CN110396672A - A kind of ion sputtering film coating method and device for realizing gradient color - Google Patents
A kind of ion sputtering film coating method and device for realizing gradient color Download PDFInfo
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- CN110396672A CN110396672A CN201910841454.4A CN201910841454A CN110396672A CN 110396672 A CN110396672 A CN 110396672A CN 201910841454 A CN201910841454 A CN 201910841454A CN 110396672 A CN110396672 A CN 110396672A
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- target
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- vacuum chamber
- pole target
- pivoted frame
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- 238000004544 sputter deposition Methods 0.000 title claims abstract description 59
- 239000007888 film coating Substances 0.000 title claims abstract description 28
- 238000009501 film coating Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000010410 layer Substances 0.000 claims abstract description 78
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 72
- 239000010936 titanium Substances 0.000 claims abstract description 65
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical group [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 49
- 239000011651 chromium Substances 0.000 claims abstract description 48
- 238000007747 plating Methods 0.000 claims abstract description 25
- 238000004140 cleaning Methods 0.000 claims abstract description 22
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 239000002344 surface layer Substances 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 178
- 229910052786 argon Inorganic materials 0.000 claims description 101
- 239000007789 gas Substances 0.000 claims description 77
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 35
- 239000001301 oxygen Substances 0.000 claims description 35
- 229910052760 oxygen Inorganic materials 0.000 claims description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 13
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000012495 reaction gas Substances 0.000 claims description 7
- 239000013077 target material Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 description 24
- -1 argon ion Chemical class 0.000 description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 20
- 239000004408 titanium dioxide Substances 0.000 description 10
- 230000002000 scavenging effect Effects 0.000 description 9
- 230000005684 electric field Effects 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 8
- 238000010849 ion bombardment Methods 0.000 description 6
- 238000005202 decontamination Methods 0.000 description 5
- 230000003588 decontaminative effect Effects 0.000 description 5
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 4
- HEGVYZJCELUPOJ-UHFFFAOYSA-N [N].[O].[Ti] Chemical group [N].[O].[Ti] HEGVYZJCELUPOJ-UHFFFAOYSA-N 0.000 description 4
- 229910000423 chromium oxide Inorganic materials 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229940097275 indigo Drugs 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- 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
- C23C14/0635—Carbides
-
- 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
- C23C14/0676—Oxynitrides
-
- 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
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3464—Sputtering using more than one target
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/46—Sputtering by ion beam produced by an external ion source
Landscapes
- Chemical & Material Sciences (AREA)
- 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 ion sputtering film coating method and devices for realizing gradient color, and the method steps are as follows: (1) hanging over the direction of workpiece gradient color on demand is flat in vacuum chamber on the hanging rod of pivoted frame;(2) it vacuumizes, makes vacuum degree≤9.0 × 10 of vacuum chamber‑ 3Pa, temperature is up to 150 DEG C;(3) aura bias cleans;(4) Ion Cleaning;(5) plating prime coat;(6) plating middle layer;(7) coating surface layer.Plated film time is 3h-6h, and film thickness is 0.8 μm -2.0 μm, and sputtering environment includes that target current is 15A-25A, bias 80V-120V, duty ratio 30%-70%.The device includes vacuum chamber, driving mechanism is installed on vacuum chamber, first pole target, the second pole target, pivoted frame are installed in vacuum chamber, driving mechanism is connected with pivoted frame, first pole target is located at the outer ring of pivoted frame, and the second pole target is located at the inner ring of pivoted frame, and the first pole target and the second pole target are symmetrically set, first pole target is titanium target, and the second pole target is chromium target.The present invention is able to produce multiple color, and color is more gorgeous, and structure is simple, easy to operate.
Description
Technical field
The present invention relates to ion sputtering film coating technical field, specially a kind of ion sputtering film coating method for realizing gradient color
And device.
