CN102505458A - Coating method for reinforcing high silica glass fiber fabric - Google Patents
Coating method for reinforcing high silica glass fiber fabric Download PDFInfo
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- CN102505458A CN102505458A CN2011103477574A CN201110347757A CN102505458A CN 102505458 A CN102505458 A CN 102505458A CN 2011103477574 A CN2011103477574 A CN 2011103477574A CN 201110347757 A CN201110347757 A CN 201110347757A CN 102505458 A CN102505458 A CN 102505458A
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- glass fibre
- resurrection glass
- fabric
- temperature
- heat treatment
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- 239000003365 glass fiber Substances 0.000 title claims abstract description 160
- 239000004744 fabric Substances 0.000 title claims abstract description 145
- 238000000576 coating method Methods 0.000 title claims abstract description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title abstract description 9
- 230000003014 reinforcing effect Effects 0.000 title abstract 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 33
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000004327 boric acid Substances 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 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 18
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 230000002708 enhancing effect Effects 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- 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
- 238000000197 pyrolysis Methods 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 3
- 238000010952 in-situ formation Methods 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 18
- 239000012298 atmosphere Substances 0.000 abstract description 17
- 230000008569 process Effects 0.000 abstract description 7
- 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
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 38
- 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
- 239000000919 ceramic Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000011152 fibreglass Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000002950 deficient Effects 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
- 238000012545 processing 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
- 238000002679 ablation Methods 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
- 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
- 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
- 230000007774 longterm Effects 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
Abstract
The invention discloses a coating method for reinforcing high silica glass fiber fabric, which employs low-temperature firing process of ceramic materials using an organic precursor conversion method; a temperature-resistant coating containing boron nitride is coated on the surface of the high silica glass fiber fabric, thereby achieving the purposes of reinforcing the mechanical property and the temperature resistance of the high silica glass fiber fabric. Pyrolytic sintering is carried out in nitrogen atmosphere, thereby overcoming the defect of easy formation of boron oxide in air atmosphere, and effectively enhancing the mechanical property of the high silica glass fiber coating fabric. The coating method disclosed by the invention comprises the steps of: dipping and coating the surface of the high silica glass fiber fabric by using ethanol solution of boric acid and triethanolamine; and then carrying out programmed heating treatment to the high silica glass fiber coating fabric at a temperature in a range from 140 DEG C to 450 DEG C; and forming the temperature-resistant coating containing boron nitride in situ on the surface of the high silica glass fiber fabric.
Description
Technical field
The present invention relates to a kind of coating process of resurrection glass fibre fabric, more specifically to a kind of coating process that strengthens the resurrection glass fibre fabric.
Background technology
Resurrection glass fibre is a kind of resistant to elevated temperatures inorfil, belongs to special glass fibre.Its SiO
2Content is normally removed impurity beyond the silicon by the sodium borosilicate glass fibre through hot acid extraction (leaching), after sintering forms more than 96%.This fiber resistance to elevated temperatures is good, can use at 900 ℃ down long-term, and the short time can anti-1200 ℃ high temperature, 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 asbestos in the world; Make resurrection glass fibre developed rapidly and use, be widely used in that the solar heat protection of high-temperature insulation material, fire prevention protective materials, high-temperature gas and liquid filtration material, aerospace craft is anti-ablates and electromagnetic wave transparent material etc.But because the intensity of this fiber is lower, be merely 1/10 of E glass fibre, intensity how to improve the resurrection glass fibre fabric also just becomes problem often to be solved.
It is to improve the easy and effective method of resurrection glass fibre fabric mechanics that surface-coated is handled.At resurrection glass fibre surface-coated organic material; Like 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, like series of products such as the BWTC of existing U.S. Armatex F, Armatexa N, Armatexa S and China, BWSC.But because the heatproof limitation of macromolecular material itself has limited the further lifting of its glass fibre coating fabric heat resistance.
