CN101328014B - Manufacturing method of doping quartz glass fibre - Google Patents
Manufacturing method of doping quartz glass fibre Download PDFInfo
- Publication number
- CN101328014B CN101328014B CN2008100486495A CN200810048649A CN101328014B CN 101328014 B CN101328014 B CN 101328014B CN 2008100486495 A CN2008100486495 A CN 2008100486495A CN 200810048649 A CN200810048649 A CN 200810048649A CN 101328014 B CN101328014 B CN 101328014B
- Authority
- CN
- China
- Prior art keywords
- quartz glass
- glass bar
- quartz
- sand
- quartz sand
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Glass Compositions (AREA)
Abstract
The invention relates to production method of a doped silica glass fiber comprising doping one or two mixtures with a total content 0.01-0.4% of the silicon dioxide substance amount in the quartz sand of the alumina and gallium oxide into a quartz sand with a purity more than 99.90% by a special doping technology, melting the mixture by an electric heating mode to draw into fine quartz glass rod, drawing the quartz glass rod into a quartz fiber which has a higher viscosity at 1200 DEG C than the normal quartz glass fiber. The method solves the problem that in the prior art a layer heat-resistant material is closely coated on the surface of the fiber, but the ideal coated fiber can not be obtained after drawing, besides the excellent electrical property of the quartz glass fiber is reduced. The production technology of the invention is simple, the prepared quartz glass fiber has a good temperature-resistant property, at the same time the other excellent property of the quartz glass is not reduced. The method is suitable for producing quartz glass fiber with good temperature-resistant property.
Description
Technical field:
The present invention relates to a kind of manufacture method of quartz glass fibre, particularly a kind of manufacture method of doping quartz glass fibre.
Background technology:
As everyone knows, the best silicate glass fiber of heat resistance is a quartz glass fibre.But, in the temperature more than 1200 ℃, even quartz glass fibre also is difficult to stand for a long time.In order to improve the heat resistance of quartz glass fibre, currently used method is closely to apply the resistant to elevated temperatures material of one deck at fiber surface, as boron nitride, and materials such as silicon carbide.The technology that is coated with one deck boron nitride or silicon carbide on the silica glass surface is very ripe, still, is applying the resistant to elevated temperatures material of one deck on the quartz glass fibre than much complicated on the resistant to elevated temperatures material technology of coating one deck on the silica glass.Wire drawing after being coated with one deck boron nitride or silicon carbide on the silica glass surface can not obtain the ideal coated fibre, and this is because boron nitride or silicon carbide can not stand the softening wire-drawing temperature of silica glass.Therefore, the resistant to elevated temperatures material of quartz glass fibre surface-coated one deck must adopt some complexity, special method.And the another one shortcoming is, the high temperature material permittivity ratio silica glass height of quartz glass fibre coating, electrical insulation capability are than silica glass difference, and this has also reduced the quartz glass fibre excellent electric performance to a certain extent.
Summary of the invention:
The objective of the invention is to: a kind of aluminum oxide or gallium oxide of mixing in quartz sand is provided, production technique is simple, the quartz glass fibre heat resistance of producing is good, does not reduce the manufacture method of doping quartz glass fibre of other excellent properties of silica glass simultaneously again.
The present invention realizes above-mentioned purpose by following technical solution:
In general, impurity enters in the quartz glass body, can reduce the viscosity of silica glass, promptly reduces the heat resistance of silica glass.Yet, when aluminum oxide or gallium oxide evenly enter in the silica glass, some unusual characteristics are arranged but under the situation of lower concentration.This is because small amount of aluminum or gallium can form complex compound with basic metal, simultaneously, forms the anoxic structure at silica glass, and such structure makes the silica structure in the silica glass tightr, thereby has caused the abnormality of performances such as viscosity, resistivity.The present invention utilizes this characteristic of silica glass to realize purpose of the present invention just.