Background technique
With the continuous development of science and technology with progress, people are higher and higher to the appearance requirement of electronic product, in order to improve city
Field competitiveness and the more consumers of attraction, make the shell of electronic product have color abundant.Especially mobile phone industry, due to
The continuous development of the communication technology, the shell of mobile phone need to make using steel or the material of more high rigidity;Such as titanium, aluminium material
The surface color processing of material, these materials is realized by ion sputtering film coating.However, in the prior art, using ion sputtering
Coating technique is mainly golden yellow, black, grey, white etc., the face being able to produce in the color for the film layer that surface of shell is formed
Color is relatively simple, it is difficult to meet consumer demand.
Summary of the invention
The present invention is in view of the above-mentioned problems of the prior art, provide a kind of ion sputtering film coating side for realizing gradient color
Method is able to produce multiple color, product lucuriant in design.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of ion sputtering film coating method for realizing gradient color, it is characterised in that: steps are as follows:
(1) in the first pole target and the second pole target are arranged in vacuum chamber, by the direction of workpiece gradient color on demand it is flat hang over it is true
In empty room on the hanging rod of pivoted frame, the door of vacuum chamber is closed, forms closed sputtering space;
(2) vacuum degree≤9.0 × 10 are evacuated to-3Pa, T:150 DEG C of vacuum room temperature≤T≤180 DEG C, setting sputtering
Environment;
(3) aura bias cleans: being powered to the first pole target, carries out aura cleaning to workpiece surface;
(4) Ion Cleaning: it is filled with argon gas to vacuum chamber, while being powered to the first pole target, argon gas is ionized as argon ion, argon
Ion bombardment workpiece surface;
(5) plating prime coat: being filled with argon gas into vacuum chamber, is powered to the first pole target or the second pole target, makes the first pole target
Or the second substance on the target of pole sputters and deposits to workpiece surface and forms metal back layer;
(6) plating middle layer: using argon gas as working gas, using oxygen, nitrogen or acetylene as reaction gas, the first pole target is given
Or second pole target be powered, so that the target material on the first pole target or the second pole target is sputtered and is deposited on the metal back layer and formed
Intermediate coat thick-layer;
(7) using argon gas as working gas, using oxygen as reaction gas, the first pole target or the second pole target coating surface layer: are given
It is powered, sputters the substance on the first pole target or the second pole target and deposits to formation surface color layer on the middle film layer.
It is preferred that first pole target is titanium target, second pole target is chromium target.
It is preferred that ion sputtering film coating with a thickness of 0.8 μm -2.0 μm.
It is preferred that sputtering environment are as follows: target current 15A-25A, bias 80V-120V, duty ratio 30%-
70%.
It is preferred that the argon flow in step (4) Ion Cleaning is 400sccm-500sccm;The step
Suddenly the argon flow in (5) plating prime coat is 80sccm-100sccm;Argon flow in step (6) the plating middle layer
For 80sccm-100sccm, the flow of nitrogen is 50sccm-100sccm, and the flow of acetylene is 40sccm-80sccm, oxygen
Flow 120sccm-180sccm.
It is preferred that the flow of the argon gas in step (7) the coating surface layer is 120sccm-140sccm, oxygen
The flow of gas is 80sccm-150sccm.
Another object of the present invention is to provide a kind of ion sputtering film coating devices for realizing gradient color, and structure is simple, at
This is low.
A kind of ion sputtering film coating device for realizing gradient color, including vacuum chamber are equipped with driving machine on the vacuum chamber
Structure, is equipped with the first pole target, the second pole target, the pivoted frame for hanging workpiece in the vacuum chamber, the driving mechanism and described
Pivoted frame connection, first pole target are located at the outer ring of the pivoted frame, and second pole target is located at the inner ring of the pivoted frame, and described
First pole target and the second pole target are symmetrically set.
It is preferred that first pole target is titanium target, second pole target is chromium target.
It is preferred that the driving mechanism includes motor, the motor is mounted on the vacuum chamber, the motor
Output shaft protrude into the vacuum chamber and be connected with driving gear.
It is preferred that the pivoted frame includes top plate, chassis, several support rods and hanger, the top plate and chassis
It is connect respectively by bogie wheel with the vacuum chamber, several support rods are circumferentially distributed, and the top of every support rod
It is connect with the top plate, the bottom end of every support rod is connect with the chassis, and the top plate periphery is provided with teeth, the top plate
It is engaged by the teeth with the driving gear, the hanger is fixedly connected with the top plate and support rod, on the hanger
It is provided with hanging rod, the direction of workpiece gradient color on demand is flat to be hung on the hanging rod.
