CN104909558B - A kind of method for preparing glassy transparent quartz sand - Google Patents
A kind of method for preparing glassy transparent quartz sand Download PDFInfo
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- CN104909558B CN104909558B CN201510316770.1A CN201510316770A CN104909558B CN 104909558 B CN104909558 B CN 104909558B CN 201510316770 A CN201510316770 A CN 201510316770A CN 104909558 B CN104909558 B CN 104909558B
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Abstract
The present invention provides a kind of method for preparing glassy transparent quartz sand, it is characterised in that：Synthesis high-purity silicon dioxide powder is placed in vacuum drying oven, is warming up to 1,100 1500 DEG C, is incubated 1 10 hours, 1,700 1800 DEG C is warming up to afterwards and is incubated 5 30 minutes, porous transparency silica glass block is made after cooling, glassy transparent quartz sand is obtained after crushing the block.
Description
Technical field
The invention belongs to quartz material preparation field, more particularly to prepares glassy transparent with synthesis high-purity silicon dioxide powder
The method of quartz sand.
Background technology
Quartz glass is the special industrial glass of silica one-component, has a variety of unique physical and chemical performances, is empty
Between indispensable material in technology, atomic energy industry, defence equipment, and the industry such as semiconductor, electric light source, communication, light industry
One of.
Preparing the raw material of quartz glass has two major classes, including the natural material such as crystal, quartz mine, and utilizes four chlorinations
The Material synthesis such as the silicon-containing compounds such as silicon, sodium metasilicate, silicon fluoride.Since earlier 1800s, quartz has been prepared using natural material
The method constantly improve of glass, its yield account for the 70-80% of whole quartz glass products.But due to natural mineral raw crystal
The limitation of structure, the problem of quartz glass quality as caused by the raw material containing impurity is bad, fail to be solved at all so that
Quartz glass prepared by natural material is unable to reach the quality requirement needed for high-end technology industry.
Although certain production cost can be increased by preparing quartz glass using synthesis material, products obtained therefrom is applied to high-end
Industry, with more market value.China Patent Publication No. CN1541194A discloses a kind of high purity synthetic vitreous silica particles
Preparation method, the quartz glass particle of high-purity, but its highest firing temperature are prepared in nitrogen atmosphere using synthesis material
For 1250 DEG C, the quartz products obtained by the firing temperature are opaque, and preparing transparency silica glass as raw material need to formulate in addition
Sintering technology, the product of transparency needed for obtaining can not be guaranteed.It is more that U.S. Patent Publication No. US6849242 discloses a kind of use
The method of hole silica gel synthetic quartz glass powder, fused silica powder is directly made without broken, but this method need to arrive 1100
1300 DEG C of progress hydrochlorinations, finally burn till, technical process is more complicated, and the sintering temperature in 1500 DEG C of helium-atmosphere
Low, obtained product is opaque, can not equally ensure that the quartz glass of required transparency can be prepared as raw material.
The content of the invention
The technical problem to be solved in the present invention is to design a kind of method of technique simple and stable, prepares high-purity glassy state
Suprasil sand.
The method for preparing glassy transparent quartz sand with synthesis high-purity silicon dioxide powder of the present invention, including：Synthesis is high
Pure silicon dioxide powder is placed in vacuum drying oven, is warming up to 1100-1500 DEG C, is incubated 1-10 hours；1700-1800 DEG C is warming up to afterwards
5-30 minutes are incubated, porous transparency silica glass block is made after cooling, glassy transparent quartz sand is obtained after crushing.
Further, the dioxide-containing silica in the synthesis high-purity silicon dioxide powder is more than 99.99%.
Further, the vacuum drying oven gas pressure intensity is less than 1Pa.
Further, the vacuum drying oven gas pressure intensity is less than or equal to 1 × 10-2Pa。
Further, 1100-1500 DEG C is warming up to, described soaking time is 4-8 hours.
Further, it is described to be warming up to 1100-1500 DEG C, including 1100 DEG C are warming up to soon, 1400- is then warming up to slowly
1500℃。
Further, it is described to be warming up to 1100-1500 DEG C, including 1100 are warming up to soon with the speed not less than 20 DEG C/min
DEG C, then 1400-1500 DEG C is warming up to slowly with the speed no more than 5 DEG C/min.
Further, the insulation 1-10 hours, afterwards to be warming up to 1700-1800 DEG C no more than 5 DEG C/min speed.
Compared with prior art, the advantage of the invention is that：It is high-purity using synthesizing using above method technique simple and stable
Silicon dioxide powder is only calcined in vacuum atmosphere, and gained quartz glass block after crushing, obtains the quartz sand of glassy state, has height
Pure transparent characteristic, can be as the raw material of the quartz glass products such as the inwall of monocrystalline silicon growing silica crucible, optical fiber.
Brief description of the drawings
Fig. 1 is the white quartz sand of the comparative example 1 of the present invention；
Fig. 2 is the white quartz sand XRD test charts shown in Fig. 1；
Fig. 3 is the white quartz sand XDR test charts of the comparative example 2 of the present invention；
Fig. 4 is the quartz glass of embodiments of the invention 1；
Fig. 5 is the glassy transparent quartz sand obtained after the quartz glass block shown in Fig. 4 is ground；
Fig. 6 is the glassy transparent quartz sand XRD test charts shown in Fig. 5.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
The method for preparing glassy transparent quartz sand of the present invention, synthesis high-purity silicon dioxide powder is placed in vacuum drying oven,
Set sintering procedure as：1100-1500 DEG C is warming up to, is incubated 1-10h；1700-1800 DEG C is warming up to, is incubated 5-30min；Treat stove
Taken out after interior quartz glass block cooling, obtain glassy transparent quartz sand after crushing.
Following examples further illustrate the present invention.
Comparative example 1：
Synthesis high-purity silicon dioxide powder (dioxide-containing silica is more than 99.99%) is placed in vacuum drying oven that (gas pressure intensity is low
In 1 × 10-2Pa), set sintering procedure as：Fast heating (speed be 20 DEG C/min) is to 1200 DEG C, and then slowly heating up, (speed is
1 DEG C/min) to 1450 DEG C insulation 8h.Taking-up obtains white quartz particles after making sample furnace cooling, after quartz particles are ground
Obtain opaque white quartz sand (referring to Fig. 1).The XRD of this white quartz sand shows that products obtained therefrom is (referring to Fig. 2)
Cristobalite crystal formation.
Comparative example 2：
Synthesis high-purity silicon dioxide powder (dioxide-containing silica is more than 99.99%) is placed in vacuum drying oven that (gas pressure intensity is low
In 1 × 10-2Pa), set sintering procedure as：Then fast heating (speed is 40 DEG C/min) is to slowly warm up to 1450 to 1100 DEG C
DEG C (speed is 1 DEG C/min) insulation 4h, heating (speed be 5 DEG C/min) is incubated 10min to 1650 DEG C slowly afterwards.Make sample with stove
Taken out after cooling and obtain white quartz particles, quartz sand is obtained after quartz particles are ground.The XRD of this white quartz sand
(referring to Fig. 3) display products obtained therefrom contains two kinds of crystal formations of vitreous silica and crystal state cristobalite.
Embodiment 1：
Synthesis high-purity silicon dioxide powder (dioxide-containing silica is more than 99.99%) is placed in vacuum drying oven that (gas pressure intensity is low
In 1 × 10-2Pa), set sintering procedure as：Then fast heating (speed is 20 DEG C/min) is to slowly warm up to 1450 to 1100 DEG C
DEG C (speed is 1 DEG C/min) insulation 4h, heating (speed be 5 DEG C/min) is incubated 10min to 1740 DEG C slowly afterwards.Make sample with stove
Taken out after cooling and obtain porous transparency silica glass block (referring to Fig. 4), suprasil sand (ginseng is obtained after quartz glass block is ground
See Fig. 5).
The XRD (referring to Fig. 6) of the suprasil sand shows that products obtained therefrom has been glassy state.
Embodiment 2：
Synthesis high-purity silicon dioxide powder (dioxide-containing silica is more than 99.99%) is placed in vacuum drying oven that (gas pressure intensity is low
In 1 × 10-2Pa), set sintering procedure as：Then fast heating (speed is 30 DEG C/min) is to slowly warm up to 1450 to 1100 DEG C
DEG C (speed is 3 DEG C/min) insulation 6h, heating (speed be 3 DEG C/min) is incubated 20min to 1760 DEG C slowly afterwards.Make sample with stove
Taken out after cooling and obtain porous transparency silica glass block, suprasil sand is obtained after quartz glass block is ground.
The XRD of the suprasil sand shows that products obtained therefrom has been glassy state.
Embodiment 3：
Synthesis high-purity silicon dioxide powder (dioxide-containing silica is more than 99.99%) is placed in vacuum drying oven that (gas pressure intensity is low
In 1 × 10-2Pa), set sintering procedure as：Then fast heating (speed is 40 DEG C/min) is to slowly warm up to 1450 to 1100 DEG C
DEG C (speed is 1 DEG C/min) insulation 8h, heating (speed be 1 DEG C/min) is incubated 30min to 1780 DEG C slowly afterwards.Make sample with stove
Taken out after cooling and obtain porous transparency silica glass block, suprasil sand is obtained after quartz glass block is ground.
The XRD of the suprasil sand shows that products obtained therefrom has been glassy state.
Comparative result table under table one, different condition
| Condition | Corresponding form |
| Comparative example 1 | The white quartz sand of cristobalite crystal formation |
| Comparative example 2 | White quartz sand containing two kinds of crystal formations of vitreous silica and crystal state cristobalite |
| Embodiment 1 | Glassy transparent quartz sand |
| Embodiment 2 | Glassy transparent quartz sand |
| Embodiment 3 | Glassy transparent quartz sand |
Claims (5)
- A kind of 1. method for preparing glassy transparent quartz sand, it is characterised in that：Synthesis high-purity silicon dioxide powder is placed in vacuum In stove, 1100 DEG C are warming up to soon with the speed not less than 20 DEG C/min, is then warming up to slowly with the speed no more than 5 DEG C/min 1400-1500 DEG C, it is incubated 4-8 hours；Afterwards to be warming up to 1700-1800 DEG C no more than 5 DEG C/min speed, 5-30 points of insulation Clock, porous transparency silica glass block is made after cooling, glassy transparent quartz sand is obtained after crushing.
- 2. the method according to claim 1 for preparing glassy transparent quartz sand, it is characterised in that：The synthesis high-purity two Dioxide-containing silica in silica powder is more than 99.99%.
- 3. the method according to claim 1 for preparing glassy transparent quartz sand, it is characterised in that：The vacuum furnace gases Pressure is less than 1Pa.
- 4. the method according to claim 3 for preparing glassy transparent quartz sand, it is characterised in that：The vacuum furnace gases Pressure is less than or equal to 1 × 10-2Pa。
- 5. the product prepared according to any described methods for preparing glassy transparent quartz sand of claim 1-4.
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| CN106365418B (en) * | 2016-08-30 | 2019-04-16 | 中国建筑材料科学研究总院 | Lightweight quartz glass and preparation method thereof |
| CN106277802B (en) * | 2016-08-30 | 2019-04-16 | 中国建筑材料科学研究总院 | Foam quartz glass, preparation method and quartz glass reflecting mirror |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0816297A1 (en) * | 1996-07-04 | 1998-01-07 | Tosoh Corporation | Opaque quartz glass and process for production thereof |
| US6360563B1 (en) * | 1999-08-13 | 2002-03-26 | Heraeus Quarzglas Gmbh & Co. Kg | Process for the manufacture of quartz glass granulate |
| CN103864292A (en) * | 2014-02-28 | 2014-06-18 | 中国科学院上海光学精密机械研究所 | Preparation method for fluorine-containing low-refractivity Yb<3+>-doped quartz glass |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4035794B2 (en) * | 1998-02-24 | 2008-01-23 | 東ソー株式会社 | Method for producing opaque quartz glass ring |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0816297A1 (en) * | 1996-07-04 | 1998-01-07 | Tosoh Corporation | Opaque quartz glass and process for production thereof |
| US6360563B1 (en) * | 1999-08-13 | 2002-03-26 | Heraeus Quarzglas Gmbh & Co. Kg | Process for the manufacture of quartz glass granulate |
| CN103864292A (en) * | 2014-02-28 | 2014-06-18 | 中国科学院上海光学精密机械研究所 | Preparation method for fluorine-containing low-refractivity Yb<3+>-doped quartz glass |
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Address after: 222313 Tuofeng new area, Donghai County, Lianyungang City, Jiangsu Province Patentee after: Jiangsu Hongwei quartz Technology Co., Ltd Address before: 222313 hump Industrial Zone, Lianyungang, Jiangsu, Donghai County Patentee before: Lianyungang Hongwei Quarts Product Co., Ltd. |
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