CN109468591B - Method for preparing colorful reflective film by vacuum evaporation process - Google Patents

Method for preparing colorful reflective film by vacuum evaporation process Download PDF

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Publication number
CN109468591B
CN109468591B CN201910021948.8A CN201910021948A CN109468591B CN 109468591 B CN109468591 B CN 109468591B CN 201910021948 A CN201910021948 A CN 201910021948A CN 109468591 B CN109468591 B CN 109468591B
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evaporation
molybdenum
vacuum
winding
film
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CN109468591A (en
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刘思远
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Hefei Huiyao Vacuum Material Co ltd
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Hefei Huiyao Vacuum Material Co ltd
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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
    • C23C14/56—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
    • 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
    • C23C14/0623—Sulfides, selenides or tellurides
    • C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/243—Crucibles for source material
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/26—Vacuum evaporation by resistance or inductive heating of the source

Abstract

The invention discloses a method for preparing a colorful reflective film by a vacuum evaporation process, which comprises the steps of loading a base film of a plant to be plated into an evaporation chamber, then carrying out low-temperature cooling on a main drum, placing molybdenum boats in which evaporation target materials are arranged in an evaporation groove, ensuring that the distances from each part of evaporation target materials to the bottom end of the central main drum are different, closing a cover plate of the evaporation groove, then sending the evaporation groove into the evaporation chamber, and vacuumizing the evaporation chamber; heating the evaporation target material to a melting point, vaporizing, opening an evaporation tank cover plate, controlling the plant base film to be plated to move at a constant speed in an evaporation chamber, and performing gradual evaporation operation; and closing the equipment after the evaporation is finished. The reflective colorful film finally obtained by the method provided by the invention has a transparent surface, is suitable for deep processing treatment in a later period, is firm and difficult to fall off, and can generate a colorful effect in a dark environment after being illuminated.

Description

Method for preparing colorful reflective film by vacuum evaporation process
Technical Field
The invention relates to the technical field of reflective films, in particular to a method for preparing a colorful reflective film by a vacuum evaporation process.
Background
The manufacturing process of the common light-reflecting plant membrane generally comprises the following steps: firstly, adhering glass beads with different particle sizes on a glued PET or PE film, and meanwhile, generally adopting the glass beads with the refractive index of 1.90-1.93, then, in order to enhance the reflection effect of the reflective film, a layer of metal film is generally evaporated on the surface of the plant film by vacuum evaporation, while the metal film is mostly an aluminum film, the common aluminum film can cause the non-transparency of the film surface of the reflective film, and the reflective film is difficult to be used as a semi-finished product in the later period, the product can be processed into other colors according to the requirement of customers, moreover, for the common rainbow film, two or more transparent thermoplastic resins with different refractive indexes (the refractive indexes are different by at least 0.03) are utilized to form at least 30 layers of uniform and parallel alternating core layers through ABABAB. The rainbow film formed by using the multilayer resin has low strength, poor light reflecting performance and complex processing technology. In addition, the common transparent dielectric film is formed by directly evaporating a zinc sulfide target material on common plastic films such as PTE (Polytetrafluoroethylene), PP (polypropylene), OPP (oriented Polypropylene) films and the like, so that the obtained dielectric film has poor light reflecting effect, and the traditional aluminized plant film has good light reflecting effect but is difficult to achieve the transparent effect.
Disclosure of Invention
Technical scheme (I)
In order to solve the defects of the prior art, the invention provides the following technical scheme: a method for preparing a colorful reflective film by a vacuum evaporation process comprises the following steps:
(1) loading the plated plant base film on two winding and unwinding rollers in a winding chamber of high vacuum coating equipment, winding the plated plant base film on the other winding and unwinding roller from one winding and unwinding roller through a central main drum, starting a forced refrigeration system and connecting a gas circuit;
(2) placing a plurality of molybdenum boats in which evaporation target materials are closely arranged in an evaporation tank of high vacuum coating equipment, ensuring that the distances from each part of evaporation target materials to the bottom end of a central main drum are different, and then connecting two electrode ends of each molybdenum boat with copper column electrodes of the evaporation tank;
(3) the evaporation tank is conveyed into an evaporation chamber after a cover plate is closed, a cabin door is closed to ensure that the evaporation chamber is in a closed state, and then a vacuum extraction device is started to extract vacuum to the evaporation chamber;
(4) switching on a power supply of the evaporation tank, heating the evaporation target material to a melting point, vaporizing the evaporation target material, and opening a cover plate of the evaporation tank;
(5) starting a winding system, entering a normal evaporation state, then controlling the plant base film to be plated to move at a constant speed in an evaporation chamber, and carrying out gradual evaporation operation;
(6) and after the evaporation is finished, closing the winding system, closing the power supply of the evaporation tank, closing the vacuum extraction equipment, returning the temperature, balancing the atmospheric pressure, and opening the chamber.
Preferably, the evaporation target specifically adopts a zinc sulfide target.
Preferably, the evaporation target material is of a cylindrical structure, the evaporation target materials are vertically arranged and then are tightly arranged on the molybdenum boat, and evaporation top surfaces formed by the arranged multiple rows of evaporation target materials are arc-shaped evaporation surfaces with different heights.
Preferably, the distance from the evaporation target to the surface of the base film of the plant to be plated at the bottom end of the central main drum is controlled to be 13.5 cm-15.5 cm.