Boron nitride ceramic material has many good physics and chemical characteristic, like high temperature resistant, anti-oxidant, resistance to chemical attack, machinability, the dielectric properties of excellence and good thermal conductivity etc.Because the heat-resisting quantity that boron nitride is excellent, lower thermal expansivity can satisfy the requirement of resurrection glass fibre face coat.Boron nitride coating can be filled up the microdefect of fiberglass surfacing; Have high-temperature oxidation resistant simultaneously and stop the low valence metal ion osmosis; Therefore be expected to significantly improve the mechanical property of glass fibre, anti-crystallization property and elevated temperature strength hold facility, thereby improve glass fabric service life at high temperature.Simultaneously in the composite Application Areas, boron nitride coating is as the interface phase, can improve fiber and combine the mechanical property of raising composite with interface between the matrix.Boron nitride ceramics often forms through high temperature sintering, and this traditional technology of preparing is difficult for making the boron nitride material of complicated shapes such as coating, film or fiber.Prepare the restriction that boron nitride coating obviously receives temperature at fiberglass surfacing, even the preferable quartz fibre of temperature tolerance just begins crystallization in the time of 950 ℃, a large amount of crystallizatioies cause tendering of fiber when being higher than 1050 ℃.Therefore, the method for the synthetic boron nitride of traditional high temperature is not suitable for preparing boron nitride coating at fiberglass surfacing.At present, the organic precursor method conversion method has become the important method of preparation ceramic coating, ceramic membrane, ceramic fibre, foamed ceramics and ceramic matric composite owing to have advantages such as easy-formation, temperature are lower.Prepare boron nitride coating with the organic precursor method conversion method at fiberglass surfacing, more can avoid the destruction of high temperature, make the novel glass fibre boron nitride coating fabric of preparation become possibility glass fibre structure.People (Materials Letters, 44,113-118,2000) such as Shampa Mondal disclose a kind of method of borate coated glass fiber, and respectively at 400 ℃ and 1000 ℃ of following pyrolysis, thermal decomposition product contains boron nitride and carbonitride in air atmosphere.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 is prone to oxidation during high temperature pyrolysis and generates boron oxide in air atmosphere, and boron oxide is as glass fibre flux commonly used, has the effect of mechanical property under fusing point and the high temperature thereof of remarkable reduction glass fibre.The TENSILE STRENGTH of resurrection glass fibre borate coated fabric in the time of 600 ℃ that experiment is illustrated in pyrolysis in the air atmosphere begins 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, and its technological process is complicated, and equipment needed thereby is more, is unfavorable for suitability for industrialized production.
Therefore need to develop the low fire ceramic material technology that combines the organic precursor method conversion method and be suitable for commercial Application; Cover boron nitride coating on the surface of resurrection glass fibre fabric with heatproof; Improve the mechanical property and the heat resistance of resurrection glass fibre fabric, enlarge the Application Areas of resurrection glass fibre fabric.
Summary of the invention
The present invention is directed to the deficiency of resurrection glass fibre fabric mechanics and the shortcoming that prior art exists; A kind of coating process that strengthens the resurrection glass fibre fabric is provided; Adopt the low fire ceramic material technology of organic precursor method conversion method; Cover to contain the heatproof coating of boron nitride at the resurrection glass fibre fabric face, realized improving the mechanical property of resurrection glass fibre fabric and the purpose of heat resistance.Directly the resurrection glass fibre fabric face is carried out dip coated with boron nitride source boric acid and triethanolamine; Then through temperature programming heat treatment; Make preparation, coating, one step of pyrolysis sintering of organic precursor method accomplish; Formed the heatproof coating that contains boron nitride in resurrection glass fibre fabric face original position, this method provides a kind of technology of simplifying step.The pyrolysis sintering carries out in blanket of nitrogen, has overcome the defective that is prone to form boron oxide in the air atmosphere, has improved the mechanical property of resurrection glass fibre coated fabric effectively.
The present invention realizes through following technical scheme:
The coating process of enhancing resurrection glass fibre fabric of the present invention; Its step is following: the ethanolic solution with boric acid and triethanolamine carries out dip coated to the resurrection glass fibre fabric face; In nitrogen atmosphere, the resurrection glass fibre coated fabric is carried out temperature programming heat treatment then, contain the heatproof coating of boron nitride in the surface in situ formation of resurrection glass fibre fabric in 140 ℃～450 ℃ temperature range.Control the chemical constitution of borate organic precursor method through the ratio of regulating boric acid and triethanolamine, need not the purifying process such as recrystallization of borate.Through regulating the coat thickness on boric acid, the triethanolamine concentration control glass surface in ethanolic solution.The resistance to elevated temperatures of boron nitride coating is excellent; 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 anti-crystallization property of resurrection glass fibre, thereby the mechanical property and the heat resistance of resurrection glass fibre have been improved effectively.
The coating process of enhancing resurrection glass fibre 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 resurrection glass fibre fabric of the present invention; Its further technical scheme can also be that described ethanolic solution with boric acid and triethanolamine carries out the dip coated step to the resurrection glass fibre fabric face and is: the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1～2 minute, and dry under 70 ℃～80 ℃ conditions.
The coating process of enhancing resurrection glass fibre fabric of the present invention; Its further technical scheme can also be describedly in nitrogen atmosphere, the resurrection glass fibre coated fabric to be carried out the heat treated step of temperature programming in 140 ℃～450 ℃ temperature range and be: earlier under 140 ℃～200 ℃ nitrogen current condition to the heat treatment of resurrection glass fibre coated fabric at the synthetic borate organic precursor method of glass surface in situ; The back in 350 ℃～450 ℃ blanket of nitrogen to the heat treatment of resurrection glass fibre coated fabric; Pyrolysis sintering borate organic precursor method forms the heatproof coating that contains boron nitride at the surface in situ of resurrection glass fibre fabric.
The coating process of enhancing resurrection glass fibre fabric of the present invention; Its technical scheme further is describedly in nitrogen atmosphere, the resurrection glass fibre coated fabric to be carried out the heat treated step of temperature programming in 140 ℃～450 ℃ temperature range and be: earlier in nitrogen current and under 140 ℃～160 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour; Again in nitrogen current and under 170 ℃～200 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour; At last 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 resurrection glass fibre fabric of the present invention, its further technical scheme can also be that method may further comprise the steps:
1) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1～2 minute, and dry under 70 ℃～80 ℃ conditions;
2) in nitrogen current and under 140 ℃～160 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour;
3) in nitrogen current 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 the 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 resurrection glass fibre fabric of the present invention, the model that its further technical scheme can also be described resurrection glass fibre fabric is BWT600.
The present invention has following beneficial effect:
1) processing step has been simplified in the preparation of organic precursor method, coating, the one step completion on the glass surface of pyrolysis sintering;
2) control the chemical constitution of borate organic precursor method through the ratio of regulating boric acid and triethanolamine, need not 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 the defective that is prone to form boron oxide in the air atmosphere, has improved the mechanical property of resurrection glass fibre coated fabric effectively;
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
Below further specify the present invention through embodiment, the resurrection glass fibre fabric among the embodiment is BWT600, TENSILE STRENGTH is pressed GBT7689.5-2001 method test.
Embodiment 1
1) weighing boric acid 61.83 grams, triethanolamine 119.35 grams and ethanol 422.75 grams are mixed with solution;
2) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1 minute, and dry under 80 ℃ of conditions;
3) in nitrogen current and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) in nitrogen current 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 the cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is seen table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, its TENSILE STRENGTH of cooling back test, test result is seen table 1.
Embodiment 2
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 492.38 grams are mixed with solution;
2) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1 minute, and dry under 70 ℃ of conditions;
3) in nitrogen current and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) in nitrogen current 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 the cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is seen table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, its TENSILE STRENGTH of cooling back test, test result is seen table 1.
Embodiment 3
1) weighing boric acid 61.83 grams, triethanolamine 223.79 grams and ethanol 1142.48 grams are mixed with solution;
2) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 2 minutes, and dry under 70 ℃ of conditions;
3) in nitrogen current and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) in nitrogen current 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 the cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is seen table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, its TENSILE STRENGTH of cooling back test, test result is seen table 1.
Embodiment 4
1) weighing boric acid 61.83 grams, triethanolamine 298.38 grams and ethanol 1440.84 grams are mixed with solution;
2) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1 minute, and dry under 80 ℃ of conditions;
3) in nitrogen current and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) in nitrogen current 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 the cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is seen table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, its TENSILE STRENGTH of cooling back test, test result is seen table 1.
Embodiment 5
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 316.53 grams are mixed with solution;
2) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 2 minutes, and dry under 70 ℃ of conditions;
3) in nitrogen current and under 140 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 2 hours;
4) in nitrogen current 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 the cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is seen table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, its TENSILE STRENGTH of cooling back test, test result is seen table 1.
Embodiment 6
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 1899.18 grams are mixed with solution;
2) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1 minute, and dry under 70 ℃ of conditions;
3) in nitrogen current and under 150 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1.5 hours;
4) in nitrogen current 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 the cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is seen table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, its TENSILE STRENGTH of cooling back test, test result is seen table 1.
Embodiment 7
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 4009.38 grams are mixed with solution;
2) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1 minute, and dry under 70 ℃ of conditions;
3) in nitrogen current and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) in nitrogen current 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 the cooling;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is seen table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, its TENSILE STRENGTH of cooling back test, test result is seen table 1.
Comparative Examples 1
1) weighing boric acid 61.83 grams, triethanolamine 149.19 grams and ethanol 492.38 grams are mixed with solution;
2) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1 minute, and dry under 70 ℃ of conditions;
3) in nitrogen current and under 160 ℃ of conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1 hour;
4) in nitrogen current 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,, obtain resurrection glass fibre coated fabric goods after the cooling to resurrection glass fibre coated fabric heat treatment 1 hour;
6) TENSILE STRENGTH of test resurrection glass fibre coated fabric goods, test result is seen table 1;
7) in air atmosphere under 800 ℃ of conditions of temperature, to resurrection glass fibre coated fabric goods heat treatment 1 hour, its TENSILE STRENGTH of cooling back test, test result is seen table 1.
Comparative Examples 2
The TENSILE STRENGTH of test resurrection glass fibre fabric, test result is seen table 1.
Comparative Examples 3
Under 800 ℃ of conditions of temperature, to resurrection glass fibre fabric heat treatment 1 hour, its TENSILE STRENGTH was tested in the cooling back in air atmosphere, and test result is seen table 1.
Table 1
Annotate: * is a TENSILE STRENGTH (MPa) of not making the original resurrection glass fibre fabric BWT600 of face coat modification.
The TENSILE STRENGTH result of table 1 shows; The TENSILE STRENGTH of the resurrection glass fibre fabric that process coating of the present invention is handled is 1.2 times before handling (comparing embodiments 2 and Comparative Examples 2); The heatproof test of 800 ℃ on warp, 1h; Its TENSILE STRENGTH is 1.6 times before handling (comparing embodiments 2 and Comparative Examples 3), has significantly improved the mechanical property and the heat resistance of resurrection glass fibre fabric.And in air atmosphere under the process conditions of pyrolysis sintering organic precursor method, the resurrection glass fibre fabric is through 800 ℃, the heatproof test of 1h, its resistance to elevated temperatures lose basically (Comparative Examples 1,3.1MPa).
Claims (7)
1. coating process that strengthens the resurrection glass fibre fabric; It is characterized in that step is following: the ethanolic solution with boric acid and triethanolamine carries out dip coated to the resurrection glass fibre fabric face; In nitrogen atmosphere, the resurrection glass fibre coated fabric is carried out temperature programming heat treatment then, contain the heatproof coating of boron nitride in the surface in situ formation of resurrection glass fibre fabric in 140 ℃～450 ℃ temperature range.
2. the coating process of enhancing resurrection glass fibre fabric according to claim 1; The ethanolic solution concentration expressed in percentage by weight that it is characterized in that described boric acid and triethanolamine is 5%～40%, and its mesoboric acid and triethanolamine mol ratio are 1: 0.8～1: 2.0.
3. the coating process of enhancing resurrection glass fibre fabric according to claim 1; It is characterized in that described ethanolic solution with boric acid and triethanolamine carries out the dip coated step to the resurrection glass fibre fabric face and is: the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1～2 minute, and dry under 70 ℃～80 ℃ conditions.
4. the coating process of enhancing resurrection glass fibre fabric according to claim 1; It is characterized in that describedly in nitrogen atmosphere, the resurrection glass fibre coated fabric being carried out the heat treated step of temperature programming and being in 140 ℃～450 ℃ temperature range: earlier under 140 ℃～200 ℃ nitrogen current condition to the heat treatment of resurrection glass fibre coated fabric at the synthetic borate organic precursor method of glass surface in situ; The back in 350 ℃～450 ℃ blanket of nitrogen to the heat treatment of resurrection glass fibre coated fabric; Pyrolysis sintering borate organic precursor method forms the heatproof coating that contains boron nitride at the surface in situ of resurrection glass fibre fabric.
5. the coating process of enhancing resurrection glass fibre fabric according to claim 4; It is characterized in that describedly in nitrogen atmosphere, the resurrection glass fibre coated fabric being carried out the heat treated step of temperature programming and being: earlier in nitrogen current and under 140 ℃～160 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour in 140 ℃～450 ℃ temperature range; Again in nitrogen current and under 170 ℃～200 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour; At last in nitrogen atmosphere and under 350 ℃～450 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 0.5～2 hour.
6. the coating process of enhancing resurrection glass fibre fabric according to claim 1 is characterized in that may further comprise the steps:
1) the resurrection glass fibre fabric is immersed in carried out surface-coated in the ethanolic solution 1～2 minute, and dry under 70 ℃～80 ℃ conditions;
2) in nitrogen current and under 140 ℃～160 ℃ conditions of temperature, to resurrection glass fibre coated fabric heat treatment 1～2 hour;
3) in nitrogen current 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 the 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.
7. according to the coating process of claim 1,3,4,5 or 6 arbitrary described enhancing resurrection glass fibre fabrics, the model that it is characterized in that described resurrection glass fibre fabric is BWT600.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103073198A (en) * | 2012-12-28 | 2013-05-01 | 四川威玻股份有限公司 | Method for treating high silica glass fibers with polyether polyol as reinforcing agent |
| CN112125649A (en) * | 2020-09-02 | 2020-12-25 | 佳木斯大学 | Preparation method of three-phase ceramic fiber composite heat insulation tile |
| CN115847987A (en) * | 2022-12-02 | 2023-03-28 | 苏州铂韬新材料科技有限公司 | Membrane material with waveguide transmission heat function 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073198A (en) * | 2012-12-28 | 2013-05-01 | 四川威玻股份有限公司 | Method for treating high silica glass fibers with polyether polyol as reinforcing agent |
| CN103073198B (en) * | 2012-12-28 | 2014-12-10 | 四川威玻股份有限公司 | Method for treating high silica glass fibers with polyether polyol as reinforcing agent |
| CN112125649A (en) * | 2020-09-02 | 2020-12-25 | 佳木斯大学 | Preparation method of three-phase ceramic fiber composite heat insulation tile |
| CN112125649B (en) * | 2020-09-02 | 2021-09-28 | 佳木斯大学 | Preparation method of three-phase ceramic fiber composite heat insulation tile |
| CN115847987A (en) * | 2022-12-02 | 2023-03-28 | 苏州铂韬新材料科技有限公司 | Membrane material with waveguide transmission heat function and preparation process thereof |
| 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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