CN102505458B - Coating method for reinforced high silica glass fiber fabric - Google Patents
Coating method for reinforced high silica glass fiber fabric Download PDFInfo
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- CN102505458B CN102505458B CN2011103477574A CN201110347757A CN102505458B CN 102505458 B CN102505458 B CN 102505458B CN 2011103477574 A CN2011103477574 A CN 2011103477574A CN 201110347757 A CN201110347757 A CN 201110347757A CN 102505458 B CN102505458 B CN 102505458B
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- 239000003365 glass fiber Substances 0.000 title claims abstract description 159
- 239000004744 fabric Substances 0.000 title claims abstract description 144
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000000576 coating method Methods 0.000 title claims abstract description 53
- 238000010438 heat treatment Methods 0.000 claims abstract description 53
- 239000011248 coating agent Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 31
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000004327 boric acid Substances 0.000 claims abstract description 26
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052582 BN Inorganic materials 0.000 claims abstract description 23
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 230000002708 enhancing effect Effects 0.000 claims abstract description 12
- 238000000197 pyrolysis Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000011065 in-situ storage Methods 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 60
- 229910052757 nitrogen Inorganic materials 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 19
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 18
- 239000012298 atmosphere Substances 0.000 abstract description 17
- 238000005516 engineering process Methods 0.000 abstract description 8
- 229910052810 boron oxide Inorganic materials 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 abstract description 5
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 39
- 239000000463 material Substances 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000012545 processing Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000011152 fibreglass Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000002679 ablation Methods 0.000 description 2
- 238000004031 devitrification Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- -1 boric acid ester compound Chemical class 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a coating method for enhancing a high silica glass fiber fabric, which adopts a low-temperature ceramic material firing technology of an organic precursor conversion method, and coats a temperature-resistant coating containing boron nitride on the surface of the high silica glass fiber fabric, thereby realizing the purpose of improving the mechanical property and the temperature resistance of the high silica glass fiber fabric. The pyrolysis sintering is carried out in nitrogen atmosphere, the defect that boron oxide is easily formed in air atmosphere is overcome, and the mechanical property of the high silica glass fiber coating fabric is effectively improved. The coating method of the reinforced high silica glass fiber fabric comprises the following steps: dipping and coating the surface of the high silica glass fiber fabric by using an ethanol solution of boric acid and triethanolamine, and then carrying out temperature programming heat treatment on the high silica glass fiber coated fabric at the temperature range of 140-450 ℃ in a nitrogen atmosphere to form a temperature-resistant coating containing boron nitride on the surface of the high silica glass fiber fabric in situ.
Description
Technical field
The present invention relates to a kind of coating process of high silica glass fiber fabric, more specifically to a kind of coating process that strengthens high silica glass fiber fabric.
Background technology
Resurrection glass fibre is a kind of resistant to elevated temperatures inorfil, belongs to special glass fibre.Its SiO
2content, more than 96%, normally, by sodium borosilicate glass fibre impurity beyond silicon is removed in hot acid extraction (leaching), forms by sintering.This fibre fire resistant is functional, can be under 900 ℃ uses for a long time, and the high temperature that the short time can anti-1200 ℃ is a kind of stable chemical performance, high temperature resistant, anti-ablation, percent thermal shrinkage is low, thermal conductivity factor is low, has the glass fiber material of good electrical insulating properties.In recent years, along with progressively forbidding in the world asbestos, make resurrection glass fibre be developed rapidly and apply, be widely used in the anti-ablation of solar heat protection of high-temperature insulation material, fire prevention protective materials, high-temperature gas and liquid filtration material, aerospace craft and electromagnetic wave transparent material etc.But because the intensity of this fiber is lower, be only 1/10 of E glass fibre, intensity how to improve high silica glass fiber fabric also just becomes problem often to be solved.
The surface coating processing is to improve the easy and effective method of high silica glass fiber fabric mechanical property.Apply organic material on the resurrection glass fibre surface, as tetrafluoroethylene, acrylic resin, organic silicon rubber etc., can improve the intensity of goods, improve its processing characteristics, make heat insulation, the fire proofing material of various uses, as the series of products such as BWTC, BWSC of existing U.S. Armatex F, Armatexa N, Armatexa S and China.But, due to the heatproof limitation of macromolecular material itself, limited the further lifting of its glass fibre coating fabric heat resistance.
Boron nitride ceramic material has many good physics and chemistry characteristics, as high temperature resistant, anti-oxidant, resistance to chemical attack, machinability, the dielectric properties of excellence and good thermal conductivity etc.Due to the heat-resisting quantity of boron nitride excellence, lower thermal expansivity, can meet the requirement of resurrection glass fibre face coat.Boron nitride coating can be filled up the microdefect of fiberglass surfacing, there is high-temperature oxidation resistant simultaneously and stop the low valence metal ion osmosis, therefore be expected to significantly improve mechanical property, devitrification resistance energy and the elevated temperature strength hold facility of glass fibre, thereby improve glass fabric service life at high temperature.In the composite Application Areas, boron nitride coating, as interface phase, can improve the interface of fiber between matrix and be combined simultaneously, improves the mechanical property of composite.Boron nitride ceramics often forms through high temperature sintering, and this traditional technology of preparing is difficult for making the boron nitride material of the complicated shapes such as coating, film or fiber.Prepare at fiberglass surfacing the restriction that boron nitride coating obviously is subject to temperature, even temperature tolerance preferably quartz fibre just start crystallization in the time of 950 ℃, a large amount of crystallizatioies during higher than 1050 ℃, cause tendering of fiber.Therefore, the method for the synthetic boron nitride of traditional high temperature, be not suitable for preparing boron nitride coating at fiberglass surfacing.At present, the organic precursor method conversion method, owing to having the advantages such as easy-formation, temperature be lower, has become the important method for preparing ceramic coating, ceramic membrane, ceramic fibre, foamed ceramics and ceramic matric composite.Prepare boron nitride coating with the organic precursor method conversion method at fiberglass surfacing, more can avoid the destruction of high temperature to glass fibre structure, making to prepare novel glass fibre boron nitride coating fabric becomes possibility.The people (Materials Letters, 44,113-118,2000) such as Shampa Mondal disclose a kind of method of borate coated glass fiber, and in air atmosphere, respectively at 400 ℃ and 1000 ℃ of lower pyrolysis, thermal decomposition product contains boron nitride and carbonitride.It is said that its glass fibre coating fabric has the potential use as the molten aluminum filtering material, but do not announce concrete heatproof and mechanical performance index.In fact boric acid ester compound easy oxidation generate boron oxide during high temperature pyrolysis in air atmosphere, boron oxide is as glass fibre flux commonly used, has the effect of mechanical property under the fusing point of remarkable reduction glass fibre and high temperature thereof.Experiment shows that the TENSILE STRENGTH of resurrection glass fibre borate coated fabric in the time of 600 ℃ of pyrolysis in air atmosphere starts obvious decline, almost loses intensity (seeing Comparative Examples 1) in the time of 800 ℃.In addition, the first borate that Shampa Mondal etc. adopt is synthetic, recrystallization purifying again, and last glass applies and the process route of high temperature pyrolysis, its technological process complexity, and equipment needed thereby is more, is unfavorable for suitability for industrialized production.
Therefore need to develop in conjunction with the organic precursor method conversion method and be suitable for the low fire ceramic material technology of commercial Application, on the surface of high silica glass fiber fabric coated with the boron nitride coating of heatproof, improve mechanical property and the heat resistance of high silica glass fiber fabric, enlarge the Application Areas of high silica glass fiber fabric.
Summary of the invention
The present invention is directed to the deficiency of high silica glass fiber fabric mechanical property and the shortcoming that prior art exists, a kind of coating process that strengthens high silica glass fiber fabric is provided, adopt the low fire ceramic material technology of organic precursor method conversion method, coated with the heatproof coating that contains boron nitride, the mechanical property of high silica glass fiber fabric and the purpose of heat resistance have been realized improving on the high silica glass fiber fabric surface.Directly dip coated is carried out in the high silica glass fiber fabric surface with boron nitride source boric acid and triethanolamine, then by temperature programming heat treatment, make preparation, coating, pyrolysis sintering one step of organic precursor method complete, formed the heatproof coating that contains boron nitride at the high silica glass fiber fabric surface in situ, the method provides a kind of technology of simplifying step.The pyrolysis sintering carries out in blanket of nitrogen, has overcome in the air atmosphere and has easily formed the defect of boron oxide, has effectively improved the mechanical property of resurrection glass fibre coated fabric.
The present invention is achieved by the following technical solutions:
The coating process of enhancing high silica glass fiber fabric of the present invention, its step is as follows: the ethanolic solution with boric acid and triethanolamine carries out dip coated to the high silica glass fiber fabric surface, then in the temperature range of 140 ℃～450 ℃, the resurrection glass fibre coated fabric is carried out to temperature programming heat treatment in nitrogen atmosphere, form the heatproof coating that contains boron nitride at the surface in situ of high silica glass fiber fabric.Control the chemical constitution of borate organic precursor method by the ratio of regulating boric acid and triethanolamine, without the purifying process such as recrystallization of borate.Control the coat thickness on glass surface by regulating boric acid, the triethanolamine concentration in ethanolic solution.The resistance to elevated temperatures excellence of boron nitride coating, can fill up the microdefect on resurrection glass fibre surface, blocking oxygen and improve the high-temperature oxidation resistance of resurrection glass fibre, and can improve the devitrification resistance energy of resurrection glass fibre, thereby mechanical property and the heat resistance of resurrection glass fibre have effectively been improved.
The coating process of enhancing high silica glass fiber fabric of the present invention, the concentration expressed in percentage by weight of the ethanolic solution that its further technical scheme is described boric acid and triethanolamine is 5%～40%, and the mol ratio of its mesoboric acid and triethanolamine is 1: 0.8～1: 2.0.
The coating process of enhancing high silica glass fiber fabric of the present invention, its further technical scheme can also be described ethanolic solution of take boric acid and triethanolamine to the high silica glass fiber fabric surface carry out the dip coated step as: high silica glass fiber fabric be immersed in ethanolic solution and carry out surface and apply 1～2 minute, and dry under 70 ℃～80 ℃ conditions.
The coating process of enhancing high silica glass fiber fabric of the present invention, its further technical scheme can also be describedly the resurrection glass fibre coated fabric to be carried out to the heat treated step of temperature programming in the temperature range of 140 ℃～450 ℃ be in nitrogen atmosphere: first under the nitrogen stream condition at 140 ℃～200 ℃ to the heat treatment of resurrection glass fibre coated fabric at the synthetic borate organic precursor method of glass surface in situ, after in the blanket of nitrogen of 350 ℃～450 ℃ to the heat treatment of resurrection glass fibre coated fabric, pyrolysis sintering borate organic precursor method, surface in situ at high silica glass fiber fabric forms the heatproof coating that contains boron nitride.
The coating process of enhancing high silica glass fiber fabric of the present invention, its further technical scheme be describedly the resurrection glass fibre coated fabric to be carried out to the heat treated step of temperature programming in the temperature range of 140 ℃～450 ℃ be in nitrogen atmosphere: first at nitrogen stream and under 140 ℃～160 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour; Again at nitrogen stream and under 170 ℃～200 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour; Finally in nitrogen atmosphere and under 350 ℃～450 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 0.5～2 hour.
The coating process of enhancing high silica glass fiber fabric of the present invention, its further technical scheme can also be that method comprises the following steps:
1) high silica glass fiber fabric is immersed in ethanolic solution and carries out surface coating 1～2 minute, and dry under 70 ℃～80 ℃ conditions;
2) at nitrogen stream and under 140 ℃～160 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour;
3) at nitrogen stream and under 170 ℃～200 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour;
4) in nitrogen atmosphere and under 350 ℃～450 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 0.5～2 hour, the resurrection glass fibre coated fabric goods that are enhanced after cooling;
The concentration expressed in percentage by weight of the ethanolic solution of wherein said boric acid and triethanolamine is 5%～40%, and the mol ratio of boric acid and triethanolamine is 1: 0.8～1: 2.0.
The coating process of enhancing high silica glass fiber fabric of the present invention, the model that its further technical scheme can also be described high silica glass fiber fabric is BWT600.
The present invention has following beneficial effect:
1) preparation of organic precursor method, coating, pyrolysis sintering complete in glass surface one step, have simplified processing step;
2) control the chemical constitution of borate organic precursor method by the ratio of regulating boric acid and triethanolamine, without the purifying process such as recrystallization of borate.
3) the pyrolysis sintering of borate organic precursor method carries out in blanket of nitrogen, has overcome in the air atmosphere and has easily formed the defect of boron oxide, has effectively improved the mechanical property of resurrection glass fibre coated fabric;
4) adopt the technology of temperature programming, can reduce the volatilization loss of boric acid, triethanolamine, reduced smoke pollution;
5) cost of material is cheap, simple, the easy row of preparation technology, and modified effect is obvious, is suitable for the industrial-scale production of resurrection glass fibre coated fabric.
The specific embodiment
Further illustrate by the following examples the present invention, the high silica glass fiber fabric in embodiment is BWT600, and TENSILE STRENGTH is pressed the test of GBT7689.5-2001 method.
Embodiment 1
1) weighing boric acid 61.83 grams, triethanolamine 119.35 grams and ethanol 422.75 grams, be mixed with solution;
2) high silica glass fiber fabric is immersed in ethanolic solution and carries out surface coating 1 minute, and dry under 80 ℃ of conditions;
3) at nitrogen stream and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) at nitrogen stream and under 180 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
5) in nitrogen atmosphere and under 350 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour, the resurrection glass fibre coated fabric goods that are enhanced after cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is in Table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, cooling its TENSILE STRENGTH of rear test, test result is in Table 1.
Embodiment 2
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 492.38 grams, be mixed with solution;
2) high silica glass fiber fabric is immersed in ethanolic solution and carries out surface coating 1 minute, and dry under 70 ℃ of conditions;
3) at nitrogen stream and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) at nitrogen stream and under 180 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
5) in nitrogen atmosphere and under 350 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour, the resurrection glass fibre coated fabric goods that are enhanced after cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is in Table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, cooling its TENSILE STRENGTH of rear test, test result is in Table 1.
Embodiment 3
1) weighing boric acid 61.83 grams, triethanolamine 223.79 grams and ethanol 1142.48 grams, be mixed with solution;
2) high silica glass fiber fabric is immersed in ethanolic solution and carries out surface coating 2 minutes, and dry under 70 ℃ of conditions;
3) at nitrogen stream and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) at nitrogen stream and under 180 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
5) in nitrogen atmosphere and under 350 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour, the resurrection glass fibre coated fabric goods that are enhanced after cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is in Table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, cooling its TENSILE STRENGTH of rear test, test result is in Table 1.
Embodiment 4
1) weighing boric acid 61.83 grams, triethanolamine 298.38 grams and ethanol 1440.84 grams, be mixed with solution;
2) high silica glass fiber fabric is immersed in ethanolic solution and carries out surface coating 1 minute, and dry under 80 ℃ of conditions;
3) at nitrogen stream and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) at nitrogen stream and under 180 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
5) in nitrogen atmosphere and under 350 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour, the resurrection glass fibre coated fabric goods that are enhanced after cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is in Table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, cooling its TENSILE STRENGTH of rear test, test result is in Table 1.
Embodiment 5
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 316.53 grams, be mixed with solution;
2) high silica glass fiber fabric is immersed in ethanolic solution and carries out surface coating 2 minutes, and dry under 70 ℃ of conditions;
3) at nitrogen stream and under 140 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 2 hours;
4) at nitrogen stream and under 200 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 2 hours;
5) in nitrogen atmosphere and under 350 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 2 hours, the resurrection glass fibre coated fabric goods that are enhanced after cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is in Table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, cooling its TENSILE STRENGTH of rear test, test result is in Table 1.
Embodiment 6
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 1899.18 grams, be mixed with solution;
2) high silica glass fiber fabric is immersed in ethanolic solution and carries out surface coating 1 minute, and dry under 70 ℃ of conditions;
3) at nitrogen stream and under 150 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1.5 hours;
4) at nitrogen stream and under 170 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1.5 hours;
5) in nitrogen atmosphere and under 400 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour, the resurrection glass fibre coated fabric goods that are enhanced after cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is in Table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, cooling its TENSILE STRENGTH of rear test, test result is in Table 1.
Embodiment 7
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 4009.38 grams, be mixed with solution;
2) high silica glass fiber fabric is immersed in ethanolic solution and carries out surface coating 1 minute, and dry under 70 ℃ of conditions;
3) at nitrogen stream and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) at nitrogen stream and under 200 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
5) in nitrogen atmosphere and under 450 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 0.5 hour, the resurrection glass fibre coated fabric goods that are enhanced after cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is in Table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, cooling its TENSILE STRENGTH of rear test, test result is in Table 1.
Comparative Examples 1
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 492.38 grams, be mixed with solution;
2) high silica glass fiber fabric is immersed in ethanolic solution and carries out surface coating 1 minute, and dry under 70 ℃ of conditions;
3) at nitrogen stream and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) at nitrogen stream and under 180 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
5), in air atmosphere and under 350 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour, obtain resurrection glass fibre coated fabric goods after cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is in Table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, cooling its TENSILE STRENGTH of rear test, test result is in Table 1.
Comparative Examples 2
The TENSILE STRENGTH of test high silica glass fiber fabric, test result is in Table 1.
Comparative Examples 3
In air atmosphere under 800 ℃ of conditions of temperature, to high silica glass fiber fabric heat treatment 1 hour, cooling its TENSILE STRENGTH of rear test, test result is in Table 1.
Table 1
Annotate: * is the TENSILE STRENGTH (MPa) of not making the original high silica glass fiber fabric BWT600 of face coat modification.