Technical essential of the present invention is: to mix total content in purity surpasses 99.90% quartz sand be the aluminum oxide of silica species amount 0.01～0.4% in the quartz sand, the mixture of one or both arbitrary proportions in the gallium oxide, then by electrically heated mode fusion, and pull into microlith English glass stick, again quartz glass bar is drawn into quartz glass fibre.
The present invention realizes by following concrete steps:
A kind of manufacture method of doping quartz glass fibre is characterized in that: it is that in the following order step is carried out:
(1) evenly to mix total content in purity surpasses 99.90% quartz sand be the aluminum oxide of silica species amount 0.01%-0.4% in the quartz sand, the mixture of one or both arbitrary proportions in the gallium oxide.
Adulterated feature also is:
(a) hotchpotch not only can be the mixture of aluminum oxide or gallium oxide or both arbitrary proportions, can also be aluminium salt or gallium salt.When mixing with aluminium salt or gallium salt, the quartz sand that also needs to mix this salt carries out roasting, and maturing temperature should be controlled between 700～1300 ℃, and soaking time should be not less than 30 minutes, made it resolve into aluminum oxide or gallium oxide.
When (b) hotchpotch added in the quartz sand with solid form or solid-liquid blended form, its particle diameter should be no more than 20 μ m, mixed to guarantee the material and the quartz sand that mix; When hotchpotch adds in the quartz sand with solid-liquid blended form, also need to mix again the quartz sand oven dry after aluminium salt or the gallium salt.Wherein, when hotchpotch is non-oxide aluminium or non-oxide gallium, also need between 700～1300 ℃, to carry out roasting, and soaking time was not less than 30 minutes, makes compound decomposition become aluminum oxide or gallium oxide.
(c) if hotchpotch is when selecting salt soluble in water, mixes with quartz sand after filler plasmogamy can being become solution, carry out roasting again between 700-1300 ℃, and soaking time should be not less than 30 minutes.The purpose of high-temperature roasting is to dry quartz sand, and decomposes the salt into oxide compound.
(2) quartz sand of uniform doping is put in crucible oven or the continuous induction melting furnace, be heated to 1800-2200 ℃, begin to draw quartz glass bar then.The diameter of quartz glass bar is controlled between the 1.53.5mm.
Feature of the present invention also is: when adopting crucible oven fused quartz sand pull-rod, the back of step (2) comprises step (3)-(6) and (12); When adopting continuous induction melting furnace fused quartz sand pull-rod, the back of step (2) comprises step (3)-(12).
(3) quartz glass bar that draws is tested, rejecting has the more and diastrophic rod of the gentle line of bubble.
(4) quartz glass bar that is up to the standards being used volume ratio with water is hydrofluoric acid dips 15-120 minute of 5-15%, and soaking temperature is controlled at 10-35 ℃.
(5) quartz glass bar behind the acid bubble is rinsed well with tap water after, rinse well greater than the deionized water of 0.5M Ω with resistivity again, until flushing afterwards the pH value of water be 6-7.
(6) quartz glass bar after will cleaning up dries naturally; If quartz glass bar is to adopt continuous induction melting furnace fused quartz sand to draw, enter step (7); If quartz glass bar is to adopt crucible oven fused quartz sand to draw, directly enter step (12).
(7) quartz glass bar of step (6) is sent into vacuum deshydroxy stove, vacuum degree control is warming up to 1000-1100 ℃ below 100Pa, keeps constant temperature more than 0.5 hour, removes metastable hydroxyl in the quartz pushrod.
(8) quartz glass bar behind the deshydroxy is tested, rejecting has diastrophic rod.
(9) the quartz glass bar volume ratio that step (8) is up to the standards is hydrofluoric acid dips 15-120 minute of 5-15%, and soaking temperature is controlled at 10-35 ℃.
(10) quartz glass bar behind the acid bubble is rinsed well with tap water after, clean up greater than the deionized water of 0.5M Ω with resistivity again and rinse well, until flushing afterwards the pH value of water be 6-7.
(11) quartz glass bar after will cleaning up dries naturally.
(12) quartz glass bar after will drying is sent into the melt drawing equipment of rod, and the control delivery speed is heated to 1750-1900 ℃ at 0.5-1.5mm/s with quartz glass bar, is drawn into quartz glass fibre with the draw rate of 20-50m/s.
The invention has the advantages that:
The doping quartz glass fibre that adopts the present invention to make has still kept all advantage performances of quartz glass fibre, and the heatproof of fiber and devitrification resistance can be greatly improved.The present invention is bigger to the purity relation of the raising of viscosity and quartz sand, and when doping was identical, greater than 99.90% quartz sand, quartz sand purity was low more for dioxide-containing silica, and the product viscosity after the doping improves big more.The quartz glass fibre of making in doping scope of the present invention, the comparable non-adulterated quartz glass fibre viscosity of its viscosity in the time of 1200 ℃ improves 0.1-10
4Doubly.
Embodiment:
That the invention will be further described is as follows below in conjunction with specific embodiment.
Embodiment 1:
(1) getting purity is 99.99% quartz sand 20kg, adds 33 gram aluminum oxide, mixes.
(2) quartz sand of uniform doping is put in the crucible oven, be heated to 1850 ℃, begin to draw quartz glass bar then.The diameter of quartz glass bar is controlled at 1.9mm.
(3) quartz glass bar of La Zhiing is tested, and rejecting has the more and diastrophic quartz glass bar of the gentle line of bubble.
(4) the quartz glass bar volume ratio that step (3) is up to the standards is 5-15% hydrofluoric acid dips 15-120 minute, and soaking temperature is controlled at 25 ℃.
(5) rinse well greater than the deionized water of 0.5M Ω with resistivity again after the quartz glass bar behind the acid bubble is rinsed well with tap water, until flushing afterwards the pH value of water be 6-7.
(6) quartz glass bar after will cleaning up dries naturally.
(7) quartz glass bar of step (6) is sent into excellent melt drawing equipment, the control delivery speed is heated to 1750-1900 ℃ at 0.5-1.5mm/s with quartz glass bar, is drawn into quartz glass fibre with 20-50m/s.
The quartz glass fibre that adopts above-mentioned steps to found, the common quartz glass fibre of 1200 ℃ ratio of viscosities is high approximately 2 times.
Embodiment 2:
(1) getting purity is 99.99% quartz sand 200kg, adds the aluminum oxide of 66g, mixes.
(2) quartz sand of uniform doping is put in the continuous induction melting furnace, be heated to 1850 ℃, begin to draw quartz glass bar then.The diameter of quartz glass bar is controlled at 1.9mm.
(3) quartz glass bar of La Zhiing is tested, and rejecting has the more and diastrophic rod of the gentle line of bubble.
(4) the quartz glass bar volume ratio that step (3) is up to the standards is 5-15% hydrofluoric acid dips 15-120 minute, and soaking temperature is controlled at 10-35 ℃.
(5) rod behind the acid bubble is rinsed well with tap water after, rinse well greater than the deionized water of 0.5M Ω with resistivity again, until flushing afterwards the pH value of water be 6-7.
(6) quartz glass bar after will cleaning up dries.
(7) quartz glass bar of step (6) is sent into vacuum deshydroxy stove, vacuum degree control is warming up to 1000～1100 ℃ below 100Pa, and constant temperature removed metastable hydroxyl in the quartz pushrod more than 0.5 hour.
(8) quartz glass bar behind the deshydroxy is tested, rejecting has diastrophic rod.
(9) the quartz glass bar volume ratio that step (8) is up to the standards is 5-15% hydrofluoric acid dips 15-120 minute, and soaking temperature is controlled at 10-35 ℃.
(10) quartz glass bar behind the acid bubble is rinsed well with tap water after, rinse well greater than the deionized water of 0.5M Ω with resistivity again, until flushing afterwards the pH value of water be 6-7.
(11) quartz glass bar after will cleaning up dries naturally.
(12) quartz glass bar of step (11) is sent into excellent melt drawing equipment, the control delivery speed is heated to 1750-1900 ℃ at 0.5-1.5mm/s with quartz glass bar, is drawn into quartz glass fibre with 20-50m/s.
The quartz glass fibre that adopts above-mentioned steps to found, the common quartz glass fibre of 1200 ℃ ratio of viscosities is high approximately 1 times.
Embodiment 3:
(1) gets the Al (NO of 7.26kg
3)
39H
20, be that the deionized water of 14kg is made into aluminum nitrate solution with weight; Get purity again and be 99.99% quartz sand 200kg.
(2) be that 99.99% 200kg quartz sand mixes with aluminum nitrate solution and purity.
(3) with the mixture of step (2) at 1100 ℃ of roastings 5 hours, naturally cooling.Obtain the uniform quartz sand of alumina doped.
(4) quartz sand of uniform doping is put in the continuous induction melting furnace, be heated to 1850 ℃, begin to draw quartz glass bar then.The diameter of quartz glass bar is controlled at 1.9mm.
(5) quartz glass bar of La Zhiing is tested, and rejecting has the more and diastrophic rod of the gentle line of bubble.
(6) the rod volume ratio that step (5) is up to the standards is 5-15% hydrofluoric acid dips 15-120 minute, and soaking temperature is controlled at 10-35 ℃.
(7) rinse well greater than the deionized water of 0.5M Ω with resistivity again after the rod behind the acid bubble is rinsed well with tap water, until flushing afterwards the pH value of water be 6-7.
(8) quartz glass bar after will cleaning up dries naturally.
(9) quartz glass bar of step (8) is sent into vacuum deshydroxy stove, vacuum degree control is warming up to 1000-1100 ℃ below 100Pa, and constant temperature removed metastable hydroxyl in the quartz pushrod more than 0.5 hour.
(10) quartz glass bar behind the deshydroxy is tested, rejecting has diastrophic rod.
(11) the rod volume ratio that step (10) is up to the standards is 5-15% hydrofluoric acid dips 15-120 minute, and soaking temperature is controlled at 10-35 ℃.
(12) rinse well greater than the deionized water of 0.5M Ω with resistivity again after the rod behind the acid bubble is rinsed well with tap water, until flushing afterwards the pH value of water be 6-7.
(13) quartz glass bar after will cleaning up dries.
(14) quartz glass bar of step (13) is sent into excellent melt drawing equipment, the control delivery speed is heated to 1750-1900 ℃ at 0.5-1.5mm/s with quartz glass bar, is drawn into quartz glass fibre with 20-50m/s.
The quartz glass fibre that adopts above-mentioned steps to found, the common quartz glass fibre of 1200 ℃ ratio of viscosities is high approximately 0.7 times.
Embodiment 4:
Get purity and be 99.99% quartz sand 20kg, add the gallium oxide of 125g, mix.Its processing step is with embodiment 1.
The quartz glass fibre that adopts embodiment 4 steps to found, the common quartz glass fibre of 1200 ℃ ratio of viscosities is high approximately 1.5 times.
Embodiment 5:
Get purity and be 99.92% quartz sand 20kg, add the gallium oxide of 63g and the aluminum oxide of 34g, mix.Its processing step is with embodiment 1.
The quartz glass fibre that adopts embodiment 5 steps to found, the common quartz glass fibre of 1200 ℃ ratio of viscosities is high approximately 30 times.
Claims (2)
1. the manufacture method of a doping quartz glass fibre is characterized in that, it is that in the following order step is carried out:
(1) evenly to mix total content in purity surpasses 99.90% quartz sand be the aluminum oxide of silica species amount 0.01%-0.4% in the quartz sand, the mixture of one or both any ratios in the gallium oxide;
(2) quartz sand of uniform doping is put in crucible oven or the continuous induction melting furnace, be heated to 1800-2200 ℃, begin to draw quartz glass bar then, the diameter of quartz glass bar is controlled between the 1.5-3.5mm;
(3) quartz glass bar that draws is tested, rejecting has the more and diastrophic rod of the gentle line of bubble;
(4) be hydrofluoric acid dips 15-120 minute of 5-15% to the quartz glass bar volume ratio that is up to the standards, soaking temperature is controlled at 10-35 ℃;
(5) quartz glass bar behind the acid bubble is rinsed well with tap water after, rinse well greater than the deionized water of 0.5M Ω with resistivity again, until flushing afterwards the pH value of water be 6-7;
(6) quartz glass bar after will cleaning up dries naturally; If quartz glass bar is to adopt continuous induction melting furnace fused quartz sand to draw, enter step (7); If quartz glass bar is to adopt crucible oven fused quartz sand to draw, directly enter step (12);
(7) quartz glass bar of step (6) is sent into vacuum deshydroxy stove, vacuum degree control is warming up to 1000-1100 ℃ below 100Pa, keeps constant temperature more than 0.5 hour, removes metastable hydroxyl in the quartz pushrod;
(8) quartz glass bar behind the deshydroxy is tested, rejecting has diastrophic rod;
(9) the quartz glass bar volume ratio that step (8) is up to the standards is hydrofluoric acid dips 15-120 minute of 5-15%, and soaking temperature is controlled at 10-35 ℃;
(10) quartz glass bar behind the acid bubble is rinsed well with tap water after, use resistivity clean again greater than the deionized water of 0.5M Ω, water ph value is 6-7 until the flushing back;
(11) quartz glass bar after will cleaning up dries naturally;
(12) quartz glass bar after will drying is sent into the melt drawing equipment of rod, and the control delivery speed is heated to 1750-1900 ℃ at 0.5-1.5mm/s with quartz glass bar, is controlled to quartz glass fibre with the draw rate of 20-50m/s.
2. the manufacture method of doping quartz glass fibre according to claim 1, it is characterized in that: the described hotchpotch of step (1) can also be aluminium salt or gallium salt, when mixing with aluminium salt or gallium salt, the quartz sand that also needs to mix this salt carries out roasting, maturing temperature should be controlled between 700-1300 ℃, soaking time should be not less than 30 minutes, made it resolve into aluminum oxide or gallium oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100486495A CN101328014B (en) | 2008-07-28 | 2008-07-28 | Manufacturing method of doping quartz glass fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100486495A CN101328014B (en) | 2008-07-28 | 2008-07-28 | Manufacturing method of doping quartz glass fibre |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101328014A CN101328014A (en) | 2008-12-24 |
| CN101328014B true CN101328014B (en) | 2010-12-22 |
Family
ID=40204066
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100486495A Active CN101328014B (en) | 2008-07-28 | 2008-07-28 | Manufacturing method of doping quartz glass fibre |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101328014B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190436A (en) * | 2010-03-16 | 2011-09-21 | 天津市硅酸盐研究所 | System and process for preparing quartz fibers |
| CN102503115B (en) * | 2011-11-08 | 2013-11-13 | 湖北菲利华石英玻璃股份有限公司 | Method for producing low-hydroxy quartz glass fibers |
| CN103387329B (en) * | 2013-07-30 | 2016-03-23 | 湖北菲利华石英玻璃股份有限公司 | A kind of preparation method of nitrating silica fiber |
| CN105693271A (en) * | 2016-01-29 | 2016-06-22 | 卓达新材料科技集团有限公司 | Preparation method of germanium oxide-silicon oxide hybrid aerogel composite material |
| CN106430952B (en) * | 2016-09-07 | 2019-06-07 | 中国建筑材料科学研究总院 | The preparation method and quartz glass of quartz glass |
| CN110903034A (en) * | 2019-12-05 | 2020-03-24 | 南京工业大学东海先进硅基材料研究院 | Preparation method of quartz glass cladding material for optical fiber and continuous melting furnace device |
| CN113354292A (en) * | 2021-06-25 | 2021-09-07 | 五河信达新材料有限公司 | Preparation method of high-strength glass fiber |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0250259A1 (en) * | 1986-06-20 | 1987-12-23 | Nippon Electric Glass Company., Ltd. | Low dielectric fiber glass composition having improved water resistance and heat resistance |
| CN1752040A (en) * | 2004-09-22 | 2006-03-29 | 台湾玻璃工业股份有限公司 | Glass having low dielectric constant |
-
2008
- 2008-07-28 CN CN2008100486495A patent/CN101328014B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0250259A1 (en) * | 1986-06-20 | 1987-12-23 | Nippon Electric Glass Company., Ltd. | Low dielectric fiber glass composition having improved water resistance and heat resistance |
| CN1752040A (en) * | 2004-09-22 | 2006-03-29 | 台湾玻璃工业股份有限公司 | Glass having low dielectric constant |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2002-80240A 2002.03.19 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101328014A (en) | 2008-12-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101328014B (en) | Manufacturing method of doping quartz glass fibre | |
| CN109608050B (en) | High-frequency low-dielectric low-loss microcrystalline glass/ceramic LTCC substrate material and preparation method thereof | |
| CN102515851B (en) | Preparation method for silicon-nitride-based coating on surface of porous ceramic | |
| TWI694976B (en) | Low dielectric constant glass composition with low bubble number and glass fiber | |
| CN103553559A (en) | CaO-B2O3-SiO2 glass and aluminum nitride ceramic composite material and preparation method thereof | |
| CN111018485A (en) | High-cold-resistance porcelain insulator and preparation method thereof | |
| TW201228965A (en) | Crystalline glass powder | |
| JPH0761852B2 (en) | Method for producing non-sintered cristobalitized silica | |
| CN109250920A (en) | A kind of low-temperature co-burning ceramic material and preparation method thereof | |
| CN106673446B (en) | A kind of low Jie's high frequency devitrified glass LTCC material and preparation method thereof | |
| CN101209898A (en) | Erbium-doped barium-yttrium-fluoride-nanocrystalline containing transparent oxyfluoride glass ceramic and preparation thereof | |
| CN104609722A (en) | Preparation method of tube-melt co-drawn bismuth-doped optical fiber | |
| EP2305612A1 (en) | Method of producing grin lens | |
| CN114835380B (en) | Melting production process for inhibiting volatilization of borosilicate glass components | |
| CN111847882B (en) | Low-temperature sealing glass and preparation method thereof | |
| CN103693939A (en) | Preparation technology of toughening/heat-conduction low-expansion purple-clay pot material | |
| JP2019163198A (en) | Method for producing porous glass member | |
| CN114873924A (en) | Modified nitride-doped microcrystalline glass composite material, and preparation method and application thereof | |
| CN105731809A (en) | Insulating material for heating wire, preparation and application method thereof | |
| CN102060440B (en) | High-pressure-resistant sealing microcrystalline glass and use thereof | |
| CN101298368B (en) | Low-temperature rapid sintered high-frequency low-consumption glass ceramic and preparation thereof | |
| CN114933418A (en) | Low dielectric constant and low dielectric loss glass fiber composition, glass fiber and application thereof | |
| JP2012193067A (en) | Borosilicate glass, porous glass, and method for producing the same | |
| JP4178179B1 (en) | Manufacturing method of GRIN lens | |
| CN110950534A (en) | Glass insulator material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A manufacturing method of doped quartz glass fiber Effective date of registration: 20230925 Granted publication date: 20101222 Pledgee: China Everbright Bank Co.,Ltd. Jingzhou Branch Pledgor: HUBEI FEILIHUA QUARTZ GLASS Co.,Ltd. Registration number: Y2023980058350 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |