CN117363211A - Large-area anti-icing and deicing coating with excellent durability and preparation method thereof - Google Patents
Large-area anti-icing and deicing coating with excellent durability and preparation method thereof Download PDFInfo
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- CN117363211A CN117363211A CN202311411523.0A CN202311411523A CN117363211A CN 117363211 A CN117363211 A CN 117363211A CN 202311411523 A CN202311411523 A CN 202311411523A CN 117363211 A CN117363211 A CN 117363211A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
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- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 41
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 41
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 41
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 39
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 34
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- 239000007788 liquid Substances 0.000 claims abstract description 6
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- 239000011203 carbon fibre reinforced carbon Substances 0.000 claims description 8
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052782 aluminium Inorganic materials 0.000 description 20
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- 238000002791 soaking Methods 0.000 description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 description 3
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- SDPQFANFRQYDAO-UHFFFAOYSA-N butyl n,n-diphenylcarbamate Chemical compound C=1C=CC=CC=1N(C(=O)OCCCC)C1=CC=CC=C1 SDPQFANFRQYDAO-UHFFFAOYSA-N 0.000 description 3
- 210000001072 colon Anatomy 0.000 description 3
- RJMRIDVWCWSWFR-UHFFFAOYSA-N methyl(tripropoxy)silane Chemical compound CCCO[Si](C)(OCCC)OCCC RJMRIDVWCWSWFR-UHFFFAOYSA-N 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 125000000304 alkynyl group Chemical group 0.000 description 2
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- LLCSWKVOHICRDD-UHFFFAOYSA-N buta-1,3-diyne Chemical group C#CC#C LLCSWKVOHICRDD-UHFFFAOYSA-N 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 230000000875 corresponding effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- XSXNZQAPLNNSCP-UHFFFAOYSA-N ethynyl-methyl-diphenylsilane Chemical compound C=1C=CC=CC=1[Si](C#C)(C)C1=CC=CC=C1 XSXNZQAPLNNSCP-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
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- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229920001709 polysilazane Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 1
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- 229920000642 polymer Polymers 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000003361 porogen Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention belongs to the technical field of anti-icing and deicing, and particularly relates to a large-area anti-icing and deicing coating with excellent durability and a preparation method thereof. The method of the invention uses SiO 2 Adding the dispersion liquid into an elastomer prepared from PDMS prepolymer and a normal temperature curing agent, and uniformly mixing to obtain a coating solution; the viscosity of the PDMS prepolymer is 3000-4000 mPa.s, and the molecular weight is 120000-130000; the mass ratio of the PDMS prepolymer to the normal temperature curing agent is 1:1; and finally, slowly and uniformly coating the coating solution on a substrate to form a film with the thickness less than or equal to 220 micrometers, so as to prepare the large-area anti-icing and deicing coating with excellent durability.
Description
Technical Field
The invention belongs to the technical field of anti-icing and deicing, and particularly relates to a large-area anti-icing and deicing coating with excellent durability and a preparation method thereof.
Background
Aircraft and wind turbine blades are often required to continue to operate in cold, harsh environments, and thus the surfaces are prone to icing. Surface icing can alter the shape of the surfaces of aircraft and wind turbine blades, increasing surface roughness, causing changes in aerodynamic performance. In severe cases, icing can even lead to aircraft failure, compromising crew life safety. In addition, the continuous ice accumulation can cause the problems of overload of the fan blades, uneven ice load distribution on the surfaces of the blades and the like, so that the wind driven generator breaks down and even stops running.
The traditional deicing technical method comprises spraying an anti-icing solution, mechanically deicing, thermally deicing and the like, but the defects of low deicing efficiency, high preparation cost and the like still exist in the whole, so that the practical application in the field of large-area deicing is limited. On the other hand, the academia suggests that bionic-based superhydrophobic and superlubricating coatings are effective methods for preventing or delaying icing. This is because there are a large number of air cushions in the micro-nano structure of the superhydrophobic coating, which can effectively delay icing and reduce the adhesive strength of ice. For example, ice is separated by a lubricant layer when it contacts the surface of the super-lubricious coating, thereby greatly reducing the adhesive strength of the ice. However, the ice adhesion of superhydrophobic and superlubricating coatings is positively correlated with the area of ice formation, and as the area of ice formation increases, the ice adhesion increases, so that it does not perform well in deicing when used in large area structures such as aircraft and turbine blade surfaces. In addition, superhydrophobic and superlubricating coatings are often less durable. The rough structure of the super-hydrophobic coating is easy to damage, and the anti-icing performance is further lost; the lubricant of the super-lubricating coating is lost during use, thereby reducing the anti-icing performance. Therefore, the conventional deicing technique and the common super-hydrophobic/super-lubricating coating which are commonly used at present are difficult to apply to large-area surfaces such as airplanes, fan blades and the like.
In addition, some scholars have produced low interfacial toughness coatings with a degree of large area deicing performance. However, the preparation method of the coating is mostly complicated, and various materials are needed to be added for preparation, but the more the types of the materials are, the higher the requirements on the preparation method are, and further the process cost is also higher, and the price of some raw materials with low interface toughness is relatively high, so that the coating is not beneficial to being expanded into industrial mass production application. On the other hand, currently reported low interfacial toughness coatings mostly lack evaluation and demonstration of durability. The patent with the application number of CN202211540809.4 and the name of a preparation method of a large-area deicing coating discloses that the surface structure of the coating is changed by adding PVC powder which is a low-interface toughness material into Ecofelx silica gel, so that wrinkles and protruding structures are generated, local stress is generated, the adhesion force of ice is reduced, and the shearing modulus of the surface of the coating is reduced by adding glycerol which is a plasticizer, so that the positive correlation characteristic of the adhesion strength and the icing area of the surface of the traditional silicon rubber coating is overcome, and the effect that the adhesion force of ice gradually tends to a lower stable value when the icing area tends to be infinite is achieved. However, the length of the condensed ice surface in the method reaches more than 80cm, so that a stable ice removing force can be realized. In addition, the method of the patent is not perfect in ice removing force measurement, and only a few distances are selected for measurement, and 20 durability tests are also selected for the measurement in the corresponding paper Soft and Rigid Integrated Durable Coating for Large-Scale Deicing. The patent with the application number of CN202010100962.X and the name of 'a porous material with low interface toughness for large-area deicing and a preparation method thereof' discloses a porous material with low interface toughness for large-area deicing, which is prepared by introducing a uniform porous structure under the surface of a smooth polymer, reducing the interface toughness of the material so as to promote the initiation and the expansion of broken cracks at the ice fixing interface. The porous elastic coating disclosed by the patent is obtained by uniformly mixing A, B components of PDMS184 and pore-forming agents (Span 80 and Tween 80) and then curing, and then removing the pore-forming agents by using absolute ethyl alcohol. However, the elastic coating is easily detached from the substrate during removal of the porogen, so that the adhesion of such elastic coating to the substrate is generally poor. In addition, the porous structure of the coating plays a role in crack initiation, but also reduces the mechanical properties of the coating, so that the coating is easy to damage in the process of cyclic icing and deicing. In summary, it is assumed that the durability of such porous elastic coatings is relatively general, and that the patent does lack long-term durability evaluation and demonstration.
Disclosure of Invention
In view of the above, the invention aims to provide a low-interface-toughness large-area anti-icing deicing coating with long durability and a preparation method thereof, and the specific technical scheme is as follows.
A preparation method of a large-area anti-icing and deicing coating with good durability comprises the following steps:
step 1: low boiling point organic solvent and SiO 2 Uniformly mixing the particles to obtain SiO 2 A dispersion;
as a preference, the dispersion can be prepared at a faster rate or with a more uniform degree by means of magnetic stirring and/or ultrasonic dispersion.
Step 2: uniformly mixing PDMS prepolymer and normal temperature curing agent to prepare an elastomer solution, and then uniformly mixing the SiO 2 Adding the dispersion liquid into the elastomer (PDMS prepolymer and normal temperature curing agent) solution, and uniformly mixing to obtain a coating solution; the viscosity of the PDMS prepolymer is 3000-4000 mPa.s, and the molecular weight is 120000-130000; the mass ratio of the PDMS prepolymer to the normal temperature curing agent is 1:1, and the SiO is 2 The particles account for 1 to 15 percent of the mass ratio of the elastomer solution (PDMS prepolymer and normal temperature curing agent);
step 3: and (3) slowly and uniformly coating the coating solution obtained in the step (2) on a substrate, and curing for 24-48h at room temperature to form the large-area anti-icing and deicing coating with the thickness of less than or equal to (less than or equal to) 220 micrometers.
As a preference, curing is carried out at room temperature for 24-48 hours to form a large-area anti-icing and deicing coating of 80-220 microns.
Further, the PDMS prepolymer has a viscosity of 3000-3500 mPas, including 3000 mPas, 3100 mPas, 3200 mPas, 3300 mPas, 3400 mPas and 3500 mPas.
Further, the PDMS prepolymer molecular weight includes 120000-121000, 121000-122000, 122000-123000, 123000-124000, 124000-125000, 125000-126000, 126000-127000, 127000-128000, 128000-129000 and 129000-130000.
Further, the substrate comprises a surface of an aircraft and/or wind turbine blade.
Further, the low boiling point organic solvent includes tetrahydrofuran (boiling point 66 ℃), chloroform (boiling point 61 ℃), methylene chloride (boiling point 39.8 ℃), ethyl acetate (boiling point 76 ℃) or n-hexane (boiling point 69 ℃).
Further, the SiO 2 The particles comprise micro-scale and/or nano-scale SiO 2 The particle size range of the particles comprises 500 nanometers to 1 micrometer or 3 to 40 nanometers。
Further, the ambient temperature curing agent is a curing agent which does not contain carbon-carbon triple bonds but contains groups capable of undergoing crosslinking (mainly, in the present invention, crosslinking with PDMS prepolymer), and the groups capable of undergoing crosslinking include amino groups, hydroxyl groups, and/or carboxyl groups.
Preferably, the normal temperature curing agent comprises methyltriethoxysilane, methyltripropoxysilane, butyl diphenylcarbamate (dbp), dibenzoyl peroxide (bpo), or the like.
Further, the SiO 2 The mass ratio of the particles to the elastomer (PDMS prepolymer plus the normal temperature curing agent) is 1%, 3%, 5%, 10% or 15%.
Preferably, the SiO 2 The mass ratio of the particles to the elastomer (PDMS prepolymer plus a curing agent at normal temperature) is 1%, 3% or 5%.
Further, the SiO 2 SiO in the dispersion 2 The mass ratio of the particles in the low-boiling point organic solvent is 0.5% -8.0%.
Further, in step 1, a low boiling point organic solvent is mixed with SiO 2 The operation of uniformly mixing the particles comprises the steps of firstly magnetically stirring for 5-15min at the speed of 300-500 r/min, and then carrying out ultrasonic vibration for 5-15min at the power of 300-1000W.
Further, siO is added in step 2 2 The operation of adding the dispersion liquid into the PDMS prepolymer and the normal temperature curing agent for uniform mixing comprises the steps of firstly magnetically stirring for 5-10min at the speed of 300-500 r/min, and then carrying out ultrasonic vibration for 5-10min at the power of 300-1000W.
Further, the method of applying the coating solution to the substrate in step 3 includes direct pouring, drop coating, blade coating, bar coating, spin coating, brush coating, and/or spray coating.
The large-area anti-icing deicing coating prepared by the preparation method is prepared.
Preferably, the large-area anti-icing and deicing coating prepared by the invention contains SiO 2 The mass fraction of the particles is 1% or 3%, and the thickness of the coating is less than or equal to 220 microns.
The large-area anti-icing deicing coating can be used for long-time anti-icing deicing of scenes such as airplanes, wind turbine blades and the like.
Beneficial technical effects
1) The invention prepares the elastomer by simplified material proportion and only crosslinking PDMS prepolymer with specific viscosity and molecular weight and normal temperature curing agent without carbon-carbon triple bond, and then further adds SiO with specific proportion into the elastomer 2 And finally, coating the particles on a substrate to obtain the low-interface-toughness large-area anti-icing and deicing coating (film) with excellent durability. The invention uses micro-scale or nano-scale SiO 2 The particles are hard in texture and do not have a low interfacial toughness per se, but are less expensive than PVC powder (soft) which is a low interfacial toughness material, but SiO is hard with this texture 2 The coating prepared by the particles and the elastomer has lower constant ice removing force and ice adhesion strength after 120 icing/deicing cycle experiments. In addition, the invention also proves that the constant deicing force and the interface toughness of the prepared coating are very low when the film thickness of the prepared coating is less than 220 microns, wherein the constant deicing force is lower than that of the research of other scholars published in the core journal in the field, and the prepared coating has excellent durability and low interface toughness, and is suitable for deicing large-area surface icing of an airplane and/or a wind turbine blade.
2) The invention crosslinks PDMS prepolymer with specific molecular weight and viscosity and curing agent without carbon-carbon triple bond, and adds SiO with specific mass ratio into the prepolymer 2 Particles, a stable elastomer-particle mixed system coating is obtained, when SiO 2 When the addition amount of the particles is 3%, the constant deicing force of the coating is reduced after a plurality of icing/deicing cycle experiments, which proves that the SiO 2 The addition of microparticles can significantly improve the durability of the coating.
3) The critical icing size of the coating prepared by the method is only tens of centimeters, which is smaller than the critical icing area/size of other coatings in the prior art and is also far smaller than the area of the aircraft wing or fan blade, so that the durable anti-icing and deicing of the scene can be completely realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. Like elements or portions are generally identified by like reference numerals throughout the several figures. In the drawings, elements or portions thereof are not necessarily drawn to scale. It will be apparent to those of ordinary skill in the art that the drawings in the following description are of some embodiments of the invention and that other drawings may be derived from these drawings without inventive faculty.
FIG. 1 is an infrared spectrum of different PDMS prepolymers and curing agents;
FIG. 2 is a coating microstructure of the present invention;
FIG. 3 is a three-dimensional topography and surface roughness of a coating according to the present invention;
FIG. 4 is a graph of a coating wettability investigation experiment of the present invention;
FIG. 5 is a graph of an experimental investigation of the de-icing force of the coating of the present invention;
FIG. 6 is a graph of an experimental investigation of apparent ice adhesion strength of a coating according to the present invention;
FIG. 7 is a summary of experimental graphs of constant de-icing force, critical length, interfacial toughness, and ice adhesion strength for a coating of the present invention;
FIG. 8 is a graph of a wettability durability test of the coating of the present invention;
FIG. 9 is a graph of experimental investigation of constant de-icing force and interfacial toughness durability of a coating according to the present invention;
FIG. 10 is a graph of experimental investigation of critical length and ice adhesion strength durability of the coating of the present invention;
FIG. 11 is a graph showing the ice detachment force test of different PDMS prepolymer coatings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Herein, "and/or" includes any and all combinations of one or more of the associated listed items.
Herein, "plurality" means two or more, i.e., it includes two, three, four, five, etc.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
As used in this specification, the term "about" is typically expressed as +/-5% of the value, more typically +/-4% of the value, more typically +/-3% of the value, more typically +/-2% of the value, even more typically +/-1% of the value, and even more typically +/-0.5% of the value.
In this specification, certain embodiments may be disclosed in a format that is within a certain range. It should be appreciated that such a description of "within a certain range" is merely for convenience and brevity and should not be construed as a inflexible limitation on the disclosed ranges. Accordingly, the description of a range should be considered to have specifically disclosed all possible sub-ranges and individual numerical values within that range. For example, a rangeThe description of (c) should be taken as having specifically disclosed sub-ranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as individual numbers within such ranges, e.g., 1,2,3,4,5, and6. the above rule applies regardless of the breadth of the range.
The low-boiling point organic solvent refers to an organic solvent with a boiling point of less than 80 ℃.
The term "normal temperature curing agent" as used herein refers to a curing agent that can crosslink with PDMS prepolymer at normal temperature, for example, at room temperature without heating.
Example 1
Scheme 1: the scheme provides a preparation method of a material which does not contain SiO 2 Method for preparing anti-icing and deicing coating
1. Material
The substrate used was 1060 aluminum plate with dimensions of 20 cm. Times.30 cm. Times.1 mm, supplied by Shenzhen Hongnian metal materials Co., ltd. PDMS prepolymer model C0030, molecular weight 128449, viscosity 3000 mPas, supplied by Hangzhou micro-Innovation technologies Co. Optional ambient temperature curing agents include methyltriethoxysilane, methyltripropoxysilane, butyl diphenylcarbamate (dbp) or dibenzoyl peroxide (bpo), without carbon-carbon triple bonds (C.ident.C bonds). Tetrahydrofuran was supplied by Colon Chemicals Inc. of Chemicals, chemie, inc. of Chemie, du. Absolute ethanol was purchased from Chongqing Chuan Dong chemical Co., ltd. All reagents were used without purification.
2. Preparation flow
Firstly, tetrahydrofuran and absolute ethyl alcohol are used for respectively soaking and cleaning the 1060 aluminum plate, so as to remove residual stains on the surface. And then deionized water is used for cleaning to remove superfluous tetrahydrofuran and absolute ethyl alcohol on the surface. And after the cleaning is finished, the aluminum plate is put into an oven for drying for standby. The mass of the PDMS prepolymer and the mass of the curing agent at normal temperature are 12g (1:1). And mixing the PDMS prepolymer and the normal-temperature curing agent to prepare an elastomer solution, slowly and uniformly pouring the fully mixed elastomer solution onto an aluminum plate inclined at 45 degrees, and vertically placing the aluminum plate for 5 minutes to remove the redundant solution. Finally, the film was cured in a room temperature environment for 36h to form a 101 μm film structure. Such as heating, may accelerate the cure time.
Scheme 2: the scheme provides SiO with different contents 2 Method for preparing anti-icing and deicing coating
1. Material
The substrate used was 1060 aluminum plate with dimensions of 20 cm. Times.30 cm. Times.1 mm, supplied by Shenzhen Hongnian metal materials Co., ltd. PDMS prepolymer model C0030, molecular weight 128449, viscosity 3000 mPas, supplied by Hangzhou micro-Innovation technologies Co. Alternative curing agents include methyltriethoxysilane, methyltripropoxysilane, butyl diphenylcarbamate (dbp) or dibenzoyl peroxide (bpo), without carbon-carbon triple bonds (C.ident.C bonds). The silica powder has an average particle diameter of 3-40nm and is purchased from Shanghai Michlin Biochemical technology Co., ltd (SiO with a particle diameter of 500 nm-1 μm may also be used) 2 Particles). Tetrahydrofuran is supplied by the Chemicals Co., ltd (other low boiling point organic solvents may be used as well as provided by the present invention). Absolute ethanol was purchased from Chongqing Chuan Dong chemical Co., ltd. All reagents were used without purification.
2. Preparation flow
Firstly, tetrahydrofuran and absolute ethyl alcohol are used for respectively soaking and cleaning the 1060 aluminum plate, so as to remove residual stains on the surface. And then deionized water is used for cleaning to remove superfluous tetrahydrofuran and absolute ethyl alcohol on the surface. And after the cleaning is finished, the aluminum plate is put into an oven for drying for standby. 50g of tetrahydrofuran and SiO of different masses 2 The microparticles were placed in a beaker (SiO) 2 The mass ratio of the particles in the tetrahydrofuran is 0.5% -8.0%), magnetic stirring is carried out for 10 minutes at the speed of 300-500 r/min, and ultrasonic vibration is carried out for 10 minutes at the power of 500-1000W to obtain SiO 2 And (3) a dispersion. Next, uniformly mixing the PDMS prepolymer and the normal temperature curing agent in a mass ratio of 1:1 to prepare an elastomer solution (the mass of the PDMS prepolymer and the normal temperature curing agent is 12 g), and further adding SiO 2 The dispersion liquid is magnetically stirred at the speed of 300-500 r/min, and is subjected to ultrasonic vibration at the power of 500-1000W for 5 minutes, so that a uniformly mixed coating solution is obtained.
To produce coatings of different mass fractions (0%, 1%, 3%, 5%, 10%, 15%, 20% and 25%), siO was added 2 The mass of the powder was 0.00g, 0.25g, 0.75g, 1.26g, 2.67g, 4.23g, 6.00g and 8, respectively.00g. And slowly and uniformly pouring the finally prepared coating solution onto an aluminum plate inclined at 45 degrees, and vertically placing the aluminum plate for 5 minutes to remove redundant solution. And finally, curing for 36h in a room temperature environment to form the large-area anti-icing and deicing coating with the 80-220 micrometer film structure. Such as heating, may accelerate the cure time.
Example 2
The present embodiment provides another material that does not contain SiO 2 Method for preparing anti-icing and deicing coating
1. Material
The substrate used was 1060 aluminum plate with dimensions of 20 cm. Times.30 cm. Times.1 mm, supplied by Shenzhen Hongnian metal materials Co., ltd. The PDMS prepolymer was C105, having a molecular weight of 30981 and a viscosity of 5000 mPas, available from Hangzhou micro-computer technology Co. The optional normal temperature curing agent contains carbon-carbon triple bonds, including methyl diphenyl ethynyl silane, organic polysilazane, diacetylene end-capped silazane or alkynyl polyethylene glycol silane, and the like. Tetrahydrofuran was supplied by Colon Chemicals Inc. of Chemicals, chemie, inc. of Chemie, du. Absolute ethanol was purchased from Chongqing Chuan Dong chemical Co., ltd. All reagents were used without purification.
2. Preparation flow
Firstly, tetrahydrofuran and absolute ethyl alcohol are used for respectively soaking and cleaning the 1060 aluminum plate, so as to remove residual stains on the surface. And then deionized water is used for cleaning to remove superfluous tetrahydrofuran and absolute ethyl alcohol on the surface. And after the cleaning is finished, the aluminum plate is put into an oven for drying for standby. The mass of the PDMS prepolymer and the mass of the curing agent at normal temperature are 12g. And (3) mixing the PDMS prepolymer and the normal-temperature curing agent to obtain a control elastomer solution 1, slowly and uniformly pouring the fully mixed solution onto an aluminum plate inclined at 45 degrees, and vertically placing the aluminum plate for 5 minutes to remove the redundant solution. Finally, curing for 48h in a room temperature environment forms a 92.4 μm film structure. Such as heating, may accelerate the cure time.
Example 3
The present embodiment provides another material that does not contain SiO 2 Method for preparing anti-icing and deicing coating
1. Material
The substrate used was 1060 aluminum plate with dimensions of 20 cm. Times.30 cm. Times.1 mm, supplied by Shenzhen Hongnian metal materials Co., ltd. The PDMS prepolymer was of type P184, molecular weight 147757 and viscosity 3500 mPa.s, available from Guangzhou photoelectric New technology Co. The optional normal temperature curing agent contains carbon-carbon triple bonds, including methyl diphenyl ethynyl silane, organic polysilazane, diacetylene end-capped silazane or alkynyl polyethylene glycol silane, and the like. Tetrahydrofuran was supplied by Colon Chemicals Inc. of Chemicals, chemie, inc. of Chemie, du. Absolute ethanol was purchased from Chongqing Chuan Dong chemical Co., ltd. All reagents were used without purification.
2. Preparation flow
Firstly, tetrahydrofuran and absolute ethyl alcohol are used for respectively soaking and cleaning the 1060 aluminum plate, so as to remove residual stains on the surface. And then deionized water is used for cleaning to remove superfluous tetrahydrofuran and absolute ethyl alcohol on the surface. And after the cleaning is finished, the aluminum plate is put into an oven for drying for standby. The mass of the PDMS prepolymer and the mass of the curing agent at normal temperature are 12g. And (3) mixing the PDMS prepolymer and the normal-temperature curing agent to obtain a control elastomer solution 2, slowly and uniformly pouring the fully mixed solution onto an aluminum plate inclined at 45 degrees, and vertically placing the aluminum plate for 5 minutes to remove the redundant solution. Finally, curing for 48h in a room temperature environment forms a film structure of 107.9 μm. Such as heating, may accelerate the cure time.
Example 4
Experiment verification
1. Characterization of
The microtopography and elemental distribution were characterized using scanning electron microscopy (SEM, zeiss Auriga, germany) and energy spectroscopy (EDS). The three-dimensional structure was observed and the surface roughness was measured using a laser confocal microscope (LEXT OLS 4000). The Contact Angle (CA) and the Contact Angle Hysteresis (CAH) were measured using a water contact angle measuring instrument (SINDIN SDC-100). The volume of the measured water drops was about 5 μl, and five positions were measured and averaged.
Measurements of ice adhesion strength and ice detachment force were performed using a semiconductor refrigeration platform of 20cm x 40 cm. Rectangular stainless steel molds with different sizes were customized. The width and the height of the die are 10mm, and the lengths are respectively: 5mm, 10mm, 20mm, 40mm, 60mm, 80mm, 100mm, 125mm, 150mm, 175mm, 200mm and 250mm. The mold was placed horizontally on the surface of the coating and tap water was injected flush with the height of the mold. The temperature of the cooling plate was set to-10 ℃ and maintained for more than 1 hour to ensure complete freezing of the water in the mold. The self-made horizontal moving guide rail is utilized to drive the thrust meter to slowly push the die at the speed of 74 mu m/s, so that the die is separated from the surface of the coating. The maximum thrust force measured at this time is the ice-breaking force. The ice adhesion strength can be calculated by dividing the ice removal force by the actual contact area of the ice with the coating. The contact point of the thrust meter was 2mm in height from the surface of the coating. All coatings were measured more than 3 times in duplicate.
2. Results
2.1 Effect of different PDMS on coating Properties
TABLE 1 coating Properties of different elastomers
The interfacial toughness value is calculated according to the constant ice-removing force, the modulus of ice and the thickness of ice, and the modulus of ice and the thickness of ice are kept unchanged in the test process, so that the interfacial toughness and the constant ice-removing force are in positive correlation. When a lower interfacial toughness means a lower constant de-icing force, de-icing is facilitated. In addition, the interface toughness also shows the expansion capability of micro cracks of the interface, and the lower the interface toughness value is, the more favorable for crack expansion and deicing. However, the lower the interfacial toughness value is, the better, and when the interfacial toughness value is too low, the durability of the coating layer is not good, so that further optimization is required from the viewpoint of the overall properties of the coating layer.
Conclusion: the test only examines the aspects of constant ice removing force and interface toughness of the coating, and the viscosity and molecular weight of different PDMS prepolymers can influence the constant ice removing force and interface toughness of the prepared coating (film). The coating (film) prepared from PDMS prepolymer with large molecular weight and low viscosity is better in deicing performance. In addition, the type of chemical bonds in the curing agent also affects the crosslinking of the PDMS prepolymer, and thus the elastomeric coating prepared from the PDMS prepolymer having the relatively minimum viscosity and molecular weight and the curing agent having no c≡c bonds was screened for further experiments. The infrared spectra of the PDMS prepolymer and the curing agent of the present example are shown in FIG. 1.
2.2 different SiO 2 Influence of quality
According to the preparation method of scheme 2 of example 1, it was verified that SiO was added in different mass ratios 2 Various properties of (3)
TABLE 2 constant de-icing force and critical length of coating
Conclusion: 1) The critical length in this experiment refers to the length of ice formation where the de-icing force is no longer changing, see fig. 5. 20% or more of SiO is added 2 After the particles, no constant de-icing force was observed in the graph of fig. 5, so 20% and 25% have no corresponding data. 2) Along with SiO 2 The addition of the particles increases the constant ice removal force, so that 1%, 3% and 5% of SiO is selected 2 The amount of the fine particles added is controlled to control the constant ice removing force within a range as small as possible.
TABLE 3 coating ice adhesion Strength and critical length
| SiO 2 Additive amount | Ice adhesion strength (kPa) | Critical value length (cm) |
| 0 | 16.38241 | 11.01 |
| 1％ | 22.08508 | 11.66 |
| 3％ | 24.72037 | 12.86 |
| 5％ | 30.04075 | 13.78 |
| 10％ | 37.83962 | 14.59 |
| 15％ | 49.24642 | 15.72 |
| 20％ | 82.61585 | / |
| 25％ | 113.81412 | / |
Conclusion: the critical value length in this experiment refers to the icing length that the ice adhesion strength is not changed any more, and the experimental chart is shown in fig. 6, as in table 2. The critical length is present, which results in a start of decrease in ice adhesion strength, consistent with the trend of ice removal force.
TABLE 4 coating durability
Conclusion: the experiment examines different SiO 2 The number of icing/deicing cycles of the particulate addition, i.e., the durability of the coating. The experimental results in Table 1 show that SiO is not added 2 The elastomeric coating of the microparticles had the best constant deicing force and interfacial toughness, and this experiment demonstrated that no SiO was added as the number of freeze/deicing cycles increased 2 The elastomeric coating of the microparticles has a constant de-icing force and ice adhesion strength exceeding the moderate amount of added SiO 2 Is a coating of (a). Wherein, when the icing/deicing cycle experiment is 60 times, siO is not added 2 The coating of (2) increased by about 173% over the constant de-icing force at 0 trials; adding 1% SiO 2 The constant de-icing force increases by about 21.4% over the coating of 0 experiments; adding 3% SiO 2 The coating of (2) increased by about 24% compared to the constant de-icing force at 0 experiments. When the icing/deicing cycle experiment was 120 experiments, no SiO was added 2 The constant de-icing force increases by about 254% compared to the coating of 0 experiments; adding 1% SiO 2 The constant de-icing force increases by about 62% compared to the coating of 0 experiments; adding 3% SiO 2 The coating of (2) increased by about 20.5% over the constant de-icing force at 0 trials. Adding 3% SiO 2 After 120 icing/deicing cycle experiments, the constant deicing force is reduced compared with 60 experiments, which indicates that a proper amount of SiO is added 2 The durability of the coating can be significantly increased.
2.3 Effect of different coating film thicknesses
According to the method of scheme 2 of example 1, siO is selected 2 The mass fraction is 1% to prepare the coatings with different thicknessesAnd (5) a layer film. The performance of coatings of different thicknesses was verified according to the de-icing force experiment.
TABLE 5 influence of different coating film thicknesses
| Film thickness | Constant ice-breaking force (N/cm) | Interfacial toughness (J/m) 2 ) |
| 79.1 micrometers | 18.24 | 0.020 |
| 93.7 micrometers | 25.75 | 0.039 |
| 125.4 micrometers | 31.39 | 0.058 |
| 185.4 micrometers | 42.07 | 0.104 |
| 253.3 micrometers | 51.87 | 0.158 |
Conclusion: the experiment examines the constant ice removing force and the interface toughness of the coating films with different thicknesses, and the experiment finds that the thicker the film is, the larger the constant ice removing force can be. However, too thin a film places high demands on the coating process and durability may be inadequate. The minimum constant ice removal force of 49.6N/cm was measured by the present scholars in the paper "A process self-assembly PTFE coating for effective large-scaling", journal Progress in Organic Coatings, and therefore the present invention chooses a 50N/cm defined value, and the thick film at this time corresponds to about 221.2 microns, and therefore the present invention chooses a preparation method in which the thickness of the coating film is less than or equal to 220 microns.
The embodiments of the present invention have been described above with reference to the accompanying drawings, but the present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and many forms may be made by those having ordinary skill in the art without departing from the spirit of the present invention and the scope of the claims, which are to be protected by the present invention.
Claims (10)
1. The preparation method of the large-area anti-icing and deicing coating with good durability is characterized by comprising the following steps of:
step 1: low boiling point organic solvent and SiO 2 Uniformly mixing the particles to obtain SiO 2 A dispersion;
step 2: uniformly mixing PDMS prepolymer and normal temperature curing agent to prepare an elastomer solution, and then uniformly mixing the SiO 2 Adding the dispersion liquid into the elastomer solution, and uniformly mixing to obtain a coating solution; the viscosity of the PDMS prepolymer is 3000-4000 mPa.s, and the molecular weight is 120000-130000; the mass ratio of the PDMS prepolymer to the normal temperature curing agent is 1:1, and the SiO is 2 The particles account for 1 to 15 percent of the mass ratio of the elastomer solution;
step 3: and (3) slowly and uniformly coating the coating solution obtained in the step (2) on a substrate, and curing for 24-48h at room temperature to form the large-area anti-icing and deicing coating with the thickness of less than or equal to 220 micrometers.
2. The method of claim 1, wherein the low boiling point organic solvent comprises tetrahydrofuran, chloroform, methylene chloride, ethyl acetate, or n-hexane.
3. The method of claim 1, wherein the SiO is 2 The particles comprise micro-scale and/or nano-scale SiO 2 The particle size range includes 500 nm to 1 micron or 3 to 40 nm.
4. The method of claim 1, wherein the ambient temperature curing agent is a curing agent that does not contain carbon-carbon triple bonds but contains crosslinkable groups including amino, hydroxyl and/or carboxyl groups.
5. The method of claim 1, wherein the SiO is 2 The particles account for 1%, 3%, 5%, 10% or 15% of the mass of the elastomer.
6. The method of claim 1, wherein the SiO is 2 SiO in the dispersion 2 The mass ratio of the particles in the low-boiling point organic solvent is 0.5% -8.0%.
7. The process according to claim 1, wherein a low-boiling organic solvent is mixed with SiO 2 The operation of uniformly mixing the particles comprises the steps of firstly magnetically stirring for 5-15min at the speed of 300-500 r/min, and then carrying out ultrasonic vibration for 5-15min at the power of 300-1000W.
8. The process according to claim 1, wherein SiO is prepared by 2 The operation of adding the dispersion liquid into the PDMS prepolymer and the normal temperature curing agent for uniform mixing comprises the steps of firstly magnetically stirring for 5-10min at the speed of 300-500 r/min, and then carrying out ultrasonic vibration for 5-10min at the power of 300-1000W.
9. The method of claim 1, wherein the method of applying the coating solution to the substrate comprises direct pouring, drop coating, knife coating, bar coating, spin coating, brush coating, and/or spray coating.
10. A large area anti-icing and deicing coating prepared by the method of any one of claims 1-9.
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