CN109705153A - A kind of purification process of ethyl orthosilicate - Google Patents
A kind of purification process of ethyl orthosilicate Download PDFInfo
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- CN109705153A CN109705153A CN201910106872.9A CN201910106872A CN109705153A CN 109705153 A CN109705153 A CN 109705153A CN 201910106872 A CN201910106872 A CN 201910106872A CN 109705153 A CN109705153 A CN 109705153A
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- ethyl orthosilicate
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- demister
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Abstract
The present invention provides a kind of purification process of ethyl orthosilicate, it include: to vaporize raw material ethyl orthosilicate in vaporizer, and the first fibre bed demister, the second fibre bed demister and third fibre bed demister on vaporizer top are passed sequentially through, obtain ethyl orthosilicate steam；The aperture of the first fibre bed demister is 1~20 μm；The aperture of the second fibre bed demister is 2~10 μm；The aperture of the third fibre bed demister is 0.1~2 μm.Compared with prior art, the present invention is handled the ethyl orthosilicate after vaporization using the fibre bed demister of three layers of different pore size, it may also function as the effect of separating metal ions Yu oils heavy hydrocarbon, therefore the present invention is also greatly reduced the content of ethyl orthosilicate steam heavy hydrocarbon and metal ion while vaporizing ethyl orthosilicate, play the role of primary purification, ensure that the quality into the ethyl orthosilicate steam of post-processing system.
Description
Technical field
The invention belongs to technical field of semiconductors more particularly to a kind of purification process of ethyl orthosilicate.
Background technique
The method that semiconductor technology forms oxide layer mainly has thermal oxide (for can form partly leading for homeostasis oxide layer
Body material), low-pressure chemical vapor phase deposition (LPCVD), plasma-reinforced chemical vapor deposition (PECVD) and atmospheric chemical vapor form sediment
Product (APCVD) etc., wherein since the throughput that APCVD is required is big, and technique generation particle is relatively more, it is most of at present partly to lead
Body technology has been rarely employed.
When ethyl orthosilicate (TEOS) is used for LPCVD, TEOS flashes to gaseous state from liquid, in 700~750 DEG C, 300mTOR
Under pressure decompose silicon chip surface deposit generate silica membrane, silica membrane deposition rate can achieve 50 à/
Min, the thickness uniformity of film is less than 3%, these excellent operational characteristiies and its distinguishing feature in terms of safety in utilization
The prevailing technology of cvd silicon dioxide film is gradually become.
Realize that silica, can be certain in the deposit on SiC wafer surface using ethyl orthosilicate (TEOS) LPCVD technology
Make up that SiC oxide layer is excessively thin and the excessively loose drawback of PECVD silicon dioxide layer in degree.Using TEOS LPCVD technology and height
The reasonable utilization of warm oxidation technology not only ensure that the compactness of oxide layer medium and the adhesive capacity with SiC wafer, but also improve
The electrical property and yield rate of device, while avoiding to obtain the deficiency of certain thickness oxide layer long-time high-temperature oxydation.Using
After this technology, the direct current yield rate of SiC chip is improved, the comparison flow of microwave power device microwave property as the result is shown
It has been significantly improved, power gain improves 1.5dB or so than original process, and power added efficiency improves nearly 10%.
But it is high-purity ethyl orthosilicate that LPCVD technique, which requires ethyl orthosilicate, and wherein metal ion content is testing product
Whether He Ge critical index, conclusive effect is played for the quality of high-purity ethyl orthosilicate.Silicon pure for superelevation
Acetoacetic ester, the content for needing to meet every metal ion species is less than or equal to 0.02ppb, and the content in raw material is end product criteria
Tens times, it is therefore desirable to each link in production process is controlled, just can guarantee the quality of final products.
In the production of high-purity ethyl orthosilicate, a most common link is vaporization, but existing carburetion system cannot be fine
The fine droplet generated in the vaporescence of ground removal raw material, cannot remove raw material so as to cause existing gasification process well
Heavy hydrocarbon and metal ion in TEOS cause certain burden to subsequent production, also make to produce high-purity ethyl orthosilicate presence
Quality risk.
