CN115304404A - SiO (silicon dioxide) 2f /SiO 2 Composite hydrophobic coating and preparation method thereof - Google Patents
SiO (silicon dioxide) 2f /SiO 2 Composite hydrophobic coating and preparation method thereof Download PDFInfo
- Publication number
- CN115304404A CN115304404A CN202210889769.8A CN202210889769A CN115304404A CN 115304404 A CN115304404 A CN 115304404A CN 202210889769 A CN202210889769 A CN 202210889769A CN 115304404 A CN115304404 A CN 115304404A
- Authority
- CN
- China
- Prior art keywords
- sio
- composite material
- hydrophobic coating
- drying
- composite
- 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
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 229910004298 SiO 2 Inorganic materials 0.000 title claims abstract description 57
- 238000000576 coating method Methods 0.000 title claims abstract description 36
- 239000011248 coating agent Substances 0.000 title claims abstract description 30
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 15
- 238000002360 preparation method Methods 0.000 title claims description 12
- 235000012239 silicon dioxide Nutrition 0.000 title claims description 10
- 239000000377 silicon dioxide Substances 0.000 title claims description 5
- 238000005507 spraying Methods 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229920002050 silicone resin Polymers 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- HUZZQXYTKNNCOU-UHFFFAOYSA-N triethyl(methoxy)silane Chemical compound CC[Si](CC)(CC)OC HUZZQXYTKNNCOU-UHFFFAOYSA-N 0.000 claims description 5
- 229910008051 Si-OH Inorganic materials 0.000 claims description 4
- 229910006358 Si—OH Inorganic materials 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- DFJDZTPFNSXNAX-UHFFFAOYSA-N ethoxy(triethyl)silane Chemical compound CCO[Si](CC)(CC)CC DFJDZTPFNSXNAX-UHFFFAOYSA-N 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 230000002787 reinforcement Effects 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 230000002152 alkylating effect Effects 0.000 abstract description 2
- 230000004888 barrier function Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 238000007789 sealing Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000029936 alkylation Effects 0.000 description 4
- 238000005804 alkylation reaction Methods 0.000 description 4
- 125000001165 hydrophobic group Chemical group 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 239000011825 aerospace material Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLXGCFTYXICXJF-UHFFFAOYSA-N ethylsilicon Chemical compound CC[Si] XLXGCFTYXICXJF-UHFFFAOYSA-N 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical compound CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 description 1
- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/82—Coating or impregnation with organic materials
- C04B41/84—Compounds having one or more carbon-to-metal of carbon-to-silicon linkages
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
- C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
- C04B41/495—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as oligomers or polymers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/522—Oxidic
- C04B2235/5228—Silica and alumina, including aluminosilicates, e.g. mullite
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses SiO 2f /SiO 2 A hydrophobic coating with the moisture absorption rate lower than 1% is obtained by alkylating a composite material and spraying organic silicon resin, and compared with the prior art, the hydrophobic coating has the advantages of high water vapor barrier, high low-temperature stability and high weather resistance, and can realize ultralow moisture resistance of an antenna cover and an antenna window stored in a severe environment.
Description
Technical Field
The invention belongs to the technical field of composite material coatings, and particularly relates to SiO 2f /SiO 2 A composite material hydrophobic coating and a preparation method thereof.
Background
The antenna housing is used as a protection part of a missile radar seeker antenna, and has excellent thermal and mechanical properties and stable wave-transmitting performance. With the continuous improvement of the flight speed, the hitting range and the guidance precision of the spacecraft, the antenna housing has to have good and stable wave-transmitting performance, better thermal shock resistance and more excellent weather resistance in a wider frequency band. The quartz fiber reinforced quartz (SiO) which is used in the existing equipment 2f /SiO 2 ) The wave-transmitting composite material has the advantages that water absorption is promoted due to free hydroxyl and holes on the surface, moisture absorption phenomena are caused, the dielectric constant and the dielectric loss tangent are increased after moisture absorption, the wave-transmitting performance is extremely reduced, and the electrical performance of the antenna housing is seriously influenced. The moisture-proof coating prepared on the surface of the material with the porous structure can effectively solve the series of problems. Existing moisture resistant coatings are divided into inorganic coatings and polymer coatings. The preparation of inorganic coatings generally requires higher temperature, has larger damage to materials, and is easy to crack and fall off because of the mismatching of the thermal expansion coefficients of the coatings and a matrix; the organic coating mainly comprises organic fluororesin (Wangxin, paint industry, 47 (10): 2017) and organic silicon resin (Zengjiaping, aerospace material technology, 3. The organic fluorine resin is unfavorable for wave permeability of the composite material and influences guidance, the moisture absorption rate of the organic silicon resin is high (generally more than 2.5 percent) although the hydrophobicity is excellent, and powder is required to be added as a hole sealing agent in the preparation of the two methods, so that the cost is increased. Patent CN110218102A discloses a hydrophobic SiO2f/SiO2 wave-transmitting material and a preparation method thereof, which, through physical adsorption bonds such as hydrogen bonds, generates cohesive force and a sealing effect on a substrate, can weaken the adsorption of water and improve the moisture resistance, but the physical adsorption bonds have small adsorption force, low stability and limited moisture resistance.
Disclosure of Invention
In view of the disadvantages of the prior art, the present invention provides a SiO 2f /SiO 2 The hydrophobic coating with the moisture absorption rate lower than 1% is obtained by generating chemical bonds and bonding surface hydrophobic groups by using the chemical bonds, and the moisture resistance is further improved.
The technical scheme adopted by the invention is as follows:
in one aspect, the present invention provides a SiO 2f /SiO 2 The preparation method of the composite material hydrophobic coating comprises the following steps:
1)SiO 2f /SiO 2 a composite material pretreatment step: firstly, siO 2f/ SiO 2 Cutting the composite material into a proper size, putting the composite material into acetone for ultrasonic soaking, removing oil stains on the surface and silica sol particles, and drying the composite material in the air to obtain pretreated SiO 2f /SiO 2 A composite material;
2)SiO 2f /SiO 2 composite material alkylation: siO pretreated in the step 1) 2f /SiO 2 Soaking the composite material in ethanol solution containing silane coupling agent, condensing and refluxing, washing with ethanol, and vacuum drying to obtain alkylated SiO 2f /SiO 2 A composite material;
3)SiO 2f /SiO 2 the preparation method of the composite material hydrophobic coating comprises the following steps: siO alkylated in step 2) 2f /SiO 2 Spraying organic silicon resin for several times, drying at room temperature, and heat treating to obtain SiO 2f /SiO 2 And (3) a composite hydrophobic coating.
Further, in step 1), siO 2f /SiO 2 The composite material mainly comprises quartz fiber reinforcement and SiO 2 Composition of matrix of SiO 2 The matrix is a porous body which is formed by converting silica sol and has a silicon-oxygen bond random network structure, and silicon hydroxyl groups ≡ Si-OH and = Si- (OH) exist on the surface of the porous body 2 。
Further, in the step 1), the ultrasonic soaking time is 1-2 h.
Further, in the step 1), drying in air for 24-36 h.
Further, in the step 2), the silane coupling agent is at least one of trimethyl methoxy silane, triethyl methoxy silane and triethyl ethoxy silane, and the mass ratio of the silane coupling agent to the ethanol is (5-8) to (110-120).
Further, in the step 2), the condensation reflux temperature is 60-90 ℃, and the condensation reflux time is 2-6 h.
Further, in the step 2), the vacuum drying temperature is 50-70 ℃, and the time is 12-24 h.
Further, in the step 3), the organic silicon resin is one or more of methyl silicon resin, ethyl silicon resin and boron-containing silicon resin.
Further, in the step 3), the spraying times are 2-3 times, and the interval between every two spraying times is 10-15min.
Further, in the step 3), drying for 6-12 h at room temperature; the heat treatment temperature is 80-120 ℃, and the time duration is 6-12 h.