Beneficial effects of the present invention:
1. compared with prior art, by selecting titanium target, chromium target, to the flow of reaction gas oxygen, nitrogen or acetylene
It designs, the control to sputtering environment, sputtering time, so that realizing can make workpiece show purple-blue, yellow-red, green-purple, indigo plant-
Green equal multiple colors, so that workpiece is lucuriant in design, and by the way that in vacuum indoor location pivoted frame, pivoted frame is by top plate, chassis, support
Bar, hanger, hanging rod composition, the direction of workpiece gradient color on demand is flat to be hung on hanging rod, and the setting of the first pole target is in pivoted frame outer ring, and the
Two pole targets are arranged in pivoted frame inner ring, and using method of the invention to workpiece sputter coating, structure is simple, easy to operate.
Detailed description of the invention
Fig. 1 is the top view for the ion sputtering film coating device that the present invention realizes gradient color;
Fig. 2 is the partial structure diagram for the ion sputtering film coating device that the present invention realizes gradient color.
In figure: 1- vacuum chamber, 2- pivoted frame, 21- top plate, the chassis 22-, 23- support rod, 24- hanger, 25- hanging rod, 3- electricity
Machine, 31- driving gear, the first pole 41- target, the second pole 42- target, 5- bogie wheel, 6-, 7- workpiece.
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 one
Referring to Fig.1, Fig. 2, a kind of ion sputtering film coating device for realizing gradient color, including vacuum chamber 1 are pacified on vacuum chamber 1
Equipped with driving mechanism, the first pole target 41, the second pole target 42, the pivoted frame 2 for hanging workpiece 7, driving machine are installed in vacuum chamber 1
Structure and pivoted frame 2 connect, and the first pole target 41 is located at the outer ring of pivoted frame 2, and the second pole target 42 is located at the inner ring of pivoted frame 2, and the first pole target
41 and second pole target 42 be symmetrically set.First pole target 41 is titanium target, and the second pole target 42 is chromium target, the first pole target 41 and second
Pole target 42 is made of purity requirement of 99.99% metal.The pivoted frame 2 is arranged in a ring in vacuum chamber.
Referring to Fig. 2, the driving mechanism includes motor 3, and the motor 3 is mounted on vacuum chamber 1.The motor 3 it is defeated
Shaft protrudes into vacuum chamber 1 and is connected with driving gear 31.The pivoted frame 2 includes top plate 21, chassis 22, several support rods 23
And hanger 24, the top plate 21 and chassis 22 are connect by bogie wheel 5 with vacuum chamber 1 respectively, several support rods 23 are circumferentially
Distribution, and the top of every support rod 23 is connect with top plate 21, the bottom end of every support rod 23 is connect with chassis 22.The top plate
21 peripheries are provided with teeth, and top plate 21 is engaged by teeth with driving gear 31.The hanger 24 and top plate 21 and support rod 23
It is fixedly connected, hanging rod 25 is provided on hanger 24.The direction of the workpiece 7 gradient color on demand is flat to be hung on hanger 24.Work
When, motor 3 drives gear 31 to rotate, and driving gear 31 is engaged with top plate 21, drives top plate 21 to rotate, is fixedly connected on top plate 21
It is rotated with the hanger 24 on support rod 23 with top plate 21 and disk 22.When the workpiece 7 on hanger 24 turn to two it is symmetrical
When between the first pole target 41 and the second pole target 42, plated film is carried out to workpiece 7.First pole target 41 is located in 2 outer ring of pivoted frame, the second pole
Target 42 is located at 2 inner ring of pivoted frame, this is not necessarily to combine, can also be 42 location swap of the first pole target 41 and the second pole target.
A kind of ion sputtering film coating method for realizing gradient color based on above-mentioned ion sputtering film coating device, steps are as follows:
(1) in the first pole target and the second pole target are arranged in vacuum chamber, by the direction of workpiece gradient color on demand it is flat hang over it is true
In empty room on the hanger of pivoted frame, the door of vacuum chamber is closed, forms closed sputtering space.First pole target is titanium target, described
Second pole target is chromium target.The titanium target and chromium target are high purity metal, and purity requirement is 99.99% or more.
(2) it vacuumizes: closed vacuum chamber being evacuated using aspiration pump, makes vacuum degree≤9.0 × 10 of vacuum chamber- 3Pa, T:150 DEG C of vacuum room temperature≤T≤180 DEG C, setting sputtering environment.
(3) aura bias cleans: in the case where sputter environment, titanium target being given to be powered, to workpiece surface progress aura cleaning, when cleaning
Between be 20min.
(4) Ion Cleaning: in the case where sputtering environment, being filled with argon gas to vacuum chamber, argon flow 400-500sccm, simultaneously
Titanium target is given to be powered, argon gas is ionized as argon ion, argon ion bombardment workpiece surface, and it is clear further to carry out decontamination to workpiece surface
It is clean, scavenging period 20min.
(5) plating prime coat: in the case where sputtering environment, argon gas is filled with into vacuum chamber, argon flow 80-100sccm gives
Titanium target or chromium target are powered, and sputter the substance on titanium target or chromium target and deposit to workpiece surface formation metal back layer.The metal bottom
Metal in layer is titanium or chromium.
(6) plating middle layer: in the case where sputtering environment, using argon gas as working gas, using oxygen, nitrogen or acetylene as reaction gas
Body, argon flow 80-100sccm, the flow of nitrogen are 50-100sccm, and the flow of acetylene is 40-80sccm.To titanium target or
Chromium target is powered, and sputters the target material on titanium target or chromium target and deposits to formation intermediate coat thick-layer on the metal back layer, should
Intermediate coat thick-layer is nitrogen oxygen titanium layer or nitrogen oxygen layers of chrome.
(7) coating surface layer: in the case where sputtering environment, using argon gas as working gas, using oxygen as reaction gas, the stream of argon gas
Amount is 120sccm-140sccm, and the flow of oxygen is 80sccm-150sccm, is powered to titanium target or chromium target, makes titanium target or chromium target
On substance sputter and deposit on the middle film layer, formed surface color layer, the surface color layer be titanium dioxide or oxygen
Change chromium.
The ion sputtering film coating with a thickness of 0.8 μm -2.0 μm, plated film time 3h-6h.The sputtering environment includes
Target current is 15A-25A, bias 80V-120V, duty ratio 30%-70%.
Ion sputtering film coating method of the invention is further elaborated using specific embodiment below.
Embodiment two
(1) it is provided with titanium target 41 and chromium target 42 in vacuum chamber 1, hangs over hanging rod for the direction of the gradient color on demand of workpiece 7 is flat
On 25, the door 6 of vacuum chamber 1 is closed, closed sputtering space is formed.Wherein titanium target 41 is the first pole target, and chromium target 42 is the second pole
Target.
(2) vacuumize: closed vacuum chamber 1 being evacuated using aspiration pump, make the vacuum degree 9.0 of vacuum chamber 1 ×
10-3Pa, temperature is up to 150 DEG C.
(3) aura bias cleans: opening motor 3, motor 3 drives the workpiece 7 on pivoted frame 2 to rotate, is powered to titanium target 41, titanium
Target current is 15A, and adjusting is biased into 100V, and duty ratio 50% carries out aura cleaning to workpiece surface, and scavenging period is
20min。
(4) Ion Cleaning: motor 3 maintains the workpiece 6 on driving pivoted frame 2 to rotate, and is filled with argon gas, argon gas stream to vacuum chamber 1
Amount is 400sccm, while being powered to titanium target 41.Titanium target electric current is 15A, and adjusting is biased into 100V, duty ratio 50%.Argon gas quilt
Ionization is argon ion, and argon ion bombardment workpiece surface further carries out decontamination cleaning to 7 surface of workpiece, and scavenging period is
20min。
(5) plating prime coat: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and argon gas, argon are filled with into vacuum chamber 1
The flow of gas is 80sccm.It being powered simultaneously to chromium target 42, chromium target current is 20A, it adjusts and is biased into 120V, duty ratio 60%,
Plating times are 10min, sputter the substance on chromium target and deposit to 7 surface of workpiece formation metal back layer, which is
Chromium film layer.