Summary of the invention
In view of this, this is pure the technical problem to be solved in the present invention is that providing a kind of purification process of ethyl orthosilicate
Change method can remove metal ion while vaporization.
The present invention provides a kind of purification process of ethyl orthosilicate, comprising:
Raw material ethyl orthosilicate is vaporized in vaporizer, and passes sequentially through the first fibre bed foam removal on vaporizer top
Device, the second fibre bed demister and third fibre bed demister, obtain ethyl orthosilicate steam；The first fibre bed demister
Aperture be 1~20 μm；The aperture of the second fibre bed demister is 2~10 μm；The hole of the third fibre bed demister
Diameter is 0.1~2 μm.
Preferably, the heat medium in the vaporizer is steam；The temperature of the steam is 160 DEG C~200 DEG C.
Preferably, the flow velocity of the raw material ethyl orthosilicate is 150~250kg/h.
Preferably, the vaporizer is provided with exhausting pipeline.
Preferably, the open degree of the exhausting pipeline is 1%~5%.
Preferably, the vaporizer is provided with sewage draining exit.
Preferably, the open degree of the sewage draining exit is 5%~10%.
Preferably, the height of the liquid level of the raw material ethyl orthosilicate and the first fibre bed demister is 2.5~3 meters.
Preferably, the distance between the first fibre bed demister and the second fibre bed demister are 0.1~0.5 meter.
Preferably, the distance between the second fibre bed demister and third fibre bed demister are 0.1~0.5 meter.
The present invention provides a kind of purification process of ethyl orthosilicate, comprising: by raw material ethyl orthosilicate in vaporizer
Vaporization, and pass sequentially through the first fibre bed demister, the second fibre bed demister and third fibre bed foam removal on vaporizer top
Device obtains ethyl orthosilicate steam；The aperture of the first fibre bed demister is 1~20 μm；The second fibre bed foam removal
The aperture of device is 2~10 μm；The aperture of the third fibre bed demister is 0.1~2 μm.Compared with prior art, of the invention
The ethyl orthosilicate after vaporization is handled using the fibre bed demister of three layers of different pore size, the positive silicic acid of gaseous state can be separated
Diameter is greater than 0.1 μm of liquid in ethyl ester, and foam removal efficiency reaches 95% or more, may also function as separating metal ions and oils heavy hydrocarbon
Effect, therefore the present invention be also greatly reduced while vaporizing ethyl orthosilicate ethyl orthosilicate steam heavy hydrocarbon and metal from
The content of son, plays the role of primary purification, ensure that the quality into the ethyl orthosilicate steam of post-processing system.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of vaporizer used in the embodiment of the present invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
The present invention provides a kind of purification process of ethyl orthosilicate, comprising: by raw material ethyl orthosilicate in vaporizer
Vaporization, and pass sequentially through the first fibre bed demister, the second fibre bed demister and third fibre bed foam removal on vaporizer top
Device obtains ethyl orthosilicate steam；The aperture of the first fibre bed demister is 1~20 μm；The second fibre bed foam removal
The aperture of device is 2~10 μm；The aperture of the third fibre bed demister is 0.1~2 μm.
Wherein, the raw material ethyl orthosilicate is ethyl orthosilicate raw material well known to those skilled in the art, usually
The purity of ethyl orthosilicate is 99%, and impurity wherein included has: moisture, ethyl alcohol, methanol, propyl alcohol and metal ion etc..
Raw material ethyl orthosilicate is vaporized in vaporizer；To make the ethyl orthosilicate amount for passing in and out vaporizer keep balance,
Continuously it can feed and discharge, the flow velocity of the raw material ethyl orthosilicate is preferably 150~250kg/h；The raw material
Ethyl orthosilicate preferably passes through canned motor pump and controls it into the amount in vaporizer；Heat medium in the vaporizer is preferably steamed
Vapour；The temperature of the steam is preferably 160 DEG C~200 DEG C, more preferably 170 DEG C~185 DEG C；The vaporizer is preferably provided with
Heat medium import and Crude product input；Heat medium steam enters from heat medium import, after heat exchange, condenses out
Hot water by Crude product input flow out vaporizer, with guarantee vaporization when heat source supply；Heat exchanger in the vaporizer
For heat exchanger well known to those skilled in the art, preferably pipe heat exchanger, more preferably spiral fin coil in the present invention
Formula heat exchanger is further preferably high frequency welding spiral fin tube formula heat exchanger.Using high frequency welding spiral fin tube formula heat exchanger, do not changing
In the case where becoming heat exchanger occupied area, total heat exchange area increases 3.5 times than original heat exchanger.