Preferably, an upper supporting cushion block and a lower supporting cushion block are sequentially placed at the bottom end of the molybdenum boat for containing the evaporation target material, and the upper supporting cushion block is square fusion casting alpha-Al matched with the molybdenum boat in size2O3Resistant firebrick, a plurality of bar grooves have been seted up to even equidistant the supporting pad top, adjacent two be formed with the support parting bead that a plurality of widths far are less than the bar groove width between the bar groove.
Preferably, the molybdenum boat is a square structure formed by splicing a plurality of molybdenum bars end to end, and is adjacent two a bar-shaped gap is formed between the molybdenum bars, two electrode ends of the molybdenum boat are end parts of the molybdenum bars located on two sides of the molybdenum boat and extending outwards, two side outer edges of the molybdenum bars in the width direction are bent to form first flanges, two side outer edges of the molybdenum bars in the length direction are spliced to form a row of silicon carbide columns, a second flange is formed, and the distance between the two adjacent silicon carbide columns is smaller than the outer diameter of the evaporation target.
Preferably, the needle valve is hermetically mounted on the sidewall of the evaporation chamber, and in the step (3), when the vacuum pumping operation is performed, the vacuum pumping operation is performed to 2.5 × 100Pa～1×10-1Pa, then utilizing a needle valve to accurately regulate and control the vacuum degree in the evaporation chamber in the evaporation process, and regulating the vacuum degree to 2.50 multiplied by 10 according to the final effect of an evaporation product0Pa～1.0×10-1Pa in the exact range.
Preferably, when the evaporation target material is heated in the step (4), the temperature is uniformly and slowly raised to 1400 ℃ within 5min, and when the temperature is raised to 1400 ℃, the temperature is kept for 2min, and then the winding system is started to enter a normal evaporation state.
Preferably, after the winding system is started in the step (5), the winding speed is kept at 48 m/min-65 m/min, the winding is carried out at a constant speed, and the film coating effect is observed in real time through an observation window to adjust the winding speed.
Preferably, the temperature of the central main drum is kept between-20 ℃ and-10 ℃ after the central main drum is cooled by a forced cooling system.
(II) advantageous effects
The invention provides a method for preparing a colorful reflective film by a vacuum evaporation process, which has the following beneficial effects:
the magic color film adopts a zinc sulfide material as a target material, because the refractive index of zinc sulfide is 2.35, the light transmission range is 400-13000nm, the magic color film has good stress and environmental durability, and the zinc sulfide is easy to sublimate when being evaporated at high temperature; for example, the anti-counterfeiting material can be processed into clothes, shoes and bags with various colors and high-quality anti-counterfeiting materials according to requirements, the colors of the clothes or the shoes and bags are the same in the daytime, the anti-counterfeiting material does not have obvious colorful effects, and the anti-counterfeiting material can have obvious colorful effects when meeting direct illumination in dark environments at night.
The key technology of the process is that the thickness of a zinc sulfide film formed by condensing the surface of a base film of a plated plant is ensured to be uneven as much as possible, the thickness difference value is 1-10 nm, because the zinc sulfide film at each different position can be regarded as a small spherical surface, the middle is thick, the edge is thin, the thickness of a circle of the zinc sulfide film around the edge is approximately equal, namely the generated optical path difference is equal, the same color light can interfere in the circle, the interfered light is colored patterns when irradiating human eyes, the color light from the center of the zinc sulfide film to the edge is red-orange yellow-green-blue-purple, and because the middle thickness is large, the wavelength of the color light is longer, and the color phenomenon can be formed;
in order to ensure that the thickness of the zinc sulfide film formed by condensation on the surface of the base film of the plant to be plated is uneven, and therefore, the distance from each part of evaporation target to the bottom end of the central main drum is different, the target 11 is set to be in a cylindrical structure and is simultaneously arranged on the molybdenum boat tightly after being cubed, the evaporation surfaces which are formed in an arc shape and have different heights can be effectively increased, the evaporation surface of the target can be effectively increased, so that the evaporation efficiency is improved, the distance from each part of target to the base film of the plant to be plated is different when each part of target is evaporated, the time for the target to reach the surface of the plant after sublimation is different, the thickness of the zinc sulfide film formed by condensation on the surface of the plant can be finally uneven, and the effect of a colorful.
The molybdenum boat is adopted as a vessel for containing the zinc sulfide target, and is high-temperature resistant and corrosion resistant, the melting point of the molybdenum boat is 2620 ℃, meanwhile, the molybdenum boat has high hardness and is not easy to deform, so that the molybdenum boat is suitable for being used as a zinc sulfide target high-temperature evaporation container; in addition, the molybdenum boat is integrally arranged to be of a square structure, so that a plurality of zinc sulfide targets can be conveniently placed at one time, and a stable supporting bottom surface is conveniently formed; the molybdenum boat is of a structure formed by splicing a plurality of molybdenum strips end to end, so that the molybdenum strips are connected in series to form a conductive material with enough length on the premise of ensuring that the bottom surface of the molybdenum boat is supported with enough area, and therefore the molybdenum boat is ensured to have enough overall resistance value, namely, after being electrified, the molybdenum boat can generate enough heat, and the zinc sulfide target material on the molybdenum boat is ensured to be quickly heated, evaporated and sublimated; according to the invention, the molybdenum boat loaded with the evaporation target material is designed into a plurality of square structures which are distributed at intervals, so that the target material can be ensured to form cross diffusion during evaporation, and the uneven surface thickness intervals of the evaporation film can be ensured.
