CN103387329B - A kind of preparation method of nitrating silica fiber - Google Patents
A kind of preparation method of nitrating silica fiber Download PDFInfo
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- CN103387329B CN103387329B CN201310324771.1A CN201310324771A CN103387329B CN 103387329 B CN103387329 B CN 103387329B CN 201310324771 A CN201310324771 A CN 201310324771A CN 103387329 B CN103387329 B CN 103387329B
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Abstract
The present invention relates to a kind of preparation method of nitrating silica fiber, belong to silica fiber production technical field.The present invention is after the nitride evenly mixing solid form that total content is 40 ~ 3000ppm or solid-liquid mixed form in quartz sand, the processing method melting of even being drawn by continuous smelting also pulls into fine quartz glass stick, then quartz glass bar is pulled into nitrating quartz glass fibre.The nitrating silica fiber heat resistance that produces of the present invention is adopted to be improved significantly, can resistance to 1200 DEG C of temperature, and maintain the original excellent properties of silica fiber, and production technique is simple, workable.Solving existing adulterating method is typically employed in the silica glass existed as silica glass particle, process in the atmosphere such as the reactant gases containing nitrogen or ammonia, nitrogen protoxide, nitrous oxide is adopted to realize N doping, doping process is complicated, and form hydrogen while ammonolysis craft, hydroxyl is also dissolved in the structure of silica glass, is unfavorable for the problem improving silica glass viscosity.
Description
Technical field
The present invention relates to a kind of preparation method of nitrating silica fiber, belong to silica fiber production technical field.
Background technology
Silica fiber has very excellent temperature tolerance, can at 1100 DEG C 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, resistance to ablation field, but when 1200 DEG C and above temperature, silica fiber is also difficult to bear for a long time.
For improving the heat resistance of silica fiber, the method usually adopted is doped element or apply the resistant to elevated temperatures material of one deck at fiber surface in silica glass.Adulterate nitrogen element in silica glass, silica glass viscosity can be improved, the method of usual employing is in the silica glass existed as silica glass particle, adopts in the atmosphere such as the reactant gases containing nitrogen or ammonia, nitrogen protoxide, nitrous oxide and processes, thus realize N doping.But this adulterating method complex process, and forming hydrogen while ammonolysis craft, hydrogen creates the melting condition of reduction, and hydroxyl is also dissolved in the structure of silica glass, is unfavorable for the viscosity improving silica glass.
Summary of the invention
The object of the invention is to, there is provided a kind of by mixing nitride in quartz sand, realize the nitrogen element that adulterates in silica glass, then manufacture heat resistance is good, do not reduce again other excellent properties of silica glass simultaneously, 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 silica glass crystalline network, there is oxygen lack hole, the oxygen position namely in lattice is unoccupied or taken by other atom, as the Siliciumatom of direct Si-Si bond and only coordination twice.The nitrogen-atoms formed because nitrogen decomposes can especially easily react with the position, existing hole of silica glass crystalline network, especially reacts with oxygen lack hole.When oxygen lack hole, the oxygen position of vacancy is taken by nitrogen, forms stable Si-N key, thus can improve the viscosity of silica glass.
Technical essential of the present invention is: in the quartz sand of silica purity more than 99.90%, 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 by continuous smelting and pull into fine quartz glass stick, then quartz glass bar is drawn into quartz glass fibre.