(6) plating middle layer: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and stops being powered to chromium target 42, give simultaneously
Titanium target 41 is powered.Wherein, titanium target electric current is 15A, bias 120V, duty ratio 60%.The gas being filled with into vacuum chamber changes
At nitrogen, oxygen and argon gas.The flow of the nitrogen is 100sccm, and the flow of oxygen is 140sccm, and the flow of argon gas is
80sccm.Argon gas is ionized as argon ion, and argon ion accelerates to fly to cathode target under electric field action, and bombards target table with high-energy
Face sputters target.In sputtering particle, titanium atom reacts to form nitrogen oxygen with oxygen, nitrogen during the motion
Titanium is deposited in chromium film layer, forms intermediate coat thick-layer, which is nitrogen oxygen titanium layer.
(7) coating surface layer: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and continues to be powered to titanium target 41.Wherein,
Titanium target electric current is 20A, bias 125V, duty ratio 50%.The gas being filled with into vacuum chamber 1 changes oxygen, argon gas, oxygen into
Flow be 120sccm, the flow of argon gas is 100sccm.Argon gas is ionized as argon ion, and argon ion accelerates under electric field action
Cathode target is flown to, and target surface is bombarded with high-energy, sputters target.In sputtering particle, titanium atom is in motion process
In react to form titanium dioxide deposition and form surface color layer on nitrogen oxygen titanium layer with oxygen, which is dioxy
Change titanium layer.
In the present embodiment, plated film time 5h, chromium film layer, nitrogen oxygen titanium layer, titanium dioxide layer thickness be respectively 0.8 μ
M, 1.2 μm, 1.8 μm, color are changed from purple to blue.
Embodiment three
(1) it is provided with titanium target 41 and chromium target 42 in vacuum chamber 1, hangs over hanging rod for the direction of the gradient color on demand of workpiece 7 is flat
On 25, the door 6 of vacuum chamber 1 is closed, closed sputtering space is formed.Wherein titanium target 41 is the first pole target, and chromium target 42 is the second pole
Target.
(2) it vacuumizes: closed vacuum chamber being evacuated using aspiration pump, makes the vacuum degree 7.0 × 10 of vacuum chamber- 3Pa, temperature is up to 150 DEG C.
(3) aura bias cleans: opening motor 3, motor 3 drives the workpiece 7 on pivoted frame 2 to rotate, is powered to titanium target 41, titanium
Target current is 15A, and adjusting is biased into 100V, and duty ratio 50% carries out aura cleaning to workpiece surface, and scavenging period is
20min。
(4) Ion Cleaning: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and is filled with argon gas, argon gas stream to vacuum chamber 1
Amount is 400sccm, while being powered to titanium target.Titanium target electric current is 15A, and adjusting is biased into 100V, duty ratio 50%.Argon gas is electric
From for argon ion, argon ion bombardment workpiece surface further carries out decontamination cleaning, scavenging period 20min to 7 surface of workpiece.
(5) plating prime coat: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and argon gas, argon are filled with into vacuum chamber 1
The flow of gas is 90sccm.It being powered simultaneously to chromium target 42, chromium target current is 25A, it adjusts and is biased into 110V, duty ratio 50%,
Plating times are 10min, sputter the substance on chromium target and deposit to workpiece surface formation metal back layer, which is chromium
Film layer.
(6) plating middle layer: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and continues to be powered to chromium target 42.Wherein,
Chromium target current is 20A, bias 110V, duty ratio 40%.The gas being filled with into vacuum chamber changes oxygen, argon gas, oxygen into
Flow be 120sccm, the flow of argon gas is 100sccm.Argon gas is ionized as argon ion, and argon ion accelerates under electric field action
Cathode target is flown to, and target surface is bombarded with high-energy, sputters target.In sputtering particle, chromium atom is in motion process
In react to form chromium oxide and be deposited in chromium film layer with oxygen, form intermediate coat thick-layer, which is chromium oxide
Layer.
