CN103332694A - Preparation method of raw material sand for quartz crucible - Google Patents
Preparation method of raw material sand for quartz crucible Download PDFInfo
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- CN103332694A CN103332694A CN2013102296000A CN201310229600A CN103332694A CN 103332694 A CN103332694 A CN 103332694A CN 2013102296000 A CN2013102296000 A CN 2013102296000A CN 201310229600 A CN201310229600 A CN 201310229600A CN 103332694 A CN103332694 A CN 103332694A
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Abstract
The invention discloses a preparation method of raw material sand for a quartz crucible. The method comprises the following steps: adopting cocoamine acetate, sodium petroleum sulfonate and pine oil to perform targeted mica flotation, iron flotation and feldspar flotation against feldspar, mica, iron oxides and the like in quartz sand so as to remove the mica, the feldspar, and iron impurities in ore, then performing acid treatment by applying hydrofluoric acid to further remove the mica, the feldspar and the iron impurities in the ore, and finally using a 20000 Gauss magnetic field to perform separation so as to remove iron and other magnetic foreign and miscellaneous matters; introducing oxygen and nitrogen for calcination under high-temperature conditions, performing high-temperature purification with hydrogen chloride gas and performing further refining to improve the purity of the quartz sand and further improve the viscosity of the quartz crucible. The raw material sand for the quartz crucible, prepared according to the invention, can be comparable to high-purity quartz sand of U.S. UNIMIN Company in the aspects of purity and viscosity, the price is just 1/2 of the high-purity quartz sand, and the localization of the high-purity quartz sand is further realized.
Description
Technical field
The present invention relates to a kind of glass sand preparation technology, specifically, that relate to is the preparation method that a kind of quartz crucible is used raw sand.
Background technology
Quartz crucible is the expendable vessel of pulling monocrystal silicon, and every production one stove silicon single crystal quartz crucible of just using up is because silicon single crystal is the main raw material of producing large-scale integrated circuit and solar cell, so very harsh to the requirement of quartz crucible.The geometrical dimension of quartz crucible and outward appearance are that production technique is determined, and purity is determined by raw material.Ingredient requirement purity height, high conformity, even particle size distribution that quartz crucible is used can influence founding of crucible when objectionable constituent are high, influence its temperature tolerance, also phenomenons such as bubble, color spot, decortication can occur, have a strong impact on the quality of quartz crucible.
Produce high-quality quartz crucible, not only Technology wants advanced, and material purity wants high, and the quartz sand that technologies such as the continuous flotation of present domestic employing, nitration mixture processing, shrend, magnetic separation are produced reasons such as bad phenomenon such as quartz crucible bubble, stain, white point and crucible viscosity are low occur and causes the work-ing life of crucible short because purity is bad.At present, domestic glass sand can not satisfy the requirement of high purity, high-quality quartz crucible; Substantially all be glass sand by import U.S. UNIMIN (You Niming) company in order to produce raw material that high-quality product China produces high-purity silica pot, though its raw materials quality is good, price is very high.Therefore improving quartz crucible quality product and output, promote the industrial development of HIGH-PURITY SILICON material, reach the quartz crucible localization of raw material, is the instant thing of China high purity quartz raw material production enterprise.
The Chinese patent publication number is 102887516A, and this patent provides a kind of production method of glass sand, and by the quartz sand secondary is added auxiliary material roasting, pickling, flotation, drying and magnetic separation, final chloridizing roasting obtains highly purified quartz sand.The present invention develops a kind of low cost, improves the method for viscosity of quartz sand.
Summary of the invention
The objective of the invention is to solve above-mentioned deficiency of the prior art, the preparation method of a kind of quartz crucible with raw sand is provided, this method has improved quartz crucible quality product and output, has promoted the industrial development of HIGH-PURITY SILICON material, has realized the production domesticization of glass sand.
For realizing above-mentioned purpose, a kind of quartz crucible of the present invention is with the preparation method of raw sand, and concrete steps are as follows:
Step 1, screening: quartz sand adopts 50mesh-150mesh vibrating screen classifier gradation sizing;
Step 2, high magnetic force magnetic separation: the quartz sand after adopting 20000gauss magnetic field to screening carries out magnetic separation;
Step 3, stage floatation: the quartz sand after step 2 processing is carried out mica flotation, iron flotation, feldspar flotation with cocoa amine acetate, petroleum sodium sulfonate and pine tar;
Step 4, acid treatment: carry out the normal temperature acid treatment with hydrofluoric acid and further remove alkali metal impurity in the quartz sand;
Step 5, washing and dehydration: residual flotation reagent and residual acid with ultrapure water removal quartz sand surface, dewater with drier then;
Step 6, high temperature drying: with 300～1000 ℃ of disposable dryings of vertical drying oven, the normal temperature cooling;
Step 7, screening: adopt 60 orders-150 order vibrating screen classifier;
Step 8, calcining: aerating oxygen and nitrogen are removed oxy-compound and other alkanes gases in the quartz sand crystal under stablizing the condition of high temperature;
Step 9, purifying: feed hydrogen chloride gas at 1000～1400 ℃ of environment, remove oxy-compound and other alkanes gas and metallic impurity in the quartz sand crystal;
Step 10, high magnetic force magnetic separation: adopt 20000gauss magnetic field magnetic separation.
Aforesaid method of the present invention can be pulverized quartz mine before carry out step 1 with jaw crusher and ball mill; Perhaps directly adopt commercially available quartz sand of not purifying, carry out above-mentioned steps.
The present invention adopts cocoa amine acetate, petroleum sodium sulfonate, pine tar that quartz mine andesine, mica and iron ore etc. are carried out the impurity that mica, feldspar and iron in the ore are removed in mica flotation targetedly, iron flotation and feldspar flotation, use hydrofluoric acid to carry out further removal mica, feldspar and iron contamination wherein of acid treatment then, sort with 20000Gauss magnetic field more at last and remove iron and other magnetic different foreign material; Adopt and stablize aerating oxygen under the hot conditions, nitrogen calcining, the hydrogen chloride gas purifying is further made with extra care and is promoted quartz sand purity to improve quartz crucible viscosity.
Beneficial effect of the present invention:
The prepared quartz crucible raw material of the present invention can match in excellence or beauty with the glass sand of U.S. UNIMIN (You Niming) company on purity and viscosity with sand, however price but just its 1/2; Realize the production domesticization of glass sand, no longer only relied on import.
Embodiment
The technical solution of the present invention is further explained below in conjunction with embodiment, but following content is not intended to limit the scope of the invention.
Embodiment 1
Present embodiment provides the preparation method of a kind of quartz crucible with raw sand, in order to prepare particle diameter at 0.1mm-0.3mm, granularity is at 60 orders-150 order, it is 99.99% that purity reaches 4N() more than, viscosity is at 1.0E+09poise(1500 ℃) more than the high-purity silica pot raw sand, concrete implementation step is as follows:
Step 1, stage reduction sort: quartz mine is pulverized with jaw crusher and ball mill;
Step 2, screening: adopt 50 orders-150 order vibrating screen classifier;
Step 3, high magnetic force magnetic separation: the magnetic separator that adopts 20000gauss;
Step 4, stage floatation: carry out mica flotation, iron flotation, feldspar flotation with cocoa amine acetate, petroleum sodium sulfonate and pine tar;