Nitrating concrete steps of the present invention are:
A preparation method for nitrating silica fiber, is characterized in that: it is made up of following steps:
The first step, in the quartz sand of silica purity more than 99.90%, evenly mix the nitride that total content is 40 ~ 3000ppm, 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 μm, and is mixed with quartz sand by the material mixed;
The nitride of described doping mixes in quartz sand with solid-liquid mixed form, carries out roasting again after being stirred, and maturing temperature is 400 DEG C ~ 1300 DEG C, and soaking time is 0.5h ~ 24h;
Second step, by uniform doping or doping roasting after quartz sand put in continuous induction melting furnace, be heated to 1800 ~ 2200 DEG C, start to draw quartz glass bar, the diameter of quartz glass bar is 1.5 ~ 3.5mm;
3rd step, to draw quartz glass bar carry out visual testing, by inspecting standard remove have bubble, gas line and bending quartz glass bar;
4th step, to the mixed solution of the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid or wherein a kind of soaked with liquid, 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 DEG C;
5th step, to the quartz glass bar tap water 1 ~ 5min after acid bubble, then to be deionized water rinsing to the pH value of 8 ~ 18M Ω by resistivity be 6 ~ 7;
6th step, naturally to be dried by the quartz glass bar after cleaning up or by oven for drying, temperature when adopting oven for drying in baking oven is 30 ~ 105 DEG C, and drying time is 10 ~ 120min;
7th step, the quartz glass bar after drying is put into vacuum deshydroxy stove and carried out deshydroxy, the vacuum tightness of vacuum deshydroxy stove is 5Pa ~ 100Pa, and the temperature of vacuum deshydroxy stove is risen to 1000 DEG C ~ 1100 DEG C, keeps 30 ~ 60min, removes metastable hydroxyl in quartz pushrod;
8th step, the quartz glass bar after deshydroxy to be tested, remove and have diastrophic quartz glass bar;
9th step, to the mixed solution of the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid or wherein a kind of soaked with liquid, 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 DEG C;
Tenth step, to the quartz glass bar tap water 1 ~ 5min after acid bubble, then to be deionized water rinsing to the pH value of 8 ~ 18M Ω by resistivity be 6 ~ 7;
11 step, naturally to be dried by the quartz glass bar after cleaning up or by oven for drying, temperature when adopting oven for drying in baking oven is 30 ~ 105 DEG C, and drying time is 10 ~ 120min;
12 step, will to dry or quartz glass bar after drying sends into melt drawing equipment, delivery speed is 0.5 ~ 1.5mm/s, adopts oxyhydrogen flame burning that quartz glass bar is heated to 1750 ~ 1900 DEG C, is drawn into silica fiber with the draw rate of 20 ~ 50m/s.
The present invention's beneficial effect is compared with prior art:
The nitrating silica fiber that the preparation method of this nitrating silica fiber produces, its heat resistance is significantly improved, can resistance to 1200 DEG C of temperature, and maintains the excellent properties of original silica fiber, and production technique is simple, workable.What solve that existing adulterating method adopts usually is in the silica glass existed as silica glass particle, process in the atmosphere such as the reactant gases containing nitrogen or ammonia, nitrogen protoxide, nitrous oxide is adopted to realize N doping, doping process is complicated, and form hydrogen while ammonolysis craft, hydroxyl is also dissolved in the structure of silica glass, is unfavorable for the problem improving silica glass viscosity.
Embodiment
Nitride to mix in quartz sand with solid form or to mix in quartz sand with solid-liquid mixed form and for raw material after carrying out roasting by the preparation method of this nitrating silica fiber, put in continuous induction melting furnace again and be drawn into quartz glass bar, then nitrating silica fiber is made, to reach the object of nitrating in silica fiber.
Below in conjunction with several specific embodiment, that the invention will be further described is as follows:
Embodiment 1:
The first step, get the silicon nitride of 50g, its total content that adulterates is made to be 40 ~ 3000ppm, silicon nitride particle diameter is 40 ~ 60 μm, join in the pure water of 2000ml, stir, then to join purity be in the quartz sand 200kg of 99.90%, mix, again by the quartz sand that the mixes temperature calcination 8 hours at 1100 DEG C that adulterates, naturally cooling.
Second step, by doping roasting after quartz sand put in continuous induction melting furnace, be heated to 1850 DEG C, then start to draw quartz glass bar, the diameter control of the quartz glass bar drawn out is at 1.7mm ± 0.2mm.
3rd step, to draw quartz glass bar carry out visual testing, by inspecting standard remove have bubble, gas line and bending quartz glass bar.
4th step, mixed liquid dipping to the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid, remove 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 DEG C.
5th step, to the quartz glass bar tap water 3min after acid bubble, then to be deionized water rinsing to the pH value of 9M Ω by resistivity be 7.
6th step, by the quartz glass bar oven for drying after cleaning up, the temperature in baking oven is 105 DEG C, and drying time is 40min.
7th step, the quartz glass bar after drying is put into vacuum deshydroxy stove and carried out deshydroxy, the vacuum tightness of vacuum deshydroxy stove is 50Pa, and the temperature of vacuum deshydroxy stove is risen to 1050 DEG C, keeps 30min, removes metastable hydroxyl in quartz pushrod.
8th step, the quartz glass bar after deshydroxy to be tested, remove and have diastrophic quartz glass bar.
9th step, mixed liquid dipping to the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid, remove 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 DEG C.
Tenth step, to the quartz glass bar tap water 3min after acid bubble, then to be deionized water rinsing to the pH value of 10M Ω by resistivity be 7.
11 step, by the quartz glass bar oven for drying after cleaning up, the temperature in baking oven is 105 DEG C, and drying time is 30min.
12 step, the quartz glass bar after drying is sent into melt drawing equipment, delivery speed is 1.5mm/s, adopts oxyhydrogen flame burning that quartz glass bar is heated to 1780 DEG C, is drawn into silica fiber with the draw rate of 20m/s.
Adopt the nitrating silica glass that embodiment 1 is obtained, viscosity when its 1200 DEG C is 1.3 times of common silica glass, and obtained nitrating silica fiber is powerful higher than common silica fiber by 5% in the tension fracture of 1000 DEG C of process after 1 hour.
Embodiment 2:
The first step, get the aluminium nitride of 250g, make its total content that adulterates be 40 ~ 3000ppm, aluminum nitride particle diameter is 80 ~ 100 μm, and joining purity is in the quartz sand 200kg of 99.90%, mixes.
Second step, put in continuous induction melting furnace by the quartz sand of uniform doping, be heated to 1780 DEG C, then start to draw quartz glass bar, diameter control is at 2.0mm ± 0.2mm.
3rd step, visual testing is carried out to the silica glass drawn, remove and have a large amount of bubble, quartz pushrod that gas line is more and bending.
4th step, mixed liquid dipping to the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid, remove 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 controls at 20 DEG C.
5th step, to the quartz glass bar tap water after acid bubble, flush time is 5min, then to be deionized water rinsing to the pH value of 10M Ω by resistivity be 6.
6th step, the quartz glass bar after cleaning up to be dried naturally or by oven for drying, bake out temperature is 105 DEG C, and drying time is 50min.
7th step, quartz glass bar is put into vacuum deshydroxy stove carry out deshydroxy, vacuum degree control, at 30Pa, is warming up to 1050 DEG C, keeps constant temperature 50min, removes metastable hydroxyl in quartz pushrod.
8th step, the quartz glass bar after deshydroxy to be tested, remove and have diastrophic rod.
9th step, mixed liquid dipping to the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid, remove 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 controls at 20 DEG C.
Tenth step, to the quartz glass bar tap water 5min after acid bubble, then to be deionized water rinsing to the pH value of 18M Ω by resistivity be 6.
11 step, the quartz glass bar after cleaning up to be dried naturally or by oven for drying, bake out temperature is 100 DEG C, drying time 50min.
12 step, the quartz glass bar feeding melt drawing equipment of will dry, control delivery speed at 1.0mm/s, adopt oxyhydrogen flame burning that quartz glass bar is heated to 1820 DEG C, be drawn into silica fiber with the draw rate of 25m/s.
Adopt the nitrating silica glass that embodiment 2 is obtained, viscosity when its 1200 DEG C is 1.8 times of common silica glass, and obtained nitrating silica fiber is powerful higher than common silica fiber by 10% in the tension fracture of 1000 DEG C of process after 1 hour.
Embodiment 3:
The first step, get the silicon nitride of 150g, its total content that adulterates is made to be 40 ~ 3000ppm, silicon nitride particle diameter is 40 ~ 60 μm, add in the pure water of 2000ml, stir, then to add purity be in the quartz sand 200kg of 99.90%, mix, again by the quartz sand that the mixes temperature calcination 12 hours at 1000 DEG C that adulterates, naturally cooling.
