CN109468591A - A kind of method that vacuum evaporation process prepares illusion-colour reflective membrane - Google Patents
A kind of method that vacuum evaporation process prepares illusion-colour reflective membrane Download PDFInfo
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- CN109468591A CN109468591A CN201910021948.8A CN201910021948A CN109468591A CN 109468591 A CN109468591 A CN 109468591A CN 201910021948 A CN201910021948 A CN 201910021948A CN 109468591 A CN109468591 A CN 109468591A
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- molybdenum
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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
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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
- C23C14/0623—Sulfides, selenides or tellurides
- C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
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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
- C23C14/24—Vacuum evaporation
- C23C14/243—Crucibles for source material
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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
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of methods that vacuum evaporation process prepares illusion-colour reflective membrane, plated plant basement membrane is packed into deposited chamber, then main drum carries out sub-cooled, is put into the molybdenum boat for being arranged with vapor deposition target in evaporator tank, and guarantee that every part vapor deposition target is variant to the distance of the center bottom end Zhu Gu, it is sent into deposited chamber after evaporator tank is closed cover board, vacuum is extracted to deposited chamber；Vapor deposition target is heated to fusing point, vaporization, opens evaporation tank cover plate, controls plated movement of the plant basement membrane in deposited chamber at the uniform velocity, carries out gradually vapor deposition operation；Pass hull closure after the completion of vapor deposition.Not only surface is transparent for the finally obtained reflective colorful film of method provided by the invention, is suitble to later period deep processing processing, while metal film is securely not easily to fall off, and in dim environment, after encountering illumination, can generate the color effect of color seven.
Description
Technical field
The present invention relates to reflective technical field of membrane, method that specially a kind of vacuum evaporation process prepares illusion-colour reflective membrane.
Background technique
The manufacture craft of common reflective bead planted film is general are as follows: first on PET the or PE film of gluing, by the glass of different-grain diameter
Pearl adheres to it, while generally using refractive index for 1.90~1.93 glass microballoon, the then reflection to enhance reflective membrane
Effect, generally can be in plant film surface by vacuum evaporation layer of metal film, and metal film mostly uses greatly aluminium film, but common aluminium
The film surface that film will cause reflective membrane is nontransparent, and the later period is difficult to be used as semi-finished product, needs to be processed into dazzling for other colors according to client
Color reflectorized material product, is usually to utilize two or more with different refractive index further for common rainbow film
Transparent thermoplastic resin's (refraction index at least differs 0.03) combines to form at least 30 through ABABAB..... or ABCABCABC...
Layer or more uniform parallel alternating sandwich layer, it is this not high using the rainbow film strength of multi-layer resinous formation, and its reflective function
Difference, the process is more complicated for simultaneous processing.Furthermore common transparent dielectric film be by zinc sulphide target be directly vaporized on PTE, PP,
On the common plastics film such as OPP film, the deielectric-coating reflecting effect obtained in this way is poor, although and traditional bead planted film reflecting effect of aluminizing
It is good, but be difficult to achieve the effect that transparent.
Summary of the invention
(1) technical solution
To solve the deficiencies in the prior art, the invention provides the following technical scheme: a kind of vacuum evaporation process prepares illusion-colour
The method of reflective membrane, includes the following steps:
(1) on the indoor two folding and unfolding windings up roller of the winding plated plant basement membrane being fitted into a high vacuum coating equipment,
Plated plant basement membrane is allowed, through the main drum in center, to be wound from one of folding and unfolding winding up roller onto another folding and unfolding winding up roller, starting is forced
Refrigeration system connects gas circuit；
(2) it is put into multiple molybdenum boats for being closely arranged with vapor deposition target in the evaporator tank of high vacuum coating equipment, and guarantees
The distance of every part vapor deposition target to the center bottom end Zhu Gu is variant, then by the copper post of two electrode tips and evaporator tank of molybdenum boat
Electrode is connected；
(3) it is sent into deposited chamber after above-mentioned evaporator tank being closed cover board, and closes hatch door, guarantees that deposited chamber is in sealed shape
State is then turned on extraction vacuum equipment, extracts vacuum to deposited chamber；
(4) evaporator tank power supply is connected, vapor deposition target is heated to fusing point, vaporization, opens evaporation tank cover plate；
(5) reel system is started, into normal evaporation state, then controls plated plant basement membrane in deposited chamber at the uniform velocity
Movement, carry out gradually vapor deposition operation；
(6) after the completion of being deposited, reel system is closed, evaporator tank power supply is turned off, finally closed and extract vacuum equipment, rise again, put down
Weigh atmospheric pressure, opens the cabin.
Preferably, the vapor deposition target specifically uses zinc sulphide target.
Preferably, the vapor deposition target is specially cylindrical structure, and the vapor deposition target stand up after be arranged closely in molybdenum
On boat, the evaporation top surface that multiple rows of vapor deposition target after placement is formed is arc and just different evaporating surfaces.
Preferably, the vapor deposition target exists to the distance controlling for being located at the plated plant membrane surface in the bottom end center Zhu Gu
13.5cm~15.5cm.
Preferably, in the molybdenum boat bottom end for holding vapor deposition target, successively supporting pad is placed with upper lip block and lower lip block,
And the upper lip block is the rectangular founding α-Al to match with molybdenum boat size2O3Refractory brick, the supporting pad top uniformly etc.
Spacing offers multiple strip grooves, and multiple width are formed between the two neighboring strip groove much smaller than bar shaped groove width
Support parting bead.
