CN103387329A - Method for preparing nitrogen-doped quartz fibers - Google Patents
Method for preparing nitrogen-doped quartz fibers Download PDFInfo
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- CN103387329A CN103387329A CN2013103247711A CN201310324771A CN103387329A CN 103387329 A CN103387329 A CN 103387329A CN 2013103247711 A CN2013103247711 A CN 2013103247711A CN 201310324771 A CN201310324771 A CN 201310324771A CN 103387329 A CN103387329 A CN 103387329A
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Abstract
The invention relates to a method for preparing nitrogen-doped quartz fibers, belonging to the field of quartz fiber production technologies. The method comprises the steps of uniformly doping nitride in a solid form or solid-liquid mixed form with a total content of 40-3,000ppm into quartz sand, then melting and drawing into thin quartz glass rods by a continuous-melting continuous-drawing process method, and then, drawing the quartz glass rods into nitrogen-doped quartz glass fibers. The temperature resistance of the nitrogen-doped quartz fibers prepared by the method is improved obviously, the nitrogen-doped quartz fibers can resist the temperature of 1,200 DEG C, the original excellent properties of quartz fibers are preserved, the production process is simple, and the operability is strong. The method solves the problems of the existing doping methods that the nitrogen doping is realized generally by processing quartz glass presenting in quartz glass particles in nitrogen-containing reacting gas or atmospheres, such as ammonia gas, nitric oxide, nitrous oxide and the like, the doping process is complicated, hydrogen is formed while ammonia is decomposed, then hydroxyl is fused into the structure of the quartz glass, and the improvement on the viscosity of the quartz glass is not facilitated.
Description
Technical field
The present invention relates to a kind of preparation method of nitrating silica fiber, belong to the silica fiber production technical field.
Background technology
Silica fiber has very excellent temperature tolerance, can be at 1100 ℃ of temperature life-time service, that in silicate glass fiber, resistance to elevated temperatures is best, be widely used in space flight military project, high temperature resistant, anti-ablation field, but when 1200 ℃ and above temperature, silica fiber also is difficult to bear for a long time.
For improving the heat resistance of silica fiber, the method that usually adopts is doped element or at fiber surface, apply the resistant to elevated temperatures material of one deck in silica glass.Doping nitrogen element in silica glass, can improve silica glass viscosity, usually the method that adopts is in the silica glass that exists as the silica glass particle, adopts in the atmosphere such as the reactant gases that contains nitrogen or ammonia, nitrogen protoxide, nitrous oxide and processes, thereby realize the nitrogen doping.Yet this adulterating method complex process, and ammonia forms hydrogen when decomposing, and hydrogen has been brought up the melting condition of reduction, and makes hydroxyl also be dissolved in the structure of silica glass, is unfavorable for improving the viscosity of silica glass.
Summary of the invention
The object of the invention is to, provide a kind of by mix nitride in quartz sand, realize doping nitrogen element in silica glass, then the manufacture heat resistance is good, do not reduce again simultaneously other excellent properties of silica glass, and production technique is simple, the preparation method of workable nitrating silica fiber.
The present invention realizes above-mentioned purpose by the following technical solutions:
The present invention based on know-why be, in the silica glass crystalline network, have the oxygen lack hole, namely the oxygen position in lattice is unoccupied or by other atom, taken, as direct Si-Si key and the Siliciumatom of twice of coordination only.Can especially easily with the position, existing hole of silica glass crystalline network, react because nitrogen decomposes the nitrogen-atoms that forms, especially with the oxygen lack hole, react.In the situation that the oxygen lack hole, the oxygen position of vacancy is taken by nitrogen, forms stable Si-N key, thereby can improve the viscosity of silica glass.
Technical essential of the present invention is: in silicon-dioxide purity, surpass in 99.90% quartz sand and mix the nitride that total content is 40～3000ppm, described nitride is silicon nitride, aluminium nitride or titanium nitride, then connect the processing method melting of drawing and pull into the fine quartz glass stick by continuous smelting, then quartz glass bar is drawn into quartz glass fibre.