Step 5, acid treatment: carry out the normal temperature acid treatment with hydrofluoric acid and further remove alkali metal impurity in the quartz sand;
Step 6, washing and dehydration: residual flotation reagent and residual acid with ultrapure water (resistivity is greater than 18M Ω * cm) removal quartz sand surface, dewater with drier then;
Step 7, high temperature drying: with the disposable drying of 300～1000 ℃ of vertical drying ovens (such as 300 ℃, 600 ℃, 1000 ℃ etc.), normal temperature cooling;
Step 8, screening: 60 orders-150 order vibrating screen classifier;
Step 9, calcining: 1000～1400 ℃ of aerating oxygen and nitrogen (such as 1000 ℃, 1200 ℃, 1400 ℃ etc.) are removed oxy-compound and other alkanes gas in the quartz sand crystal;
Step 10, purifying: feed 1000～1400 ℃ of hydrogen chloride gas (such as 1000 ℃, 1200 ℃, 1400 ℃ etc.) and remove oxy-compound and other alkanes gas and metallic impurity in the quartz sand crystal;
Step 11, high magnetic force magnetic separation: the magnetic separator that adopts 20000gauss;
Present embodiment adopts cocoa amine acetate, petroleum sodium sulfonate, pine tar that quartz mine andesine, mica and iron ore etc. are carried out mica flotation targetedly, iron flotation and feldspar flotation and goes out the impurity of mica, feldspar and iron in the ore, use hydrofluoric acid to carry out further removal mica, feldspar and iron contamination wherein of acid treatment then, sort with 20000Gauss magnetic field more at last and remove iron and other magnetic different foreign material.Employing aerating oxygen, nitrogen calcining and feeding hydrogen chloride gas purifying under 1000～1400 ℃ of conditions are further made with extra care and are promoted quartz sand purity to improve quartz crucible viscosity.
The prepared quartz crucible raw material of present embodiment can match in excellence or beauty with the glass sand of U.S. UNIMIN (You Niming) company on purity and viscosity with sand, price but just its 1/2, realized the production domesticization of glass sand.
Embodiment 2
Present embodiment provides the preparation method of a kind of quartz crucible with raw sand, in order to prepare particle diameter at 0.1mm-0.3mm, granularity is at 60 orders-150 order, it is 99.99% that purity reaches 4N() more than, viscosity is at 1.0E+09poise(1500 ℃) more than the high-purity silica pot raw sand, concrete implementation step is as follows:
Step 1, directly buy without the quartz sand of purifying;
Step 2, screening: adopt 50 orders-150 order vibrating screen classifier;
Step 3, high magnetic force magnetic separation: the magnetic separator that adopts 20000gauss;
Step 4, stage floatation: carry out mica flotation, iron flotation, feldspar flotation with cocoa amine acetate, petroleum sodium sulfonate and pine tar;
Step 5, acid treatment: carry out the normal temperature acid treatment with hydrofluoric acid and further remove alkali metal impurity in the quartz sand;
Step 6, washing and dehydration: residual flotation reagent and residual acid with ultrapure water (resistivity is greater than 18M Ω * cm) removal quartz sand surface, dewater with drier then;
Step 7, high temperature drying: with 300～1000 ℃ of disposable dryings of vertical drying oven, the normal temperature cooling;
Step 8, screening: 60 orders-150 order vibrating screen classifier;
Step 9, calcining: 1000～1400 ℃ of oxy-compound and other alkanes gases of removing in the quartz sand crystal of aerating oxygen and nitrogen;
Step 10, purifying: feed oxy-compound and other alkanes gas and metallic impurity in 1000～1400 ℃ of removals of hydrogen chloride gas quartz sand crystal;
Step 11, high magnetic force magnetic separation: the magnetic separator that adopts 20000gauss;
In the present embodiment, directly buy without the quartz sand of purifying, adopt above-mentioned steps to make with extra care purification then, so more use manpower and material resources sparingly.
