CN102925044A - Preparation method of hole-sealing coating on surface of physical vapor deposition (PVD) aluminum coating - Google Patents

Preparation method of hole-sealing coating on surface of physical vapor deposition (PVD) aluminum coating Download PDF

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CN102925044A
CN102925044A CN2012104199903A CN201210419990A CN102925044A CN 102925044 A CN102925044 A CN 102925044A CN 2012104199903 A CN2012104199903 A CN 2012104199903A CN 201210419990 A CN201210419990 A CN 201210419990A CN 102925044 A CN102925044 A CN 102925044A
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coating
component
pvd
aluminium coat
butyl acetate
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宋仁国
李鑫伟
王超
姜冬
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Changzhou University
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Changzhou University
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Abstract

The invention relates to a preparation method of a hole-sealing coating on the surface of a physical vapor deposition (PVD) aluminum coating. The preparation method solves the problem that the existing PVD aluminum coating has an uneven surface and a lot of pores and micro-cracks. The hole-sealing coating obtained by the preparation method is a fluorocarbon coating which can effectively seal pores and micro-cracks of an aluminum coating and can improve corrosion resistance, chemical resistance and weatherability of an aluminum coating. The preparation method belongs to the technical field of coating processing.

Description

A kind of preparation method of PVD aluminium coat surface-sealing coating
Technical field
The present invention relates to a kind of preparation method of PVD aluminium coat surface-sealing coating, mainly be for PVD aluminium coat surface irregularity, there are a lot of pores and tiny crack, prepare and a kind ofly can effectively seal pore in the aluminium coat and the fluororine-carbon coating of tiny crack, can improve simultaneously erosion resistance, chemical resistant properties and the weathering resistance of aluminium coat, belong to the coating processing technique field.
Background technology
The corrosion of metallic substance is a common problem; utilize thin film technique to improve its corrosion resistance and obtained certain progress; utilize the film preparing technologies such as PVD or CVD to play the coating of buffer action at metal material surface preparation and corrosive medium; can play certain protective effect to metallic material parts; yet; all exist the microscopic void of some micron dimensions in these coating; in storage process; steam in the environment; the corrosive mediums such as oxygen can cause matrix corrosion by coating hole and metal material matrix generation chemical reaction; migration along with the time; the accumulation of corrosion product also can cause the bubbling of coating; peel off; find through the literature search to prior art; Chen Yuhua etc. adopt the LG3 hole sealing agent that aluminium coat is carried out sealing of hole in " gray prediction of sealing of hole aluminum coating high temperature resistance atmospheric oxidation performance "; the result from the electromicroscopic photograph as seen; still there are a lot of crackles in the gained film coated surface; therefore need more excellent the filming of a kind of performance to solve these problems; therefore be coated with filming of one deck excellent performance at aluminium coat, the protection aluminium coat is very important.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of metal material matrix PVD aluminium coat surface-sealing coating, improve erosion resistance, chemical resistant properties and the weathering resistance of aluminium coat.
For reaching goal of the invention the technical solution used in the present invention be: a kind of PVD aluminium coat surface-sealing coating is characterized in that being achieved through the following technical solutions:
Find through the literature search to prior art, Wu S K etc. adopt radio-frequency (RF) sputtering method to deposit the approximately pure aluminium film of 2 μ m of thickness at the AZ91D Mg alloy surface in " A study of r.f.-sputtered Al and Ni thin film on AZ91D magnesium alloy ", behind 350 ℃ of high vacuum thermal treatment 24h, generated new mutually (Mg in the responding layer (thick approximately 5 μ m) that forms at the interface of aluminium and matrix magnesium 17Al 12); this phase fragility is larger; and responding layer contains than multiple cracks, so that aluminium coat wear resistance and solidity to corrosion all are subject to certain impact, and just there is the shortcoming of pore and crackle in this patent for PVD aluminium coat surface; studied hole sealing coating; the fluorocarbon coating that the preparation hole sealing coating adopts can be good at being attached on the PVD aluminium coat, and coating is comparatively fine and close, can effectively prevent the infiltration of sealing and oxygen; thereby well protect the PVD aluminium coat, improve corrosion resistance nature.
A kind of PVD aluminium coat surface-sealing coating of the present invention, the component that comprises and mass percent are:
The first component:
Fluorocarbon resin 60-70%;
Flow agent (BYK-306) 0.2%;
Flow agent (EFKA-3777) 0.5%;
Catalyzer dibutyl tin laurate (DBTDL) 0.01-0.1%;
N-BUTYL ACETATE 15-20%;
Ethylene glycol ether acetate (CAC) surplus.
The second component:
HDI trimer curing agent 60-70%;
N-BUTYL ACETATE 30-40%.
The thinner proportioning:
N-BUTYL ACETATE 15-30%;
Dimethylbenzene 50%;
Ethylene glycol ether acetate (CAC) 20-35%.
Formulation parameter:
The mol ratio of NCO in the HDI tripolymer and the OH of fluorocarbon resin=1.1: 1.
The preparation method of described PVD aluminium coat surface-sealing coating comprises the steps:
(1) in paint mixing cylinder, adds successively fluorocarbon resin, BYK-306, EFKA-3777, catalyzer DBTDL according to the batching order, add N-BUTYL ACETATE and CAC solvent, be adjusted to corresponding solid part, obtain the first component;
Solid part refers to the content of non-volatile matter in the coating, namely forms the coating content of dry coating film, and generally the mass percent with non-volatile matter represents; Solid part of the first component of preparing according to the percentage composition scope of each material in the first component listed above is different, and how many this percentage compositions that will see that every kind of material adds is, is adjusted to thus corresponding solid part.
(2) first, component B is mixed, and be diluted to suitable viscosity with thinner, parameter is as follows: the mass ratio of dilution is: first component: component B: thinner=10: 1: 2-4.
Coating of the present invention is sprayed at PVD alclad sheet surface, working viscosity: 23 ± 2 ℃, be coated with-4 glasss, 18-20s under the environment of Air drying; Spray pressure 0.2-0.4MPa carries out the oil removing skimming treatment to the alclad sheet surface before filming.
The beneficial effect of PVD aluminium coat surface-sealing coating of the present invention is mainly reflected in: (1) described PVD aluminium coat surface-sealing coating can be sealed pore and the crackle on PVD aluminium coat surface, and aluminium coat is played a very good protection; (2) improve the corrosion resistance nature of aluminium coat; (3) raw material is inexpensive, and technique is simple, and cost is low, is beneficial to suitability for industrialized production.
Description of drawings
Fig. 1 is the shape appearance figure of PVD aluminium coat;
Fig. 2 be embodiment 1-3 the PVD aluminium coat is carried out the surface topography map of the fluororine-carbon coating of sealing of hole.
Embodiment
The present invention is described further below in conjunction with concrete mode:
Matrix is the Q235 steel, and the thickness of aluminium plated film is 2 ± 0.5 μ m, and the PVD alclad sheet is of a size of 70mm * 180mm * 2mm.
Embodiment 1:
The first component:
Fluorocarbon resin 63%;
Flow agent (BYK-306) 0.2%;
Flow agent (EFKA-3777) 0.5%;
Catalyzer (DBTDL) 0.03%;
N-BUTYL ACETATE 20%;
Ethylene glycol ether acetate (CAC) surplus.
The second component:
HDI trimer curing agent 65%;
N-BUTYL ACETATE 35%.
The thinner proportioning:
N-BUTYL ACETATE 20%;
Dimethylbenzene 50%;
Ethylene glycol ether acetate (CAC) 30%.
Formulation parameter:
NCO∶OH=1.1∶1。
The first step: in paint mixing cylinder, add successively fluorocarbon coating, BYK-306, EFKA-3777, DBTDL auxiliary agent according to the batching order, add again N-BUTYL ACETATE and CAC solvent, be adjusted to corresponding solid part;
Second step: first, component B is mixed, and be diluted to suitable viscosity with thinner, parameter is as follows: Dilution ratio: first component: component B: thinner=10: 1: 2.
Working viscosity: 23 ± 2 ℃, be coated with-4 glasss, 19s spray pressure, 0.3MPa.
Embodiment 2:
The first component:
Fluorocarbon resin 68%;
Flow agent (BYK-306) 0.2%;
Flow agent (EFKA-3777) 0.5%;
Catalyzer (DBTDL) 0.05%;
N-BUTYL ACETATE 18%;
Ethylene glycol ether acetate (CAC) surplus.
The second component:
HDI trimer curing agent 67%;
N-BUTYL ACETATE 33%.
The thinner proportioning:
N-BUTYL ACETATE 22%;
Dimethylbenzene 50%;
Ethylene glycol ether acetate (CAC) 28%.
Formulation parameter:
NCO∶OH=1.1∶1。
The first step: in paint mixing cylinder, add successively fluorocarbon coating, BYK-306, EFKA-3777, DBTDL auxiliary agent according to the batching order, add again N-BUTYL ACETATE and CAC solvent, be adjusted to corresponding solid part;
Second step: first, component B is mixed, and be diluted to suitable viscosity with thinner, parameter is as follows: Dilution ratio: first component: component B: thinner=10: 1: 3.
Working viscosity: 23 ± 2 ℃, be coated with-4 glasss, 20s; Spray pressure, 0.4MPa.
Embodiment 3:
The first component:
Fluorocarbon resin 70%;
Flow agent (BYK-306) 0.2%;
Flow agent (EFKA-3777) 0.5%;
Catalyzer (DBTDL) 0.07%;
N-BUTYL ACETATE 16%;
Ethylene glycol ether acetate (CAC) surplus.
The second component:
HDI trimer curing agent 63%;
N-BUTYL ACETATE 37%.
The thinner proportioning:
N-BUTYL ACETATE 18%;
Dimethylbenzene 50%;
Ethylene glycol ether acetate (CAC) 32%.
Formulation parameter:
NCO∶OH=1.1∶1。
The first step: in paint mixing cylinder, add successively fluorocarbon coating, BYK-306, EFKA-3777, DBTDL auxiliary agent according to the batching order, add again N-BUTYL ACETATE and CAC equal solvent, be adjusted to corresponding solid part;
Second step: first, component B is mixed, and be diluted to suitable viscosity with thinner, parameter is as follows: Dilution ratio: first component: component B: thinner=10: 1: 4.
Working viscosity: 23 ± 2 ℃, be coated with-4 glasss, 18s; Spray pressure 0.2MPa.
Prepared PVD aluminium coat surface-sealing coating detects and scanning electronic microscope (SEM) testing coating performance and observation surface topography through every GB.
(1) performance test
Figure 168495DEST_PATH_IMAGE001
By table as seen, fluororine-carbon coating have good corrosion resistance nature, acid-proof alkaline, hardness and with the bonding force of matrix, the actual drying time, only about 24h, therefore, fluororine-carbon coating played a very good protection to the PVD aluminium coat.
(2) SEM observes
With sem observation PVD aluminium coat with the PVD aluminium coat is carried out the surface topography of the fluororine-carbon coating of sealing of hole; As seen from Figure 1, middle aluminium coat is not fine and close, and the surface is also rough smooth, has many pores even crackle; And it is still smooth smooth through the fluororine-carbon coating surface after the 500h salt-fog test among Fig. 2, fine and close, without obvious pore and crackle, the Fluorocarbon resin coating of having prepared the smooth surface densification in the success of PVD aluminium coat surface is described, originally the porous characteristic disappear of aluminium coat.
(3) gas permeation rate
The rate of permeation of FEVE coating
Figure 10549DEST_PATH_IMAGE002
Fluorocarbon resin coating sees the following form to the transmitance of oxygen and carbon dioxide, and the result shows that the air penetrability of Fluorocarbon resin coating is low, good weatherability, and the rate of permeation of three embodiment is basic identical.

Claims (4)

1. PVD aluminium coat surface-sealing coating, it is characterized in that: the component that comprises and mass percent are:
The first component:
Fluorocarbon resin 60-70%;
Flow agent (BYK-306) 0.2%;
Flow agent (EFKA-3777) 0.5%;
Catalyzer dibutyl tin laurate (DBTDL) 0.01-0.1%;
N-BUTYL ACETATE 15-20%;
Ethylene glycol ether acetate (CAC) surplus;
The second component:
HDI trimer curing agent 60-70%;
N-BUTYL ACETATE 30-40%;
The thinner proportioning:
N-BUTYL ACETATE 15-30%;
Dimethylbenzene 50%;
Ethylene glycol ether acetate (CAC) 20-35%.
2. a kind of PVD aluminium coat surface-sealing coating as claimed in claim 1, it is characterized in that: the mol ratio of the NCO in the HDI tripolymer and the OH of fluorocarbon resin is 1.1: 1.
3. the preparation method of a kind of PVD aluminium coat surface-sealing coating as claimed in claim 1 is characterized in that comprising the steps:
(1) in paint mixing cylinder, adds successively fluorocarbon resin, BYK-306, EFKA-3777, catalyzer DBTDL according to the batching order, add solvent butyl acetate and CAC, be adjusted to corresponding solid part, obtain the first component;
(2) first, component B is mixed, and be diluted to suitable viscosity with thinner, parameter is as follows: the mass ratio of dilution is: first component: component B: thinner=10: 1: 2-4.
4. a kind of PVD aluminium coat surface-sealing coating spraying as claimed in claim 1 is in the method on PVD alclad sheet surface, it is characterized in that: described coating is sprayed at PVD alclad sheet surface under the environment of Air drying, working viscosity: 23 ± 2 ℃, be coated with-4 glasss, 18-20s; Spray pressure 0.2-0.4MPa carries out the oil removing skimming treatment to the alclad sheet surface before filming.
CN2012104199903A 2012-10-29 2012-10-29 Preparation method of hole-sealing coating on surface of physical vapor deposition (PVD) aluminum coating Pending CN102925044A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103865371A (en) * 2014-03-17 2014-06-18 常州大学 Preparation method of modified trifluoro-FEVE (Fluorinated Ethylene Vinyl Ether) fluorocarbon coating
CN109594056A (en) * 2018-12-18 2019-04-09 国家电投集团科学技术研究院有限公司 Substrate and preparation method, sealing of hole system, cladding tubes
CN110416782A (en) * 2019-08-27 2019-11-05 问问智能信息科技有限公司 A kind of charging contact composite structure and preparation method thereof
CN112852237A (en) * 2021-01-05 2021-05-28 北京动力机械研究所 Hole sealing agent for thermal spraying sealing coating and use method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01146965A (en) * 1987-12-02 1989-06-08 Kansai Paint Co Ltd Primer composition for fluorocarbon resin paint
CN1580154A (en) * 2004-05-18 2005-02-16 大连振邦氟涂料股份有限公司 Fluorocarbon coating and its preparing method
CN101280139A (en) * 2008-04-30 2008-10-08 杭州油漆有限公司 High-weather resistance fluorocarbon paint and construction method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01146965A (en) * 1987-12-02 1989-06-08 Kansai Paint Co Ltd Primer composition for fluorocarbon resin paint
CN1580154A (en) * 2004-05-18 2005-02-16 大连振邦氟涂料股份有限公司 Fluorocarbon coating and its preparing method
CN101280139A (en) * 2008-04-30 2008-10-08 杭州油漆有限公司 High-weather resistance fluorocarbon paint and construction method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103865371A (en) * 2014-03-17 2014-06-18 常州大学 Preparation method of modified trifluoro-FEVE (Fluorinated Ethylene Vinyl Ether) fluorocarbon coating
CN103865371B (en) * 2014-03-17 2016-07-13 常州大学 A kind of preparation method of modified three fluorine-type FEVE fluororine-carbon coatings
CN109594056A (en) * 2018-12-18 2019-04-09 国家电投集团科学技术研究院有限公司 Substrate and preparation method, sealing of hole system, cladding tubes
CN109594056B (en) * 2018-12-18 2021-02-12 国家电投集团科学技术研究院有限公司 Substrate, preparation method, hole sealing system and cladding tube
CN110416782A (en) * 2019-08-27 2019-11-05 问问智能信息科技有限公司 A kind of charging contact composite structure and preparation method thereof
CN112852237A (en) * 2021-01-05 2021-05-28 北京动力机械研究所 Hole sealing agent for thermal spraying sealing coating and use method thereof

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Application publication date: 20130213