In addition, the both sides outward flange of molybdenum strip length direction is pegged graft the second flange of constituteing by many carborundum posts, and guarantee that the interval is less than the evaporation coating target external diameter between two adjacent carborundum posts, so design, can utilize first flange and second flange to enclose the retaining with the cylindric zinc sulfide target of cube, avoid its problem that drops, and the carborundum post that designs the second flange for the interval setting, the flange structure of direct molybdenum strip bending type of utilizing of comparison, can effectively reduce the conducting area of outside molybdenum strip, thereby guarantee that the conducting area of many molybdenum strips keeps unanimous, thereby make the heating temperature evenly distributed at each position of molybdenum boat bottom surface, and carborundum itself is high temperature resistant insulating material, can avoid electrically conductive problem, make heating current flow along the molybdenum strip all the time.
According to the invention, the top end of the upper supporting cushion block is provided with the plurality of strip-shaped grooves, and a plurality of supporting parting beads with smaller width are formed, when in supporting, the supporting parting beads are contacted with the bottom surface of the molybdenum boat to form local contact, rather than the whole upper surface of the upper supporting cushion block is contacted with the bottom surface of the molybdenum boat, so that the contact area between the supporting cushion block and the molybdenum boat can be greatly reduced, the supporting strength can be ensured, and the phenomenon of adhesion between the upper supporting cushion block and the molybdenum boat caused by thermal deformation in the repeated high-temperature evaporation process can be avoided; the plurality of strip-shaped grooves are arranged into groove-shaped structures which are not directly communicated with the bottom ends of the upper supporting cushion blocks, so that heat can be ensured to circulate in the strip-shaped grooves, and heat loss is effectively reduced;
in addition, will supportThe supporting cushion block adopts fusion casting alpha-Al2O3The refractory brick is cut and polished to be made, the texture structure of the refractory material is compact, the refractoriness and high-temperature structural strength are high, and the high-temperature chemical stability is good, so that the upper supporting cushion block made of the material is not easy to generate thermal deformation and evaporation after repeated high-temperature heating, and cannot become impurity particles of an evaporation target material after high-temperature evaporation, and the purity of the evaporation target material for forming steam molecules can be ensured.
And all set up supporting pad and molybdenum boat to the independent square structure of mutual matching, arrange the molybdenum boat interval, so design can conveniently get alone and put molybdenum boat and supporting pad, damages or when needing to be changed when certain molybdenum boat or supporting pad, just can change alone, and need not whole changes, convenient nimble use.
The method provided by the invention controls the vacuum degree to be 1 x 10 when the vacuum is extracted from the evaporation chamber-1Pa～2.5×100Pa, because when the degree of vacuum is 2.5X 100When the pressure is higher than Pa, the surface of a vapor deposition film can be blackened or yellowed, the effect of a final finished product is influenced, and a zinc sulfide metal film formed by vapor deposition is not firm enough because a small amount of air molecules exist in a vapor deposition chamber, so that high-temperature zinc sulfide vapor molecules collide with the small amount of air molecules in the upward flying process, the firmness of the formed zinc sulfide metal film is influenced finally, and the problem of blackening and yellowing after oxidation also exists because of the small amount of air molecules; the vacuum degree is not required to be too low, so that good evaporation effect can be achieved, and particularly, the vacuum degree is lower than 1 multiplied by 10-1After Pa, the operation burden of the whole cooling system is greatly increased, and the problem of damage of the system in the long-time operation process is caused; in addition, because install the needle valve that can carry out the accuracy regulation and control to vacuum on this coiling evaporation plating equipment's the evaporation plating room, the installation of this needle valve can be with the indoor vacuum of traditional evaporation plating adjust to its next order of magnitude within range, this is the effect that traditional vacuum evaporation plating industry can't reach, after the vacuum degree carries out more accurate regulation and control, can regulate and control the gorgeous degree that dazzling various reflective membrane after the evaporation plating finally appears and the width of the seven various strips that form, effectively stop the membrane face simultaneouslyThe problem of blackening and yellowing can be realized according to different customer's demands like this, will dazzle various reflective membrane and regulate and control to different gorgeous degrees, adjust into the seven various strips of different width simultaneously.
When the power supply of the evaporation tank is switched on for heating evaporation operation, the temperature is uniformly and slowly increased to 1400 ℃ within 5min, and the temperature is kept for 2min after the temperature is increased to 1400 ℃, so that the operation can ensure that all parts of the target can be uniformly increased, and meanwhile, the target can be fully evaporated by keeping the temperature for 2min after the evaporation temperature is reached, thereby achieving the purpose of full evaporation.
In conclusion, according to the method for preparing the colorful reflective film by the vacuum evaporation process, the finally obtained reflective colorful film is transparent in surface and suitable for deep processing in the later period, and meanwhile, the metal film is firm and is not easy to fall off, and in a dim environment, a colorful effect can be generated after illumination.
Drawings
FIG. 1 is a schematic view of an evaporation process according to the present invention;
FIG. 2 is a schematic view of the internal structure of the evaporation tank without the target material;
FIG. 3 is a schematic top view of the molybdenum boat of the present invention;
FIG. 4 is a schematic diagram of a top view of the molybdenum boat after being filled with the target material;
FIG. 5 is a schematic view of the arrangement of targets according to the present invention;
FIG. 6 is a schematic view of the upper support pad structure of the present invention;
FIG. 7 is a schematic layout of the lower support pad, the upper support pad and the molybdenum boat of the present invention.
