CN111559872A - Glass sight glass with anticorrosive coating and preparation method thereof - Google Patents
Glass sight glass with anticorrosive coating and preparation method thereof Download PDFInfo
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- CN111559872A CN111559872A CN202010460702.3A CN202010460702A CN111559872A CN 111559872 A CN111559872 A CN 111559872A CN 202010460702 A CN202010460702 A CN 202010460702A CN 111559872 A CN111559872 A CN 111559872A
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- 239000011521 glass Substances 0.000 title claims abstract description 113
- 239000011248 coating agent Substances 0.000 title claims abstract description 56
- 238000000576 coating method Methods 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000005507 spraying Methods 0.000 claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 238000005498 polishing Methods 0.000 claims abstract description 5
- 238000007711 solidification Methods 0.000 claims abstract description 4
- 230000008023 solidification Effects 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 3
- 238000005260 corrosion Methods 0.000 claims description 13
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 5
- 229920001780 ECTFE Polymers 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 4
- 239000002390 adhesive tape Substances 0.000 claims description 4
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- 229920009441 perflouroethylene propylene Polymers 0.000 claims description 3
- 229920011301 perfluoro alkoxyl alkane Polymers 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 5
- 239000011241 protective layer Substances 0.000 abstract description 4
- 239000002344 surface layer Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 18
- 238000001514 detection method Methods 0.000 description 8
- 230000006872 improvement Effects 0.000 description 8
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- 230000007797 corrosion Effects 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
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- 230000002950 deficient Effects 0.000 description 3
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 210000004905 finger nail Anatomy 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
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- 229920000742 Cotton Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- OWIKHYCFFJSOEH-UHFFFAOYSA-N Isocyanic acid Chemical compound N=C=O OWIKHYCFFJSOEH-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- 239000011253 protective coating Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/001—General methods for coating; Devices therefor
- C03C17/002—General methods for coating; Devices therefor for flat glass, e.g. float glass
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B11/00—Cleaning flexible or delicate articles by methods or apparatus specially adapted thereto
- B08B11/04—Cleaning flexible or delicate articles by methods or apparatus specially adapted thereto specially adapted for plate glass, e.g. prior to manufacture of windshields
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a glass sight glass with an anticorrosive coating and a preparation method thereof, wherein the preparation method comprises the following steps: (1) polishing and cleaning the edge of the glass, and putting the glass into a high-temperature furnace with a clean inner cavity; (2) preheating the glass at the temperature of 120-220 ℃ for 15-30 min; (3) taking out the preheated glass, selecting raw material powder for manufacturing an anticorrosive coating, and spraying the single side of the glass; (4) and putting the glass into a high-temperature furnace again, sintering at the temperature of 260-380 ℃ for 30-60min, then cooling to the cooling solidification point of the coating material at the cooling speed of 50-80 ℃/h, taking out and putting into a room for natural cooling. The method can coat a layer of protective layer on the surface of the glass surface layer for manufacturing the sight glass, and the protective layer can limit and prevent the sight glass from being corroded and discolored in use, greatly prolong the service life of the flange sight glass, reduce the leakage fault probability of the flange sight glass in a device area, and does not influence the transparency of the sight glass.
Description
Technical Field
The invention belongs to the technical field of coating of an anti-corrosion coating, and particularly relates to a glass sight glass with an anti-corrosion coating and a preparation method thereof.
Background
In the chemical production process, particularly in the production of high-corrosivity chemicals, the devices and equipment are all provided with sight glasses which are convenient for operators to observe. In the process, chemicals are attached to the glass sight glass due to volatilization, sputtering and the like, some chemical reagents such as isocyanic acid fluoride and hydrofluoric acid corrode the glass sight glass to generate punctiform corrosion, the strength of the glass sight glass is gradually weakened due to long-time corrosion action with the lapse of time, the glass sight glass is damaged and leaked, and equipment maintenance is troublesome. Meanwhile, the glass corrosion also influences the observation and maintenance of the interior of the device.
Disclosure of Invention
Aiming at the problems, the invention provides a specific preparation method for forming a protective coating with high corrosion resistance on the surface of the sight glass by manufacturing a coating capable of resisting high-corrosion chemical agents on the surface of the sight glass.
The technical purpose is achieved, the technical effect is achieved, and the invention is realized through the following technical scheme:
a preparation method of a glass sight glass with an anticorrosive coating is characterized by comprising the following steps:
(1) polishing and cleaning the edge of the glass, and putting the glass into a high-temperature furnace with a clean inner cavity;
(2) preheating the glass at the temperature of 120-220 ℃ for 15-30 min;
(3) taking out the preheated glass, selecting raw material powder with certain fineness for manufacturing an anticorrosive coating, and spraying the single surface of the glass;
(4) and putting the glass into a high-temperature furnace again, sintering at the temperature of 260-380 ℃ for 30-60min, then cooling to the cooling solidification point of the coating material at the cooling speed of 50-80 ℃/h, taking out and putting into a room for natural cooling.
As a further improvement of the invention, the raw material for preparing the anticorrosive coating selected in the step (3) comprises any one of PTFE, PFA, FEP, ETFE, HALAR-ECTFE and PVDF.
As a further improvement of the invention, the particle size of the raw material powder is 20-200 um.
As a further improvement of the invention, the single-side spraying is carried out on the surface of the glass by adopting an electrostatic powder spraying method, and the uniformity of the coating is controlled by adopting a flat plate spraying method and combining with circumferential movement.
As a further improvement of the invention, the steps (2) to (4) can be repeated for a plurality of times starting from any one of the steps, and the production is repeated for each time until the step (4) is finished.
As a further improvement of the invention, the step (1) also comprises the steps of firstly pasting a layer of tin foil paper and a layer of high-temperature adhesive tape on one side of the glass, and then putting the glass into a high-temperature furnace.
As a further improvement of the invention, in the step (1), the glass edge is polished to a chamfer having a width of not less than 2 mm.
As a further improvement of the invention, the glass is placed in a high temperature furnace by a suspension method.
The invention also provides a glass sight glass with the anti-corrosion coating, and the anti-corrosion coating is manufactured on one side or two sides of the glass based on the preparation method.
As a further improvement of the invention, the thickness of the anticorrosive coating is uniform and is 50-1800 um.
The invention has the beneficial effects that: the method can coat a protective layer with high corrosion resistance on the surface of the glass surface layer for manufacturing the sight glass, and the protective layer can prevent the sight glass from being corroded and discolored in use, greatly prolong the service life of the sight glass, reduce the leakage fault probability of the sight glass in a device area and not influence the transparency of the sight glass.
Drawings
FIG. 1 is a schematic view showing the distribution of sight glass placed in a high temperature furnace during the manufacturing process,
wherein, 1-coating; 2-sight glass; 3-tinfoil paper; 4-hooking; 5-hanging points in the furnace; 6-furnace chamber.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The method for manufacturing the anti-corrosion PFA coating on the surface of the sight glass comprises the following specific steps:
the first step is as follows: procedure before furnace entry
1.1 cleaning and cleaning a high-temperature furnace:
the type of the high-temperature furnace adopted by the invention is an electric heating type constant-temperature hot air circulating furnace, the maximum heating temperature is 500 ℃, the effective capacity of an inner cavity is 1 m wide, 1 m deep and 0.8 m high, and the maximum air speed of hot air circulation is 1 m/s.
The inside of the furnace chamber is swept for 2 minutes by a clean compressed air gun before each use, then the inner wall of the furnace chamber 6, an inner chamber heat insulation layer, an air inlet, an air outlet and other positions are swept by a dust collector, finally the inner surface of the furnace chamber is wiped by rags, and filter screens are arranged at the air inlet and the air outlet, wherein the mesh number of the filter screens is not less than 100 meshes. The cleaning aims to prevent the flying of the residue or the heat insulation fiber cotton in the furnace chamber in the coating manufacturing process and avoid the increase of the product rejection rate caused by the stain formed on the surface of the glass.
1.2 mirror glass circumference chamfer and burr of polishing:
removing the outer package of the sight glass, and blowing the surface of the sight glass by using a clean compressed air gun for pre-cleaning.
And (3) chamfering and polishing the pre-cleaned sight glass 2 along the edge of the glass, wherein the chamfer width is not less than 2 mm. Care was taken not to mark the mirror surface during grinding.
The polished sight glass 2 can avoid the coating from being punctured and the coating from being broken due to stress concentration in the cooling process.
1.3 cleaning glass:
before the glass 2 enters the furnace for the first time, dust on the surface of the glass is wiped by using dust-free paper, greasy dirt and impurities on the surface of stubborn stains are washed away by using an alkaline detergent, and then the glass is completely washed by using high-purity water and dried.
1.4 pasting high-temperature-resistant tin foil paper:
the side that does not spray temporarily among them is selected, pastes tinfoil paper 3 and glues firmly with yellow high temperature sticky tape, and tinfoil paper 3 provides electrically conductive basic unit, makes the glass heated more evenly when heating simultaneously, avoids local temperature overheat to cause the glass phenomenon of bursting apart. The invention selects the polyimide gold finger high-temperature adhesive tape (such as 3M 5413D type). The high-temperature adhesive tape can bear the temperature of 300-400 ℃, has an abnormally smooth surface, is not dissolved or adhered with coating raw materials needing to be sprayed, and is easy to wipe and clean with absolute ethyl alcohol at the later stage.
1.5. And (3) cleaning the glass again:
the surface of the sight glass used for manufacturing the coating is wiped again by the hand with the dust-free glove, and dust and finger prints on the surface are removed.
The second step is that: glass spraying process
2.1 preheating in a glass furnace:
as shown in figure 1, the sight glass prepared to be qualified in the previous process is vertically suspended by a hook 4 and placed in a furnace chamber 6, and the top wall of the furnace chamber 6 is provided with a furnace hanging point 5. And (4) switching on a power supply of the high-temperature furnace, starting preheating until the temperature in the furnace reaches 220 ℃ and keeping the temperature for 30 minutes. In this process, it should be noted that the suspended mirror glasses need to maintain a certain distance therebetween and be uniformly placed in the temperature stable region of the oven cavity, and they cannot contact each other.
2.2. Production raw material and equipment
Preparing raw materials:
the starting material used in the present invention was a DuPont PFA clear coating powder (e.g., TEFLON 532G) with a single spray thickness of about 25 microns. Because of probably having the caking in transportation and the storage process, in order to guarantee coating thickness and smoothness, need filter raw materials powder mesh screen twice, the filter screen mesh number is 500 meshes, and raw materials powder particle size does not exceed 20 microns after the filtration.
Electrostatic spraying equipment:
the spraying equipment adopted in the invention is a Gema high-voltage electrostatic spray gun GA03 and an Optistar CG08 intelligent controller. A flat plate spraying mode is selected, a spraying controller is calibrated through powder discharge, the powder amount required by spraying is calculated according to the surface area, the coating thickness and the coating density of the sight glass, and the parameters can be input into the controller, so that the controller can accurately control the coating thickness and repeatability.
2.3. Preheating glass spraying:
taking out the preheated sight glass hung in a high-temperature furnace, immediately spraying raw material powder on the surface of the sight glass by adopting electrostatic powder spraying equipment, slowly moving a spraying gun in a circular form for 20-40 seconds (the spraying time is determined by the thickness of the coating and the surface area of the sight glass under the condition that powder output parameters are consistent), forming a uniform thin film coating on the surface of the sight glass, and enabling a spray gun to be in full-range non-contact with the surface of the sight glass in the spraying process. The sprayed powder stays stably on the glass surface due to the electrostatic effect.
The following two points need to be noticed in the spraying process:
(1) and (4) checking the glass temperature by using an infrared thermometer, and if the glass temperature is lower than 180 ℃ before spraying, preheating again and continuing spraying.
(2) After the circular motion spraying action is finished, if a coating omission position with obviously less local coating density is found, the residual point is quickly aligned to carry out the additional spraying by using the additional spraying mode of the spray gun.
And after the spraying is finished, the next sintering process is carried out.
2.4. Sintering in a high-temperature furnace:
the sprayed mirror glass is hung in a high-temperature furnace according to the arrangement form in the figure, and the furnace door is closed for high-temperature baking. The maximum baking temperature set in this example was 380 deg.C, and the temperature rise gradient was about 400 deg.C/hr. The sintering residence time after reaching the maximum temperature was 1 hour. After sintering, the furnace door can be opened slowly to dissipate heat and cool, and cooling at nearly constant speed is carried out at 50-80 ℃/h. When the temperature in the furnace is reduced to 200 ℃, namely the temperature is lower than the solidification temperature of the manufactured coating, after the coating is solidified, the glass is taken out and still suspended and placed in a room temperature environment for natural cooling, and the cooling cannot be carried out in a forced air convection mode. The cooling mode is adopted to avoid cracks of the coating caused by rapid cooling.
The finished coated mirror, cooled to room temperature, can be laid on a soft, dust-free table or cardboard prepared in advance for further testing.
When sintering, a plurality of glasses can be put into a high-temperature furnace for simultaneous sintering, but the placing density needs to be controlled so as to prevent the phenomenon that the heating or cooling temperature of the coating is not uniform due to overlarge density, and pockmarks, stripes or other situations occur. For the high temperature furnace used in this embodiment, the number of the internally placed glass mirrors cannot exceed 8.
The third step: finished product inspection
Inspecting a coating film:
before carrying the coated sight glass, the operator is careful to check the length of the fingernail or remove the hand ornaments, and is provided with safety gloves to ensure that the coated surface of the sight glass cannot be scratched.
The items examined mainly include:
1. visual inspection including pockmarks, black spots, impurities, air holes, peeling, powder particles, fingernail scratches, finger prints, and the like. These visual inspection defects are mostly caused by poor cleanliness of the glass surfaces and the interior of the high temperature furnace, or by the operator not operating according to the correct specifications mentioned above. .
2. And (3) film thickness detection: for the products sprayed and sintered in the same batch, a certain number of finished products are extracted for thickness detection, and the detection process refers to the standard HG/T4077-.
In the embodiment, a PositeTector 200 ultrasonic coating tester is adopted for coating detection, and the detector can detect the thickness of a film of 10 micrometers to 2 millimeters. The instrument is calibrated using a standard plate prior to detection.
The thickness of the film layer after sampling detection can be used as the classification basis of the thickness of the coating of the products sprayed and sintered in the same batch: for this example, the PFA coating thickness was in the acceptable range of 40 microns to 80 microns.
The product for sampling detection is slightly separated from the glass surface due to local compression and deformation of the coating at the detection point, and can be placed in a high-temperature furnace for a sintering process again.
The fourth step: defective product remediation
For defective products caused by uneven coating thickness, the defective products can be remedied by repeating the glass spraying process of the second step, the whole process of the second step can be completely repeated, or the process can be started from any partial step of the second step, but the process can be finished to the last step of the second step from any step.
Other examples are summarized
Besides the PFA raw material in this embodiment, the anticorrosive coating raw material that can be used includes PTFE, PFA, FEP, ETFE, HALAR-ECTFE, PVDF, etc., and the process parameters for implementing various raw materials are summarized as follows (heating and spraying equipment are not changed).
Table 1: corresponding process parameters for preparing coating from different raw materials
Except for the PFA raw material in the embodiment, the first step and the second step can be repeated for coating raw materials such as ETFE, ECTFE, PTFE, PVDF and the like, and double-sided anticorrosive coating spraying is carried out.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A preparation method of a glass sight glass with an anticorrosive coating is characterized by comprising the following steps:
polishing and cleaning the edge of the glass, and putting the glass into a high-temperature furnace with a clean inner cavity;
preheating the glass at the temperature of 120-220 ℃ for 15-30 min;
taking out the preheated glass, selecting raw material powder for manufacturing an anticorrosive coating, and spraying the single side of the glass;
and putting the glass into a high-temperature furnace again, sintering at the temperature of 260-380 ℃ for 30-60min, then cooling to the cooling solidification point of the coating material at the cooling speed of 50-80 ℃/h, taking out and putting into a room for natural cooling.
2. The method of claim 1, wherein: the raw material for preparing the anticorrosive coating selected in the step (3) comprises any one of PTFE, PFA, FEP, ETFE, HALAR-ECTFE and PVDF.
3. The method of claim 2, wherein: the particle size of the raw material powder is 20-200 um.
4. The method of claim 1, wherein: and (3) carrying out single-side spraying on the surface of the glass by adopting an electrostatic powder spraying method, and controlling the uniformity of the coating by adopting a flat plate spraying method and combining circumferential movement.
5. The method of claim 1, wherein: the steps (2) to (4) can be repeated for a plurality of times from any one of the steps, and the manufacturing is repeated for each time until the step (4) is finished.
6. The method of claim 1, wherein: the step (1) also comprises the step of firstly sticking a layer of tin foil paper and a layer of high-temperature adhesive tape on one side of the glass, and then putting the glass into a high-temperature furnace.
7. The method of claim 1, wherein: in the step (1), the glass edge is polished to a chamfer with a width of not less than 2 mm.
8. The method of claim 1, wherein: the glass is put into a high-temperature furnace by a suspension method.
9. A glass sight glass with an anticorrosive coating is characterized in that: the method of any one of claims 1 to 8 is used to produce an anti-corrosion coating on one or both sides of the glass.
10. The glass sight glass with an anticorrosive coating according to claim 9, wherein: the thickness of the anti-corrosion coating is uniform and is 50-1800 um.
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2020
- 2020-05-27 CN CN202010460702.3A patent/CN111559872A/en active Pending
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JPH11269672A (en) * | 1998-01-19 | 1999-10-05 | Nakabohtec Corrosion Protecting Co Ltd | Coating corrosion preventing method by organic material |
EP1490217A1 (en) * | 2002-03-05 | 2004-12-29 | Ke-Burgmann A/S | High-flexible laminate for use by protection against aggressive medias and a method for manufacture of same |
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US20190135686A1 (en) * | 2016-04-26 | 2019-05-09 | Pilkington Group Limited | Corrosion resistant coated glass substrate |
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