CN109457226A - A kind of insulator surface coating sputtering preparation method - Google Patents

A kind of insulator surface coating sputtering preparation method Download PDF

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Publication number
CN109457226A
CN109457226A CN201811062872.5A CN201811062872A CN109457226A CN 109457226 A CN109457226 A CN 109457226A CN 201811062872 A CN201811062872 A CN 201811062872A CN 109457226 A CN109457226 A CN 109457226A
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CN
China
Prior art keywords
insulator
sputtering
coating
surface coating
target
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811062872.5A
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Chinese (zh)
Inventor
季昆玉
王健
毛锋
翁蓓蓓
杨君中
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
State Grid Jiangsu Electric Power Co Ltd
Taizhou Power Supply Co of Jiangsu Electric Power Co
Taizhou Power Supply Co of State Grid Jiangsu Electric Power Co Ltd
Original Assignee
State Grid Jiangsu Electric Power Co Ltd
Taizhou Power Supply Co of Jiangsu Electric Power Co
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Filing date
Publication date
Application filed by State Grid Jiangsu Electric Power Co Ltd, Taizhou Power Supply Co of Jiangsu Electric Power Co filed Critical State Grid Jiangsu Electric Power Co Ltd
Priority to CN201811062872.5A priority Critical patent/CN109457226A/en
Publication of CN109457226A publication Critical patent/CN109457226A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5846Reactive treatment

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  • 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 belongs to distribution structure water-proofing treatment technical fields more particularly to a kind of insulator surface coating to sputter preparation method.Compared with the micron scale construction of traditional completion method coating, traditional micron scale construction is honeycomb, and water droplet will receive certain air negative pressure effect when being detached from from nest hole and adhesion strength is larger;The nanoscale protrusion of completion method coating is depend on resin to bond and is packed together between nanoparticle microballoon, and the surface of the coating based on the method for the present invention manufacture is nanoscale baculum, droplet and the true solid-liquid contact area on surface are smaller, and the resistance being subject in water drop motion is smaller.