In the figure: the device comprises a main drum 1, an evaporation tank 2, a plant base film 3, a copper sheet 4, a molybdenum boat 5, a cover plate 6, a molybdenum boat electrode end 7, a strip-shaped gap 8, a molybdenum strip 9, a silicon carbide column 10, a target 11, an evaporation top surface 12, a strip-shaped groove 13, a support spacer 14, an upper support cushion block 15, a lower support cushion block 16 and a copper column electrode 17.
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 method for preparing a colorful reflective film by a vacuum evaporation process comprises the following steps:
(1) loading the plated plant base film on two winding and unwinding rollers in a winding chamber of a high vacuum coating device, winding the plated plant base film on the other winding and unwinding roller from one winding and unwinding roller through a central main drum, starting a forced refrigeration system, switching on a gas circuit, and cooling the main drum to-20 ℃ for later use;
(2) placing a plurality of molybdenum boats closely arranged with zinc sulfide targets in an evaporation tank of high vacuum coating equipment, wherein the zinc sulfide targets are cylindrical structures, the targets are closely arranged on the molybdenum boats after being vertically placed, evaporation top surfaces formed by the multiple rows of targets after being placed are arc-shaped evaporation surfaces with different heights, sequentially supporting the bottom ends of the molybdenum boats containing the evaporation targets by upper supporting cushion blocks and lower supporting cushion blocks, and the upper supporting cushion blocks are square fusion casting alpha-Al with the sizes matched with those of the molybdenum boats2O3The top end of the supporting pad is uniformly provided with a plurality of strip-shaped grooves at equal intervals, a plurality of supporting parting beads with the width far smaller than that of the strip-shaped grooves are formed between every two adjacent strip-shaped grooves, and the supporting parting beads are supported on the bottom surface of the molybdenum boat; supporting by using a supporting cushion block with proper height, and finally ensuring that the distance from the zinc sulfide target material to the surface of the plant base film to be plated at the bottom end of the central main drum is 13.5 cm; then connecting two electrode ends of the molybdenum boat with copper column electrodes of the evaporation tank through copper sheets;
(3) closing the cover plate of the evaporation tank and feeding the evaporation tank into an evaporation chamber, wherein a needle valve is hermetically arranged on the side wall of the evaporation chamber in advance, a chamber door is closed to ensure that the evaporation chamber is in a closed state, and a vacuum pump set is firstly utilized to vacuumize to 1 x 10-1Pa, then utilizing a needle valve to accurately regulate and control the vacuum degree in the evaporation chamber in the evaporation process, and controlling the vacuum degree at the final effect of the evaporation productAdjusting within the precise range of the next order of magnitude;
(4) switching on an evaporation tank power supply, uniformly and slowly heating to 1400 ℃ within 5min, and keeping the temperature for 2min after the temperature rises to 1400 ℃, so that the evaporation target material is heated to a melting point and vaporized, and a cover plate of the evaporation tank is opened;
(5) starting a winding system, entering a normal evaporation state, keeping the winding speed at 48m/min, carrying out uniform winding, then observing the film coating effect in real time through an observation window to adjust the winding speed, and carrying out gradual evaporation operation;
(6) and after the evaporation is finished, closing the winding system, closing the power supply of the evaporation tank, closing the vacuum extraction equipment, returning the temperature, balancing the atmospheric pressure, and opening the chamber.
The molybdenum boat is preferably of a square structure formed by splicing a plurality of molybdenum bars end to end, a bar-shaped gap is formed between every two adjacent molybdenum bars, two electrode ends of the molybdenum boat are end parts extending outwards of the molybdenum bars positioned on two sides of the molybdenum boat, the outer edges of two sides of the molybdenum bars in the width direction are bent to form first flanges, the outer edges of two sides of the molybdenum bars in the length direction are spliced with a row of silicon carbide columns to form second flanges, and the distance between every two adjacent silicon carbide columns is smaller than the outer diameter of an evaporation target.
Example 2
A method for preparing a colorful reflective film by a vacuum evaporation process comprises the following steps:
(1) loading the plated plant base film on two winding and unwinding rollers in a winding chamber of a high vacuum coating device, winding the plated plant base film on the other winding and unwinding roller from one winding and unwinding roller through a central main drum, starting a forced refrigeration system, switching on a gas circuit, and cooling the main drum to-16 ℃ for later use;
(2) put into a plurality of molybdenum boats that closely arrange and have zinc sulfide target in high vacuum coating equipment's evaporation tank, wherein zinc sulfide target is cylindrical structure, and closely arrange on the molybdenum boat after the target is put immediately, and the evaporation top surface that the multirow target formed after putting is the evaporation surface of arc and difference in height, puts supporting pad and lower support pad at the molybdenum boat bottom that holds the coating by vaporization target in proper order supporting pad, andthe upper supporting cushion block is square fusion casting alpha-Al matched with the molybdenum boat in size2O3The top end of the supporting pad is uniformly provided with a plurality of strip-shaped grooves at equal intervals, a plurality of supporting parting beads with the width far smaller than that of the strip-shaped grooves are formed between every two adjacent strip-shaped grooves, and the supporting parting beads are supported on the bottom surface of the molybdenum boat; supporting by using a supporting cushion block with proper height, and finally ensuring that the distance from the zinc sulfide target material to the surface of the plant base film to be plated at the bottom end of the central main drum is 14.2 cm; then connecting two electrode ends of the molybdenum boat with copper column electrodes of the evaporation tank through copper sheets;
(3) closing the cover plate of the evaporation tank and feeding the evaporation tank into an evaporation chamber, wherein the side wall of the evaporation chamber is provided with a needle valve in advance in a sealing manner, the chamber door is closed to ensure that the evaporation chamber is in a closed state, and a vacuum pump set is firstly utilized to pump vacuum to 9 multiplied by 10-1Pa, then utilizing a needle valve to accurately regulate and control the vacuum degree in the evaporation chamber in the evaporation process, and regulating the vacuum degree within the accurate range of the next order of magnitude according to the final effect of an evaporation product;
(4) switching on an evaporation tank power supply, uniformly and slowly heating to 1400 ℃ within 5min, and keeping the temperature for 2min after the temperature rises to 1400 ℃, so that the evaporation target material is heated to a melting point and vaporized, and a cover plate of the evaporation tank is opened;
(5) starting a winding system, entering a normal evaporation state, keeping the winding speed at 54m/min, carrying out uniform winding, then observing the film coating effect in real time through an observation window to adjust the winding speed, and carrying out gradual evaporation operation;
(6) and after the evaporation is finished, closing the winding system, closing the power supply of the evaporation tank, closing the vacuum extraction equipment, returning the temperature, balancing the atmospheric pressure, and opening the chamber.
The molybdenum boat is preferably of a square structure formed by splicing a plurality of molybdenum bars end to end, a bar-shaped gap is formed between every two adjacent molybdenum bars, two electrode ends of the molybdenum boat are end parts extending outwards of the molybdenum bars positioned on two sides of the molybdenum boat, the outer edges of two sides of the molybdenum bars in the width direction are bent to form first flanges, the outer edges of two sides of the molybdenum bars in the length direction are spliced with a row of silicon carbide columns to form second flanges, and the distance between every two adjacent silicon carbide columns is smaller than the outer diameter of an evaporation target.
Example 3
A method for preparing a colorful reflective film by a vacuum evaporation process comprises the following steps:
(1) loading the plated plant base film on two winding and unwinding rollers in a winding chamber of a high vacuum coating device, winding the plated plant base film on the other winding and unwinding roller from one winding and unwinding roller through a central main drum, starting a forced refrigeration system, switching on a gas circuit, and cooling the main drum to-13 ℃ for later use;
(2) placing a plurality of molybdenum boats closely arranged with zinc sulfide targets in an evaporation tank of high vacuum coating equipment, wherein the zinc sulfide targets are cylindrical structures, the targets are closely arranged on the molybdenum boats after being vertically placed, evaporation top surfaces formed by the multiple rows of targets after being placed are arc-shaped evaporation surfaces with different heights, sequentially supporting the bottom ends of the molybdenum boats containing the evaporation targets by upper supporting cushion blocks and lower supporting cushion blocks, and the upper supporting cushion blocks are square fusion casting alpha-Al with the sizes matched with those of the molybdenum boats2O3The top end of the supporting pad is uniformly provided with a plurality of strip-shaped grooves at equal intervals, a plurality of supporting parting beads with the width far smaller than that of the strip-shaped grooves are formed between every two adjacent strip-shaped grooves, and the supporting parting beads are supported on the bottom surface of the molybdenum boat; supporting by using a supporting cushion block with proper height, and finally ensuring that the distance from the zinc sulfide target material to the surface of the plant base film to be plated at the bottom end of the central main drum is 14.8 cm; then connecting two electrode ends of the molybdenum boat with copper column electrodes of the evaporation tank through copper sheets;
(3) closing the cover plate of the evaporation tank and feeding the evaporation tank into an evaporation chamber, wherein the side wall of the evaporation chamber is provided with a needle valve in advance in a sealing manner, the chamber door is closed to ensure that the evaporation chamber is in a closed state, and a vacuum pump set is firstly utilized to vacuumize to 1.7 multiplied by 100Pa, then utilizing a needle valve to accurately regulate and control the vacuum degree in the evaporation chamber in the evaporation process, and regulating the vacuum degree within the accurate range of the next order of magnitude according to the final effect of an evaporation product;
(4) switching on an evaporation tank power supply, uniformly and slowly heating to 1400 ℃ within 5min, and keeping the temperature for 2min after the temperature rises to 1400 ℃, so that the evaporation target material is heated to a melting point and vaporized, and a cover plate of the evaporation tank is opened;
(5) starting a winding system, entering a normal evaporation state, keeping the winding speed at 60m/min, carrying out uniform winding, then observing the film coating effect in real time through an observation window to adjust the winding speed, and carrying out gradual evaporation operation;
(6) and after the evaporation is finished, closing the winding system, closing the power supply of the evaporation tank, closing the vacuum extraction equipment, returning the temperature, balancing the atmospheric pressure, and opening the chamber.
The molybdenum boat is preferably of a square structure formed by splicing a plurality of molybdenum bars end to end, a bar-shaped gap is formed between every two adjacent molybdenum bars, two electrode ends of the molybdenum boat are end parts extending outwards of the molybdenum bars positioned on two sides of the molybdenum boat, the outer edges of two sides of the molybdenum bars in the width direction are bent to form first flanges, the outer edges of two sides of the molybdenum bars in the length direction are spliced with a row of silicon carbide columns to form second flanges, and the distance between every two adjacent silicon carbide columns is smaller than the outer diameter of an evaporation target.
Example 4
A method for preparing a colorful reflective film by a vacuum evaporation process comprises the following steps:
(1) loading the plated plant base film on two winding and unwinding rollers in a winding chamber of a high vacuum coating device, winding the plated plant base film on the other winding and unwinding roller from one winding and unwinding roller through a central main drum, starting a forced refrigeration system, switching on a gas circuit, and cooling the main drum to-10 ℃ for later use;
(2) placing a plurality of molybdenum boats closely arranged with zinc sulfide targets in an evaporation tank of high vacuum coating equipment, wherein the zinc sulfide targets are cylindrical structures, the targets are closely arranged on the molybdenum boats after being vertically placed, evaporation top surfaces formed by the multiple rows of targets after being placed are arc-shaped evaporation surfaces with different heights, sequentially supporting the bottom ends of the molybdenum boats containing the evaporation targets by upper supporting cushion blocks and lower supporting cushion blocks, and the upper supporting cushion blocks are square fusion casting alpha-Al with the sizes matched with those of the molybdenum boats2O3Resistant firebrick, even equidistant a plurality of bar grooves of seting up in supporting pad top form a plurality of widths between two adjacent bar grooves and far be less than the support of bar groove width and separateThe bar is supported on the bottom surface of the molybdenum boat by utilizing a supporting parting strip; supporting by using a supporting cushion block with proper height, and finally ensuring that the distance from the zinc sulfide target material to the surface of the plant base film to be plated at the bottom end of the central main drum is 15.5 cm; then connecting two electrode ends of the molybdenum boat with copper column electrodes of the evaporation tank through copper sheets;
(3) closing the cover plate of the evaporation tank and feeding the evaporation tank into an evaporation chamber, wherein the side wall of the evaporation chamber is provided with a needle valve in advance in a sealing manner, the chamber door is closed to ensure that the evaporation chamber is in a closed state, and a vacuum pump set is firstly utilized to vacuumize to 2.5 multiplied by 100Pa, then utilizing a needle valve to accurately regulate and control the vacuum degree in the evaporation chamber in the evaporation process, and regulating the vacuum degree within the accurate range of the next order of magnitude according to the final effect of an evaporation product;
(4) switching on an evaporation tank power supply, uniformly and slowly heating to 1400 ℃ within 5min, and keeping the temperature for 2min after the temperature rises to 1400 ℃, so that the evaporation target material is heated to a melting point and vaporized, and a cover plate of the evaporation tank is opened;
(5) starting a winding system, entering a normal evaporation state, keeping the winding speed at 65m/min, carrying out uniform winding, then observing the film coating effect in real time through an observation window to adjust the winding speed, and carrying out gradual evaporation operation;
(6) and after the evaporation is finished, closing the winding system, closing the power supply of the evaporation tank, closing the vacuum extraction equipment, returning the temperature, balancing the atmospheric pressure, and opening the chamber.
The molybdenum boat is preferably of a square structure formed by splicing a plurality of molybdenum bars end to end, a bar-shaped gap is formed between every two adjacent molybdenum bars, two electrode ends of the molybdenum boat are end parts extending outwards of the molybdenum bars positioned on two sides of the molybdenum boat, the outer edges of two sides of the molybdenum bars in the width direction are bent to form first flanges, the outer edges of two sides of the molybdenum bars in the length direction are spliced with a row of silicon carbide columns to form second flanges, and the distance between every two adjacent silicon carbide columns is smaller than the outer diameter of an evaporation target.
The magic color film adopts a zinc sulfide material as a target material, because the refractive index of zinc sulfide is 2.35, the light transmission range is 400-13000nm, the magic color film has good stress and environmental durability, and the zinc sulfide is easy to sublimate when being evaporated at high temperature; for example, the color-changeable decorative cloth or the shoe bag can be processed into various colors according to the requirement, the colors of the decorative cloth or the shoe bag are the colors of the decorative cloth or the shoe bag in the daytime, the obvious colorful effect is not achieved, and the obvious colorful effect can be achieved when direct illumination is met in a dark environment at night.
The key technology of the process is that the thickness of zinc sulfide films formed by condensation on the surface of a base film of a plated plant is guaranteed to be uneven as much as possible, because the zinc sulfide films at different positions can be regarded as a small spherical surface, the middle is thick, and the edge is thin, the thickness of a circle of zinc sulfide film surrounding the edge is approximately equal, namely, the generated optical path difference is equal, so that the same color light can interfere in the circle, the interfered light irradiates human eyes to form color patterns, the color light from the center of the zinc sulfide film to the edge is red, orange, yellow, green, blue and purple, because the middle thickness is large, the wavelength of the color light is longer, and the color phenomenon can be formed;
in order to ensure that the thickness of the zinc sulfide film formed by condensation on the surface of the base film of the plant to be plated is uneven, and therefore, the distance from each part of evaporation target to the bottom end of the central main drum is different, the target 11 is set to be in a cylindrical structure and is simultaneously arranged on the molybdenum boat tightly after being cubed, the evaporation surfaces which are formed in an arc shape and have different heights can be effectively increased, the evaporation surface of the target can be effectively increased, so that the evaporation efficiency is improved, the distance from each part of target to the base film of the plant to be plated is different when each part of target is evaporated, the time for the target to reach the surface of the plant after sublimation is different, the thickness of the zinc sulfide film formed by condensation on the surface of the plant can be finally uneven, and the effect of a colorful.
The molybdenum boat is used as a vessel for containing the zinc sulfide target, and is high-temperature resistant and corrosion resistant, the melting point of the molybdenum boat is 2620 ℃, and the molybdenum boat is high in hardness and difficult to deform, so that the molybdenum boat is suitable for being used as a zinc sulfide target high-temperature evaporation container; in addition, the molybdenum boat is integrally arranged to be of a square structure, so that a plurality of zinc sulfide targets can be conveniently placed at one time, and a stable supporting bottom surface is conveniently formed; the molybdenum boat is of a structure formed by splicing a plurality of molybdenum strips end to end, so that the molybdenum strips are connected in series to form a conductive material with enough length on the premise of ensuring that the bottom surface of the molybdenum boat is supported with enough area, and therefore the molybdenum boat is ensured to have enough overall resistance value, namely, after being electrified, the molybdenum boat can generate enough heat, and the zinc sulfide target material on the molybdenum boat is ensured to be quickly heated, evaporated and sublimated; according to the invention, the molybdenum boat loaded with the evaporation target material is designed into a plurality of square structures which are distributed at intervals, so that the target material can be ensured to form cross diffusion during evaporation, and the uneven surface thickness intervals of the evaporation film can be ensured.
In addition, the both sides outward flange of molybdenum strip length direction is pegged graft the second flange of constituteing by many carborundum posts, and guarantee that the interval is less than the evaporation coating target external diameter between two adjacent carborundum posts, so design, can utilize first flange and second flange to enclose the retaining with the cylindric zinc sulfide target of cube, avoid its problem that drops, and the carborundum post that designs the second flange for the interval setting, the flange structure of direct molybdenum strip bending type of utilizing of comparison, can effectively reduce the conducting area of outside molybdenum strip, thereby guarantee that the conducting area of many molybdenum strips keeps unanimous, thereby make the heating temperature evenly distributed at each position of molybdenum boat bottom surface, and carborundum itself is high temperature resistant insulating material, can avoid electrically conductive problem, make heating current flow along the molybdenum strip all the time.
According to the invention, the top end of the upper supporting cushion block is provided with the plurality of strip-shaped grooves, and a plurality of supporting parting beads with smaller width are formed, when in supporting, the supporting parting beads are contacted with the bottom surface of the molybdenum boat to form local contact, rather than the whole upper surface of the upper supporting cushion block is contacted with the bottom surface of the molybdenum boat, so that the contact area between the supporting cushion block and the molybdenum boat can be greatly reduced, the supporting strength can be ensured, and the phenomenon of adhesion between the upper supporting cushion block and the molybdenum boat caused by thermal deformation in the repeated high-temperature evaporation process can be avoided; the plurality of strip-shaped grooves are arranged into groove-shaped structures which are not directly communicated with the bottom ends of the upper supporting cushion blocks, so that heat can be ensured to circulate in the strip-shaped grooves, and heat loss is effectively reduced;
in addition, the upper supporting cushion block adopts fusion casting alpha-Al2O3The refractory brick is cut and polished to be made, the texture structure of the refractory material is compact, the refractoriness and high-temperature structural strength are high, and the high-temperature chemical stability is good, so that the upper supporting cushion block made of the material is not easy to generate thermal deformation and evaporation after repeated high-temperature heating, and cannot become impurity particles of an evaporation target material after high-temperature evaporation, and the purity of the evaporation target material for forming steam molecules can be ensured.
And all set up supporting pad and molybdenum boat to the independent square structure of mutual matching, and arrange the molybdenum boat interval, so design, can conveniently get alone and put molybdenum boat and supporting pad, damage or when needing to be changed when certain molybdenum boat or supporting pad, just can change alone, and need not whole changes, convenient nimble use.
The method provided by the invention controls the vacuum degree to be 1 x 10 when the vacuum is extracted from the evaporation chamber-1Pa～2.5×100Pa, because when the degree of vacuum is 2.5X 100When the pressure is higher than Pa, the surface of a vapor deposition film can be blackened or yellowed, the effect of a final finished product is influenced, and a zinc sulfide metal film formed by vapor deposition is not firm enough because a small amount of air molecules exist in a vapor deposition chamber, so that high-temperature zinc sulfide vapor molecules collide with the small amount of air molecules in the upward flying process, the firmness of the formed zinc sulfide metal film is influenced finally, and the problem of blackening and yellowing after oxidation also exists because of the small amount of air molecules; the vacuum degree is not required to be too low, so that good evaporation effect can be achieved, and particularly when the vacuum degree is lower than 1 multiplied by 10-1After Pa, just can increase whole cooling system's operation burden greatly, cause the damage problem of the long-time operation in-process of system, in addition, because install the needle valve that can carry out accurate regulation and control to vacuum on this coiling evaporation plating equipment's the evaporation plating chamber, the installation of this needle valve can be adjusted traditional indoor vacuum of evaporation plating to its next order of magnitude within range, this is the effect that traditional vacuum evaporation plating industry can't reach, after the vacuum degree carries out more accurate regulation and control, can regulate and control the evaporation plating after, can regulate and control the evaporation platingThe gorgeous degree that dazzles various reflective membrane and the width of the seven various strips that form that finally appear simultaneously effectively stop the blackish yellow problem of membrane face, just so can realize according to different customer's demand, will dazzle various reflective membrane and regulate and control to different gorgeous degrees, adjust into the seven various strips of different widths simultaneously.