Embodiment 3
At SiO
2Purity reaches the quartz sand more than 98%, directly adopts embodiment 1 described step 3,5,6,7,8,9,10,11 direct purifications to get final product.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (2)
1. a quartz crucible is characterized in that this method may further comprise the steps with the preparation method of raw sand:
Step 1, screening: quartz sand is adopted 50 orders-150 order vibrating screen classifier gradation sizing;
Step 2, high magnetic force magnetic separation: the quartz sand after adopting 20000gauss magnetic field to screening carries out magnetic separation;
Step 3, stage floatation: the quartz sand after step 2 processing is carried out mica flotation, iron flotation, feldspar flotation with cocoa amine acetate, petroleum sodium sulfonate and pine tar;
Step 4, acid treatment: carry out the normal temperature acid treatment with hydrofluoric acid and further remove alkali metal impurity in the quartz sand;
Step 5, washing and dehydration: with residual flotation reagent and the residual acid of resistivity greater than the ultrapure water removal quartz sand surface of 18M Ω * cm, dewater with drier then;
Step 6, high temperature drying: with 300～1000 ℃ of disposable dryings of vertical drying oven, the normal temperature cooling;
Step 7, screening: adopt 60 orders-150 order vibrating screen classifier;
Step 8, calcining: aerating oxygen and nitrogen are removed oxy-compound and other alkanes gases in the quartz sand crystal under 1000～1400 ℃ of conditions;
Step 9, purifying: feed hydrogen chloride gas under 1000～1400 ℃ of conditions and remove oxy-compound and other alkanes gas and metallic impurity in the quartz sand crystal;
Step 10, high magnetic force magnetic separation: adopt 20000gauss magnetic field magnetic separation, obtain described quartz crucible raw sand.
2. a kind of quartz crucible according to claim 1 is with the preparation method of raw sand, it is characterized in that: in the described step 3, carry out mica, iron, the continuous flotation raising of feldspar classification dioxide-containing silica respectively with cocoa amine acetate, petroleum sodium sulfonate and pine tar.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103964444A (en) * | 2014-05-05 | 2014-08-06 | 临沂晟泉矿业有限公司 | Method for producing high-purity quartz sand |
| CN106000621A (en) * | 2016-06-01 | 2016-10-12 | 安徽晶晶石英科技有限公司 | Method for purifying quartz sand by compounding chlorination with acid leaching |
| CN109336116A (en) * | 2018-10-31 | 2019-02-15 | 黄冈师范学院 | A method of photovoltaic high purity quartz emery dust is prepared containing feldspar ore type quartzite |
| CN109534347A (en) * | 2018-11-06 | 2019-03-29 | 黄冈师范学院 | A method of use for electronic products high purity quartz emery dust is prepared containing feldspar ore type quartzite |
| CN109665528A (en) * | 2019-01-22 | 2019-04-23 | 黄冈师范学院 | Method containing corundum type quartzite preparation use for electronic products high purity quartz emery dust |
| CN110817886A (en) * | 2019-12-02 | 2020-02-21 | 凯盛石英材料（太湖）有限公司 | Quartz sand flotation and pesticide removal method |
| CN110862091A (en) * | 2019-12-25 | 2020-03-06 | 苏州纳迪微电子有限公司 | High-purity quartz sand and preparation method and application thereof |
| CN111874913A (en) * | 2020-07-24 | 2020-11-03 | 武汉理工大学 | Method for purifying quartz by chloridizing roasting |
| CN115231909A (en) * | 2021-04-22 | 2022-10-25 | 新沂市中鑫光电科技有限公司 | Preparation method of quartz crucible air bubble layer |
| CN115246704A (en) * | 2021-04-27 | 2022-10-28 | 新沂市中鑫光电科技有限公司 | Method for eliminating impurity elements in transparent layer of quartz crucible |
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| US5037625A (en) * | 1990-02-06 | 1991-08-06 | The Feldspar Corporation | Purified quartz and process for purifying quartz |
| CN101337767A (en) * | 2008-08-15 | 2009-01-07 | 杜建中 | Purification method in process of production of high-pure quartz sand as raw material of quartz glass |
| CN101367609A (en) * | 2008-08-15 | 2009-02-18 | 刘少云 | Preparation and purification process of quartz sand and quartz powder and products thereof |
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| US5037625A (en) * | 1990-02-06 | 1991-08-06 | The Feldspar Corporation | Purified quartz and process for purifying quartz |
| CN101337767A (en) * | 2008-08-15 | 2009-01-07 | 杜建中 | Purification method in process of production of high-pure quartz sand as raw material of quartz glass |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103964444B (en) * | 2014-05-05 | 2016-08-24 | 临沂晟泉矿业有限公司 | A kind of production method of glass sand |
| CN103964444A (en) * | 2014-05-05 | 2014-08-06 | 临沂晟泉矿业有限公司 | Method for producing high-purity quartz sand |
| CN106000621A (en) * | 2016-06-01 | 2016-10-12 | 安徽晶晶石英科技有限公司 | Method for purifying quartz sand by compounding chlorination with acid leaching |
| CN106000621B (en) * | 2016-06-01 | 2019-04-19 | 安徽晶晶石英科技有限公司 | A kind of method of the compound purifying quartz sand of chlorination-acidleach |
| CN109336116B (en) * | 2018-10-31 | 2020-10-13 | 黄冈师范学院 | Method for preparing photovoltaic high-purity quartz sand powder from feldspar ore type quartzite |
| CN109336116A (en) * | 2018-10-31 | 2019-02-15 | 黄冈师范学院 | A method of photovoltaic high purity quartz emery dust is prepared containing feldspar ore type quartzite |
| CN109534347A (en) * | 2018-11-06 | 2019-03-29 | 黄冈师范学院 | A method of use for electronic products high purity quartz emery dust is prepared containing feldspar ore type quartzite |
| CN109534347B (en) * | 2018-11-06 | 2021-11-02 | 黄冈师范学院 | Method for preparing high-purity quartz sand powder for electronic products from feldspar ore type quartzite |
| CN109665528B (en) * | 2019-01-22 | 2021-11-02 | 黄冈师范学院 | Method for preparing high-purity quartz sand powder for electronic products from corundum-containing quartzite |
| CN109665528A (en) * | 2019-01-22 | 2019-04-23 | 黄冈师范学院 | Method containing corundum type quartzite preparation use for electronic products high purity quartz emery dust |
| CN110817886A (en) * | 2019-12-02 | 2020-02-21 | 凯盛石英材料（太湖）有限公司 | Quartz sand flotation and pesticide removal method |
| CN110862091A (en) * | 2019-12-25 | 2020-03-06 | 苏州纳迪微电子有限公司 | High-purity quartz sand and preparation method and application thereof |
| CN110862091B (en) * | 2019-12-25 | 2022-08-02 | 苏州西丽卡电子材料有限公司 | High-purity quartz sand and preparation method and application thereof |
| CN111874913A (en) * | 2020-07-24 | 2020-11-03 | 武汉理工大学 | Method for purifying quartz by chloridizing roasting |
| CN115231909A (en) * | 2021-04-22 | 2022-10-25 | 新沂市中鑫光电科技有限公司 | Preparation method of quartz crucible air bubble layer |
| CN115246704A (en) * | 2021-04-27 | 2022-10-28 | 新沂市中鑫光电科技有限公司 | Method for eliminating impurity elements in transparent layer of quartz crucible |
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Effective date of registration: 20150727 Address after: 750021 No. 23 Guangming West Road, Yinchuan economic and Technological Development Zone, the Ningxia Hui Autonomous Region Patentee after: Ferrotec (Ningxia) Advanced Quartz Material Co., Ltd. Address before: 750021, Guangming West Road, Yinchuan economic and Technological Development Zone, Yinchuan, the Ningxia Hui Autonomous Region, 23 Patentee before: Ferrotec (Ningxia) Advanced Quartz Material Co., Ltd. Patentee before: Advanced Quartz Material (Hangzhou) Co., Ltd. |
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Address after: 750021 No. 23, Guangming West Road, Yinchuan economic and Technological Development Zone, Ningxia Hui Autonomous Region Patentee after: Ningxia dunyuan poly core semiconductor technology Co.,Ltd. Address before: 750021 No. 23, Guangming West Road, Yinchuan economic and Technological Development Zone, Ningxia Hui Autonomous Region Patentee before: FERROTEC (NINGXIA) ADVANCED QUARTZ MATERIAL Co.,Ltd. |