CN103772424A - Preparation method of electronic grade tetraethoxysilane - Google Patents
Preparation method of electronic grade tetraethoxysilane Download PDFInfo
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- CN103772424A CN103772424A CN201310747619.4A CN201310747619A CN103772424A CN 103772424 A CN103772424 A CN 103772424A CN 201310747619 A CN201310747619 A CN 201310747619A CN 103772424 A CN103772424 A CN 103772424A
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- preparation
- tetraethyl orthosilicate
- distillation
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- product
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000004821 distillation Methods 0.000 claims abstract description 34
- 239000012535 impurity Substances 0.000 claims abstract description 31
- 238000009835 boiling Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000010453 quartz Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 32
- 239000000706 filtrate Substances 0.000 claims description 15
- 125000002091 cationic group Chemical group 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 229910021654 trace metal Inorganic materials 0.000 abstract description 3
- 230000000536 complexating effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005341 cation exchange Methods 0.000 abstract 1
- 239000008139 complexing agent Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- 238000012423 maintenance Methods 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- 238000000207 volumetry Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910000103 lithium hydride Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to a preparation method of electronic grade tetraethoxysilane and particularly relates to a preparation method of electronic grade tetraethoxysilane for chemical vapor deposition in semiconductor industry. The preparation method comprises the steps of firstly complexing most of metal impurities in raw materials by using a complexing agent, and then filtering by using a microporous filter of 0.1 micron; passing through a cation exchange tower, a quartz plate type distillation tower and a sub-boiling distiller, strictly controlling temperature, and removing trace metal impurities, ethanol, other organic impurities and water. The preparation method provided by the invention adopts conventional purification equipment and has the advantages of convenience in operation, effect of being conductive to industrial large-scale production and low product cost.
Description
Technical field
The present invention relates to a kind of preparation method of electronic-grade tetraethyl orthosilicate, relate in particular to a kind of preparation method for semicon industry chemical vapour deposition electronic-grade tetraethyl orthosilicate.
Background technology
In the manufacture of semi-conductor electricity sub-element, must be by element encases in glass, or with glass as interlayer insulating film.Conventionally, glass coating is to be produced on the SiO in wafer surface by chemical vapor deposition (CVD) method
2layer.
Initial use be the inflammable silane of severe toxicity as vapor deposition source, along with the update of electronic material and technology, people in the high-performance of pursuing product simultaneously, more focus on its feature such as nontoxic, green, environmental friendliness.The relative silane toxicity of tetraethyl orthosilicate reduces greatly, is liquid at normal temperatures, operates more easy.And the density than forming silane film improves greatly, thereby reduce the possibility of leaking electricity between layers of multilayer circuit board and layer.
Industry tetraethyl orthosilicate by general preparation after content can reach 99%, but still contain the impurity up to 1%, wherein metal ion is electrically active impurity, can reduce and be deposited on semiconducter device SiO
2thin film layer insulating property, can cause micron-sized circuit mutually to be connected, thereby cause circuit card to be scrapped; Non-electrically active impurity wherein can affect even film layer and the planarization of deposition as moisture content, organism.
In U.S. Pat 5840953, use gas-chromatography to prepare tetraethyl orthosilicate, and with lithium hydride removal water impurity, product (in the metallic impurity) purity obtaining is not less than 99.999999% tetraethyl orthosilicate, water content is less than 2PPM, because gas chromatograph is mainly used in micro-analyzing and testing, and gas chromatograph apparatus expensive, has improved production cost.
Summary of the invention
The object of the invention is to overcome the defect of prior art; provide a kind of and be not less than 99.999999%(w/w in its purity of metallic impurity) preparation method of electronic-grade tetraethyl orthosilicate; the content of organic impurity (with alcohol meter) is lower than 1ppm; water content is lower than 0.3ppm; adopt conventional Preparation equipment, easy to operate, be beneficial to industrial scale and produce; product cost is low, and quality can meet the requirement of semicon industry vapor deposition source.
The present invention achieves the above object by following measures:
(1) first the present invention uses most of metallic impurity in analytically pure EDTA complex agent complexing raw material, through fully mixing, stirring, with the millipore filter filtration of 0.1 micron;
(2) by the filtrate process cationic exchange column device of collecting, collect product, further remove trace metal impurities.
(3) the present invention adopts quartzy plate tower, by efficient distillation, strict control device extraction cut temperature, treat that cut temperature is controlled within the scope of 159.0～166.0 ℃, after total reflux 7～16h hour, start extraction fraction from tower top, ethanol and organic impurity content thereof are less than 1ppm, and metallic impurity total content is less than 5ppm.
(4) fraction of collecting is distilled through sub-boiling distillation device, strictly control 90～100 ℃ of distillation temperatures, further remove moisture, other inorganic phase impurity in material, the water content in product is to 0.3ppm.
In whole production process, product does not contact the external world, and wherein said strainer, cationic exchange coloum and pipe material adopt tetrafluoroethylene, and plate tower, sub-boiling distillation equipment matter adopt quartz.
A kind of preparation method for semicon industry chemical vapor deposition (CVD) source electronic-grade tetraethyl orthosilicate of the present invention.Realize by following steps:
(1) in technical grade tetraethyl orthosilicate raw material, add the agent of analytical pure EDTA complex, fully mix, stir 30-60 minute, the millipore filter that enters 0.1 micron filters; (2) by the filtrate process cationic exchange column device of collecting, collect product, further remove trace metal impurities; (3) add distillation tower to distill filtration gained filtrate, after total reflux 7～16h hour, gather 159.0～166.0 ℃ of fractions from tower top; (4) fraction of collecting is distilled through sub-boiling distillation device, regulate sub-boiling distillation device heating unit voltage, maintenance medium surface temperature, at 90～100 ℃, is collected 90～100 ℃ of distillation product; (5) products obtained therefrom is not more than thousand grades, part in entirety and is not more than the clean room of hundred grades, adopts quartz source bottle to carry out filling, obtains electronic-grade tetraethyl orthosilicate product.
Preparation method of the present invention, the wherein said analytical pure EDTA complex agent quality adding is the 3-10% of raw material tetraethyl orthosilicate quality, the mix and blend time is preferably 40-50 minute.
Preparation method of the present invention, wherein said millipore filter filter membrane is using tetrafluoroethylene as mould material.
Preparation method of the present invention, wherein said distillation tower adopts quartzy plate tower, and tower top gathers fraction and is preferably 164～166.0 ℃.
Preparation method of the present invention, wherein said sub-boiling distillation temperature remains on 95～98 ℃.
Preparation method of the present invention, wherein said strainer, cationic exchange coloum and pipe material adopt tetrafluoroethylene, and plate tower, sub-boiling distillation equipment matter adopt quartz.
Preparation method of the present invention, is characterized in that the tetraethyl orthosilicate product purity obtaining with aforesaid method is not less than 99.999999%(w/w), the content < 1ppm of organic impurity (with alcohol meter); Water-content < 0.3ppm.
Effect of the present invention: the present invention adopts millipore filtration, column plate distillation, sub-boiling distillation to combine; adopt conventional equipment for purifying; easy to operate; can effectively remove solid impurity in raw material, metallic impurity, low-boiling-point substance, micro-moisture; product purity (in metallic impurity) is not less than 99.999999%(w/w); and our bright preparation method is beneficial to industrial scale and produces, and product cost is low, and quality can meet the requirement of semicon industry vapor deposition source.
The advantages such as it is high that product of the present invention has purity, safe, nontoxic, difficult combustion, environmental pollution is little.
Product of the present invention adopts quartz source bottle packing, and client is easy to use.
Product of the present invention can be semicon industry, unicircuit, semiconductor separation part and provides that high-efficiency environment friendly is nontoxic, low cost silicon depositing source, promotes semicon industry sustainable and stable development.
Embodiment
For the present invention is described, provide following case study on implementation.But be interpreted as claim of the present invention and be not subject to the restriction of following embodiment.
Embodiment 1:
A kind of preparation method of electronic-grade tetraethyl orthosilicate: (1) gets the synthetic tetraethyl orthosilicate crude product 12kg of industry in the polytetrafluoroethylcontainer container of 20L, add the agent of 0.36kg analytical pure EDTA complex, fully mix, stir 30 minutes, then filter with the millipore filter of 0.1 micron; (2) by the filtrate process cationic exchange column device of collecting, further remove metallic impurity, collect filtrate; (3) filtrate of collection is added board-like quartzy distillation tower distill, after total reflux 7 hours, gather 163 ℃ of fractions from tower top; (4) fraction of collecting is distilled through sub-boiling distillation device, regulate sub-boiling distillation device heating unit voltage, maintenance medium surface temperature, at 95 ℃, is collected 95 ℃ of distillation product, and sampling detects; (5) products obtained therefrom is not more than thousand grades, part in entirety and is not more than the clean room of hundred grades, adopts quartz source bottle to carry out filling, obtains electronic-grade tetraethyl orthosilicate product.
Icp ms for product (ICP-MS) detects conventional 17 kinds of metals content impurities such as Li, Na, Mg, Al wherein, detect the organic impurity contents such as ethanol with gas chromatograph-mass spectrometer (GC-MS), with Ka Er-Fei Xiu (KF) volumetry detection water-content.
Detected result sees attached list.
Embodiment 2:
A kind of preparation method of electronic-grade tetraethyl orthosilicate: (1) gets the synthetic tetraethyl orthosilicate crude product 12kg of industry in the polytetrafluoroethylcontainer container of 20L, add the agent of 0.72kg analytical pure EDTA complex, fully mix, stir 45 minutes, then filter with the millipore filter of 0.1 micron; (2) by the filtrate process cationic exchange column device of collecting, further remove metallic impurity, collect filtrate; (3) filtrate of collection is added board-like quartzy distillation tower distill, after total reflux 10 hours, gather 165 ℃ of fractions from tower top; (4) fraction of collecting is distilled through sub-boiling distillation device, regulate sub-boiling distillation device heating unit voltage, maintenance medium surface temperature, at 98 ℃, is collected 98 ℃ of distillation product, and sampling detects; (5) products obtained therefrom is not more than thousand grades, part in entirety and is not more than the clean room of hundred grades, adopts quartz source bottle to carry out filling, obtains electronic-grade tetraethyl orthosilicate product.
Icp ms for product (ICP-MS) detects conventional 17 kinds of metals content impurities such as Li, Na, Mg, Al wherein, detect the organic impurity contents such as ethanol with gas chromatograph-mass spectrometer (GC-MS), with Ka Er-Fei Xiu (KF) volumetry detection water-content.
Detected result sees attached list.
Embodiment 3:
A kind of preparation method of electronic-grade tetraethyl orthosilicate: (1) gets the synthetic tetraethyl orthosilicate crude product 12kg of industry in the polytetrafluoroethylcontainer container of 20L, add the agent of 1.2kg analytical pure EDTA complex, fully mix, stir 60 minutes, then filter with the millipore filter of 0.1 micron; (2) by the filtrate process cationic exchange column device of collecting, further remove metallic impurity, collect filtrate; (3) filtrate of collection is added board-like quartzy distillation tower distill, after total reflux 15 hours, gather 163 ℃ of fractions from tower top; (4) fraction of collecting is distilled through sub-boiling distillation device, regulate sub-boiling distillation device heating unit voltage, maintenance medium surface temperature, at 90 ℃, is collected 90 ℃ of distillation product, and sampling detects; (5) products obtained therefrom is not more than thousand grades, part in entirety and is not more than the clean room of hundred grades, adopts quartz source bottle to carry out filling, obtains electronic-grade tetraethyl orthosilicate product.
Icp ms for product (ICP-MS) detects conventional 17 kinds of metals content impurities such as Li, Na, Mg, Al wherein, detect the organic impurity contents such as ethanol with gas chromatograph-mass spectrometer (GC-MS), with Ka Er-Fei Xiu (KF) volumetry detection water-content.
Detected result sees attached list.
?
Subordinate list
Ppm of the present invention, ppb refer to mass concentration unit, 1ppm=1000ppb.
Claims (7)
1. a preparation method for electronic-grade tetraethyl orthosilicate, is characterized in that comprising the steps:
(1) in technical grade tetraethyl orthosilicate raw material, add the agent of analytical pure EDTA complex, fully mix, stir 30-60 minute, the millipore filter that enters 0.1 micron filters;
(2) will filter gained filtrate through cationic exchange column device, collect filtrate;
(3) add distillation tower to distill the filtrate of collection, after total reflux 7～16h hour, gather 159～166 ℃ of fractions from tower top;
(4) fraction of collecting is distilled through sub-boiling distillation device, regulate sub-boiling distillation device heating unit voltage, keep liquid level temperature at 90～100 ℃, collect 90～100 ℃ of distillation product;
(5) the distillation product of collecting are not more than to thousand grades, part in entirety and are not more than the clean room of hundred grades, carry out fillingly with quartz source bottle, obtain electronic-grade tetraethyl orthosilicate product.
2. preparation method according to claim 1, the wherein said analytical pure EDTA complex agent quality adding is the 3-10% of raw material tetraethyl orthosilicate quality, the mix and blend time is preferably 40-50 minute.
3. preparation method according to claim 1, wherein said millipore filter filter membrane is using tetrafluoroethylene as mould material.
4. preparation method according to claim 1, wherein said distillation tower adopts quartzy plate tower, and tower top gathers fraction and is preferably 164～166.0 ℃.
5. preparation method according to claim 1, wherein said sub-boiling distillation temperature maintains 95～98 ℃.
6. according to the preparation method described in claim 1-5, wherein said strainer, cationic exchange coloum and pipe material adopt tetrafluoroethylene, and plate tower, sub-boiling distillation equipment matter adopt quartz.
7. according to the preparation method described in claim 1-5, it is characterized in that the tetraethyl orthosilicate product obtaining with aforesaid method is not less than 99.999999%w/w in metallic impurity purity, organic impurity is with the content < 1ppm of alcohol meter; Water-content < 0.3ppm.
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|---|---|---|---|
| CN201310747619.4A CN103772424B (en) | 2013-12-31 | 2013-12-31 | A kind of preparation method of electronic-grade tetraethyl orthosilicate |
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| CN201310747619.4A CN103772424B (en) | 2013-12-31 | 2013-12-31 | A kind of preparation method of electronic-grade tetraethyl orthosilicate |
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| CN103772424B CN103772424B (en) | 2016-01-27 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438495A (en) * | 2018-12-25 | 2019-03-08 | 苏州金宏气体股份有限公司 | A kind of production method and production system of high-purity ethyl orthosilicate |
| CN109459539A (en) * | 2018-12-29 | 2019-03-12 | 苏州金宏气体股份有限公司 | The detection method and detection system of micro-moisture in a kind of high-purity ethyl orthosilicate |
| CN109705153A (en) * | 2019-02-02 | 2019-05-03 | 苏州金宏气体股份有限公司 | A kind of purification process of ethyl orthosilicate |
| CN113121583A (en) * | 2021-04-21 | 2021-07-16 | 洛阳中硅高科技有限公司 | Preparation device and preparation method of electronic-grade ethyl orthosilicate |
| CN115304632A (en) * | 2022-07-21 | 2022-11-08 | 湖北新蓝天新材料股份有限公司 | Preparation method and application of electronic-grade tetraalkoxysilane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5840953A (en) * | 1995-11-16 | 1998-11-24 | Eagle-Picher Industries, Inc. | Purified tetraethoxysilane and method of purifying |
| EP0879821B1 (en) * | 1997-05-20 | 2004-07-07 | Air Products And Chemicals, Inc. | Purification of organosilanes of group 13 (IIIA) and 15 (VA) impurities |
-
2013
- 2013-12-31 CN CN201310747619.4A patent/CN103772424B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5840953A (en) * | 1995-11-16 | 1998-11-24 | Eagle-Picher Industries, Inc. | Purified tetraethoxysilane and method of purifying |
| EP0879821B1 (en) * | 1997-05-20 | 2004-07-07 | Air Products And Chemicals, Inc. | Purification of organosilanes of group 13 (IIIA) and 15 (VA) impurities |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438495A (en) * | 2018-12-25 | 2019-03-08 | 苏州金宏气体股份有限公司 | A kind of production method and production system of high-purity ethyl orthosilicate |
| CN109438495B (en) * | 2018-12-25 | 2023-05-26 | 金宏气体股份有限公司 | Production method and production system of high-purity ethyl silicate |
| CN109459539A (en) * | 2018-12-29 | 2019-03-12 | 苏州金宏气体股份有限公司 | The detection method and detection system of micro-moisture in a kind of high-purity ethyl orthosilicate |
| CN109459539B (en) * | 2018-12-29 | 2024-03-22 | 金宏气体股份有限公司 | Method and system for detecting trace moisture in high-purity ethyl silicate |
| CN109705153A (en) * | 2019-02-02 | 2019-05-03 | 苏州金宏气体股份有限公司 | A kind of purification process of ethyl orthosilicate |
| CN109705153B (en) * | 2019-02-02 | 2020-04-07 | 苏州金宏气体股份有限公司 | Purifying method of ethyl orthosilicate |
| CN113121583A (en) * | 2021-04-21 | 2021-07-16 | 洛阳中硅高科技有限公司 | Preparation device and preparation method of electronic-grade ethyl orthosilicate |
| CN113121583B (en) * | 2021-04-21 | 2024-07-05 | 洛阳中硅高科技有限公司 | Preparation device and preparation method of electronic grade ethyl orthosilicate |
| CN115304632A (en) * | 2022-07-21 | 2022-11-08 | 湖北新蓝天新材料股份有限公司 | Preparation method and application of electronic-grade tetraalkoxysilane |
| CN115304632B (en) * | 2022-07-21 | 2023-08-29 | 湖北新蓝天新材料股份有限公司 | Preparation method and application of electronic-grade tetraalkoxysilane |
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