Preferably, the molybdenum boat is the square structure being spliced that joined end to end by multiple molybdenum items, and two neighboring described
Strip crevice is formed between molybdenum item, two electrode tips of the molybdenum boat are positioned at the outwardly extending end of molybdenum item of molybdenum boat two sides
Part, and the two sides outer edge of the molybdenum width direction has been bent to form the first rib, the two sides of the molybdenum length direction
Outer edge is plugged with row carbonization silicon column, forms the second rib, spacing is less than evaporation targets between adjacent two carbonization silicon columns
Material outer diameter.
Preferably, needle-valve is sealed and installed on deposited chamber side wall, above-mentioned steps (3) are first when carrying out vacuum pumping
2.5 × 10 are evacuated to first with vacuum pump group0Pa~1 × 10-1Then Pa utilizes needle-valve in deposited chamber during vapor deposition
Vacuum degree carries out accuracy controlling, adjusts vacuum degree to 2.50 × 10 according to evaporation product final effect0Pa~1.0 × 10-1Pa's
In exact extension.
Preferably, it when above-mentioned steps (4) carry out heating heating to vapor deposition target, is primarily remain in 5min uniformly slowly
1400 DEG C are warming up to, heat preservation 2min is needed after temperature rises to 1400 DEG C, then restarts reel system, into normal vapor deposition
State.
Preferably, after above-mentioned steps (5) start reel system, winding speed should be kept in 48m/min~65m/min,
It is at the uniform velocity wound, and the adjusting that coating effects are wound speed is observed by watch window in real time.
Preferably, in the main drum in the center after forcing cooling system cooling, temperature is maintained at -20 DEG C~-10 DEG C.
(2) beneficial effect
The present invention provides a kind of method that vacuum evaporation process prepares illusion-colour reflective membrane, have it is following the utility model has the advantages that
This kind of colorful film uses zinc sulphide materials for target, be due to zinc sulphide refractive index be 2.35, transparency range exists
400-13000nm has good stress and good environment durability, and zinc sulphide easily distils in high temperature evaporation, this
Outer zinc sulphide plated film itself had both had metal film to the strong reflection effect of light, while its transparency is also preferable, therefore manufactured unreal
Color film itself has no color, facilitates as semi-finished product, the later period needs to be made the product of various colors according to client；For example, can be with
It is processed into the anti-fake material of assorted dress ornament, shoes packet and high-quality as needed, is dress ornament or shoes packet itself on daytime
Color, have no apparent seven color effect, in night dim environment, encounter direct light photograph, apparent seven color effects will occur
Fruit.
The key technology of the technique is, should guarantee that plated plant membrane surface agglomerates the ZnS-film thickness to be formed as far as possible
Unevenness, difference in thickness value is in 1%-10% nm, because the zinc sulphide plated film of each different location may be considered a bead
Face, thick middle, thin edge, so the a-circle-by-a-circle local thickness around zinc sulphide plating film edge is approximately equal, that is,
Say that the optical path difference generated is equal, so same coloured light will be interfered in this circle, the light interfered is being irradiated to people
In the eyes it is exactly chromatic pattern, should is red, orange, yellow, green, indigo, azure, purple from the zinc sulphide plating extrorse coloured light of center membrane, because of thick middle
Degree is big, so the wavelength of colourama is longer, will form colored phenomenon；
To guarantee that plated plant membrane surface agglomerates the ZnS-film uneven thickness to be formed, therefore it should ensure that every part vapor deposition
The distance of target to the center bottom end Zhu Gu is variant, by setting cylindrical structure for target 11, while will be tight after its cube
Solid matter is listed on molybdenum boat, and the arc formed at this time and just different evaporating surfaces can effectively increase the evaporating surface of target, thus
Improve vapor deposition efficiency, additionally it is possible to guarantee every part target in evaporation, the distance between plated plant base film surface is different, therefore
The time that plant film surface is reached after the target distillation of various pieces is different, so eventually realizing that plant film surface agglomerates the sulphur to be formed
Change zinc non-uniform film thickness, and then achievees the effect that colorful film.
The present invention as vessel holds zinc sulphide target using molybdenum boat, be since molybdenum boat itself has corrosion-and high-temp-resistant,
Its fusing point is up to 2620 DEG C, while hardness is larger is unlikely to deform, molybdenum boat, therefore is suitable for being used as zinc sulphide target high temperature deposition to hold
Vessel；Furthermore it is square structure by molybdenum boat whole installation, conveniently disposably can holds multiple zinc sulphide targets, while facilitating shape
At stable support bottom surface；And the structure being spliced that joined end to end by multiple molybdenum items is set by molybdenum boat, it can guarantee in foot
Under the premise of the support bottom surface of enough areas, while multiple molybdenum items being made to be composed in series sufficiently long conductive material, so that guaranteeing should
Molybdenum boat overall resistance is sufficiently large, i.e., after powered up, can generate the calorific value of sufficient amount, guarantees that zinc sulphide target thereon is fast
Speed heating evaporation distillation；The molybdenum boat for loading evaporation target is designed as the multiple square structures being spaced apart, Neng Goubao by the present invention
Card target forms cross-diffusion in evaporation, to guarantee evaporation film surface thickness interval unevenness.
In addition, the second rib that the two sides outer edge grafting of molybdenum length direction is made of the more silicon columns that are carbonized, and guarantee
Spacing is less than vapor deposition target outer diameter between adjacent two carbonizations silicon column, is designed in this way, can utilize the first rib and the second rib
By cube columned zinc sulphide target carry out enclosing, avoid the problem that it falls, and the second rib is designed as being spaced
The carbonization silicon column of setting can effectively reduce outermost molybdenum item compared to the rib structure being relatively directly bent to form using molybdenum item
Conductive area, to guarantee that the conductive area of more molybdenum items is consistent, so that the heating temperature at each position in molybdenum boat bottom surface
Degree is uniformly distributed, and silicon carbide sheet can be avoided conductive problem as high-temperature insulation material, so that heated current edge always
The flowing of molybdenum item.
The present invention opens up multiple strip grooves on upper lip block top, and forms the lesser support parting bead of multiple width,
It when support, is contacted using support parting bead with molybdenum boat bottom surface, formation localized contact, rather than by the entire upper surface of upper lip block
It is contacted with molybdenum boat bottom surface, in this way, the contact area of lip block and molybdenum boat just can be greatly decreased, can be realized and guaranteeing to support
While intensity, avoid because during high temperature deposition repeatedly, due to upper lip block or molybdenum boat generate thermal deformation caused by two
The viscous glutinous phenomenon of person；And multiple strip grooves are arranged to not be connected to the bathtub construction of lip block bottom end directly, can protect in this way
Card heat recycles in strip groove, effectively reduces heat loss；
In addition, upper lip block is used founding α-Al2O3Refractory brick cutting is polished to, the tissue of this kind of refractory material
Compact structure, refractoriness and thermal structure intensity are higher, while stability at elevated temperature is good, therefore on made of this kind of material
Lip block after being repeatedly heated at high temperature repeatedly, is being not easy to produce thermal deformation and Evaporation Phenomenon, therefore will not become evaporation
Target is in high temperature evaporation rear impurity particle, so as to guarantee to evaporate the purity of target formation steam molecule.
And lip block and molybdenum boat are all provided with the independent square structure for being set to and being mutually matched, molybdenum boat is intervally arranged, so
Design conveniently can individually pick and place molybdenum boat and lip block, when a certain molybdenum boat or lip block damage or when needing replacing, just
It can be carried out and be individually replaced, without whole replacements, convenient, flexible use.
Method provided by the invention is when extracting vacuum to deposited chamber, by vacuum degree control 1 × 10-1Pa~2.5 ×
100Pa is because when vacuum degree is 2.5 × 100When Pa or more, it will cause vapor deposition film surface and black or turn to be yellow, influence final finished
Effect, while the zinc sulphide metal film that formation is deposited is also not secured enough, this is because having a small amount of air molecule in deposited chamber, therefore
High temperature vulcanized zinc fume molecule can collide in upward flight course with a small amount of air molecule, final to influence to form vulcanization
The fastness of zinc metal film, while the jaundice that blacks after oxidation can be also deposited because of a small amount of there are problems that for air molecule；And it is true
Reciprocal of duty cycle does not need too low, just can reach good evaporation effect, especially when vacuum degree is lower than 1 × 10-1After Pa, it will increase
The operation burden of big entire cooling system, causes the damage problem during system long-play；Further, since the winding steams
The needle-valve that accuracy controlling can be carried out to vacuum degree is installed, the installation of the needle-valve can will be traditional on the deposited chamber of coating apparatus
Indoor vacuum degree is deposited to be adjusted within the scope of its next order of magnitude, this is the effect that traditional vacuum vapor deposition industry is unable to reach,
After vacuum degree carries out more accuracy controlling, the gorgeous degree that finally presents of colorful reflective membrane and formation after vapor deposition can be regulated and controled
The width of seven colour bars, while effectively preventing the problem of film surface nigrescence is turned to be yellow, it is just able to achieve the demand according to different clients in this way, it will
Colorful reflective membrane regulates and controls to different gorgeous degree, while being adjusted to seven colour bars of different in width.
When the present invention connects the progress heating evaporation operation of evaporator tank power supply, it is primarily remain in 5min and is uniformly to slowly warm up to
1400 DEG C, heat preservation 2min is needed after temperature rises to 1400 DEG C, so operation both can guarantee that target each section can uniformly heat up,
Simultaneously when reach evaporating temperature after heat preservation 2min operation, can guarantee the abundant evaporation of target, be sufficiently deposited to reach
Purpose.
In conclusion the method that vacuum evaporation process provided by the invention prepares illusion-colour reflective membrane, finally obtained reflective
Not only surface is transparent for colorful film, is suitble to later period deep processing processing, while metal film is securely not easily to fall off, and in dim environment,
After encountering illumination, the color effect of color seven can be generated.
Detailed description of the invention
Fig. 1 is present invention vapor deposition process schematic；
Fig. 2 is the evaporator tank schematic diagram of internal structure that the present invention does not put target；
Fig. 3 is molybdenum boat overlooking structure diagram of the invention；
Fig. 4 is that the present invention is booked molybdenum boat overlooking structure diagram after target；
Fig. 5 is target arrangement architecture schematic diagram of the invention；
Fig. 6 is upper lip block structural schematic diagram of the invention；
Fig. 7 is the arrangement schematic diagram of lower lip block of the invention, upper lip block and molybdenum boat.
In figure: main drum 1, evaporator tank 2, plant basement membrane 3, copper sheet 4, molybdenum boat 5, cover board 6, molybdenum boat electrode tip 7, strip crevice 8,
Molybdenum item 9, carbonization silicon column 10, target 11, evaporation top surface 12, strip groove 13, support parting bead 14, upper lip block 15, lower supporting pad
Block 16, copper post electrode 17.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
A kind of method that vacuum evaporation process prepares illusion-colour reflective membrane, includes the following steps:
(1) on the indoor two folding and unfolding windings up roller of the winding plated plant basement membrane being fitted into a high vacuum coating equipment,
Plated plant basement membrane is allowed, through the main drum in center, to be wound from one of folding and unfolding winding up roller onto another folding and unfolding winding up roller, starting is forced
Refrigeration system, connect gas circuit, by main drum be cooled to -20 DEG C it is spare；
(2) multiple molybdenum boats for being closely arranged with zinc sulphide target are put into the evaporator tank of high vacuum coating equipment, wherein
Zinc sulphide target is cylindrical structure, and target stand up after be arranged closely on molybdenum boat, the steaming that multiple rows of target after placement is formed
It sends out top surface and is arc and just different evaporating surfaces, successively supporting pad puts lip block in the molybdenum boat bottom end for holding vapor deposition target
With lower lip block, and upper lip block is the rectangular founding α-Al to match with molybdenum boat size2O3Refractory brick, supporting pad top
Multiple strip grooves are uniformly opened up at equal intervals, and the branch that multiple width are much smaller than bar shaped groove width is formed between two neighboring strip groove
Parting bead is supportted, is supported on molybdenum boat bottom surface using support parting bead；It is supported using the lip block of proper height, it is final to guarantee vulcanization
Zinc target is 13.5cm to being located at the bottom end center Zhu Gu to be plated the distance of plant membrane surface；Then by two electrode tips of molybdenum boat
It is connected by copper sheet with the copper post electrode of evaporator tank；
(3) deposited chamber is sent into after above-mentioned evaporator tank being closed cover board, wherein is sealed and installed with needle in advance on deposited chamber side wall
Valve, and hatch door is closed, guarantee that deposited chamber is in air-tight state, is evacuated to 1 × 10 first with vacuum pump group-1Then Pa exists
Accuracy controlling is carried out to vacuum degree in deposited chamber using needle-valve during vapor deposition, according to evaporation product final effect, by vacuum degree
It is adjusted in the exact extension of its next order of magnitude；
(4) evaporator tank power supply is connected, is primarily remain in 5min and is uniformly to slowly warm up to 1400 DEG C, when temperature rises to
Heat preservation 2min is needed after 1400 DEG C, so that vapor deposition target is heated to fusing point, vaporization, opens evaporation tank cover plate；
(5) reel system is started, into normal evaporation state, holding winding speed is 48m/min, and is at the uniform velocity rolled up
Around then observing the adjusting that coating effects are wound speed in real time by watch window, carry out gradually vapor deposition operation；
(6) after the completion of being deposited, reel system is closed, evaporator tank power supply is turned off, finally closed and extract vacuum equipment, rise again, put down
Weigh atmospheric pressure, opens the cabin.
Wherein, molybdenum boat is preferably joined end to end the square structure being spliced by multiple molybdenum items, and two neighboring molybdenum item it
Between be formed with strip crevice, two electrode tips of molybdenum boat are the outwardly extending end portion of molybdenum item positioned at molybdenum boat two sides, and molybdenum
The two sides outer edge of width direction has been bent to form the first rib, and the two sides outer edge of molybdenum length direction is plugged with row's carbon
SiClx column forms the second rib, and spacing is less than vapor deposition target outer diameter between adjacent two carbonizations silicon column.
Embodiment 2
A kind of method that vacuum evaporation process prepares illusion-colour reflective membrane, includes the following steps:
(1) on the indoor two folding and unfolding windings up roller of the winding plated plant basement membrane being fitted into a high vacuum coating equipment,
Plated plant basement membrane is allowed, through the main drum in center, to be wound from one of folding and unfolding winding up roller onto another folding and unfolding winding up roller, starting is forced
Refrigeration system, connect gas circuit, by main drum be cooled to -16 DEG C it is spare；
(2) multiple molybdenum boats for being closely arranged with zinc sulphide target are put into the evaporator tank of high vacuum coating equipment, wherein
Zinc sulphide target is cylindrical structure, and target stand up after be arranged closely on molybdenum boat, the steaming that multiple rows of target after placement is formed
It sends out top surface and is arc and just different evaporating surfaces, successively supporting pad puts lip block in the molybdenum boat bottom end for holding vapor deposition target
With lower lip block, and upper lip block is the rectangular founding α-Al to match with molybdenum boat size2O3Refractory brick, supporting pad top
Multiple strip grooves are uniformly opened up at equal intervals, and the branch that multiple width are much smaller than bar shaped groove width is formed between two neighboring strip groove
Parting bead is supportted, is supported on molybdenum boat bottom surface using support parting bead；It is supported using the lip block of proper height, it is final to guarantee vulcanization
Zinc target is 14.2cm to being located at the bottom end center Zhu Gu to be plated the distance of plant membrane surface；Then by two electrode tips of molybdenum boat
It is connected by copper sheet with the copper post electrode of evaporator tank；
(3) deposited chamber is sent into after above-mentioned evaporator tank being closed cover board, wherein is sealed and installed with needle in advance on deposited chamber side wall
Valve, and hatch door is closed, guarantee that deposited chamber is in air-tight state, is evacuated to 9 × 10 first with vacuum pump group-1Then Pa exists
Accuracy controlling is carried out to vacuum degree in deposited chamber using needle-valve during vapor deposition, according to evaporation product final effect, by vacuum degree
It is adjusted in the exact extension of its next order of magnitude；
(4) evaporator tank power supply is connected, is primarily remain in 5min and is uniformly to slowly warm up to 1400 DEG C, when temperature rises to
Heat preservation 2min is needed after 1400 DEG C, so that vapor deposition target is heated to fusing point, vaporization, opens evaporation tank cover plate；
(5) reel system is started, into normal evaporation state, holding winding speed is 54m/min, and is at the uniform velocity rolled up
Around then observing the adjusting that coating effects are wound speed in real time by watch window, carry out gradually vapor deposition operation；
(6) after the completion of being deposited, reel system is closed, evaporator tank power supply is turned off, finally closed and extract vacuum equipment, rise again, put down
Weigh atmospheric pressure, opens the cabin.
Wherein, molybdenum boat is preferably joined end to end the square structure being spliced by multiple molybdenum items, and two neighboring molybdenum item it
Between be formed with strip crevice, two electrode tips of molybdenum boat are the outwardly extending end portion of molybdenum item positioned at molybdenum boat two sides, and molybdenum
The two sides outer edge of width direction has been bent to form the first rib, and the two sides outer edge of molybdenum length direction is plugged with row's carbon
SiClx column forms the second rib, and spacing is less than vapor deposition target outer diameter between adjacent two carbonizations silicon column.
Embodiment 3
A kind of method that vacuum evaporation process prepares illusion-colour reflective membrane, includes the following steps:
(1) on the indoor two folding and unfolding windings up roller of the winding plated plant basement membrane being fitted into a high vacuum coating equipment,
Plated plant basement membrane is allowed, through the main drum in center, to be wound from one of folding and unfolding winding up roller onto another folding and unfolding winding up roller, starting is forced
Refrigeration system, connect gas circuit, by main drum be cooled to -13 DEG C it is spare；
(2) multiple molybdenum boats for being closely arranged with zinc sulphide target are put into the evaporator tank of high vacuum coating equipment, wherein
Zinc sulphide target is cylindrical structure, and target stand up after be arranged closely on molybdenum boat, the steaming that multiple rows of target after placement is formed
It sends out top surface and is arc and just different evaporating surfaces, successively supporting pad puts lip block in the molybdenum boat bottom end for holding vapor deposition target
With lower lip block, and upper lip block is the rectangular founding α-Al to match with molybdenum boat size2O3Refractory brick, supporting pad top
Multiple strip grooves are uniformly opened up at equal intervals, and the branch that multiple width are much smaller than bar shaped groove width is formed between two neighboring strip groove
Parting bead is supportted, is supported on molybdenum boat bottom surface using support parting bead；It is supported using the lip block of proper height, it is final to guarantee vulcanization
Zinc target is 14.8cm to being located at the bottom end center Zhu Gu to be plated the distance of plant membrane surface；Then by two electrode tips of molybdenum boat
It is connected by copper sheet with the copper post electrode of evaporator tank；
(3) deposited chamber is sent into after above-mentioned evaporator tank being closed cover board, wherein is sealed and installed with needle in advance on deposited chamber side wall
Valve, and hatch door is closed, guarantee that deposited chamber is in air-tight state, is evacuated to 1.7 × 10 first with vacuum pump group0Pa, then
Accuracy controlling is carried out to vacuum degree in deposited chamber using needle-valve during vapor deposition, according to evaporation product final effect, by vacuum
Degree is adjusted in the exact extension of its next order of magnitude；
(4) evaporator tank power supply is connected, is primarily remain in 5min and is uniformly to slowly warm up to 1400 DEG C, when temperature rises to
Heat preservation 2min is needed after 1400 DEG C, so that vapor deposition target is heated to fusing point, vaporization, opens evaporation tank cover plate；
(5) reel system is started, into normal evaporation state, holding winding speed is 60m/min, and is at the uniform velocity rolled up
Around then observing the adjusting that coating effects are wound speed in real time by watch window, carry out gradually vapor deposition operation；
(6) after the completion of being deposited, reel system is closed, evaporator tank power supply is turned off, finally closed and extract vacuum equipment, rise again, put down
Weigh atmospheric pressure, opens the cabin.
Wherein, molybdenum boat is preferably joined end to end the square structure being spliced by multiple molybdenum items, and two neighboring molybdenum item it
Between be formed with strip crevice, two electrode tips of molybdenum boat are the outwardly extending end portion of molybdenum item positioned at molybdenum boat two sides, and molybdenum
The two sides outer edge of width direction has been bent to form the first rib, and the two sides outer edge of molybdenum length direction is plugged with row's carbon
SiClx column forms the second rib, and spacing is less than vapor deposition target outer diameter between adjacent two carbonizations silicon column.
Embodiment 4
A kind of method that vacuum evaporation process prepares illusion-colour reflective membrane, includes the following steps:
(1) on the indoor two folding and unfolding windings up roller of the winding plated plant basement membrane being fitted into a high vacuum coating equipment,
Plated plant basement membrane is allowed, through the main drum in center, to be wound from one of folding and unfolding winding up roller onto another folding and unfolding winding up roller, starting is forced
Refrigeration system, connect gas circuit, by main drum be cooled to -10 DEG C it is spare；
(2) multiple molybdenum boats for being closely arranged with zinc sulphide target are put into the evaporator tank of high vacuum coating equipment, wherein
Zinc sulphide target is cylindrical structure, and target stand up after be arranged closely on molybdenum boat, the steaming that multiple rows of target after placement is formed
It sends out top surface and is arc and just different evaporating surfaces, successively supporting pad puts lip block in the molybdenum boat bottom end for holding vapor deposition target
With lower lip block, and upper lip block is the rectangular founding α-Al to match with molybdenum boat size2O3Refractory brick, supporting pad top
Multiple strip grooves are uniformly opened up at equal intervals, and the branch that multiple width are much smaller than bar shaped groove width is formed between two neighboring strip groove
Parting bead is supportted, is supported on molybdenum boat bottom surface using support parting bead；It is supported using the lip block of proper height, it is final to guarantee vulcanization
Zinc target is 15.5cm to being located at the bottom end center Zhu Gu to be plated the distance of plant membrane surface；Then by two electrode tips of molybdenum boat
It is connected by copper sheet with the copper post electrode of evaporator tank；
(3) deposited chamber is sent into after above-mentioned evaporator tank being closed cover board, wherein is sealed and installed with needle in advance on deposited chamber side wall
Valve, and hatch door is closed, guarantee that deposited chamber is in air-tight state, is evacuated to 2.5 × 10 first with vacuum pump group0Pa, then
Accuracy controlling is carried out to vacuum degree in deposited chamber using needle-valve during vapor deposition, according to evaporation product final effect, by vacuum
Degree is adjusted in the exact extension of its next order of magnitude；
(4) evaporator tank power supply is connected, is primarily remain in 5min and is uniformly to slowly warm up to 1400 DEG C, when temperature rises to
Heat preservation 2min is needed after 1400 DEG C, so that vapor deposition target is heated to fusing point, vaporization, opens evaporation tank cover plate；
(5) reel system is started, into normal evaporation state, holding winding speed is 65m/min, and is at the uniform velocity rolled up
Around then observing the adjusting that coating effects are wound speed in real time by watch window, carry out gradually vapor deposition operation；
(6) after the completion of being deposited, reel system is closed, evaporator tank power supply is turned off, finally closed and extract vacuum equipment, rise again, put down
Weigh atmospheric pressure, opens the cabin.
Wherein, molybdenum boat is preferably joined end to end the square structure being spliced by multiple molybdenum items, and two neighboring molybdenum item it
Between be formed with strip crevice, two electrode tips of molybdenum boat are the outwardly extending end portion of molybdenum item positioned at molybdenum boat two sides, and molybdenum
The two sides outer edge of width direction has been bent to form the first rib, and the two sides outer edge of molybdenum length direction is plugged with row's carbon
SiClx column forms the second rib, and spacing is less than vapor deposition target outer diameter between adjacent two carbonizations silicon column.
This kind of colorful film uses zinc sulphide materials for target, be due to zinc sulphide refractive index be 2.35, transparency range exists
400-13000nm has good stress and good environment durability, and zinc sulphide easily distils in high temperature evaporation, this
Outer zinc sulphide plated film itself had both had metal film to the strong reflection effect of light, while its transparency is also preferable, therefore manufactured unreal
Color film itself has no color, facilitates as semi-finished product, the later period needs to be made the product of various colors according to client；For example, can be with
It is processed into assorted dress ornament perhaps its color on daytime for dress ornament or shoes packet of shoes packet itself as needed, has no apparent
Seven color effects encounter direct light photograph, apparent seven color effect will occur in night dim environment.
The key technology of the technique is, should guarantee that plated plant membrane surface agglomerates the ZnS-film thickness to be formed as far as possible
Unevenness, because the zinc sulphide plated film of each different location may be considered a small sphere of exterior rearview, thick middle, thin edge, so surrounding
Zinc sulphide plating film edge a-circle-by-a-circle local thickness it is approximately equal, the optical path difference that is generated is equal, so together
A kind of coloured light will be interfered in this circle, and the light interfered is exactly chromatic pattern in human eye being irradiated to, from zinc sulphide
Plating the extrorse coloured light of center membrane should be red, orange, yellow, green, indigo, azure, purple, because interior thickness is big, the wavelength of colourama is longer,
Colored phenomenon will be formed；
To guarantee that plated plant membrane surface agglomerates the ZnS-film uneven thickness to be formed, therefore it should ensure that every part vapor deposition
The distance of target to the center bottom end Zhu Gu is variant, by setting cylindrical structure for target 11, while will be tight after its cube
Solid matter is listed on molybdenum boat, and the arc formed at this time and just different evaporating surfaces can effectively increase the evaporating surface of target, thus
Improve vapor deposition efficiency, additionally it is possible to guarantee every part target in evaporation, the distance between plated plant base film surface is different, therefore
The time that plant film surface is reached after the target distillation of various pieces is different, so eventually realizing that plant film surface agglomerates the sulphur to be formed
Change zinc non-uniform film thickness, and then achievees the effect that colorful film.
The present invention as vessel holds zinc sulphide target using molybdenum boat, be since molybdenum boat itself has corrosion-and high-temp-resistant,
Its fusing point is up to 2620 DEG C, while hardness is larger is unlikely to deform, therefore is suitable for being used as zinc sulphide target high temperature deposition holding vessel；
Furthermore by molybdenum boat whole installation be square structure, can conveniently disposably hold multiple zinc sulphide targets, while facilitate to be formed it is flat
Steady support bottom surface；And the structure being spliced that joined end to end by multiple molybdenum items is set by molybdenum boat, it can guarantee in enough faces
Under the premise of long-pending support bottom surface, while multiple molybdenum items being made to be composed in series sufficiently long conductive material, to guarantee the molybdenum boat
Overall resistance is sufficiently large, i.e., after powered up, can generate the calorific value of sufficient amount, guarantees that zinc sulphide target thereon quickly rises
Temperature evaporation distillation；The molybdenum boat for loading evaporation target is designed as the multiple square structures being spaced apart by the present invention, can guarantee target
Material forms cross-diffusion in evaporation, to guarantee evaporation film surface thickness interval unevenness.
In addition, the second rib that the two sides outer edge grafting of molybdenum length direction is made of the more silicon columns that are carbonized, and guarantee
Spacing is less than vapor deposition target outer diameter between adjacent two carbonizations silicon column, is designed in this way, can utilize the first rib and the second rib
By cube columned zinc sulphide target carry out enclosing, avoid the problem that it falls, and the second rib is designed as being spaced
The carbonization silicon column of setting can effectively reduce outermost molybdenum item compared to the rib structure being relatively directly bent to form using molybdenum item
Conductive area, to guarantee that the conductive area of more molybdenum items is consistent, so that the heating temperature at each position in molybdenum boat bottom surface
Degree is uniformly distributed, and silicon carbide sheet can be avoided conductive problem as high-temperature insulation material, so that heated current edge always
The flowing of molybdenum item.
The present invention opens up multiple strip grooves on upper lip block top, and forms the lesser support parting bead of multiple width,
It when support, is contacted using support parting bead with molybdenum boat bottom surface, formation localized contact, rather than by the entire upper surface of upper lip block
It is contacted with molybdenum boat bottom surface, in this way, the contact area of lip block and molybdenum boat just can be greatly decreased, can be realized and guaranteeing to support
While intensity, avoid because during high temperature deposition repeatedly, due to upper lip block or molybdenum boat generate thermal deformation caused by two
The viscous glutinous phenomenon of person；And multiple strip grooves are arranged to not be connected to the bathtub construction of lip block bottom end directly, can protect in this way
Card heat recycles in strip groove, effectively reduces heat loss；
In addition, upper lip block is used founding α-Al2O3Refractory brick cutting is polished to, the tissue of this kind of refractory material
Compact structure, refractoriness and thermal structure intensity are higher, while stability at elevated temperature is good, therefore on made of this kind of material
Lip block after being repeatedly heated at high temperature repeatedly, is being not easy to produce thermal deformation and Evaporation Phenomenon, therefore will not become evaporation
Target is in high temperature evaporation rear impurity particle, so as to guarantee to evaporate the purity of target formation steam molecule.
And lip block and molybdenum boat are all provided with the independent square structure for being set to and being mutually matched, and molybdenum boat is intervally arranged, such as
This design conveniently can individually pick and place molybdenum boat and lip block, when a certain molybdenum boat or lip block damage or when needing replacing,
Just it can be carried out and be individually replaced, without whole replacements, convenient, flexible use.
Method provided by the invention is when extracting vacuum to deposited chamber, by vacuum degree control 1 × 10-1Pa~2.5 ×
100Pa is because when vacuum degree is 2.5 × 100When Pa or more, it will cause vapor deposition film surface and black or turn to be yellow, influence final finished
Effect, while the zinc sulphide metal film that formation is deposited is also not secured enough, this is because having a small amount of air molecule in deposited chamber, therefore
High temperature vulcanized zinc fume molecule can collide in upward flight course with a small amount of air molecule, final to influence to form vulcanization
The fastness of zinc metal film, while the jaundice that blacks after oxidation can be also deposited because of a small amount of there are problems that for air molecule；And it is true
Reciprocal of duty cycle does not need too low, and change can reach good evaporation effect, especially when vacuum degree is lower than 1 × 10-1After Pa, it will increase
The operation burden of big entire cooling system, causes the damage problem during system long-play, further, since the winding steams
The needle-valve that accuracy controlling can be carried out to vacuum degree is installed, the installation of the needle-valve can will be traditional on the deposited chamber of coating apparatus
Indoor vacuum degree is deposited to be adjusted within the scope of its next order of magnitude, this is the effect that traditional vacuum vapor deposition industry is unable to reach,
After vacuum degree carries out more accuracy controlling, the gorgeous degree that finally presents of colorful reflective membrane and formation after vapor deposition can be regulated and controled
The width of seven colour bars, while effectively preventing the problem of film surface nigrescence is turned to be yellow, it is just able to achieve the demand according to different clients in this way, it will
Colorful reflective membrane regulates and controls to different gorgeous degree, while being adjusted to seven colour bars of different in width.
When the present invention connects the progress heating evaporation operation of evaporator tank power supply, it is primarily remain in 5min and is uniformly to slowly warm up to
1400 DEG C, heat preservation 2min is needed after temperature rises to 1400 DEG C, so operation both can guarantee that target each section can uniformly heat up,
Simultaneously when reach evaporating temperature after heat preservation 2min operation, can guarantee the abundant evaporation of target, be sufficiently deposited to reach
Purpose.
To sum up, the method that vacuum evaporation process provided by the invention prepares illusion-colour reflective membrane, finally obtained reflective colorful
Not only surface is transparent for film, is suitble to later period deep processing processing, while metal film is securely not easily to fall off, and in dim environment, encounters
After illumination, the color effect of color seven can be generated.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (10)
1. a kind of method that vacuum evaporation process prepares illusion-colour reflective membrane, characterized by the following steps:
(1) on the indoor two folding and unfolding windings up roller of the winding plated plant basement membrane being fitted into a high vacuum coating equipment, allow by
Plant basement membrane is plated from one of folding and unfolding winding up roller through the main drum in center, winds onto another folding and unfolding winding up roller, starts forced refrigeration
System connects gas circuit；
(2) it is put into multiple molybdenum boats for being closely arranged with vapor deposition target in the evaporator tank of high vacuum coating equipment, and guarantees every portion
Divide the distance of vapor deposition target to the center bottom end Zhu Gu variant, then by two electrode tips of molybdenum boat and the copper post electrode of evaporator tank
It is connected；
(3) it is sent into deposited chamber after above-mentioned evaporator tank being closed cover board, and closes hatch door, guarantees that deposited chamber is in air-tight state, so
It opens afterwards and extracts vacuum equipment, vacuum is extracted to deposited chamber；
(4) evaporator tank power supply is connected, vapor deposition target is heated to fusing point, vaporization, opens evaporation tank cover plate；
(5) reel system is started, into normal evaporation state, then controls plated shifting of the plant basement membrane in deposited chamber at the uniform velocity
It is dynamic, carry out gradually vapor deposition operation；
(6) after the completion of being deposited, reel system is closed, evaporator tank power supply is turned off, finally closed and extract vacuum equipment, rise again, balance is big
Air pressure is opened the cabin.
2. the method that a kind of vacuum evaporation process according to claim 1 prepares illusion-colour reflective membrane, it is characterised in that: described
Vapor deposition target specifically uses zinc sulphide target.
3. the method that a kind of vacuum evaporation process according to claim 2 prepares illusion-colour reflective membrane, it is characterised in that: described
Vapor deposition target is specially cylindrical structure, and the vapor deposition target stand up after be arranged closely on molybdenum boat, multiple rows of steaming after placement
It plates the evaporation top surface that target is formed and is arc and just different evaporating surfaces.
4. the method that a kind of vacuum evaporation process according to any one of claim 1-3 prepares illusion-colour reflective membrane, special
Sign is: the vapor deposition target arrive be located at the distance controlling of the plated plant membrane surface in the bottom end center Zhu Gu 13.5cm~
15.5cm。
5. the method that a kind of vacuum evaporation process according to claim 4 prepares illusion-colour reflective membrane, it is characterised in that: containing
Putting the molybdenum boat bottom end of vapor deposition target, successively supporting pad is placed with lip block and lower lip block, and the upper lip block be with
The rectangular founding α-Al that molybdenum boat size matches2O3Refractory brick, the supporting pad top uniformly offer multiple bar shapeds at equal intervals
Slot is formed with the support parting bead that multiple width are much smaller than bar shaped groove width between the two neighboring strip groove.
6. the method that a kind of vacuum evaporation process according to claim 4 prepares illusion-colour reflective membrane, it is characterised in that: described
Molybdenum boat is the square structure being spliced that joined end to end by multiple molybdenum items, and bar shaped seam is formed between the two neighboring molybdenum item
Gap, two electrode tips of the molybdenum boat are the outwardly extending end portion of molybdenum item positioned at molybdenum boat two sides, and the molybdenum width
The two sides outer edge in direction has been bent to form the first rib, and the two sides outer edge of the molybdenum length direction is plugged with row carbonization
Silicon column forms the second rib, and spacing is less than vapor deposition target outer diameter between adjacent two carbonization silicon columns.
7. the method that a kind of vacuum evaporation process according to any one of claim 1-3 prepares illusion-colour reflective membrane, special
Sign is: needle-valve is sealed and installed on deposited chamber side wall, above-mentioned steps (3) are when carrying out vacuum pumping, first with true
Empty pump group is evacuated to 2.5 × 100Pa~1 × 10-1Pa, then during vapor deposition using needle-valve to vacuum degree in deposited chamber into
Row accuracy controlling adjusts vacuum degree to 2.50 × 10 according to evaporation product final effect0Pa~1.0 × 10-1The exact extension of Pa
It is interior.
8. the method that a kind of vacuum evaporation process according to any one of claim 1-3 prepares illusion-colour reflective membrane, special
Sign is: when above-mentioned steps (4) carry out heating heating to vapor deposition target, being primarily remain in 5min and is uniformly to slowly warm up to
1400 DEG C, heat preservation 2min is needed after temperature rises to 1400 DEG C, then restarts reel system, into normal evaporation state.
9. the method that a kind of vacuum evaporation process according to any one of claim 1-3 prepares illusion-colour reflective membrane, special
Sign is: after above-mentioned steps (5) start reel system, winding speed should be kept in 48m/min~65m/min, carried out at the uniform velocity
Winding, and the adjusting that coating effects are wound speed is observed by watch window in real time.
10. the method that a kind of vacuum evaporation process according to any one of claim 1-3 prepares illusion-colour reflective membrane, special
Sign is: in the main drum in the center after forcing cooling system cooling, temperature is maintained at -20 DEG C~-10 DEG C.
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| CN113564556A (en) * | 2020-04-28 | 2021-10-29 | 合肥市辉耀真空材料有限责任公司 | Method for manufacturing colorful reflective film with blue front surface |
| CN115323329A (en) * | 2022-10-12 | 2022-11-11 | 苏州东杏表面技术有限公司 | Serial-type multifunctional molybdenum boat assembly and evaporation method based on same |
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| CN109468591B (en) | 2020-11-13 |
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