The TENSILE STRENGTH result of table 1 shows, the TENSILE STRENGTH of the high silica glass fiber fabric of processing through coating of the present invention is 1.2 times (comparing embodiment 2 and Comparative Examples 2) before processing, through 800 ℃, the test of the heatproof of 1h, its TENSILE STRENGTH is 1.6 times (comparing embodiment 2 and Comparative Examples 3) before processing, has significantly improved mechanical property and the heat resistance of high silica glass fiber fabric.And in air atmosphere under the process conditions of pyrolysis sintering organic precursor method, high silica glass fiber fabric is through 800 ℃, the heatproof test of 1h, its resistance to elevated temperatures substantially lose (Comparative Examples 1,3.1MPa).
Claims (5)
1. a coating process that strengthens high silica glass fiber fabric, it is characterized in that step is as follows: the ethanolic solution with boric acid and triethanolamine carries out dip coated to the high silica glass fiber fabric surface, then in the temperature range of 140 ℃～450 ℃, the resurrection glass fibre coated fabric is carried out to temperature programming heat treatment in nitrogen atmosphere, form the heatproof coating that contains boron nitride at the surface in situ of high silica glass fiber fabric; Wherein said ethanolic solution of take boric acid and triethanolamine to the high silica glass fiber fabric surface carry out the dip coated step as: high silica glass fiber fabric be immersed in ethanolic solution and carry out surface and apply 1～2 minute, and dry under 70 ℃～80 ℃ conditions; Describedly the resurrection glass fibre coated fabric is carried out to the heat treated step of temperature programming in the temperature range of 140 ℃～450 ℃ be in nitrogen atmosphere: first under the nitrogen stream condition at 140 ℃～200 ℃ to the heat treatment of resurrection glass fibre coated fabric at the synthetic borate organic precursor method of glass surface in situ, after in the blanket of nitrogen of 350 ℃～450 ℃ to the heat treatment of resurrection glass fibre coated fabric, pyrolysis sintering borate organic precursor method, form the heatproof coating that contains boron nitride at the surface in situ of high silica glass fiber fabric.
2. the coating process of enhancing high silica glass fiber fabric according to claim 1, the concentration expressed in percentage by weight that it is characterized in that the ethanolic solution of described boric acid and triethanolamine is 5%～40%, and the mol ratio of its mesoboric acid and triethanolamine is 1:0.8～1:2.0.
3. the coating process of enhancing high silica glass fiber fabric according to claim 1 is characterized in that describedly in the temperature range of 140 ℃～450 ℃, the resurrection glass fibre coated fabric being carried out to the heat treated step of temperature programming be in nitrogen atmosphere:
First at nitrogen stream and under 140 ℃～160 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour;
Again at nitrogen stream and under 170 ℃～200 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour;
Finally in nitrogen atmosphere and under 350 ℃～450 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 0.5～2 hour.
4. the coating process of enhancing high silica glass fiber fabric according to claim 1 is characterized in that comprising the following steps:
1) high silica glass fiber fabric is immersed in the ethanolic solution of boric acid and triethanolamine and carries out surface and apply 1～2 minute, and dry under 70 ℃～80 ℃ conditions;
2) at nitrogen stream and under 140 ℃～160 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour;
3) at nitrogen stream and under 170 ℃～200 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour;
4) in nitrogen atmosphere and under 350 ℃～450 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 0.5～2 hour, the resurrection glass fibre coated fabric goods that are enhanced after cooling;
The concentration expressed in percentage by weight of the ethanolic solution of wherein said boric acid and triethanolamine is 5%～40%, and the mol ratio of boric acid and triethanolamine is 1:0.8～1:2.0.
5. according to the coating process of claim 1,3 or 4 arbitrary described enhancing high silica glass fiber fabrics, the model that it is characterized in that described high silica glass fiber fabric is BWT600.
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| CN112125649B (en) * | 2020-09-02 | 2021-09-28 | 佳木斯大学 | Preparation method of three-phase ceramic fiber composite heat insulation tile |
| CN115847987B (en) * | 2022-12-02 | 2023-12-08 | 苏州铂韬新材料科技有限公司 | Film material with wave-transmitting and heat-conducting functions and preparation process thereof |
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| CN1214329A (en) * | 1997-10-13 | 1999-04-21 | 向阳春 | Preparation of boron nitride ceramic material with boron and nitrogen containing organic precursor |
| CN102167612A (en) * | 2011-01-14 | 2011-08-31 | 中国人民解放军国防科学技术大学 | Preparation method of boron nitride coating on fiber surface |
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| CN1214329A (en) * | 1997-10-13 | 1999-04-21 | 向阳春 | Preparation of boron nitride ceramic material with boron and nitrogen containing organic precursor |
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