Description

A kind of insulator surface coating sputtering preparation method
Technical field
The invention belongs to distribution structure water-proofing treatment technical field more particularly to a kind of sputtering preparations of insulator surface coating Method.
Background technique
The insulation performance of insulator can be effectively improved by preparing waterproof coating in insulator surface, substantially reduce it in sleet Weather lower surface conduction probability, while insulator surface spot adhesive force is greatly reduced, prevent pollution flashover.Insulator surface coating system Preparation Method is numerous, and cladding process is simple and easy, easy to produce, but can only carry out preparing simple glue and cover coating, and coat adhering power is poor, It is affected by larger, it is difficult to meet some pairs of more demanding occasions of surface property.
Summary of the invention
The purpose of the invention is that providing one kind can apply in the nanoscale waterproof that insulator surface constructs high quality Layer, it is smaller to the structure change of insulator surface, it is small by external environment influence.
To achieve the above object, the invention adopts the following technical scheme that.
A kind of insulator surface coating of the invention sputters preparation method, includes the following steps:
It is cleaned by ultrasonic 10min respectively Step 1: insulator is put into enough deionized water and dehydrated alcohol and dries For use;
Step 2: insulator is fixed on magnetic control sputtering device and is protected, 5 are evacuated down to by mechanical pump and molecular pump ×10-3Pa is passed through work argon gas into operating room, is 1Pa by the air pressure that pressure controller controls operating room;
Step 3: opening radio-frequency power supply preheats 10min, it is then turned on power supply and gradually increases voltage up to build-up of luminance, by power It is adjusted to 120W, pre-sputtering 10min, sputters purity to remove the impurity of target material surface and improve it;
Step 4: removing the protection structure of insulator, at the uniform velocity rotating insulated son carries out magnetron sputtering to insulator surface Film;
Step 5: terminating sputtering, radio-frequency power supply is closed, argon gas is passed through into sputtering chamber reverts to operating room's air pressure often Pressure takes out insulator;
Step 6: the insulator after magnetron sputtering is subjected to oxidizing annealing in Muffle furnace, 10 DEG C/min of heating rate, 30-50min is kept at 400 DEG C, then cools to room temperature with the furnace;
Step 7: the mass ratio of modulation hexadecyl trimethoxy silane and ethyl alcohol is the mixed solution of 2:98, with 60r/ The revolving speed of min carries out magnetic agitation 60min to carry out dispersion hydrolysis;Insulator is put into mixing 30-50min, makes silane molecule Self assembly is carried out in zinc oxide surface, it is modified that low-surface-energy is carried out to it;
Step 8: taking out insulator, rinsed well using ethyl alcohol, is put into 90 DEG C of air dry ovens dry 30-50min;
The beneficial effect is that:
Compared with the micron scale construction of traditional completion method coating, traditional micron scale construction is honeycomb, and water droplet is from nest It will receive certain air negative pressure effect when being detached from hole and adhesion strength is larger;The nanoscale protrusion of completion method coating is nanoparticle It depends on resin to bond between sub- microballoon to be packed together, and the surface of the coating based on the method for the present invention manufacture is that nanoscale is rodlike prominent It rises, the true solid-liquid contact area on droplet and surface is smaller, and the resistance being subject in water drop motion is smaller.Utilize cetyl three After methoxy silane is modified, so that there are the long chain alkanes that carbon atom number is greater than 4 for the film surface of coating, so that film layer has There is lower surface energy, makes surface that there is super-hydrophobic characteristic.The solid-liquid contact area value of the super-hydrophobic film layer of magnetron sputtering method connects Nearly 4.0% is less than the 6.3% of the coating of the particle-filled method preparation of Conventional nano, therefore its structure is more conducive to reduction solid-liquid and connects Contacting surface is long-pending to obtain better anti-glaze ability with smaller roll angle and contact angle hysteresis with solid-liquid adhesion strength with this.
Detailed description of the invention
Fig. 1 is sputtering coating schematic diagram;
Fig. 2 different moments correct the comparison of front and back covering ice for insulator area ratio and Hydrophobic glass, common insulator.
Specific embodiment
It elaborates below in conjunction with specific embodiment to the invention.
The principle of coating is sputtered as shown in Figure 1, mainly carrying out electronics punching to insulator surface using its principle in the present invention It hits, generates nanoscale film layer to control insulator surface to realize hydrophobic performance.
It is cleaned by ultrasonic 10min respectively Step 1: insulator is put into enough deionized water and dehydrated alcohol and dries For use;
Step 2: insulator is fixed on magnetic control sputtering device and is protected, 5 are evacuated down to by mechanical pump and molecular pump ×10-3Pa is passed through work argon gas into operating room, is 1Pa by the air pressure that pressure controller controls operating room;
Step 3: opening radio-frequency power supply preheats 10min, it is then turned on power supply and gradually increases voltage up to build-up of luminance, by power It is adjusted to 120W, pre-sputtering 10min, sputters purity to remove the impurity of target material surface and improve it;
Step 4: removing the protection structure of insulator, at the uniform velocity rotating insulated son carries out magnetron sputtering to insulator surface Film;
Step 5: terminating sputtering, radio-frequency power supply is closed, argon gas is passed through into sputtering chamber reverts to operating room's air pressure often Pressure takes out insulator;
Step 6: the insulator after magnetron sputtering is subjected to oxidizing annealing in Muffle furnace, 10 DEG C/min of heating rate, 30-50min is kept at 400 DEG C, then cools to room temperature with the furnace;
Step 7: the mass ratio of modulation hexadecyl trimethoxy silane and ethyl alcohol is the mixed solution of 2:98, with 60r/ The revolving speed of min carries out magnetic agitation 60min to carry out dispersion hydrolysis;Insulator is put into mixing 30-50min, makes silane molecule Self assembly is carried out in zinc oxide surface, it is modified that low-surface-energy is carried out to it;
Step 8: taking out insulator, rinsed well using ethyl alcohol, is put into 90 DEG C of air dry ovens dry 30-50min;
Hydrophobic stability test is carried out to the above-mentioned insulator containing anti-icing film layer, (dropping liquid is straight using acid rain impingement attack 15min 15 μ L of diameter, height 27cm, 1 drop of rate of addition/s) hydrophobic method to be tested afterwards is tested, test result is as shown in table 1:
1 film layer hydrophobic stability test result of table
Impregnating in the solution of PH=7 and PH=14 slightly reduces with the film layer after water impact, film layer ultra-hydrophobicity And still maintain ultra-hydrophobicity.Illustrate that film layer alkali corrosion resistance ability is stronger, although this is because zinc oxide be amphoteric oxide, But zinc oxide nano rod is wrapped up by long chain alkane and forms protective layer, while the superhydrophobic characteristic that film layer has makes true solid-liquid Contact area is smaller, so that film layer and aqueous slkali reaction speed are slower.
After the mechanism of sand impact and Sandpapering, film layer is still able to maintain certain ultra-hydrophobicity.This is Because the ethyl alcohol of hexadecyl trimethoxy silane is molten when modified to film layer progress surface using hexadecyl trimethoxy silane Liquid can penetrate among film surface coarse structure, and the zinc oxide inside film layer in " loose vitellarium " gap is also modified.Cause Under the mechanism of sand impact and Sandpapering, the part coarse structure of film surface is likely to be broken, but is exposed for this The part come still has the effect of super-hydrophobic.After Sandpapering, worn area still has a large amount of nanometers coarse from the point of view of microcosmic Structure composition, such structure make film layer can continue to keep super-hydrophobic performance.The super-hydrophobic film layer of magnetron sputtering is water-fast stream Impact, sand impact, mechanical friction and alkali corrosion resistance ability are stronger, and the ability of acid corrosion-resistant is slightly weak, has centainly hydrophobic Stability.
Insulator, common insulator and Hydrophobic glass Jing Guo above method prepares coating is subjected to ice-coating test, i.e., The icing area for observing its surface at room temperature is compared, and obtains comparison diagram shown in Fig. 2.According to revised data, warp Icing area ratio of insulator surface after icing is reduced to 29.6% after crossing processing, and the area ratio of no icing is 70.4%, illustrate after treatment have excellent anti-glaze icing ability.
Finally it should be noted that above embodiments are only to illustrate the technical solution of the invention, rather than to this hair It is bright create protection scope limitation, although being explained in detail referring to preferred embodiment to the invention, this field it is general Lead to it will be appreciated by the skilled person that can be modified or replaced equivalently to the technical solution of the invention, without departing from this The spirit and scope of innovation and creation technical solution.

Claims (3)

1. a kind of insulator surface coating sputters preparation method, which is characterized in that
It is cleaned by ultrasonic 10min respectively Step 1: insulator is put into enough deionized water and dehydrated alcohol and dries stand-by;
Step 2: insulator is fixed on magnetic control sputtering device and is protected, 5 × 10 are evacuated down to by mechanical pump and molecular pump-3Pa is passed through work argon gas into operating room, is 1Pa by the air pressure that pressure controller controls operating room;
Step 3: opening radio-frequency power supply preheats 10min, it is then turned on power supply and gradually increases voltage until build-up of luminance, power is adjusted to 120W, pre-sputtering 10min sputter purity to remove the impurity of target material surface and improve it;
Step 4: removing the protection structure of insulator, at the uniform velocity rotating insulated son carries out magnetron sputtering plating to insulator surface;
Step 5: terminating sputtering, radio-frequency power supply is closed, argon gas is passed through into sputtering chamber makes operating room's air pressure revert to normal pressure, takes Insulator out;
Step 6: the insulator after magnetron sputtering is carried out oxidizing annealing, 10 DEG C/min of heating rate, 400 in Muffle furnace 30-50min is kept at DEG C, then cools to room temperature with the furnace;
Step 7: the mass ratio of modulation hexadecyl trimethoxy silane and ethyl alcohol is the mixed solution of 2:98, with 60r/min's Revolving speed carries out magnetic agitation 60min to carry out dispersion hydrolysis;Insulator is put into mixing 30-50min, is aoxidizing silane molecule Zinc surface carries out self assembly, and it is modified that low-surface-energy is carried out to it;
Step 8: taking out insulator, rinsed well using ethyl alcohol, is put into 90 DEG C of air dry ovens dry 30-50min.
2. a kind of insulator surface coating sputters preparation method according to claim 1, which is characterized in that the target refers to Zinc target, zinc target purity are not less than 99%, and the purity of the work argon gas is not less than 99%.
3. a kind of insulator surface coating sputters preparation method according to claim 1, which is characterized in that the step 4 In, target-substrate distance is not less than 10cm when sputtering, and sputtering time is no less than 15min.
CN201811062872.5A 2018-09-12 2018-09-12 A kind of insulator surface coating sputtering preparation method Pending CN109457226A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111180150A (en) * 2020-01-03 2020-05-19 天津大学 Preparation method of nonlinear insulator with optimized surface conductance
CN114496424A (en) * 2022-03-31 2022-05-13 萍乡华创电气有限公司 Column type insulator and manufacturing method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105623503A (en) * 2016-03-23 2016-06-01 华北电力大学 Silicone rubber hydrophobic coating used for insulator and preparation method thereof
CN105820644A (en) * 2016-04-26 2016-08-03 国网河南省电力公司电力科学研究院 Superhydrophobic coating, anti-pollution-flashover superhydrophobic insulator and preparation technique thereof
CN207367703U (en) * 2017-08-10 2018-05-15 国网河南宝丰县供电公司 Insulator with anti-ice-flashing, pollution flashover coating

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105623503A (en) * 2016-03-23 2016-06-01 华北电力大学 Silicone rubber hydrophobic coating used for insulator and preparation method thereof
CN105820644A (en) * 2016-04-26 2016-08-03 国网河南省电力公司电力科学研究院 Superhydrophobic coating, anti-pollution-flashover superhydrophobic insulator and preparation technique thereof
CN207367703U (en) * 2017-08-10 2018-05-15 国网河南宝丰县供电公司 Insulator with anti-ice-flashing, pollution flashover coating

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
RUIJIN LIAO ET.AL: "Anti-icing performance in glaze ice of nanostructured film prepared by RF magnetron sputtering", 《APPLIED SURFACE SCIENCE》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111180150A (en) * 2020-01-03 2020-05-19 天津大学 Preparation method of nonlinear insulator with optimized surface conductance
CN114496424A (en) * 2022-03-31 2022-05-13 萍乡华创电气有限公司 Column type insulator and manufacturing method thereof
CN114496424B (en) * 2022-03-31 2024-04-26 萍乡华创电气有限公司 Column insulator and manufacturing method thereof

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Application publication date: 20190312