When the power supply of the evaporation tank is switched on for heating evaporation operation, the temperature is uniformly and slowly increased to 1400 ℃ within 5min, and the temperature is kept for 2min after the temperature is increased to 1400 ℃, so that the operation can ensure that all parts of the target can be uniformly increased, and meanwhile, the target can be fully evaporated by keeping the temperature for 2min after the evaporation temperature is reached, thereby achieving the purpose of full evaporation.
In conclusion, according to the method for preparing the colorful reflective film by the vacuum evaporation process, the finally obtained reflective colorful film is transparent in surface and suitable for deep processing in the later period, and meanwhile, the metal film is firm and is not easy to fall off, and in a dim environment, a colorful effect can be generated after illumination.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
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 (8)

1. A method for preparing a colorful reflective film by a vacuum evaporation process is characterized by comprising the following steps: the method comprises the following steps:
(1) loading the plated plant base film on two winding and unwinding rollers in a winding chamber of high vacuum coating equipment, winding the plated plant base film on the other winding and unwinding roller from one winding and unwinding roller through a central main drum, starting a forced refrigeration system and connecting a gas circuit;
(2) placing a plurality of molybdenum boats in which evaporation target materials are closely arranged in an evaporation tank of high vacuum coating equipment, ensuring that the distances from each part of evaporation target materials to the bottom end of a central main drum are different, and then connecting two electrode ends of each molybdenum boat with copper column electrodes of the evaporation tank; the evaporation target material is a zinc sulfide target material, the evaporation target material is a cylindrical structure, the evaporation target material is vertically arranged and then closely arranged on a molybdenum boat, and evaporation top surfaces formed by a plurality of rows of the arranged evaporation target materials are arc-shaped evaporation surfaces with different heights;
(3) the evaporation tank is conveyed into an evaporation chamber after a cover plate is closed, a cabin door is closed to ensure that the evaporation chamber is in a closed state, and then a vacuum extraction device is started to extract vacuum to the evaporation chamber;
(4) switching on a power supply of the evaporation tank, heating the evaporation target material to a melting point, vaporizing the evaporation target material, and opening a cover plate of the evaporation tank;
(5) starting a winding system, entering a normal evaporation state, then controlling the plant base film to be plated to move at a constant speed in an evaporation chamber, and carrying out gradual evaporation operation;
(6) and after the evaporation is finished, closing the winding system, closing the power supply of the evaporation tank, closing the vacuum extraction equipment, returning the temperature, balancing the atmospheric pressure, and opening the chamber.
2. The method for preparing the multicolor reflecting film by the vacuum evaporation process according to claim 1, which is characterized in that: the distance from the evaporation target to the surface of the plant base film to be plated at the bottom end of the central main drum is controlled to be 13.5 cm-15.5 cm.
3. The method for preparing the multicolor reflecting film by the vacuum evaporation process according to claim 2, which is characterized in that: molybdenum boat for holding evaporation target materialThe bottom end of the device is sequentially provided with an upper supporting cushion block and a lower supporting cushion block, and the upper supporting cushion block is square fusion casting alpha-Al matched with the molybdenum boat in size2O3Resistant firebrick, a plurality of bar grooves have been seted up to even equidistant the supporting pad top, adjacent two be formed with the support parting bead that a plurality of widths far are less than the bar groove width between the bar groove.
4. The method for preparing the multicolor reflecting film by the vacuum evaporation process according to claim 2, which is characterized in that: the molybdenum boat is the square structure that forms by the concatenation of a plurality of molybdenum strip end to end, and adjacent two be formed with the bar gap between the molybdenum strip, two electrode terminals of molybdenum boat are for being located the end part of the molybdenum strip outside extension of molybdenum boat both sides, just the both sides outward flange bending type of molybdenum strip width direction is formed with first flange, the both sides outward flange of molybdenum strip length direction is pegged graft and is had one row of carborundum post, forms the second flange, adjacent two the interval is less than the evaporation coating target external diameter between the carborundum post.
5. The method for preparing the multicolor reflecting film by the vacuum evaporation process according to claim 1, which is characterized in that: the needle valve is hermetically arranged on the side wall of the evaporation chamber, and in the step (3), when the vacuumizing operation is carried out, the vacuum pump set is firstly used for vacuumizing to 2.5 multiplied by 100Pa～1×10-1Pa, then utilizing a needle valve to accurately regulate and control the vacuum degree in the evaporation chamber in the evaporation process, and regulating the vacuum degree to 2.50 multiplied by 10 according to the final effect of an evaporation product0Pa～1.0×10-1Pa in the exact range.
6. The method for preparing the multicolor reflecting film by the vacuum evaporation process according to claim 1, which is characterized in that: when the evaporation target material is heated in the step (4), the temperature is uniformly and slowly increased to 1400 ℃ within 5min, the temperature is kept for 2min after the temperature is increased to 1400 ℃, and then the winding system is started to enter a normal evaporation state.
7. The method for preparing the multicolor reflecting film by the vacuum evaporation process according to claim 1, which is characterized in that: after the winding system is started in the step (5), the winding speed is kept at 48-65 m/min, the uniform winding is carried out, and the film coating effect is observed in real time through an observation window to adjust the winding speed.
8. The method for preparing the multicolor reflecting film by the vacuum evaporation process according to claim 1, which is characterized in that: after the central main drum is cooled by a forced cooling system, the temperature of the central main drum is kept between minus 20 ℃ and minus 10 ℃.
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