Second step, by doping roasting after quartz sand put in continuous induction melting furnace, be heated to 1800 DEG C, then start to draw quartz glass bar, the diameter control of the quartz glass bar drawn out is at 2.5mm ± 0.2mm.
3rd step, to draw quartz glass bar carry out visual testing, by inspecting standard remove have bubble, gas line and bending quartz glass bar.
4th step, mixed liquid dipping to the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid, remove 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 controls at 20 DEG C.
5th step, to the quartz glass bar tap water 2min after acid bubble, then to be deionized water rinsing to the pH value of 12M Ω by resistivity be 7.
6th step, by the quartz glass bar oven for drying after cleaning up, the temperature in baking oven is 80 DEG C, and drying time is 100min.
7th step, the quartz glass bar after drying is put into vacuum deshydroxy stove and carried out deshydroxy, the vacuum tightness of vacuum deshydroxy stove is 30Pa, and the temperature of vacuum deshydroxy stove is risen to 1100 DEG C, keeps 50min, removes metastable hydroxyl in quartz pushrod.
8th step, the quartz glass bar after deshydroxy to be tested, remove and have diastrophic quartz glass bar.
9th step, mixed liquid dipping to the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid, remove 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 controls at 20 DEG C.
Tenth step, to the quartz glass bar tap water 2min after acid bubble, then to be deionized water rinsing to the pH value of 12M Ω by resistivity be 7.
11 step, by the quartz glass bar oven for drying after cleaning up, the temperature in baking oven is 80 DEG C, and drying time is 100min.
12 step, the quartz glass bar after drying is sent into melt drawing equipment, delivery speed is 0.8mm/s, adopts oxyhydrogen flame burning that quartz glass bar is heated to 1850 DEG C, is drawn into silica fiber with the draw rate of 30m/s.
Adopt the nitrating silica glass that embodiment 3 is obtained, the common silica glass of its ratio of viscosities of 1200 DEG C is about high 1.7 times, and obtained nitrating silica fiber is powerful higher than common silica fiber by 9% in the tension fracture of 1000 DEG C of process after 1 hour.
Embodiment 4:
The first step, get the aluminium nitride of 400g, make its total content that adulterates be 40 ~ 3000ppm, aluminum nitride particle diameter is 80 ~ 100 μm, and joining purity is in the quartz sand 200kg of 99.90%, mixes.
Second step, put in continuous induction melting furnace by the quartz sand of uniform doping, be heated to 1830 DEG C, then start to draw quartz glass bar, diameter control is at 3.0mm ± 0.2mm.
3rd step, visual testing is carried out to the silica glass drawn, remove and have a large amount of bubble, quartz pushrod that gas line is more and bending.
4th step, to the quartz glass bar hydrofluoric acid dips be 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 controls at 30 DEG C.
5th step, to the quartz glass bar tap water after acid bubble, flush time is 2min, then to be deionized water rinsing to the pH value of 12M Ω by resistivity be 6 ~ 7.
6th step, the quartz glass bar after cleaning up to be dried naturally or by oven for drying, bake out temperature is 80 DEG C, and drying time is 100min.
7th step, quartz glass bar is put into vacuum deshydroxy stove carry out deshydroxy, vacuum degree control, at 20Pa, is warming up to 1080 DEG C, keeps constant temperature 60min, removes metastable hydroxyl in quartz pushrod.
8th step, the quartz glass bar after deshydroxy to be tested, remove and have diastrophic rod.
9th step, to the quartz glass bar hydrofluoric acid immersion bubble be 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 controls at 35 DEG C.
Tenth step, to the quartz glass bar tap water 1min after acid bubble, then to be deionized water rinsing to the pH value of 16M Ω by resistivity be 6 ~ 7.
11 step, the quartz glass bar after cleaning up to be dried naturally or by oven for drying, bake out temperature is 80 DEG C, drying time 100min.
12 step, the quartz glass bar feeding melt drawing equipment of will dry, control delivery speed at 0.6mm/s, adopt oxyhydrogen flame burning that quartz glass bar is heated to 1880 DEG C, be drawn into silica fiber with the draw rate of 40m/s.
Adopt the nitrating silica glass that embodiment 4 is obtained, viscosity when its 1200 DEG C is 2 times of common silica glass, and obtained nitrating silica fiber is powerful higher than common silica fiber by 15% in the tension fracture of 1000 DEG C of process after 1 hour.
Embodiment 5:
The first step, get the titanium nitride of 500g, its total content that adulterates is made to be 40 ~ 3000ppm, titanium nitride particles diameter is 20 ~ 50 μm, add in the pure water of 5000ml, stir, then to add purity be in the quartz sand 200kg of 99.90%, mix, again by the quartz sand that the mixes temperature calcination 20 hours at 800 DEG C that adulterates, naturally cooling.
Second step, by doping roasting after quartz sand put in continuous induction melting furnace, be heated to 1850 DEG C, then start to draw quartz glass bar, the diameter control of the quartz glass bar drawn out is at 3.2mm ± 0.2mm.
3rd step, to draw quartz glass bar carry out visual testing, by inspecting standard remove have bubble, gas line and bending quartz glass bar.
4th step, to the quartz glass bar hydrofluoric acid dips be 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 controls at 25 DEG C.
5th step, to the quartz glass bar tap water 4min after acid bubble, then to be deionized water rinsing to the pH value of 16M Ω by resistivity be 7.
6th step, by the quartz glass bar oven for drying after cleaning up, the temperature in baking oven is 60 DEG C, and drying time is 120min.
7th step, the quartz glass bar after drying is put into vacuum deshydroxy stove and carried out deshydroxy, the vacuum tightness of vacuum deshydroxy stove is 20Pa, and the temperature of vacuum deshydroxy stove is risen to 1120 DEG C, keeps 60min, removes metastable hydroxyl in quartz pushrod.
8th step, the quartz glass bar after deshydroxy to be tested, remove and have diastrophic quartz glass bar.
9th step, to the quartz glass bar hydrofluoric acid dips be 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 controls at 25 DEG C.
Tenth step, to the quartz glass bar tap water 4min after acid bubble, then to be deionized water rinsing to the pH value of 16M Ω by resistivity be 7.
11 step, by the quartz glass bar oven for drying after cleaning up, the temperature in baking oven is 60 DEG C, and drying time is 120min.
12 step, the quartz glass bar after drying is sent into melt drawing equipment, delivery speed is 0.5mm/s, adopts oxyhydrogen flame burning that quartz glass bar is heated to 1820 DEG C, is drawn into silica fiber with the draw rate of 50m/s.
Adopt the nitrating silica glass that embodiment 5 is obtained, viscosity when its 1200 DEG C is 2 times of common quartz, and obtained nitrating silica fiber is powerful higher than common silica fiber by 14% in the tension fracture of 1000 DEG C of process after 1 hour.
The above is the embodiment of this invention, above-mentioned illustrating is not construed as limiting flesh and blood of the present invention, person of an ordinary skill in the technical field can make an amendment above-mentioned embodiment or be out of shape after having read this specification sheets, and does not deviate from the spirit and scope of the invention.
Claims (1)
1. a preparation method for nitrating silica fiber, is characterized in that: it is made up of following steps:
The first step, at silica purity be more than 99.90% quartz sand in evenly mix the nitride that total content is 40 ~ 3000ppm, 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 μm, and is mixed with quartz sand by the material mixed;
Second step, put in continuous induction melting furnace by the quartz sand after uniform doping, be heated to 1800 ~ 2200 DEG C, start to draw quartz glass bar, the diameter of quartz glass bar is 1.5 ~ 3.5mm;
3rd step, to draw quartz glass bar carry out visual testing, by inspecting standard remove have bubble, gas line and bending quartz glass bar;
4th step, to the mixed solution of the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid or wherein a kind of soaked with liquid, 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 DEG C;
5th step, to the quartz glass bar tap water 1 ~ 5min after acid bubble, then to be deionized water rinsing to the pH value of 8 ~ 18M Ω by resistivity be 6 ~ 7;
6th step, naturally to be dried by the quartz glass bar after cleaning up or by oven for drying, temperature when adopting oven for drying in baking oven is 30 ~ 105 DEG C, and drying time is 10 ~ 120min;
7th step, the quartz glass bar after drying is put into vacuum deshydroxy stove and carried out deshydroxy, the vacuum tightness of vacuum deshydroxy stove is 5Pa ~ 100Pa, and the temperature of vacuum deshydroxy stove is risen to 1000 DEG C ~ 1100 DEG C, keeps 30 ~ 60min, removes metastable hydroxyl in quartz pushrod;
8th step, the quartz glass bar after deshydroxy to be tested, remove and have diastrophic quartz glass bar;
9th step, to the mixed solution of the quartz glass bar hydrofluoric acid be up to the standards and hydrochloric acid or wherein a kind of soaked with liquid, 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 DEG C;
Tenth step, to the quartz glass bar tap water 1 ~ 5min after acid bubble, then to be deionized water rinsing to the pH value of 8 ~ 18M Ω by resistivity be 6 ~ 7;
11 step, naturally to be dried by the quartz glass bar after cleaning up or by oven for drying, temperature when adopting oven for drying in baking oven is 30 ~ 105 DEG C, and drying time is 10 ~ 120min;
12 step, will to dry or quartz glass bar after drying sends into melt drawing equipment, delivery speed is 0.5 ~ 1.5mm/s, adopts oxyhydrogen flame burning that quartz glass bar is heated to 1750 ~ 1900 DEG C, is drawn into silica fiber with the draw rate of 20 ~ 50m/s.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1894986A2 (en) * | 2006-08-31 | 2008-03-05 | Chevron Oronite Company LLC | Method for forming tetraoxy-silane derived antiwear films and lubricating oil compositions therefrom |
| 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 |
| CN101568497A (en) * | 2006-12-22 | 2009-10-28 | 赫罗伊斯石英玻璃股份有限两合公司 | Quartz glass component with reflector layer and method for producing the same |
| CN101600663A (en) * | 2006-09-29 | 2009-12-09 | 赫罗伊斯石英玻璃股份有限两合公司 | Be used to make the silicon-dioxide slurry of silica glass and the purposes of this slurry |
| CN101622204A (en) * | 2007-02-27 | 2010-01-06 | 赫罗伊斯石英玻璃股份有限两合公司 | Optical component used in micro-lithographic exposure and projection systems for producing highly integrated circuits consists of synthetic quartz glass containing hydroxyl groups and chemically bound |
| CN101687680A (en) * | 2007-06-30 | 2010-03-31 | 赫罗伊斯石英玻璃股份有限两合公司 | Method for the production of a composite body from a basic body of opaque quartz glass and a tight sealing layer |
| 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 |
| CN102575377A (en) * | 2009-10-06 | 2012-07-11 | Lg矽得荣株式会社 | Quartz crucible and method of manufacturing the same |
-
2013
- 2013-07-30 CN CN201310324771.1A patent/CN103387329B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1894986A2 (en) * | 2006-08-31 | 2008-03-05 | Chevron Oronite Company LLC | Method for forming tetraoxy-silane derived antiwear films and lubricating oil compositions therefrom |
| CN101600663A (en) * | 2006-09-29 | 2009-12-09 | 赫罗伊斯石英玻璃股份有限两合公司 | Be used to make the silicon-dioxide slurry of silica glass and the purposes of this slurry |
| CN101568497A (en) * | 2006-12-22 | 2009-10-28 | 赫罗伊斯石英玻璃股份有限两合公司 | Quartz glass component with reflector layer and method for producing the same |
| CN101622204A (en) * | 2007-02-27 | 2010-01-06 | 赫罗伊斯石英玻璃股份有限两合公司 | Optical component used in micro-lithographic exposure and projection systems for producing highly integrated circuits consists of synthetic quartz glass containing hydroxyl groups and chemically bound |
| CN101687680A (en) * | 2007-06-30 | 2010-03-31 | 赫罗伊斯石英玻璃股份有限两合公司 | Method for the production of a composite body from a basic body of opaque quartz glass and a tight sealing layer |
| 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 |