The top of the vaporizer is disposed with the first fibre bed demister, the second fibre bed demister and third fiber
Bed demister；It is vaporization space between heat exchanger and the first fibre bed demister；The heat exchanger and the first fibre bed demister
The distance between preferably 2.5~3 meters；The aperture of the first fibre bed demister is 1~20 μm, after capturing vaporization
The droplet that diameter is 5~10 μm in ethyl orthosilicate；The thickness of the first fibre bed demister is preferably 0.1~0.15 meter；
Between first fibre bed demister and the second fibre bed demister and the second fibre bed demister and third fibre bed demister it
Between be ethyl orthosilicate primary purification space, the distance between the first fibre bed demister and the second fibre bed demister
Preferably 0.1~0.5 meter；The distance between the second fibre bed demister and third bed fiber demister preferably 0.1~
0.5 meter；The aperture of second fibre bed demister is 2~10 μm, is 2~5 μ to capture diameter in the ethyl orthosilicate after vaporizing
The droplet of m；The thickness of the second fibre bed demister is preferably 0.1~0.15 meter；The aperture of third fibre bed demister is
0.1~2 μm, to capture the droplet that diameter is 0.1~2 μm in the ethyl orthosilicate after vaporizing；The third fibre bed foam removal
The thickness of device is preferably 0.1~0.15 meter；The ethyl orthosilicate steam (vapor) outlet of the vaporizer is preferably provided with the top of vaporizer
Portion, the ethyl orthosilicate after vaporization pass sequentially through the first fibre bed demister, the second fibre bed demister and third fibre bed and remove
Foam device is not contain more than 0.1 μm of droplet in the ethyl orthosilicate steam made, greatly reduces heavy hydrocarbon and metal ion exists
Content in gas ensure that the quality into the ethyl orthosilicate steam of aftertreatment systems.
In the present invention, the vaporizer is preferably additionally provided with exhausting pipeline；The exhausting pipeline is preferably placed at the first fibre
In the lower sidewalls for tieing up bed demister；In vaporescence, the open degree of the exhausting pipeline is preferably 1%~5%, can part
Remove the light component in ethyl orthosilicate steam.
The vaporizer is preferably additionally provided with sewage draining exit；The sewage draining exit is preferably placed at the bottom of vaporizer；It was vaporizing
Cheng Zhong, the open degree of the sewage draining exit are preferably 5%~10%, so that in vaporizer bottom by the heavy hydrocarbon and metal ion of cathode
It is discharged vaporizer.
According to the present invention, it is preferably additionally provided with liquidometer in the vaporizer, to monitor ethyl orthosilicate in vaporizer
The amount of liquid can monitor the load of vaporizer at any time, guarantee the effect of vaporization.
In the present invention, the equipment such as the heat exchanger in the vaporizer, each component and duct coupling are preferably using electrolysis
The 316L stainless steel material of polishing is made.
The present invention is handled the ethyl orthosilicate after vaporization using the fibre bed demister of three layers of different pore size, can be with
The liquid that diameter in gaseous state ethyl orthosilicate is greater than 0.1 μm is separated, foam removal efficiency reaches 95% or more, may also function as separation metal
The effect of ion and oils heavy hydrocarbon, therefore the present invention is also greatly reduced ethyl orthosilicate steaming while vaporizing ethyl orthosilicate
The content of vapour heavy hydrocarbon and metal ion plays the role of primary purification, ensure that the ethyl orthosilicate into post-processing system
The quality of steam.
In order to further illustrate the present invention, with reference to embodiments to a kind of purifying of ethyl orthosilicate provided by the invention
Method is described in detail.
Reagent used in following embodiment is commercially available.
Embodiment
Using vaporizer shown in FIG. 1, wherein 1 is vaporizer, 2 be ethyl orthosilicate steam (vapor) outlet, and 3 be exhausting pipeline, 4
It is heat medium import for ethyl orthosilicate material inlet, 5,6 be fibre bed demister, and 7 change for high frequency welding spiral fin tube formula
Hot device, 8 be liquidometer mouth, and 9 be sewage draining exit, and 10 be Crude product input；Between heat exchanger and the first fibre bed demister away from
From being 3 meters；The distance between first fibre bed demister and the second fibre bed demister are 0.5 meter；Second fibre bed demister
The distance between third fibre bed demister is 0.5 meter；First fibre bed demister, the second fibre bed demister and third are fine
The thickness for tieing up bed demister is 0.15 meter.
Using steam as heat source, steam enters ratio-frequency welding spiral by the steam inlet (5) on vaporizer for TEOS vaporization
Finned tube exchanger (7) is come into full contact with by heat exchanger tube (7) with raw material TEOS, guarantees the vaporization of raw material TEOS, the heat after heat exchange
Vaporizer is discharged through hot water outlet (10) in water.
Vaporizer side wall is connected with exhausting pipeline (3), can be by nitrogen, oxygen, the methane in raw material TEOS through exhausting pipeline (3)
Etc. light components be vented.Liquidometer (8) are installed on vaporizer, the load of vaporizer can be monitored at any time, guarantee the effect of vaporization
Fruit.
(1) raw material TEOS (wherein the composition of metal ion is shown in Table 1) is continuous via TEOS material inlet (4) by canned motor pump
Constantly enter inside vaporizer, 150~250kg/h maintained by the amount of TEOS that canned motor pump control enters vaporizer, make into
The TEOS amount of vaporizer keeps balance out, continuously can feed and discharge.
(2) the heated medium entrance of steam (5) enters in high frequency welding spiral fin tube (7), controls the temperature of steam 160
DEG C to 200 DEG C or so, is heated by steam, vaporize raw material TEOS sufficiently, the hot water being condensed is gone out by heat medium
Mouth (10) outflow vaporizer (1).
(3) TEOS after overflash enters three layers of fibre bed demister (6), and the aperture of first layer fibre bed demister is
1~20 micron, preferably 10 microns, to capture droplet of the diameter at 5~10 microns in TEOS；Second layer fibre bed demister
Aperture be 2~10 microns, preferably 2 microns, to capture droplet of the diameter at 2~5 microns in TEOS；Third layer fibre bed foam removal
The aperture of device be 0.1~2 micron, preferably 0.1 micron, to capture droplet of the diameter at 0.1~2 micron in TEOS.Pass through three
Layer fibre bed demister, ensure that in the TEOS steam entered in unstrpped gas outlet conduit (2) after vaporizing and is not contain more than 0.1
The droplet of micron, greatly reduces the content of heavy hydrocarbon and metal ion in gas, ensure that the TEOS raw material into rear system
The quality of gas.
(4) it is maintained at the open degree of exhausting pipeline (3) 1%~5% in gasification, can partially be removed light in unstripped gas
Component；The open degree for keeping sewage draining exit (9) 5%~10%, so that the heavy hydrocarbon and metal ion quilt that are enriched in vaporizer bottom
Vaporizer is discharged.
Select three kinds of different vapor (steam) temperatures as heat source respectively, the temperature of selection is respectively 160~170 degree, 170~
185 DEG C, 185~200 DEG C, three layers of fiber demister are 1~20 micron of first layer, 2~10 microns of the second layer, third layer 0.1~2
Micron.Analysis the results are shown in Table 2, by different temperatures select it can be found that when select vapor (steam) temperature be 160~170 DEG C when, though
Metal ion content so after vaporization in TEOS is lower, but evaporating capacity is obviously insufficient, affects subsequent yield；Select steam
When temperature is 185~200 degree, the metal ion content highest in TEOS is exported.The vapor (steam) temperature selection of optimization is 170~
185 degree.
For fiber demister, three layers 10 microns, 2 microns and 0.1 micron of fiber demister is individually selected to carry out
Research, result of study are shown in Table 3, by these analysis results it can be found that individually micro- using three layers 1~20 micron and 2~10
The fiber demister of rice, vaporizer is poor for short grained droplet removal effect, and metal ion removal effect is undesirable；Individually
Using 0.1~2 micron of fiber demister, resistance is larger, affects evaporating capacity, also just affects yield, in practical application not
Give exclusive use.Therefore, 1~20 micron of first layer is used in industrial production, 2~10 microns of the second layer, third layer 0.1~2 is micro-
The fiber demister of rice is the selection optimized.
Metal ion detection result in 1 raw material ethyl orthosilicate of table and final products
Metal ion detection result in the ethyl orthosilicate steam obtained under the different implementation conditions of table 2
Metal ion detection result (adopt by three layers of demister in the ethyl orthosilicate steam obtained under the different implementation conditions of table 3
With different size)
Remarks: A: three layers of demister of condition are 1~20 micron.
B: three layers of demister of condition are 2~10 microns.
Condition C: three layers of demister specification are respectively 1~20 micron of first layer, and 2~10 microns of the second layer, third layer 0.1~
2 microns.
Claims (10)
1. a kind of purification process of ethyl orthosilicate characterized by comprising
Raw material ethyl orthosilicate is vaporized in vaporizer, and passes sequentially through the first fibre bed demister on vaporizer top,
Two fibre bed demisters and third fibre bed demister, obtain ethyl orthosilicate steam；The hole of the first fibre bed demister
Diameter is 1~20 μm；The aperture of the second fibre bed demister is 2~10 μm；The aperture of the third fibre bed demister is
0.1~2 μm.
2. purification process according to claim 1, which is characterized in that the heat medium in the vaporizer is steam；Institute
The temperature for stating steam is 160 DEG C~200 DEG C.
3. purification process according to claim 1, which is characterized in that the flow velocity of the raw material ethyl orthosilicate be 150~
250kg/h。
4. purification process according to claim 1, which is characterized in that the vaporizer is provided with exhausting pipeline.
5. purification process according to claim 4, which is characterized in that the open degree of the exhausting pipeline is 1%~5%.
6. purification process according to claim 1, which is characterized in that the vaporizer is provided with sewage draining exit.
7. purification process according to claim 6, which is characterized in that the open degree of the sewage draining exit is 5%~10%.
8. purification process according to claim 1, which is characterized in that the liquid level of the raw material ethyl orthosilicate and the first fibre
The height for tieing up bed demister is 2.5~3 meters.
9. purification process according to claim 1, which is characterized in that the first fibre bed demister and the second fibre bed
The distance between demister is 0.1~0.5 meter.
10. purification process according to claim 1, which is characterized in that the second fibre bed demister and third fiber
The distance between bed demister is 0.1~0.5 meter.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910106872.9A CN109705153B (en) | 2019-02-02 | 2019-02-02 | Purifying method of ethyl orthosilicate |
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| CN201910106872.9A CN109705153B (en) | 2019-02-02 | 2019-02-02 | Purifying method of ethyl orthosilicate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203095627U (en) * | 2012-11-28 | 2013-07-31 | 苏州金宏气体股份有限公司 | Device for preparing ultra pure ammonia by vaporizing liquid ammonia |
| CN103772424A (en) * | 2013-12-31 | 2014-05-07 | 贵州威顿晶磷电子材料有限公司 | Preparation method of electronic grade tetraethoxysilane |
| CN108640943A (en) * | 2018-04-20 | 2018-10-12 | 居焕龙 | A method of producing ethyl orthosilicate using silica flour |
-
2019
- 2019-02-02 CN CN201910106872.9A patent/CN109705153B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203095627U (en) * | 2012-11-28 | 2013-07-31 | 苏州金宏气体股份有限公司 | Device for preparing ultra pure ammonia by vaporizing liquid ammonia |
| CN103772424A (en) * | 2013-12-31 | 2014-05-07 | 贵州威顿晶磷电子材料有限公司 | Preparation method of electronic grade tetraethoxysilane |
| CN108640943A (en) * | 2018-04-20 | 2018-10-12 | 居焕龙 | A method of producing ethyl orthosilicate using silica flour |
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| CN109705153B (en) | 2020-04-07 |
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Address after: 215152 Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Jinhong Gas Co.,Ltd. Address before: 215152 No. 6 Anmin Road, Panyang Industrial Park, Huangdi Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee before: SUZHOU JINHONG GAS Co.,Ltd. |
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