Nitrating concrete steps of the present invention are:
A kind of preparation method of nitrating silica fiber is characterized in that: it consists of following steps:
The first step, evenly mix the nitride that total content is 40～3000ppm in silicon-dioxide purity surpasses 99.90% quartz sand, nitride is the wherein a kind of of silicon nitride, aluminium nitride or titanium nitride;
The nitride of described doping mixes in quartz sand with solid form, its particle diameter≤200 μ m, and the material that will mix mixes with quartz sand;
The nitride of described doping mixes in quartz sand with the solid-liquid mixed form, carries out roasting after it is stirred again, and maturing temperature is 400 ℃～1300 ℃, and soaking time is 0.5h～24h;
Second step, the quartz sand after roasting is put in continuous induction melting furnace with uniform doping or doping, is heated to 1800～2200 ℃, starts to draw quartz glass bar, and the diameter of quartz glass bar is 1.5～3.5mm;
The 3rd step, the quartz glass bar that draws is carried out visual testing, remove by inspecting standard bubble is arranged, gas line and crooked quartz glass bar;
The 4th step, to the quartz glass bar that is up to the standards with the mixed solution of hydrofluoric acid and hydrochloric acid or a kind of soaked with liquid wherein, remove the impurity on quartz glass bar surface; The concentration of described hydrofluoric acid is 5～15%, and the concentration of hydrochloric acid is 5～15%, and soak time is 10～60min, and soaking temperature is 10～35 ℃;
The 5th step, the quartz glass bar after acid bubble is rinsed 1～5 min with tap water, then be that deionized water rinsing to the pH value of 8～18M Ω is till 6～7 with resistivity;
The 6th step, the quartz glass bar after cleaning up naturally dry or use oven for drying, and while adopting oven for drying, the interior temperature of baking oven is 30～105 ℃, and drying time is 10～120min;
The 7th step, the quartz glass bar after drying are put into vacuum deshydroxy stove and are carried out deshydroxy, the vacuum tightness of vacuum deshydroxy stove is 5Pa～100Pa, the temperature of vacuum deshydroxy stove is risen to 1000 ℃～1100 ℃, keep 30～60 min, remove metastable hydroxyl in quartz pushrod;
The 8th goes on foot, the quartz glass bar after deshydroxy is tested, and removes diastrophic quartz glass bar is arranged;
The 9th step, to the quartz glass bar that is up to the standards with the mixed solution of hydrofluoric acid and hydrochloric acid or a kind of soaked with liquid wherein, remove the impurity on quartz glass bar surface; The concentration of described hydrofluoric acid is 5～15%, and the concentration of hydrochloric acid is 5～15%, and soak time is 10～60min, and soaking temperature is 10～35 ℃;
The tenth step, the quartz glass bar after acid bubble is rinsed 1～5min with tap water, then be that deionized water rinsing to the pH value of 8～18M Ω is till 6～7 with resistivity;
The 11 step, the quartz glass bar after cleaning up naturally dry or use oven for drying, and while adopting oven for drying, the interior temperature of baking oven is 30～105 ℃, and drying time is 10～120min;
The 12 step, the quartz glass bar after will drying or dry are sent into melt drawing equipment, and delivery speed is 0.5～1.5mm/s, adopt oxyhydrogen flame to burn quartz glass bar is heated to 1750～1900 ℃, with the draw rate of 20～50m/s, are drawn into silica fiber.
The present invention's beneficial effect compared with prior art is:
The nitrating silica fiber that the preparation method of this nitrating silica fiber produces, its heat resistance is significantly improved, can anti-1200 ℃ of temperature, and kept the excellent properties of original silica fiber, and production technique is simple, and workable.What solved the common employing of existing adulterating method is in the silica glass that exists as the silica glass particle, employing contains in the atmosphere such as the reactant gases of nitrogen or ammonia, nitrogen protoxide, nitrous oxide to be processed and realizes the nitrogen doping, doping process is complicated, and when decomposing, ammonia forms hydrogen, make hydroxyl also be dissolved in the structure of silica glass, be unfavorable for improving the problem of silica glass viscosity.
Embodiment
The preparation method of this nitrating silica fiber be nitride is mixed in quartz sand with solid form or take the solid-liquid mixed form mix in quartz sand and carry out roasting after as raw material, again it is put in continuous induction melting furnace and is drawn into quartz glass bar, then make the nitrating silica fiber, to reach the purpose of nitrating in silica fiber.
That the invention will be further described is as follows below in conjunction with several specific embodiments:
Embodiment 1:
The first step, get the silicon nitride of 50g, the silicon nitride particle diameter is 40～60 μ m, join in the pure water of 2000ml, stir, join again purity and be in 99.90% quartz sand 200kg, mix, then the quartz sand that doping is mixed is at the temperature roasting of 1100 ℃ 8 hours, naturally cooling.
Quartz sand after second step, the roasting of adulterating is put in continuous induction melting furnace, is heated to 1850 ℃, then starts to draw quartz glass bar, and the diameter control of the quartz glass bar that draws out is at 1.7mm ± 0.2mm.
The 3rd step, the quartz glass bar that draws is carried out visual testing, remove by inspecting standard bubble is arranged, gas line and crooked quartz glass bar.
The 4th goes on foot, the quartz glass bar that is up to the standards is used the mixed liquid dipping of hydrofluoric acid and hydrochloric acid, removes the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 10%, and the concentration of hydrochloric acid is 5%, and soak time is 30min, and soaking temperature is 25 ℃.
The 5th step, the quartz glass bar after acid bubble is rinsed 3min with tap water, then be that deionized water rinsing to the pH value of 9M Ω is till 7 with resistivity.
The 6th step, the quartz glass bar oven for drying after cleaning up, the interior temperature of baking oven is 105 ℃, drying time is 40min.
The 7th step, the quartz glass bar after dry are put into vacuum deshydroxy stove and are carried out deshydroxy, and the vacuum tightness of vacuum deshydroxy stove is 50Pa, and the temperature of vacuum deshydroxy stove is risen to 1050 ℃, keep 30 min, remove the interior metastable hydroxyl of quartz pushrod.
The 8th goes on foot, the quartz glass bar after deshydroxy is tested, and removes diastrophic quartz glass bar is arranged.
The 9th goes on foot, the quartz glass bar that is up to the standards is used the mixed liquid dipping of hydrofluoric acid and hydrochloric acid, removes the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 10%, and the concentration of hydrochloric acid is 5%, and soak time is 30min, and soaking temperature is 25 ℃.
The tenth step, the quartz glass bar after acid bubble is rinsed 3min with tap water, then be that deionized water rinsing to the pH value of 10M Ω is till 7 with resistivity.
The 11 step, the quartz glass bar oven for drying after cleaning up, the interior temperature of baking oven is 105 ℃, drying time is 30min.
The 12 step, the quartz glass bar after dry are sent into melt drawing equipment, and delivery speed is 1.5mm/s, adopt oxyhydrogen flame to burn quartz glass bar is heated to 1780 ℃, with the draw rate of 20m/s, are drawn into silica fiber.
The nitrating silica glass that adopts embodiment 1 to make, the viscosity in the time of its 1200 ℃ is 1.3 times of common silica glass, the nitrating silica fiber that makes is higher by 5% than common silica fiber in the tension fracture brute force of 1000 ℃ of processing after 1 hour.
Embodiment 2:
The first step, get the aluminium nitride of 250g, the aluminum nitride particle diameter is 80～100 μ m, joins purity and is in 99.90% quartz sand 200kg, mixes.
Second step, the quartz sand of uniform doping is put in continuous induction melting furnace, be heated to 1780 ℃, then start to draw quartz glass bar, diameter control is at 2.0mm ± 0.2mm.
The 3rd step, the silica glass that draws is carried out visual testing, remove a large amount of bubbles are arranged, quartz pushrod that the gas line is more and crooked.
The 4th goes on foot, the quartz glass bar that is up to the standards is used the mixed liquid dipping of hydrofluoric acid and hydrochloric acid, removes the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 15%, and the concentration of hydrochloric acid is 10%, and soak time is 20min, and soaking temperature is controlled at 20 ℃.
The 5th step, the quartz glass bar after acid bubble is rinsed with tap water, flush time is 5min, then is that deionized water rinsing to the pH value of 10M Ω is till 6 with resistivity.
The 6th step, the quartz glass bar after cleaning up naturally dries or uses oven for drying, bake out temperature is 105 ℃, and drying time is 50min.
The 7th step, quartz glass bar is put into vacuum deshydroxy stove carry out deshydroxy, vacuum degree control, at 30Pa, is warming up to 1050 ℃, keeps constant temperature 50min, removes metastable hydroxyl in quartz pushrod.
The 8th goes on foot, the quartz glass bar after deshydroxy is tested, and removes diastrophic rod is arranged.
The 9th goes on foot, the quartz glass bar that is up to the standards is used the mixed liquid dipping of hydrofluoric acid and hydrochloric acid, removes the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 15%, and the concentration of hydrochloric acid is 10%, and soak time is 20min, and soaking temperature is controlled at 20 ℃.
The tenth step, the quartz glass bar after acid bubble is rinsed 5min with tap water, then be that deionized water rinsing to the pH value of 18M Ω is till 6 with resistivity.
The 11 step, the quartz glass bar after cleaning up naturally dries or uses oven for drying, bake out temperature is 100 ℃, drying time 50min.
The 12 step, the quartz glass bar that will dry are sent into melt drawing equipment, control delivery speed at 1.0mm/s, adopt oxyhydrogen flame to burn quartz glass bar is heated to 1820 ℃, with the draw rate of 25m/s, are drawn into silica fiber.
The nitrating silica glass that adopts embodiment 2 to make, the viscosity in the time of its 1200 ℃ is 1.8 times of common silica glass, the nitrating silica fiber that makes is higher by 10% than common silica fiber in the tension fracture brute force of 1000 ℃ of processing after 1 hour.
Embodiment 3:
The first step, get the silicon nitride of 150g, the silicon nitride particle diameter is 40～60 μ m, add in the pure water of 2000ml, stir, adding purity is in 99.90% quartz sand 200kg again, mix, then the quartz sand that doping is mixed is at the temperature roasting of 1000 ℃ 12 hours, naturally cooling.
Quartz sand after second step, the roasting of adulterating is put in continuous induction melting furnace, is heated to 1800 ℃, then starts to draw quartz glass bar, and the diameter control of the quartz glass bar that draws out is at 2.5mm ± 0.2mm.
The 3rd step, the quartz glass bar that draws is carried out visual testing, remove by inspecting standard bubble is arranged, gas line and crooked quartz glass bar.
The 4th goes on foot, the quartz glass bar that is up to the standards is used the mixed liquid dipping of hydrofluoric acid and hydrochloric acid, removes the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 15%, and the concentration of hydrochloric acid is 15%, and soak time is 15min, and soaking temperature is controlled at 20 ℃.
The 5th step, the quartz glass bar after acid bubble is rinsed 2min with tap water, then be that deionized water rinsing to the pH value of 12M Ω is till 7 with resistivity.
The 6th step, the quartz glass bar oven for drying after cleaning up, the interior temperature of baking oven is 80 ℃, drying time is 100min.
The 7th step, the quartz glass bar after dry are put into vacuum deshydroxy stove and are carried out deshydroxy, and the vacuum tightness of vacuum deshydroxy stove is 30Pa, and the temperature of vacuum deshydroxy stove is risen to 1100 ℃, keep 50min, remove the interior metastable hydroxyl of quartz pushrod.
The 8th goes on foot, the quartz glass bar after deshydroxy is tested, and removes diastrophic quartz glass bar is arranged.
The 9th goes on foot, the quartz glass bar that is up to the standards is used the mixed liquid dipping of hydrofluoric acid and hydrochloric acid, removes the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 15%, and the concentration of hydrochloric acid is 15%, and soak time is 15min, and soaking temperature is controlled at 20 ℃.
The tenth step, the quartz glass bar after acid bubble is rinsed 2min with tap water, then be that deionized water rinsing to the pH value of 12M Ω is till 7 with resistivity.
The 11 step, the quartz glass bar oven for drying after cleaning up, the interior temperature of baking oven is 80 ℃, drying time is 100min.
The 12 step, the quartz glass bar after dry are sent into melt drawing equipment, and delivery speed is 0.8mm/s, adopt oxyhydrogen flame to burn quartz glass bar is heated to 1850 ℃, with the draw rate of 30m/s, are drawn into silica fiber.
The nitrating silica glass that adopts embodiment 3 to make, the common silica glass of its ratio of viscosities of 1200 ℃ is approximately high 1.7 times, and the nitrating silica fiber that makes is higher by 9% than common silica fiber in the tension fracture brute force of 1000 ℃ of processing after 1 hour.
Embodiment 4:
The first step, get the aluminium nitride of 400g, the aluminum nitride particle diameter is 80～100 μ m, joins purity and is in 99.90% quartz sand 200kg, mixes.
Second step, the quartz sand of uniform doping is put in continuous induction melting furnace, be heated to 1830 ℃, then start to draw quartz glass bar, diameter control is at 3.0mm ± 0.2mm.
The 3rd step, the silica glass that draws is carried out visual testing, remove a large amount of bubbles are arranged, quartz pushrod that the gas line is more and crooked.
The 4th step, the quartz glass bar hydrofluoric acid dips to being up to the standards, remove the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 5%, and soak time is 50min, and soaking temperature is controlled at 30 ℃.
The 5th step, the quartz glass bar after acid bubble is rinsed with tap water, flush time is 2min, then is that deionized water rinsing to the pH value of 12M Ω is till 6～7 with resistivity.
The 6th step, the quartz glass bar after cleaning up naturally dries or uses oven for drying, bake out temperature is 80 ℃, and drying time is 100min.
The 7th step, quartz glass bar is put into vacuum deshydroxy stove carry out deshydroxy, vacuum degree control, at 20Pa, is warming up to 1080 ℃, keeps constant temperature 60min, removes metastable hydroxyl in quartz pushrod.
The 8th goes on foot, the quartz glass bar after deshydroxy is tested, and removes diastrophic rod is arranged.
The 9th goes on foot, the quartz glass bar that is up to the standards is steeped with the hydrofluoric acid immersion, removes the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 5%, and soak time is 50min, and soaking temperature is controlled at 35 ℃.
The tenth step, the quartz glass bar after acid bubble is rinsed 1min with tap water, then be that deionized water rinsing to the pH value of 16M Ω is till 6～7 with resistivity.
The 11 step, the quartz glass bar after cleaning up naturally dries or uses oven for drying, bake out temperature is 80 ℃, drying time 100min.
The 12 step, the quartz glass bar that will dry are sent into melt drawing equipment, control delivery speed at 0.6mm/s, adopt oxyhydrogen flame to burn quartz glass bar is heated to 1880 ℃, with the draw rate of 40m/s, are drawn into silica fiber.
The nitrating silica glass that adopts embodiment 4 to make, the viscosity in the time of its 1200 ℃ is 2 times of common silica glass, the nitrating silica fiber that makes is higher by 15% than common silica fiber in the tension fracture brute force of 1000 ℃ of processing after 1 hour.
Embodiment 5:
The first step, get the titanium nitride of 500g, the titanium nitride particles diameter is 20～50 μ m, adds in the pure water of 5000ml, stir, then to add purity be in 99.90% quartz sand 200kg, to mix, the quartz sand that again doping is mixed is at the temperature roasting of 800 ℃ 20 hours, naturally cooling.
Quartz sand after second step, the roasting of adulterating is put in continuous induction melting furnace, is heated to 1850 ℃, then starts to draw quartz glass bar, and the diameter control of the quartz glass bar that draws out is at 3.2mm ± 0.2mm.
The 3rd step, the quartz glass bar that draws is carried out visual testing, remove by inspecting standard bubble is arranged, gas line and crooked quartz glass bar.
The 4th step, the quartz glass bar hydrofluoric acid dips to being up to the standards, remove the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 12%, and soak time is 30min, and soaking temperature is controlled at 25 ℃.
The 5th step, the quartz glass bar after acid bubble is rinsed 4min with tap water, then be that deionized water rinsing to the pH value of 16M Ω is till 7 with resistivity.
The 6th step, the quartz glass bar oven for drying after cleaning up, the interior temperature of baking oven is 60 ℃, drying time is 120min.
The 7th step, the quartz glass bar after dry are put into vacuum deshydroxy stove and are carried out deshydroxy, and the vacuum tightness of vacuum deshydroxy stove is 20Pa, and the temperature of vacuum deshydroxy stove is risen to 1120 ℃, keep 60min, remove the interior metastable hydroxyl of quartz pushrod.
The 8th goes on foot, the quartz glass bar after deshydroxy is tested, and removes diastrophic quartz glass bar is arranged.
The 9th step, the quartz glass bar hydrofluoric acid dips to being up to the standards, remove the impurity on quartz glass bar surface.Wherein the concentration of hydrofluoric acid is 12%, and soak time is 30min, and soaking temperature is controlled at 25 ℃.
The tenth step, the quartz glass bar after acid bubble is rinsed 4min with tap water, then be that deionized water rinsing to the pH value of 16M Ω is till 7 with resistivity.
The 11 step, the quartz glass bar oven for drying after cleaning up, the interior temperature of baking oven is 60 ℃, drying time is 120min.
The 12 step, the quartz glass bar after dry are sent into melt drawing equipment, and delivery speed is 0.5mm/s, adopt oxyhydrogen flame to burn quartz glass bar is heated to 1820 ℃, with the draw rate of 50m/s, are drawn into silica fiber.
The nitrating silica glass that adopts embodiment 5 to make, the viscosity in the time of its 1200 ℃ is 2 times of common quartz, the nitrating silica fiber that makes is higher by 14% than common silica fiber in the tension fracture brute force of 1000 ℃ of processing after 1 hour.
