the substrate layer under the continuous high temperature condition is further reduced, and the heat stability of the whole film is ensured. Moreover, radiant heat is reflected for multiple times in the gap through the reflection characteristics of the transition layer and the high reflection layer, so that the reflectivity is greatly improved, and the radiant heat transfer is reduced.
Further optimization is carried out, and the thickness of the base layer is 25-30 mu m.
Further optimizing, the thickness of the high reflection layer is 100-200 nm.
Preferably, the cobalt content of the high reflection layer is less than 0.1 wt.%.
Further optimization is carried out, and the thickness of the protective layer is 10-50 nm.
Further optimized, the thickness ratio of the transition layer, the high reflection layer and the protective layer is 1:20 (1-5).
The preparation method of the light irradiation-resistant high-reflectivity film is characterized by comprising the following steps of:
a. opening the vacuum chamber, installing the membrane material, measuring the diameter of the membrane material at the coiling and uncoiling positions, and adjusting the tension; then closing the vacuum chamber, turning on a power supply, and checking whether the coating drum can work normally; opening cooling water switch of pump set, opening preceding stage pump set, vacuumizing after 5min to vacuum degree less than 5 × 10-3When Pa, preparing a coating; checking the temperature of the coating drum and the cryogenic temperature, opening a cathode cooling water and a pretreatment heater, adjusting the tension, and starting to coil;
b. rotating the metal copper target material, and adjusting the distance between the substrate and the target material, wherein the distance between the metal copper target material and the substrate is 4-10 cm; introducing argon, cleaning a gas pipeline, keeping the duration for 3-5 min, keeping the pressure at 0.1-0.8 Pa, and starting sputtering;
c. after the metal copper sputtering is finished, replacing a low-cobalt stainless steel target, and adjusting the distance between a substrate and the target, wherein the distance between the low-cobalt stainless steel target and the substrate is 4-10 cm; introducing argon, cleaning a gas pipeline, keeping the duration for 3-5 min, keeping the pressure at 0.1-0.8 Pa, and starting sputtering;
d. after the low-cobalt stainless steel sputtering is finished, replacing the silicon target, and adjusting the distance between the substrate and the target, wherein the distance between the silicon target and the substrate is 8-16 cm; introducing argon and oxygen, keeping the pressure at 0.1-0.8 Pa, and starting sputtering;
e. after the silicon sputtering is finished, the sputtering power supply and the gas are closed, the steps a to d are repeated, and the residual reverse side sputtering is finished;
f. and e, after the sputtering is finished, closing a sputtering power supply and gas.
Further optimizing, the argon flow in the step b and the step c is 30-500 sccm.
And c, further optimizing, wherein the power of the metal copper sputtering in the step b is 200-300W, and the sputtering time is 2-5 min.
And c, further optimizing, wherein the sputtering power of the low-cobalt stainless steel in the step c is 250-350W, and the sputtering time is 8-12 min.
And d, further optimizing, wherein the argon flow in the step d is 10-60 sccm, and the oxygen flow in the step d is 30-80 sccm.
And (d) further optimizing, wherein the silicon sputtering power in the step d is 150-250W, and the sputtering time is 2-3 min.
The invention has the following technical effects:
according to the invention, the transition layer, the high-reflection layer and the protective layer are prepared on the polyimide film, so that the whole film has lower surface density, and the light characteristic of the film is ensured; meanwhile, the whole film has high reflectivity through the matching of the transition layer and the high reflection layer, so that excellent radiation resistance is ensured, and the excellent thermal stability of the whole film is ensured through the thermal expansion coefficient difference of the base layer, the transition layer and the high reflection layer, so that the uniformity and the stability of reflection characteristics are ensured; the high-reflection layer is protected by the transition layer and the protective layer, and the phenomenon that the high-reflection layer falls off from the base layer due to thermal deformation and the reflectivity is reduced due to oxidation is avoided, so that the service life of the whole film is obviously prolonged.
The light irradiation-resistant high-reflectivity film prepared by the invention has the advantages of simple preparation process, easily obtained used materials, high maturity and wide application range, and can be used on the surfaces of most high-temperature equipment or pipelines.
Drawings
FIG. 1 is a schematic view of the structure of a polyimide film according to the present invention.
FIG. 2 is a schematic diagram of a thermal insulation performance testing system according to the present invention.
Wherein, 1, a substrate layer; 2. a transition layer; 3. a highly reflective layer; 4. a protective layer; 10. a data recorder; 20. a computer; 30. an intelligent temperature control addition system; 101. a temperature sensor; 102. a support; 103. sealing the cover body; 104. a high and low temperature chamber; 105. a heater; 106. a sample; 107. a sample holder; 108. a fastener.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of a light irradiation-resistant high-reflectivity film is characterized by comprising the following steps:
a. firstly, opening a vacuum chamber, installing a membrane material, measuring the diameter of the membrane material at the coiling and uncoiling positions, and adjusting the tension; then closing the vacuum chamber, turning on a power supply, and checking whether the coating drum can work normally; opening cooling water switch of pump set, opening preceding stage pump set, vacuumizing after 5min to vacuum degree less than 5 × 10-3When Pa, preparing a coating; checking the temperature of the coating drum and the cryogenic temperature, turning on the cathode cooling water and the pretreatment heater, adjusting the tension, and starting the coiled material.
b. Rotating the metal copper target material, and adjusting the distance between the substrate and the target material, wherein the distance between the metal copper target material and the substrate is 10 cm; introducing argon gas with the flow rate of 30sccm, cleaning a gas pipeline, lasting for 5min, keeping the pressure at 0.1Pa, and starting sputtering; the sputtering power is 200W, and the sputtering time is 2 min.
c. After the metal copper sputtering is finished, replacing the low-cobalt stainless steel target, and adjusting the distance between the substrate and the target, wherein the distance between the low-cobalt stainless steel target and the substrate is 10 cm; introducing argon gas with the flow rate of 30sccm, cleaning a gas pipeline, lasting for 3min, keeping the pressure at 0.1Pa, and starting sputtering; the sputtering power is 250W, and the sputtering time is 8 min.
d. After the low-cobalt stainless steel sputtering is finished, replacing the silicon target, and adjusting the distance between the substrate and the target, wherein the distance between the silicon target and the substrate is 14 cm; introducing argon and oxygen, wherein the flow of the argon is 20sccm, the flow of the oxygen is 40sccm, the pressure is kept at 0.3Pa, and starting sputtering; the sputtering power is 180W, and the sputtering time is 2.5 min.
e. After the silicon sputtering is finished, the sputtering power supply and the gas are closed, the steps a to d are repeated, and the residual reverse side sputtering is finished;
f. and e, after the sputtering is finished, closing a sputtering power supply and gas.
The finally obtained light irradiation-resistant high-reflectivity film is shown in figure 1 and sequentially comprises a protective layer 4, a high-reflection layer 3, a transition layer 2, a substrate layer 1, a transition layer 2, a high-reflection layer 3 and a protective layer 4 from top to bottom; wherein, the substrate layer 1 is a polyimide film with the thickness of 25 μm; the transition layer 2 is made of metal copper and has the thickness of 5 nm; the high reflection layer 3 is low cobalt stainless steel, the cobalt content is less than 0.1wt.%, and the thickness of the high reflection layer 3 is 100 nm; the protective layer 4 is silicon oxide and has a thickness of 25 nm. The light irradiation-resistant high-reflectivity film has a reflectivity of 0.85 and an area density of 47.5 g/m2(ii) a After heating at 300 ℃ for 2h, the reflectance was 0.84.
Example 2:
a preparation method of a light irradiation-resistant high-reflectivity film is characterized by comprising the following steps:
a. firstly, opening a vacuum chamber, installing a membrane material, measuring the diameter of the membrane material at the coiling and uncoiling positions, and adjusting the tension; then closing the vacuum chamber, turning on a power supply, and checking whether the coating drum can work normally; opening cooling water switch of pump set, opening preceding stage pump set, vacuumizing after 5min to vacuum degree less than 5 × 10-3When Pa, preparing a coating; checking the temperature of the coating drum and the cryogenic temperature, turning on the cathode cooling water and the pretreatment heater, adjusting the tension, and starting the coiled material.
b. Rotating the metal copper target material, and adjusting the distance between the substrate and the target material, wherein the distance between the metal copper target material and the substrate is 6 cm; introducing argon gas with the flow rate of 200sccm, cleaning a gas pipeline, lasting for 4min, keeping the pressure at 0.5Pa, and starting sputtering; the sputtering power is 250W, and the sputtering time is 3 min.
c. After the metal copper sputtering is finished, replacing the low-cobalt stainless steel target, and adjusting the distance between the substrate and the target, wherein the distance between the low-cobalt stainless steel target and the substrate is 6 cm; introducing argon gas with the flow rate of 200sccm, cleaning a gas pipeline, lasting for 4min, keeping the pressure at 0.5Pa, and starting sputtering; the sputtering power is 300W, and the sputtering time is 10 min.
d. After the low-cobalt stainless steel sputtering is finished, replacing the silicon target, and adjusting the distance between the substrate and the target, wherein the distance between the silicon target and the substrate is 16 cm; introducing argon and oxygen, wherein the flow of the argon is 15sccm, the flow of the oxygen is 35sccm, the pressure is kept at 0.3Pa, and sputtering is started; the sputtering power is 160W, and the sputtering time is 2 min.
e. After the silicon sputtering is finished, the sputtering power supply and the gas are closed, the steps a to d are repeated, and the residual reverse side sputtering is finished;
f. and e, after the sputtering is finished, closing a sputtering power supply and gas.
The finally obtained light irradiation-resistant high-reflectivity film is shown in figure 1 and sequentially comprises a protective layer 4, a high-reflection layer 3, a transition layer 2, a substrate layer 1, a transition layer 2, a high-reflection layer 3 and a protective layer 4 from top to bottom; wherein, the substrate layer 1 is a polyimide film with the thickness of 27 μm; the transition layer 2 is made of metal copper and has the thickness of 7.5 nm; the high reflection layer 3 is low cobalt stainless steel, the cobalt content is less than 0.1wt.%, and the thickness of the high reflection layer 3 is 150 nm; the protective layer 4 is silicon oxide and has a thickness of 15 nm. The light irradiation-resistant high-reflectivity film has a reflectivity of 0.86 and an area density of 47.6g/m2(ii) a After heating at 300 ℃ for 2h, the reflectance was 0.85.
Example 3:
a preparation method of a light irradiation-resistant high-reflectivity film is characterized by comprising the following steps:
a. firstly, opening a vacuum chamber, installing a membrane material, measuring the diameter of the membrane material at the coiling and uncoiling positions, and adjusting the tension; then the vacuum is turned offThe chamber is powered on, and whether the coating drum can work normally is checked; opening cooling water switch of pump set, opening preceding stage pump set, vacuumizing after 5min to vacuum degree less than 5 × 10-3When Pa, preparing a coating; checking the temperature of the coating drum and the cryogenic temperature, turning on the cathode cooling water and the pretreatment heater, adjusting the tension, and starting the coiled material.
b. Rotating the metal copper target material, and adjusting the distance between the substrate and the target material, wherein the distance between the metal copper target material and the substrate is 4 cm; introducing argon gas with the flow rate of 500sccm, cleaning a gas pipeline, lasting for 5min, keeping the pressure at 0.8Pa, and starting sputtering; the sputtering power is 300W, and the sputtering time is 5 min.
c. After the metal copper sputtering is finished, replacing the low-cobalt stainless steel target material, and adjusting the distance between the substrate and the target material, wherein the distance between the low-cobalt stainless steel target material and the substrate is 4 cm; introducing argon gas with the flow rate of 500sccm, cleaning a gas pipeline, lasting for 5min, keeping the pressure at 0.8Pa, and starting sputtering; the sputtering power is 350W, and the sputtering time is 12 min.
d. After the low-cobalt stainless steel sputtering is finished, replacing the silicon target, and adjusting the distance between the substrate and the target, wherein the distance between the silicon target and the substrate is 8 cm; introducing argon and oxygen, wherein the flow of the argon is 60sccm, the flow of the oxygen is 80sccm, the pressure is kept at 0.8Pa, and sputtering is started; the sputtering power is 250W, and the sputtering time is 3 min.
e. After the silicon sputtering is finished, the sputtering power supply and the gas are closed, the steps a to d are repeated, and the residual reverse side sputtering is finished;
f. and e, after the sputtering is finished, closing a sputtering power supply and gas.
The finally obtained light irradiation-resistant high-reflectivity film is shown in figure 1 and sequentially comprises a protective layer 4, a high-reflection layer 3, a transition layer 2, a substrate layer 1, a transition layer 2, a high-reflection layer 3 and a protective layer 4 from top to bottom; wherein the substrate layer 1 is a polyimide film with the thickness of 30 μm; the transition layer 2 is made of metal copper and has the thickness of 10 nm; the high reflection layer 3 is low cobalt stainless steel, the cobalt content is less than 0.1wt.%, and the thickness of the high reflection layer 3 is 200 nm; the protective layer 4 is silicon oxide and has a thickness of 50 nm. The light irradiation-resistant high-reflectivity film has a reflectivity of 0.87 and an area density of 47.9g/m2；3After heating at 00 ℃ for 2h, the reflectance was 0.85.
Preparing a test sample of a multilayer composite heat-insulating product, and testing the heat-insulating property according to the southwest technical engineering institute enterprise standard Q/CD 3229-:
standard sample 1, sample 2 and sample 3 having a length of 350mm, a width of 250mm and a thickness of 50mm were prepared. Wherein the sample 1 is a heat-insulating layer formed by alternately laminating stainless steel foil and composite ceramic fiber, the thickness of the stainless steel foil is 0.03mm, the reflectivity is 0.77, and the surface density is 237g/m2(ii) a Sample 2 is a heat-insulating layer formed by alternately laminating the light radiation-resistant high-reflectivity film and the composite ceramic fiber, the thickness of the film is 0.03mm, the reflectivity is 0.86, and the surface density is 47.9g/m2(ii) a The sample 3 does not adopt the transition layer 2, the structures and materials of the other layers are consistent with those of the sample 2, the high-reflection layer 3 and the protective layer 4 are consistent with those of the sample 2, the thin film and the composite ceramic fiber are alternately laminated to form the heat-insulating layer, the thickness of the thin film is 0.03mm, the reflectivity is 0.82, and the areal density is 47.9g/m2. The schematic diagram of the thermal insulation performance test is shown in fig. 2, a sample is fixed on heating equipment, 3 temperature measuring points are arranged on the cold surface of the sample, and the temperature of the cold surface of the sample is continuously collected by a thermocouple. Tests show that the hot surface temperature is 300 ℃, the environment temperature is 23 ℃, the heat preservation time is 2 hours, the cold surface highest temperature of the sample 1 is 47 ℃, the cold surface highest temperature of the sample 2 is 30 ℃, and the cold surface highest temperature of the sample 3 is 35 ℃, which shows that the heat insulation material has more obvious heat insulation effect compared with the traditional heat preservation layer (namely the sample 1) and also has better heat insulation effect compared with the sample 3 without the transition layer 2. Meanwhile, the temperature of each point of the cold surface of the test sample 2 has a positive and negative deviation value not exceeding 1.5 ℃, and the temperature of each point of the cold surface of the test sample 3 has a positive and negative deviation value exceeding 4 ℃, so that the invention is proved to have good heat insulation uniformity, good thermal stability of the film and no large thermal deformation, and further ensures the heat insulation uniformity.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A light irradiation-resistant high-reflectivity film is used for coating the surface of equipment or a pipeline and is characterized in that: the light-emitting diode comprises a base layer (1), a transition layer (2), a high-reflection layer (3) and a protective layer (4), wherein the protective layer (4), the high-reflection layer (3), the transition layer (2), the base layer (1), the transition layer (2), the high-reflection layer (3) and the protective layer (4) are arranged from inside to outside in sequence;
wherein the substrate layer (1) adopts a polyimide film; the transition layer (2) is made of metal copper; the high-reflection layer (3) is made of low-cobalt stainless steel; the protective layer (4) is made of silicon oxide.
2. The lightweight radiation-resistant high reflectivity film of claim 1, wherein: the thickness of the substrate layer (1) can be 25-30 μm.
3. The lightweight radiation-resistant high reflectivity film of claim 1, wherein: the thickness of the protective layer (4) can be 10-50 nm.
4. A preparation method of a light irradiation-resistant high-reflectivity film is characterized by comprising the following steps:
a. opening the vacuum chamber, installing the membrane material, measuring the diameter of the membrane material at the coiling and uncoiling positions, and adjusting the tension; then closing the vacuum chamber, turning on a power supply, and checking whether the coating drum can work normally; opening cooling water switch of pump set, opening preceding stage pump set, vacuumizing after 5min to vacuum degree less than 5 × 10-3When Pa, preparing a coating; checking the temperature of the coating drum and the cryogenic temperature, opening a cathode cooling water and a pretreatment heater, adjusting the tension, and starting to coil;
b. rotating the metal copper target material, and adjusting the distance between the substrate and the target material, wherein the distance between the metal copper target material and the substrate is 4-10 cm; introducing argon, cleaning a gas pipeline, keeping the duration for 3-5 min, keeping the pressure at 0.1-0.8 Pa, and starting sputtering;
c. after the metal copper sputtering is finished, replacing a low-cobalt stainless steel target, and adjusting the distance between a substrate and the target, wherein the distance between the low-cobalt stainless steel target and the substrate is 4-10 cm; introducing argon, cleaning a gas pipeline, keeping the duration for 3-5 min, keeping the pressure at 0.1-0.8 Pa, and starting sputtering;
d. after the low-cobalt stainless steel sputtering is finished, replacing the silicon target, and adjusting the distance between the substrate and the target, wherein the distance between the silicon target and the substrate is 8-16 cm; introducing argon and oxygen, keeping the pressure at 0.1-0.8 Pa, and starting sputtering;
e. after the silicon sputtering is finished, the sputtering power supply and the gas are closed, the steps a to d are repeated, and the residual reverse side sputtering is finished;
f. and e, after the sputtering is finished, closing a sputtering power supply and gas.
5. The method for preparing the light irradiation-resistant high-reflectivity film according to claim 4, wherein the method comprises the following steps: the argon flow in the steps b and c is 30-500 sccm.
6. The method for preparing the light irradiation-resistant high-reflectivity film according to claim 4, wherein the method comprises the following steps: and b, sputtering the metal copper in the step b at the power of 200-300W for 2-5 min.
7. The method for preparing the light irradiation-resistant high-reflectivity film according to claim 4, wherein the method comprises the following steps: in the step c, the power of the low-cobalt stainless steel sputtering is 250-350W, and the sputtering time is 8-12 min.
8. The method for preparing the light irradiation-resistant high-reflectivity film according to claim 4, wherein the method comprises the following steps: in the step d, the argon flow is 10-60 sccm, and the oxygen flow is 30-80 sccm.
9. The method for preparing the light irradiation-resistant high-reflectivity film according to claim 4, wherein the method comprises the following steps: and d, in the step d, the silicon sputtering power is 150-250W, and the sputtering time is 2-3 min.
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CN104962861A (en) * 2015-06-03 2015-10-07 东莞市明谷一纳米材料有限公司 Alloy composite material and preparation method thereof
CN106799872A (en) * 2016-12-27 2017-06-06 兰州空间技术物理研究所 A kind of controllable heat controlled thin film of emissivity
CN110001160A (en) * 2019-04-02 2019-07-12 中国兵器工业第五九研究所 A kind of multi-layered composite heat-insulating component resistant to high temperature and preparation method thereof
CN110802885A (en) * 2019-11-11 2020-02-18 中国兵器工业第五九研究所 Nuclear-grade modular heat-insulating layer and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN102260854A (en) * 2011-07-18 2011-11-30 东莞理工学院 Self-cleaning solar high-reflectivity nano film and manufacturing method
CN104962861A (en) * 2015-06-03 2015-10-07 东莞市明谷一纳米材料有限公司 Alloy composite material and preparation method thereof
CN106799872A (en) * 2016-12-27 2017-06-06 兰州空间技术物理研究所 A kind of controllable heat controlled thin film of emissivity
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