On the other hand, the invention also provides SiO 2f /SiO 2 The composite material hydrophobic coating is prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
SiO for use in the invention 2f /SiO 2 The composite material mainly comprises quartz fiber reinforcement and SiO 2 Composition of matrix of SiO 2 The matrix is a porous body having a silicon-oxygen bond random network structure formed by converting a silica sol, and a large number of silicon hydroxyl groups (≡ Si-OH and = Si- (OH) are present on the surface of the porous body 2 ) The invention uses at least one of silane coupling agent trimethyl methoxy silane, triethyl methoxy silane and triethyl ethoxy silane to combine with ≡ Si-OH or = Si- (OH) on the surface of primary particle 2 The groups are subjected to condensation reaction, so that the number of hydrophilic-OH groups on the surface of the porous body is reduced, and the hydrophobicity Si-CH on the surface of the porous body is increased 3 Radicals or Si-CH 2 CH 3 The quantity and the micromolecule hydrophobic group of the silane coupling agent can also close smaller holes on the surface of the porous body, so that the surface hydrophobic property of the porous body is greatly changed, the adsorption of water is weakened, and compared with the prior art (CN 110218102A), the surface hydrophobic property of the invention is hydrophobicThe active groups are bonded through chemical bonds and can cover the inner surface and the outer surface of the composite material, the existing process is a physical adsorption bond, and the nanometer silica sol particles are easy to agglomerate to block the pore passages of the composite material, so that the hydrophobic groups in the pore passages are not uniformly distributed, and the moisture resistance is greatly reduced. And the preparation of the hydrophobic coating is combined, so that the ultralow moisture resistance of the antenna housing and the antenna window in severe environment storage can be realized.
Drawings
FIG. 1 shows a SiO solid of the present invention 2f /SiO 2 A flow chart of a preparation method of the composite material hydrophobic coating.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
Step 1: siO2 2f /SiO 2 The composite material is pretreated by firstly preparing SiO 2f/ SiO 2 Cutting the composite material into a proper size, putting the composite material into acetone for ultrasonic immersion for 1h to remove surface oil stains and silica sol particles, and then drying the composite material in the air for 24h;
and 2, step: siO2 2f /SiO 2 Alkylating the composite material, namely, the SiO pretreated in the step 1 2f /SiO 2 Soaking the composite material in an ethanol solution containing trimethyl methoxy silane, wherein the mass ratio of the two is 5;
and step 3: siO2 2f /SiO 2 Preparing hydrophobic coating of composite material by using the alkylated SiO obtained in the step 2 2f /SiO 2 The composite material is prepared by spraying methyl silicone resin for 3 times (15 min interval between every spraying), drying at room temperature for 8h, and performing heat treatment at 100 ℃ for 6h. The properties of the hydrophobic coating of the composite obtained in this example are shown in table 1.
Example 2
Step 1: siO2 2f /SiO 2 The composite material is pretreated by firstly preparing SiO 2f/ SiO 2 Cutting the composite material into proper size, putting the composite material into acetone, and ultrasonically soaking the composite material for 1.5hRemoving oil stains on the surface and silica sol particles, and then drying in the air for 30 hours;
and 2, step: siO2 2f /SiO 2 Sealing holes with the composite material, namely sealing the SiO pretreated in the step 1 2f /SiO 2 Soaking the composite material in an ethanol solution containing triethyl methoxy silane, wherein the mass ratio of the triethyl methoxy silane to the ethanol solution is 8;
and 3, step 3: siO2 2f /SiO 2 Preparing hydrophobic coating of composite material by using the alkylated SiO obtained in the step 2 2f /SiO 2 The composite material is sprayed with ethyl silicone resin for 3 times (with the interval of 13min between every spraying), dried at room temperature for 12h, and heat treated at 80 ℃ for 12h to obtain the required coating. The properties of the hydrophobic coating of the composite obtained in this example are shown in table 1.