The above is the embodiment of this invention, above-mentioned not illustrating is construed as limiting flesh and blood of the present invention, the person of an ordinary skill in the technical field can make an amendment or be out of shape above-mentioned embodiment after having read this specification sheets, and does not deviate from the spirit and scope of the invention.
Claims (1)
1. the preparation method of a nitrating silica fiber, it is characterized in that: it consists of following steps:
The first step, evenly mix the nitride that total content is 40～3000ppm in silicon-dioxide purity surpasses 99.90% quartz sand, nitride is the wherein a kind of of silicon nitride, aluminium nitride or titanium nitride;
The nitride of described doping mixes in quartz sand with solid form, its particle diameter≤200 μ m, and the material that will mix mixes with quartz sand;
The nitride of described doping mixes in quartz sand with the solid-liquid mixed form, carries out roasting after it is stirred again, and maturing temperature is 400 ℃～1300 ℃, and soaking time is 0.5h～24h;
Second step, the quartz sand after roasting is put in continuous induction melting furnace with uniform doping or doping, is heated to 1800～2200 ℃, starts to draw quartz glass bar, and the diameter of quartz glass bar is 1.5～3.5mm;
The 3rd step, the quartz glass bar that draws is carried out visual testing, remove by inspecting standard bubble is arranged, gas line and crooked quartz glass bar;
The 4th step, to the quartz glass bar that is up to the standards with the mixed solution of hydrofluoric acid and hydrochloric acid or a kind of soaked with liquid wherein, remove the impurity on quartz glass bar surface; The concentration of described hydrofluoric acid is 5～15%, and the concentration of hydrochloric acid is 5～15%, and soak time is 10～60min, and soaking temperature is 10～35 ℃;
The 5th step, the quartz glass bar after acid bubble is rinsed 1～5 min with tap water, then be that deionized water rinsing to the pH value of 8～18M Ω is till 6～7 with resistivity;
The 6th step, the quartz glass bar after cleaning up naturally dry or use oven for drying, and while adopting oven for drying, the interior temperature of baking oven is 30～105 ℃, and drying time is 10～120min;
The 7th step, the quartz glass bar after drying are put into vacuum deshydroxy stove and are carried out deshydroxy, the vacuum tightness of vacuum deshydroxy stove is 5Pa～100Pa, the temperature of vacuum deshydroxy stove is risen to 1000 ℃～1100 ℃, keep 30～60 min, remove metastable hydroxyl in quartz pushrod;
The 8th goes on foot, the quartz glass bar after deshydroxy is tested, and removes diastrophic quartz glass bar is arranged;
The 9th step, to the quartz glass bar that is up to the standards with the mixed solution of hydrofluoric acid and hydrochloric acid or a kind of soaked with liquid wherein, remove the impurity on quartz glass bar surface; The concentration of described hydrofluoric acid is 5～15%, and the concentration of hydrochloric acid is 5～15%, and soak time is 10～60min, and soaking temperature is 10～35 ℃;
The tenth step, the quartz glass bar after acid bubble is rinsed 1～5min with tap water, then be that deionized water rinsing to the pH value of 8～18M Ω is till 6～7 with resistivity;
The 11 step, the quartz glass bar after cleaning up naturally dry or use oven for drying, and while adopting oven for drying, the interior temperature of baking oven is 30～105 ℃, and drying time is 10～120min;
The 12 step, the quartz glass bar after will drying or dry are sent into melt drawing equipment, and delivery speed is 0.5～1.5mm/s, adopt oxyhydrogen flame to burn quartz glass bar is heated to 1750～1900 ℃, with the draw rate of 20～50m/s, are drawn into silica fiber.
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| CN102099304A (en) * | 2008-07-19 | 2011-06-15 | 赫罗伊斯石英玻璃股份有限两合公司 | Method for producing quartz glass doped with nitrogen and quartz glass grains suitable for carrying out the method |
| CN101328014A (en) * | 2008-07-28 | 2008-12-24 | 湖北菲利华石英玻璃股份有限公司 | Manufacturing method of doping quartz glass fibre |
| CN102575377A (en) * | 2009-10-06 | 2012-07-11 | Lg矽得荣株式会社 | Quartz crucible and method of manufacturing the same |
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Denomination of invention: A preparation method of nitrogen doped quartz fibers Effective date of registration: 20230925 Granted publication date: 20160323 Pledgee: China Everbright Bank Co.,Ltd. Jingzhou Branch Pledgor: HUBEI FEILIHUA QUARTZ GLASS Co.,Ltd. Registration number: Y2023980058350 |