CN104909558A - Method for preparing glassy state transparent quartz sand - Google Patents
Method for preparing glassy state transparent quartz sand Download PDFInfo
- Publication number
- CN104909558A CN104909558A CN201510316770.1A CN201510316770A CN104909558A CN 104909558 A CN104909558 A CN 104909558A CN 201510316770 A CN201510316770 A CN 201510316770A CN 104909558 A CN104909558 A CN 104909558A
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- China
- Prior art keywords
- quartz sand
- transparent quartz
- warming
- glassy transparent
- method preparing
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 239000006004 Quartz sand Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000010792 warming Methods 0.000 claims description 24
- 230000015572 biosynthetic process Effects 0.000 claims description 15
- 238000009413 insulation Methods 0.000 claims description 13
- 238000003786 synthesis reaction Methods 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 238000013467 fragmentation Methods 0.000 claims description 5
- 238000006062 fragmentation reaction Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 9
- 239000010453 quartz Substances 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 239000004576 sand Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000005755 formation reaction Methods 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007038 hydrochlorination reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
- Glass Compositions (AREA)
Abstract
The invention provides a method for preparing glassy state transparent quartz sand. The method is characterized by comprising the following steps: placing synthesized high-purity silicon dioxide powder in a vacuum furnace, raising temperature to 1100-1500 DEG C, keeping temperature for 1-10 hours, and then raising temperature to 1700-1800 DEG C to keep temperature for 5-30 min, cooling to prepare a porous transparent quartz glass block, and crushing the block body to obtain the glassy state transparent quartz sand.
Description
Technical field
The invention belongs to quartz material preparation field, particularly prepare the method for glassy transparent quartz sand with synthesis high-purity silicon dioxide powder.
Background technology
One of silica glass is the special industrial glass of silicon-dioxide one-component, has the physical and chemical performance of multiple uniqueness, is space technology, nuclear industry, defence equipment, and material indispensable in the industry such as semi-conductor, electric light source, communication, light industry.
The raw material preparing silica glass has two large classes, comprises the natural matter such as crystal, quartz mine, and utilizes the Material synthesis such as silicon-containing compound such as silicon tetrachloride, water glass, silicon fluoride.Since earlier 1800s, the method that employing natural matter prepares silica glass is constantly perfect, and its output accounts for the 70-80% of whole quartz glass products.But due to the restriction of natural mineral raw crystalline structure, the bad problem of the quartz glass quality caused by the raw material containing impurity fails to be solved at all, make the silica glass prepared by natural matter cannot reach specification of quality needed for high-end technology industry.
Although adopt synthesis material to prepare silica glass can increase certain production cost, products obtained therefrom is applied to higher-end businesses, has more marketable value.China Patent Publication No. CN1541194A discloses a kind of preparation method of high purity synthetic vitreous silica particles, adopt synthesis material in nitrogen atmosphere, prepare highly purified silica glass particle, but its highest firing temperature is 1250 DEG C, the quartz products of this firing temperature gained is opaque, prepare transparency silica glass as raw material and need formulate sintering technology in addition, the product obtaining required transparency cannot be guaranteed.U.S. Patent Publication No. US6849242 discloses a kind of method of porous silica gel synthetic quartz glass powder, without fragmentation directly obtained fused silica powder, but this method need carry out hydrochlorination at 1100 to 1300 DEG C, finally burn till in the helium-atmosphere of 1500 DEG C, technological process is more complicated, and this sintering temperature is low, obtained product is opaque, cannot ensure the silica glass preparing required transparency as raw material equally.
Summary of the invention
The technical problem to be solved in the present invention designs a kind of method of technique simple and stable, prepares high-purity glassy transparent quartz sand.
Synthesis high-purity silicon dioxide powder of the present invention prepares the method for glassy transparent quartz sand, comprising: synthesis high-purity silicon dioxide powder is placed in vacuum oven, is warming up to 1100-1500 DEG C, insulation 1-10 hour; Be warming up to 1700-1800 DEG C of insulation 5-30 minute afterwards, after cooling, obtained porous transparency silica glass block, obtains glassy transparent quartz sand after fragmentation.
Further, the dioxide-containing silica in described synthesis high-purity silicon dioxide powder is greater than 99.99%.
Further, described vacuum oven gas pressure intensity is less than 1Pa.
Further, described vacuum oven gas pressure intensity is less than or equal to 1 × 10
-2pa.
Further, be warming up to 1100-1500 DEG C, described soaking time is 4-8 hour.
Further, described in be warming up to 1100-1500 DEG C, comprise and be warming up to 1100 DEG C soon, be then warming up to 1400-1500 DEG C slowly.
Further, described in be warming up to 1100-1500 DEG C, the speed comprising being not less than 20 DEG C/min is warming up to 1100 DEG C soon, is then warming up to 1400-1500 DEG C slowly with the speed being not more than 5 DEG C/min.
Further, described insulation 1-10 hour, afterwards to be not more than 5 DEG C/min ramp to 1700-1800 DEG C.
Compared with prior art, the invention has the advantages that: adopt aforesaid method technique simple and stable, synthesis high-purity silicon dioxide powder is utilized only to calcine in vacuum atmosphere, gained quartz glass block is after fragmentation, obtain the quartz sand of vitreous state, there is the characteristic of high-purity transparent, can be used as the raw material of the quartz glass products such as the inwall of monocrystalline silicon growing quartz crucible, photoconductive fiber.
Accompanying drawing explanation
Fig. 1 is the white quartz sand of comparative example 1 of the present invention;
Fig. 2 is the white quartz sand XRD test pattern shown in Fig. 1;
Fig. 3 is the white quartz sand XDR test pattern of comparative example 2 of the present invention;
Fig. 4 is the silica 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 being ground;
Fig. 6 is the glassy transparent quartz sand XRD test pattern shown in Fig. 5.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
The method preparing glassy transparent quartz sand of the present invention, synthesis high-purity silicon dioxide powder is placed in vacuum oven, and setting sintering procedure is: be warming up to 1100-1500 DEG C, insulation 1-10h; Be warming up to 1700-1800 DEG C, insulation 5-30min; Until taking out after quartz glass block cooling in stove, after fragmentation, obtain glassy transparent quartz sand.
Following examples further illustrate the present invention.
Comparative example 1:
High-purity silicon dioxide powder (dioxide-containing silica is greater than 99.99%) will be synthesized be placed in vacuum oven (gas pressure intensity is lower than 1 × 10
-2pa), setting sintering procedure is: fast heat up (speed is 20 DEG C/min), to 1200 DEG C, then slowly heat up (speed is 1 DEG C/min) is to 1450 DEG C of insulation 8h.Take out after making sample furnace cooling and obtain white quartz particles, after quartz particles is ground, obtain opaque white quartz sand (see Fig. 1).The XRD figure (see Fig. 2) of this white quartz sand shows that products obtained therefrom is cristobalite crystal formation.
Comparative example 2:
High-purity silicon dioxide powder (dioxide-containing silica is greater than 99.99%) will be synthesized be placed in vacuum oven (gas pressure intensity is lower than 1 × 10
-2pa), setting sintering procedure is: fast heat up (speed is 40 DEG C/min) is to 1100 DEG C, then be slowly warming up to 1450 DEG C (speed is 1 DEG C/min) and be incubated 4h, heat up slowly afterwards (speed is 5 DEG C/min) is to 1650 DEG C of insulation 10min.Take out after making sample furnace cooling and obtain white quartz particles, after quartz particles is ground, obtain quartz sand.The XRD figure (see Fig. 3) of this white quartz sand shows products obtained therefrom and contains vitreous silica and crystal state ashlar English two kinds of crystal formations.
Embodiment 1:
High-purity silicon dioxide powder (dioxide-containing silica is greater than 99.99%) will be synthesized be placed in vacuum oven (gas pressure intensity is lower than 1 × 10
-2pa), setting sintering procedure is: fast heat up (speed is 20 DEG C/min) is to 1100 DEG C, then be slowly warming up to 1450 DEG C (speed is 1 DEG C/min) and be incubated 4h, heat up slowly afterwards (speed is 5 DEG C/min) is to 1740 DEG C of insulation 10min.Take out after making sample furnace cooling and obtain porous transparency silica glass block (see Fig. 4), after quartz glass block is ground, obtain vitreous silica sand (see Fig. 5).
It has been vitreous state that the XRD figure (see Fig. 6) of this vitreous silica sand shows products obtained therefrom.
Embodiment 2:
High-purity silicon dioxide powder (dioxide-containing silica is greater than 99.99%) will be synthesized be placed in vacuum oven (gas pressure intensity is lower than 1 × 10
-2pa), setting sintering procedure is: fast heat up (speed is 30 DEG C/min) is to 1100 DEG C, then be slowly warming up to 1450 DEG C (speed is 3 DEG C/min) and be incubated 6h, heat up slowly afterwards (speed is 3 DEG C/min) is to 1760 DEG C of insulation 20min.Take out after making sample furnace cooling and obtain porous transparency silica glass block, after quartz glass block is ground, obtain vitreous silica sand.
The XRD figure display products obtained therefrom of this vitreous silica sand has been vitreous state.
Embodiment 3:
High-purity silicon dioxide powder (dioxide-containing silica is greater than 99.99%) will be synthesized be placed in vacuum oven (gas pressure intensity is lower than 1 × 10
-2pa), setting sintering procedure is: fast heat up (speed is 40 DEG C/min) is to 1100 DEG C, then be slowly warming up to 1450 DEG C (speed is 1 DEG C/min) and be incubated 8h, heat up slowly afterwards (speed is 1 DEG C/min) is to 1780 DEG C of insulation 30min.Take out after making sample furnace cooling and obtain porous transparency silica glass block, after quartz glass block is ground, obtain vitreous silica sand.
The XRD figure display products obtained therefrom of this vitreous silica sand has been vitreous 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 vitreous silica and crystal state ashlar English two kinds of crystal formations |
| Embodiment 1 | Glassy transparent quartz sand |
| Embodiment 2 | Glassy transparent quartz sand |
| Embodiment 3 | Glassy transparent quartz sand |
Claims (9)
1. prepare a method for glassy transparent quartz sand, it is characterized in that: synthesis high-purity silicon dioxide powder is placed in vacuum oven, is warming up to 1100-1500 DEG C, insulation 1-10 hour; Be warming up to 1700-1800 DEG C of insulation 5-30 minute afterwards, after cooling, obtained porous transparency silica glass block, obtains glassy transparent quartz sand after fragmentation.
2. the method preparing glassy transparent quartz sand according to claim 1, is characterized in that: the dioxide-containing silica in described synthesis high-purity silicon dioxide powder is greater than 99.99%.
3. the method preparing glassy transparent quartz sand according to claim 1, is characterized in that: described vacuum oven gas pressure intensity is less than 1Pa.
4. the method preparing glassy transparent quartz sand according to claim 3, is characterized in that: described vacuum oven gas pressure intensity is less than or equal to 1 × 10
-2pa.
5. the method preparing glassy transparent quartz sand according to claim 1, is characterized in that: be warming up to 1100-1500 DEG C, and described soaking time is 4-8 hour.
6. the method preparing glassy transparent quartz sand according to claim 1, is characterized in that: described in be warming up to 1100-1500 DEG C, comprise and be warming up to 1100 DEG C soon, be then warming up to 1400-1500 DEG C slowly.
7. the method preparing glassy transparent quartz sand according to claim 6, it is characterized in that: described in be warming up to 1100-1500 DEG C, the speed comprising being not less than 20 DEG C/min is warming up to 1100 DEG C soon, is then warming up to 1400-1500 DEG C slowly with the speed being not more than 5 DEG C/min.
8. the method preparing glassy transparent quartz sand according to claim 1, is characterized in that: described insulation 1-10 hour, afterwards to be not more than 5 DEG C/min ramp to 1700-1800 DEG C.
9. product prepared by the method preparing glassy transparent quartz sand according to claim 1-8.
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| CN201510316770.1A CN104909558B (en) | 2015-06-10 | 2015-06-10 | A kind of method for preparing glassy transparent quartz sand |
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| CN201510316770.1A CN104909558B (en) | 2015-06-10 | 2015-06-10 | A kind of method for preparing glassy transparent quartz sand |
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| Publication Number | Publication Date |
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| CN104909558A true CN104909558A (en) | 2015-09-16 |
| CN104909558B CN104909558B (en) | 2018-01-23 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277802A (en) * | 2016-08-30 | 2017-01-04 | 中国建筑材料科学研究总院 | Foaming quartz glass, preparation method and quartz glass reflecting mirror |
| CN106365418A (en) * | 2016-08-30 | 2017-02-01 | 中国建筑材料科学研究总院 | Light-weight quartz glass and preparing method thereof |
Citations (4)
| 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 |
| JPH11236234A (en) * | 1998-02-24 | 1999-08-31 | Tosoh Corp | Method for manufacturing opaque quartz glass ring |
| 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 of fluorine-containing low refractive index Yb3+ doped quartz glass |
-
2015
- 2015-06-10 CN CN201510316770.1A patent/CN104909558B/en active Active
Patent Citations (4)
| 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 |
| JPH11236234A (en) * | 1998-02-24 | 1999-08-31 | Tosoh Corp | Method for manufacturing opaque quartz glass ring |
| 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 of fluorine-containing low refractive index Yb3+ doped quartz glass |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277802A (en) * | 2016-08-30 | 2017-01-04 | 中国建筑材料科学研究总院 | Foaming quartz glass, preparation method and quartz glass reflecting mirror |
| CN106365418A (en) * | 2016-08-30 | 2017-02-01 | 中国建筑材料科学研究总院 | Light-weight quartz glass and preparing method thereof |
| 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 |
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| Publication number | Publication date |
|---|---|
| CN104909558B (en) | 2018-01-23 |
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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. |