Example 3
Step 1: siO2 2f /SiO 2 The composite material is pretreated by firstly preparing SiO 2f/ SiO 2 Cutting the composite material into a proper size, putting the composite material into acetone for ultrasonic soaking for 2 hours to remove surface oil stains and silica sol particles, and then drying the composite material in air for 36 hours;
step 2: siO2 2f /SiO 2 Sealing holes with the composite material, namely sealing the SiO pretreated in the step 1 2f /SiO 2 Soaking the composite material in an ethanol solution containing triethyl ethoxysilane, wherein the mass ratio of the two is 6;
and step 3: siO2 2f /SiO 2 Preparing hydrophobic coating of composite material by using the alkylated SiO obtained in the step 2 2f /SiO 2 The composite material is sprayed with borosilicate-containing resin for 2 times (with the interval of 10min between every spraying), dried at room temperature for 6h, and heat-treated at 120 ℃ for 8h to obtain the required coating. The properties of the hydrophobic coating of the composite obtained in this example are shown in table 1.
Comparative example 1
The difference from example 1 is that: no SiO 2f /SiO 2 Composite alkylation this step. The properties of the composite hydrophobic coating obtained in this comparative example are shown in table 1.
Comparative example 2
The difference from example 2 is that: step 3 is not performed.
COMPARATIVE EXAMPLE 3 (CN 110218102A)
The difference from example 3 is in step 2: siO2 2f /SiO 2 Sealing holes with wave-transmitting material, namely, sealing the SiO pretreated in the step 1 2f /SiO 2 The wave-transmitting material is soaked in silica sol modified by trimethyl methoxy silane, TEOS and trimethyl methoxy silane are used as raw materials, ethanol and water are used as solvents, ammonia water (mass fraction is 23% -25%) is used as a catalyst, and the mass ratio of the substances is 0.4; circulating water is introduced for condensing reflux at 70 ℃ for 3 hours, and then the solution is kept stand for 24 hours to obtain colorless transparent sol, and new smaller holes are generated or exist due to the volatilization of the solution, so that the process needs to be repeated for 3 times;
the properties of the composite hydrophobic coating obtained in this comparative example are shown in table 1.
Table 1 results of performance test of hydrophobic coating layer of composite material obtained in examples and comparative examples
Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
Moisture absorption Rate (%) | 1.0 | 0.8 | 0.8 | 2.3 | 1.4 | 1.3 |
Dielectric constant | 2.98 | 2.92 | 2.93 | 3.32 | 3.21 | 3.15 |
From Table 1 it can be seen that the present invention provides a composite hydrophobic coating having a moisture pick-up of less than 1%, while comparative examples 1 and 2 show SiO 2f /SiO 2 Alkylation of the composite material and spraying of the coating are important, chemical bonds are formed through alkylation, and hydrophobic groups on the surface are bonded through the formed chemical bonds in spraying, so that the hydrophobic and moisture-proof performance of the coating is directly promoted. Compared with the prior art (CN 110218102A), the preparation method of the invention has better physical bond bonding performance and better moisture-proof effect through chemical bond bonding.
The present invention is not described in detail and is well known to those skilled in the art.
Although the present invention has been described with reference to the above embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. SiO (silicon dioxide) 2f /SiO 2 Composite hydrophobicThe preparation method of the coating is characterized by comprising the following steps:
1) Firstly, siO 2f/ SiO 2 Cutting the composite material into blocks, putting the blocks into acetone for ultrasonic soaking, removing oil stains on the surface and silica sol particles, and drying the blocks in the air to obtain pretreated SiO 2f /SiO 2 A composite material;
2) Pretreated SiO 2f /SiO 2 Soaking the composite material in ethanol solution containing silane coupling agent, condensing and refluxing, washing with ethanol, and vacuum drying to obtain alkylated SiO 2f /SiO 2 A composite material;
3) Alkylated SiO 2f /SiO 2 Spraying the composite material with organic silicon resin for several times, drying at room temperature, and heat treating to obtain SiO 2f /SiO 2 And (3) a composite hydrophobic coating.