(7) coating surface layer: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and stops being powered to chromium target 42, give simultaneously
Titanium target 41 is powered.Wherein, titanium target target current is 25A, bias 20V, duty ratio 70%.The gas being filled with into vacuum chamber changes
At oxygen, argon gas, the flow of oxygen is 100sccm, and the flow of argon gas is 90sccm.Argon gas is ionized as argon ion, argon ion
Accelerate to fly to cathode target under electric field action, and target surface is bombarded with high-energy, sputters target.In sputtering particle,
Titanium atom reacts with oxygen during the motion to be formed titanium dioxide deposition and forms surface color layer on chromium oxide layer, should
Surface color layer is titanium dioxide layer.
In the present embodiment, plated film time 6h, chromium film layer, chromium oxide layer, titanium dioxide layer thickness be respectively 1.0 μ
M, 1.6 μm, 2.0 μm, color are changed from yellow to red.
Example IV
(1) it is provided with titanium target 41 and chromium target 42 in vacuum chamber 1, hangs over hanging rod for the direction of the gradient color on demand of workpiece 7 is flat
On 25, it is provided with titanium target 41 and chromium target 42 in vacuum chamber 1, closes the door 6 of vacuum chamber 1, forms closed sputtering space.Wherein titanium
Target 41 is the first pole target, and chromium target 42 is the second pole target.
(2) it vacuumizes: closed vacuum chamber being evacuated using aspiration pump, makes the vacuum degree 5.0 × 10 of vacuum chamber- 3Pa, temperature is up to 150 DEG C.
(3) aura bias cleans: opening motor 3, motor 3 drives the workpiece 7 on pivoted frame 2 to rotate, is powered to titanium target 41, titanium
Target current is 15A, and adjusting is biased into 100V, and duty ratio 50% carries out aura cleaning to workpiece surface, and scavenging period is
20min。
(4) Ion Cleaning: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and is filled with argon gas, argon gas stream to vacuum chamber 1
Amount is 400sccm, while being powered to titanium target 41.Titanium target electric current is 15A, and adjusting is biased into 100V, duty ratio 50%.Argon gas quilt
Ionization is argon ion, and argon ion bombardment workpiece surface further carries out decontamination cleaning, scavenging period 20min to workpiece surface.
(5) plating prime coat: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and argon gas, argon are filled with into vacuum chamber 1
The flow of gas is 100sccm.It being powered simultaneously to chromium target 42, chromium target current is 15A, it adjusts and is biased into 80V, duty ratio 70%,
Plating times are 10min, sputter the substance on chromium target and deposit to workpiece surface formation metal back layer.The metal back layer is chromium
Film layer.
(6) plating middle layer: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and stops being powered to chromium target 42, give simultaneously
Titanium target 41 is powered.Wherein, titanium target electric current is 18A, bias 100V, duty ratio 50%.The gas being filled with into vacuum chamber changes
At oxygen, argon gas and acetylene.The flow of the oxygen is 90sccm, and the flow of argon gas is 80sccm, and the flow of acetylene is
120sccm.Argon gas is ionized as argon ion, and argon ion accelerates to fly to cathode target under electric field action, and bombards target with high-energy
Surface sputters target.In sputtering particle, titanium atom reacts with acetylene during the motion, and to form titanium carbide heavy
Product forms intermediate coat thick-layer in chromium film layer, which is titanium carbide layer.
(7) coating surface layer: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and continues to be powered to titanium target 41.Wherein,
Titanium target electric current is 25A, bias 20V, duty ratio 50%.The gas being filled with into vacuum chamber changes oxygen, argon gas into, oxygen
Flow is 120sccm, and the flow of argon gas is 100sccm.Argon gas is ionized as argon ion, and argon ion accelerates to fly under electric field action
Target surface is bombarded to cathode target, and with high-energy, sputters target.In sputtering particle, titanium atom is during the motion
It reacts with oxygen and to form titanium dioxide deposition and form surface color layer on titanium carbide layer, which is titanium dioxide
Titanium layer.
In the present embodiment, plated film time 4h, chromium film layer, titanium carbide layer, titanium dioxide layer thickness be respectively 0.9 μ
M, 1.5 μm, 1.8 μm, color are changed from green to purple.
Embodiment five
(1) it is provided with titanium target 41 and chromium target 42 in vacuum chamber 1, hangs over hanging rod for the direction of the gradient color on demand of workpiece 7 is flat
On 25, the door 6 of vacuum chamber 1 is closed, closed sputtering space is formed.
(2) vacuumize: closed vacuum chamber being evacuated using aspiration pump, make the vacuum degree 6.0 of vacuum chamber 1 ×
10-3Pa, temperature is up to 150 DEG C.
(3) aura bias cleans, and opens motor 3, and motor 3 drives the workpiece 7 on pivoted frame 2 to rotate, gives 41 energization titanium of titanium target
Target current is 15A, and adjusting is biased into 100V, and duty ratio 50% carries out aura cleaning to 7 surface of workpiece, and scavenging period is
20min。
(4) Ion Cleaning: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and is filled with argon gas, argon gas stream to vacuum chamber 1
Amount is 400sccm, while being powered to titanium target 41 that titanium target electric current is 15A, and adjusting is biased into 100V, duty ratio 50%.Argon gas quilt
Ionization is argon ion, and argon ion bombardment workpiece surface further carries out decontamination cleaning, scavenging period 20min to workpiece surface.
(5) plating prime coat: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and argon gas, argon are filled with into vacuum chamber 1
The flow of gas is 100sccm.It being powered simultaneously to titanium target 41, titanium target electric current is 20A, it adjusts and is biased into 120V, duty ratio 60%,
Plating times are 10min, sputter the substance in titanium target and deposit to 7 surface of workpiece formation metal back layer, which is
Titanium film layer.
6) plating middle layer: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and continues to be powered to titanium target 41.Wherein, titanium
Target current is 20A, bias 120V, duty ratio 60%.The gas being filled with into vacuum chamber changes oxygen, argon gas and acetylene into.
The flow of the oxygen is 80sccm, and the flow of argon gas is 100sccm, and the flow of acetylene is 120sccm.Argon gas is ionized as argon
Ion, argon ion accelerates to fly to cathode target under electric field action, and bombards target surface with high-energy, sputters target.In
In sputtering particle, titanium atom, which reacts to form titanium carbide and be deposited on titanium film layer during the motion with acetylene, forms intermediate coat
Thick-layer, the intermediate coat thick-layer are titanium carbide layer.
(7) coating surface layer: motor 3 maintains the workpiece 7 on driving pivoted frame 2 to rotate, and continues to be powered to titanium target 41.Wherein,
Titanium target electric current is 20A, bias 25V, duty ratio 40%.The gas being filled with into vacuum chamber changes oxygen, argon gas into, oxygen
Flow is 100sccm, and the flow of argon gas is 80sccm.Argon gas is ionized as argon ion, and argon ion accelerates to fly under electric field action
Target surface is bombarded to cathode target, and with high-energy, sputters target.In sputtering particle, titanium atom is during the motion
It reacts with oxygen and to form titanium dioxide deposition and form surface color layer on titanium carbide layer, which is titanium dioxide
Titanium layer.
In the present embodiment, plated film time 6h, titanium film layer, titanium carbide layer, titanium dioxide layer thickness be respectively 0.8 μ
M, 1.6 μm, 2.0 μm, color are changed from blue to green.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, In
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (10)
1. a kind of ion sputtering film coating method for realizing gradient color, it is characterised in that: steps are as follows:
(1) in the first pole target and the second pole target are arranged in vacuum chamber, vacuum chamber is hung over by the direction of workpiece gradient color on demand is flat
On the hanging rod of interior pivoted frame, the door of vacuum chamber is closed, forms closed sputtering space;
(2) vacuum degree≤9.0 × 10 are evacuated to-3Pa, T:150 DEG C of vacuum room temperature≤T≤180 DEG C, setting sputtering environment;
(3) aura bias cleans: being powered to the first pole target, carries out aura cleaning to workpiece surface;
(4) Ion Cleaning: it is filled with argon gas to vacuum chamber, while being powered to the first pole target, argon gas is ionized as argon ion, argon ion
Bombard workpiece surface;
(5) plating prime coat: being filled with argon gas into vacuum chamber, is powered to the first pole target or the second pole target, makes the first pole target or the
Substance on two pole targets, which sputters and deposits to workpiece surface, forms metal back layer;
(6) plating middle layer: using argon gas as working gas, using oxygen, nitrogen or acetylene as reaction gas, to the first pole target or the
Two pole targets are powered, and sputter the target material on the first pole target or the second pole target and deposit on the metal back layer among formation
Film thickness layer;
(7) coating surface layer: using argon gas as working gas, using oxygen as reaction gas, being powered to the first pole target or the second pole target,
It sputters the substance on the first pole target or the second pole target and deposits to formation surface color layer on the middle film layer.
2. a kind of ion sputtering film coating method for realizing gradient color according to claim 1, it is characterised in that: first pole
Target is titanium target, and second pole target is chromium target.
3. a kind of ion sputtering film coating method for realizing gradient color according to claim 2, it is characterised in that: ion sputtering plating
Film with a thickness of 0.8 μm -2.0 μm.
4. a kind of ion sputtering film coating method for realizing gradient color according to claim 3, it is characterised in that: sputtering environment
Are as follows: target current 15A-25A, bias 80V-120V, duty ratio 30%-70%.
5. a kind of ion sputtering film coating method for realizing gradient color according to claim 4, it is characterised in that:
Argon flow in step (4) Ion Cleaning is 400sccm-500sccm;In step (5) the plating prime coat
Argon flow be 80sccm-100sccm;Argon flow in step (6) the plating middle layer is 80sccm-100sccm,
The flow of nitrogen is 50sccm-100sccm, and the flow of acetylene is 40sccm-80sccm, the flow 120sccm- of oxygen
180sccm。
6. a kind of ion sputtering film coating method for realizing gradient color according to claim 5, it is characterised in that: the step
(7) flow of the argon gas in coating surface layer is 120sccm-140sccm, and the flow of oxygen is 80sccm-150sccm.
7. a kind of ion sputtering film coating device for realizing gradient color, including vacuum chamber (1), it is characterised in that: the vacuum chamber (1)
On driving mechanism is installed, the first pole target (41), the second pole target (42) are installed, for hanging workpiece in the vacuum chamber (1)
(7) pivoted frame (2), the driving mechanism and the pivoted frame (2) connection, first pole target (41) are located at the pivoted frame (2)
Outer ring, second pole target (42) are located at the inner ring of the pivoted frame (2), and first pole target (41) and second pole target (42) phase
Mutually it is symmetrical arranged.
8. a kind of ion sputtering film coating device for realizing gradient color according to claim 7, it is characterised in that: first pole
Target (41) is titanium target, and second pole target (42) is chromium target.
9. a kind of ion sputtering film coating device for realizing gradient color according to claim 7, it is characterised in that: the driving machine
Structure (3) includes motor (3), and the motor (3) is mounted on the vacuum chamber (1), and the output shaft of the motor (3) protrudes into described
In vacuum chamber (1) and it is connected with driving gear (31).
10. a kind of ion sputtering film coating device for realizing gradient color according to claim 9, it is characterised in that: the pivoted frame
It (2) include top plate (21), chassis (22), several support rods (23) and hanger (24), the top plate (21) and chassis (22) are divided
Not Tong Guo bogie wheel (5) connect with the vacuum chamber (1), several support rods (23) are circumferentially distributed, and every support
The top of bar (23) is connect with the top plate (21), and the bottom end of every support rod (23) is connect with the chassis (22), the top
Disk (21) periphery is provided with teeth, and the top plate (21) is engaged by the teeth with the driving gear (31), the hanger
(24) it is fixedly connected with the top plate (21) and support rod (23), is provided with hanging rod (25), the workpiece on the hanger (24)
(7) direction of gradient color is flat on demand hangs on the hanging rod (25).
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