2. The method of claim 1, wherein in step 1), the SiO is 2f /SiO 2 The composite material mainly comprises quartz fiber reinforcement and SiO 2 Composition of matrix of SiO 2 The matrix is a porous body which is formed by converting silica sol and has a silicon-oxygen bond random network structure, and silicon hydroxyl groups ≡ Si-OH and = Si- (OH) exist on the surface of the porous body 2 。
3. The method of claim 1, wherein in step 1), the ultrasonic soaking time is 1-2 hours, and the drying in air is 24-36 hours.
4. The method of claim 1, wherein in the step 2), the silane coupling agent is at least one of trimethyl methoxy silane, triethyl methoxy silane and triethyl ethoxy silane, and the mass ratio of the silane coupling agent to the ethanol is (5-8) to (110-120).
5. The method of claim 1, wherein in step 2), the condensation reflux temperature is 60-90 ℃ and the condensation reflux time is 2-6 h.
6. The method of claim 1, wherein in step 2), the vacuum drying temperature is 50-70 ℃ and the time is 12-24 h.
7. The method of claim 1, wherein in step 3), the silicone resin is one or more of a methyl silicone resin, an ethyl silicone resin, and a boron-containing silicone resin.
8. The method as claimed in claim 1, wherein in the step 3), the spraying times are 2-3 times, and the interval between every spraying time is 10-15min.
9. The method according to claim 1, wherein in step 3), drying is carried out for 6 to 12 hours at room temperature; the heat treatment temperature is 80-120 ℃, and the time duration is 6-12 h.
10. SiO (silicon dioxide) 2f /SiO 2 A hydrophobic coating for a composite material, obtainable by a process as claimed in any one of claims 1 to 9.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210889769.8A CN115304404A (en) | 2022-07-27 | 2022-07-27 | SiO (silicon dioxide) 2f /SiO 2 Composite hydrophobic coating and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210889769.8A CN115304404A (en) | 2022-07-27 | 2022-07-27 | SiO (silicon dioxide) 2f /SiO 2 Composite hydrophobic coating and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN115304404A true CN115304404A (en) | 2022-11-08 |
Family
ID=83858293
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210889769.8A Pending CN115304404A (en) | 2022-07-27 | 2022-07-27 | SiO (silicon dioxide) 2f /SiO 2 Composite hydrophobic coating and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115304404A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116730743A (en) * | 2023-07-03 | 2023-09-12 | 航天特种材料及工艺技术研究所 | Hydrophobic silicon dioxide ceramic composite material and preparation method thereof |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015059054A (en) * | 2013-09-18 | 2015-03-30 | 信越化学工業株式会社 | Surface organic resin-coated hydrophobic spherical silica fine particle, production method of the same, and toner external additive for electrostatic charge image development using the same |
CN110218102A (en) * | 2019-05-09 | 2019-09-10 | 航天特种材料及工艺技术研究所 | Hydrophobic type SiO2f/SiO2Electromagnetic wave transparent material and preparation method thereof |
CN110436966A (en) * | 2019-09-03 | 2019-11-12 | 江西嘉捷信达新材料科技有限公司 | A kind of Nano-meter SiO_22The antenna house of enhancing/antenna windows moisture barrier coatings preparation method and application |
CN111718206A (en) * | 2019-03-20 | 2020-09-29 | 山东工业陶瓷研究设计院有限公司 | SiO (silicon dioxide)2f/SiO2Ceramic moisture-proof sealing coating and preparation method thereof |
CN111718603A (en) * | 2020-07-01 | 2020-09-29 | 中国石油大学(北京) | Silicon dioxide surface modification method |
CN113930136A (en) * | 2021-11-26 | 2022-01-14 | 江苏博云塑业股份有限公司 | Hydrophobic coating, preparation method thereof and composite material with hydrophobic coating |
-
2022
- 2022-07-27 CN CN202210889769.8A patent/CN115304404A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015059054A (en) * | 2013-09-18 | 2015-03-30 | 信越化学工業株式会社 | Surface organic resin-coated hydrophobic spherical silica fine particle, production method of the same, and toner external additive for electrostatic charge image development using the same |
CN111718206A (en) * | 2019-03-20 | 2020-09-29 | 山东工业陶瓷研究设计院有限公司 | SiO (silicon dioxide)2f/SiO2Ceramic moisture-proof sealing coating and preparation method thereof |
CN110218102A (en) * | 2019-05-09 | 2019-09-10 | 航天特种材料及工艺技术研究所 | Hydrophobic type SiO2f/SiO2Electromagnetic wave transparent material and preparation method thereof |
CN110436966A (en) * | 2019-09-03 | 2019-11-12 | 江西嘉捷信达新材料科技有限公司 | A kind of Nano-meter SiO_22The antenna house of enhancing/antenna windows moisture barrier coatings preparation method and application |
CN111718603A (en) * | 2020-07-01 | 2020-09-29 | 中国石油大学(北京) | Silicon dioxide surface modification method |
CN113930136A (en) * | 2021-11-26 | 2022-01-14 | 江苏博云塑业股份有限公司 | Hydrophobic coating, preparation method thereof and composite material with hydrophobic coating |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116730743A (en) * | 2023-07-03 | 2023-09-12 | 航天特种材料及工艺技术研究所 | Hydrophobic silicon dioxide ceramic composite material and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110218102B (en) | Hydrophobic SiO2f/SiO2Wave-transparent material and preparation method thereof | |
JP3703032B2 (en) | Airgel coated film | |
KR100300801B1 (en) | How to form an SI-O-containing film | |
CN101817980B (en) | Sol-gel preparation method of silica-based superhydrophobic thin films | |
CN108373609B (en) | Coating for preparing transparent super-hydrophobic coating and preparation and use methods thereof | |
US9351405B2 (en) | Hydrophobic silane coating for preventing conductive anodic filament (CAF) growth in printed circuit boards | |
WO2008060883A2 (en) | Hydrophobic organic-inorganic hybrid silane coatings | |
CN109336545A (en) | A kind of silicon dioxide silica aerogel composite material, preparation method and application | |
CN115304404A (en) | SiO (silicon dioxide) 2f /SiO 2 Composite hydrophobic coating and preparation method thereof | |
CN104311161B (en) | The dampproof method of the compound quartzy ceramic material of porous | |
CN109575509B (en) | Method for preparing high-temperature-resistant phenolic organic silicon composite light block material by drying under normal pressure | |
CN109913855A (en) | A kind of hydrophobic material and plate hydrophobic film method | |
CN111718206A (en) | SiO (silicon dioxide)2f/SiO2Ceramic moisture-proof sealing coating and preparation method thereof | |
CN113026369B (en) | Ceramizable coating coated fiber and preparation method and application thereof | |
US10865303B2 (en) | Composite structure having an inorganic coating adhered thereto and method of making same | |
US5863595A (en) | Thick ceramic coatings for electronic devices | |
CN109626954A (en) | A kind of heatproof damp-proof silicon dioxide silica aerogel composite material and its preparation method and application | |
CN113980554B (en) | Moisture-coating anti-condensation heat-insulation coating and preparation method thereof | |
CN115710456A (en) | Water-based functional coating and preparation method thereof | |
CN102714232A (en) | Substrate having a metal film for producing photovoltaic cells | |
CN114249575A (en) | Surface densification method for aerogel heat-proof material | |
Li et al. | Facile synthesis of atomic oxygen-resistant methyl silicone rubber-coated Kapton film for photovoltaic solar array blanket in low Earth orbit | |
CN115625099B (en) | Hydrophobic moisture-proof layer of wave-transmitting material and preparation method thereof | |
CN115849956B (en) | Composite quartz ceramic material with hydrophobic moisture-proof coating and preparation method thereof | |
KR102398152B1 (en) | Method for producing polysilazane-based film |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |