CN109438495A - A kind of production method and production system of high-purity ethyl orthosilicate - Google Patents
A kind of production method and production system of high-purity ethyl orthosilicate Download PDFInfo
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Abstract
The present invention provides a kind of production methods of high-purity ethyl orthosilicate, comprising: S1) by ethyl orthosilicate crude product after moisture adsorbent is adsorbed, the ethyl orthosilicate for the moisture that is removed；S2) by the ethyl orthosilicate of the adsorption moisture after metal ion-modified materials are handled, the ethyl orthosilicate that obtains that treated；S3) treated that ethyl orthosilicate is distilled by described, obtains high-purity ethyl orthosilicate.Compared with prior art, the present invention is by dewatered ethyl orthosilicate after metal ion-modified materials are handled, heavier compounds are converted by therein phosphorous and/or boracic light component substance, high-purity ethyl orthosilicate can be obtained after distillation condensation again, production method is easily operated, high degree of automation, it can carry out continuous production, the product quality that work efficiency is high and obtains is also higher, while distillation only being needed to also reduce energy consumption, energy saving and cost lowering.
Description
Technical field
The invention belongs to the production methods and production system of technical field of semiconductors more particularly to a kind of high-purity ethyl orthosilicate
System.
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%.
The Chinese patent of Publication No. CN201310747619.4 discloses a kind of preparation side of electron level ethyl orthosilicate
Method, this method first with after most of metal impurities in complexing agent complexing raw material, are filtered, then with 0.1 micron of millipore filter
Pass sequentially through cation exchange tower, quartzy plate tower, sub-boiling distillation device, strict temperature control, removal trace metal impurities,
Ethyl alcohol and other organic impurities and moisture, but new impurity metal ion is easily quoted using complexing agent, and pass through sub-boiling distillation
Mode difficulty of processing is big, high energy consumption and efficiency is low, so that the production cost increases for product, and is unable to continuous production.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that one kind is provided can continuous production and lower-cost high-purity
The production method and production system of ethyl orthosilicate.
The present invention provides a kind of production methods of high-purity ethyl orthosilicate, comprising:
S1) by ethyl orthosilicate crude product after moisture adsorbent is adsorbed, the ethyl orthosilicate for the moisture that is removed；
S2) by the dewatered ethyl orthosilicate after metal ion-modified materials are handled, obtain that treated just
Silester；
S3) treated that ethyl orthosilicate is distilled by described, obtains high-purity ethyl orthosilicate.
Preferably, the moisture adsorbent is selected from 3A molecular sieve.
Preferably, the metal ion-modified materials are selected as the modified silica-alumina gel of carried noble metal.
Preferably, the S3) specifically:
Treated by described in, and ethyl orthosilicate carries out first time distillation, the positive silicic acid after condensation, after obtaining single flash
Ethyl ester；
Ethyl orthosilicate after the single flash is carried out second to distill, after condensation, is obtained after second distillation just
Silester；
Ethyl orthosilicate after the second distillation is subjected to third time distillation, after condensation, obtains high-purity ethyl orthosilicate.
Preferably, after distillation, condensation after Electrostatic Absorption is handled, obtains high-purity ethyl orthosilicate.
The present invention also provides a kind of production systems of high-purity ethyl orthosilicate, comprising:
Water adsorption device；The water adsorption device includes ethyl orthosilicate crude product entrance and outlet；
Metal ion-modified device；The outlet of the moisture absorbing device is connected with the metal ion-modified device；
Destilling tower；The destilling tower is connected with metal ion-modified device.
It preferably, further include condensing unit；The condensing unit is connected with the tower top of destilling tower.
It preferably, further include secondary distillation tower and the second condensing unit；The secondary distillation tower and the condensing unit phase
Connection；The tower top of the secondary distillation tower is connected with the second condensing unit.
It preferably, further include three-stage distillation tower and third condensing unit；The three-stage distillation tower and second condensation fill
It sets and is connected；The tower top of the three-stage distillation tower is connected with third condensing unit.
It preferably, further include metal ion electrostatic adsorption device, the metal ion electrostatic adsorption device and the third
Condensing unit is connected.
The present invention provides a kind of production methods of high-purity ethyl orthosilicate, comprising: S1) by ethyl orthosilicate crude product through water
After dividing adsorbent absorption, the ethyl orthosilicate for the moisture that is removed；S2) by the ethyl orthosilicate of the adsorption moisture through metal from
After the processing of sub- modified material, the ethyl orthosilicate that obtains that treated；S3) treated that ethyl orthosilicate is distilled by described,
Obtain high-purity ethyl orthosilicate.Compared with prior art, the present invention is by dewatered ethyl orthosilicate through metal ion-modified
After material processing, heavier compounds are converted by therein phosphorous and/or boracic light component substance, then after distillation condensation
High-purity ethyl orthosilicate can be obtained, production method is easily operated, high degree of automation, can carry out continuous production, working efficiency
Product quality that is high and obtaining is also higher, while distillation only being needed to also reduce energy consumption, energy saving and cost lowering.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of high-purity ethyl orthosilicate production system provided by the invention；
Fig. 2 is the structural schematic diagram of high-purity ethyl orthosilicate production system provided by the 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 production methods of high-purity ethyl orthosilicate, comprising: S1) by ethyl orthosilicate crude product through water
After dividing adsorbent absorption, the ethyl orthosilicate for the moisture that is removed；S2) by the dewatered ethyl orthosilicate through metal from
After the processing of sub- modified material, the ethyl orthosilicate that obtains that treated；S3) treated that ethyl orthosilicate is distilled by described,
Obtain high-purity ethyl orthosilicate.
Wherein the ethyl orthosilicate crude product is ethyl orthosilicate crude product well known to those skilled in the art, usual positive silicic acid
The purity of ethyl ester is 99%, and impurity wherein included has: moisture, ethyl alcohol, methanol, propyl alcohol and metal ion etc..
By ethyl orthosilicate crude product after moisture adsorbent is adsorbed, the ethyl orthosilicate for the moisture that is removed；The moisture
Adsorbent is moisture adsorbent well known to those skilled in the art, has no special limitation, and preferably 3A divides in the present invention
Son sieve, the aperture of this molecular sieve analog is smaller, similar with hydrone diameter, therefore adsorbable hydrone；The positive silicic acid second
The flow velocity of ester crude product is preferably 1~5 meter per second, more preferably 3 meter per seconds.
By the dewatered ethyl orthosilicate after metal ion-modified materials are handled, the positive silicic acid that obtains that treated
Ethyl ester；The metal ion-modified materials are preferably the modified silica-alumina gel of carried noble metal, and more preferably palladium and/or platinum is modified
Silica-alumina gel；Wherein silica-alumina gel includes silica and aluminum oxide；The matter of the silica and aluminum oxide
Amount is than being preferably (1~2): 1, more preferably 1.5:1；(i.e. the quality of noble metal is Silica hydrogel quality to the load capacity of noble metal
Percentage) it is preferably 0.1%~1%；Some III races and group Ⅴ element, as phosphorus and boron will form POCl in ethyl orthosilicate3、
BOCl3、PCl3、BCl3Equal compounds.These compounds can exist during TEOS distills as light component, therefore steam
During evaporating, finished pot can be entered with stream flow, these impurity is caused just not can be removed.The present invention first with metal from
Sub- modified material handles the ethyl orthosilicate for moisture of going out, by being adsorbed on changing for the upper surface of molecular sieve filled object load
Property material, by POCl3、BOCl3、PCl3、BCl3Etc. light components compound, be modified to heavier compounds, then again to TEOS into
Row distillation, such impurity can be exhausted as heavy constituent, and the TEOS that light component comes out will be purified.
Treated that ethyl orthosilicate is distilled by described；The temperature of the distillation is preferably 165 DEG C~170 DEG C.For
The quality of the high-purity ethyl orthosilicate further increased, present invention preferably employs three-stage distillations, are particularly preferred as: will be described
Treated, and ethyl orthosilicate carries out first time distillation, the ethyl orthosilicate after condensation, after obtaining single flash；It will be described primary
Ethyl orthosilicate after distillation carries out second and distills, the ethyl orthosilicate after condensation, after obtaining second distillation；It will be described secondary
Ethyl orthosilicate after distillation carries out third time distillation, after condensation, obtains high-purity ethyl orthosilicate；First time distillation, the
Second distillation and the temperature of third time distillation are preferably 165 DEG C~170 DEG C each independently；The method of the condensation is preferably this
Method known to the technical staff of field has no special limitation, and present invention preferably employs recirculated cooling waters to be condensed；Institute
The temperature for stating recirculated cooling water is preferably 20 DEG C~30 DEG C, more preferably 25 DEG C.
Through three-stage distillation, impurity metal ion can be removed, in such a way that heavy constituent is discharged to be further reduced metal
The content of ionic impurity handles through Electrostatic Absorption after preferably condensing, obtains high-purity ethyl orthosilicate；The electricity of the Electrostatic Absorption
Pressure is preferably 300~700 volts/rice, and more preferably 400~600 volts/rice is further preferably 500 volts/rice；It can be into one through Electrostatic Absorption
Step removes positively charged metal ion.
The present invention by dewatered ethyl orthosilicate after metal ion-modified materials are handled, by it is therein it is phosphorous and/
Or the light component substance of boracic is converted into heavier compounds, then high-purity ethyl orthosilicate can be obtained after distillation condensation, it is raw
Production method is easily operated, high degree of automation, can carry out continuous production, and work efficiency is high and obtained product quality is also higher,
Distillation is only needed to also reduce energy consumption, energy saving and cost lowering simultaneously.
The present invention also provides a kind of production systems of high-purity ethyl orthosilicate, comprising:
Water adsorption device；The water adsorption device includes ethyl orthosilicate crude product entrance and outlet；
Metal ion-modified device；The outlet of the moisture absorbing device is connected with the metal ion-modified device；
Destilling tower；The destilling tower is connected with metal ion-modified device.
Referring to Fig. 1 and Fig. 2, Fig. 1 and Fig. 2 is the structural representation of high-purity ethyl orthosilicate production system provided by the invention
Figure.
High-purity ethyl orthosilicate provided by the invention is just producing system and is preferably including head tank, thick for storing ethyl orthosilicate
Product；The outlet of the head tank is connected with the ethyl orthosilicate crude product entrance of water adsorption device.
It is preferably provided with molecular sieve in the water adsorption device, is more preferably provided with 3A molecular sieve；The water adsorption
The ratio of height to diameter of device is preferably (5~12): 1, more preferably (7~12): 1, it is further preferably 7:1.
The outlet of the water adsorption device is connected with metal ion-modified device；In the metal ion-modified device
Filled with metal ion-modified materials；The preferably loaded modified silica-alumina gel of the metal ion-modified materials；The metal from
The ratio of height to diameter of sub- reforming apparatus is preferably (5~12): 1, more preferably (5~10): 1, be further preferably (7~10): 1, most preferably
For 7:1.
According to the present invention, it is also preferable to include spare metal ion-modified devices；The spare metal ion-modified device and water
The outlet of adsorbent equipment is divided to be connected；Metal ion-modified materials are filled in the spare metal ion-modified device；It is described
Metal ion-modified materials are preferably the modified silica-alumina gel of carried noble metal；The metal ion-modified materials are same as above,
Details are not described herein.Spare metal ion-modified device can be used simultaneously with metal ion-modified device, also be used interchangeably, with
Both less burden can also make production that can continue to carry out.
The metal ion-modified device is connected with destilling tower respectively with spare metal ion-modified device；In destilling tower
The interior ethyl orthosilicate to after metal ion-modified distills；The destilling tower is distillation well known to those skilled in the art
Tower has no special limitation, and preferably using oil bath as heating method, the destilling tower is provided with heretofore described destilling tower
Heat conducting oil inlet and conduction oil outlet；Heat conducting oil inlet is connected with conduction oil outlet with heating heat conduction oil tank；In order to be conducive to follow
Ring, the heating heat conduction oil tank preferably pass through circulating pump and are connected with the heat conducting oil inlet of the destilling tower.
According to the present invention, it is also preferable to include condensing units for the production system；The tower top of the condensing unit and destilling tower
It is connected；The ethyl orthosilicate steam that destilling tower distills out is condensed by condensing unit；The condensing unit is preferably provided with
There are cooling water inlet and cooling water outlet；The cooling water inlet is connected with chilled water tank with cooling water outlet.
In order to improve the purity of ethyl orthosilicate, it is also preferable to include secondary distillation towers and the second condensing unit；The second level
Destilling tower is connected with condensing unit；The tower top of the secondary distillation tower is connected with the second condensing unit.Guarantee to improve
The flow of ethyl orthosilicate liquid in secondary distillation tower；The condensing unit preferably passes through the first fluid cushion tank and secondary distillation
Tower is connected；The secondary distillation tower is destilling tower well known to those skilled in the art, has no special limitation, the present invention
Described in secondary distillation tower preferably using oil bath as heating method, the secondary distillation tower is provided with heat conducting oil inlet and goes out with conduction oil
Mouthful；The heat conducting oil inlet of secondary distillation tower is connected with conduction oil outlet with heating heat conduction oil tank；It is described to add in order to be conducive to circulation
Hot heat conduction oil tank preferably passes through circulating pump and is connected with the heat conducting oil inlet of the secondary distillation tower；Second condensing unit is excellent
Choosing is provided with cooling water inlet and cooling water outlet；The cooling water inlet of second condensing unit and cooling water outlet and cooling
Water pot is connected.
It is also preferable to include three-stage distillation towers and third condensing unit for production system provided by the invention；The three-stage distillation tower
It is connected with the second condensing unit；The tower top of the three-stage distillation tower is connected with third condensing unit.In order to improve guarantee three
The flow of ethyl orthosilicate liquid in grade destilling tower；The condensing unit preferably passes through second liquid surge tank and three-stage distillation tower
It is connected；The three-stage distillation tower is destilling tower well known to those skilled in the art, has no special limitation, in the present invention
Preferably using oil bath as heating method, the three-stage distillation tower is provided with heat conducting oil inlet and goes out with conduction oil the three-stage distillation tower
Mouthful；The heat conducting oil inlet of three-stage distillation tower is connected with conduction oil outlet with heating heat conduction oil tank；It is described to add in order to be conducive to circulation
Hot heat conduction oil tank preferably passes through circulating pump and is connected with the heat conducting oil inlet of the three-stage distillation tower；The third condensing unit is excellent
Choosing is provided with cooling water inlet and cooling water outlet；The cooling water inlet of the third condensing unit and cooling water outlet and cooling
Water pot is connected.
It, can be miscellaneous by metal ion in such a way that destilling tower, secondary distillation tower and three-stage distillation tower tower bottom heavy constituent are discharged
Matter removal, in order to further remove positively charged metal ion, production system provided by the invention it is also preferable to include metal from
Sub- electrostatic adsorption device；The metal ion electrostatic adsorption device is connected with the third condensing unit, in order to guarantee metal
Metal ion electrostatic adsorption device described in the flow of ethyl orthosilicate liquid preferably passes through third liquid in ion electrostatic adsorption device
Body surge tank is connected with third condensing unit；Negative electrode plate is provided in the metal ion electrostatic adsorption device；It is described negative
Electrode plate is connected with the cathode of power supply；The width of the negative electrode plate is preferably 0.1~0.5 meter, more preferably 0.2~0.3
Rice, is further preferably 0.2 meter；The length of negative electrode plate is preferably 0.5~2 meter, and more preferably 0.8~1.5 meter, be further preferably 1 meter；
The specification of negative electrode plate used is preferably 0.2 meter * 1 meter in the present invention；The plus earth of power supply.Ethyl orthosilicate liquid is in negative electricity
Adsorbable positively charged metal ion is flowed through on pole plate, to obtain high-purity ethyl orthosilicate.
It is also preferable to include finished pots for production system provided by the invention；The finished pot and metal ion electrostatic adsorption device
It is connected, to store high-purity ethyl orthosilicate.
In order to further illustrate the present invention, with reference to embodiments to a kind of high-purity ethyl orthosilicate provided by the invention
Production method and production system are described in detail.
Reagent used in following embodiment is commercially available.
Embodiment 1
It is prepared using Fig. 1 and production system shown in Fig. 2, is wherein provided with 3A molecular sieve in water adsorption device,
The ratio of height to diameter of water adsorption device is 7:1；Filled with the silica-alumina gel (40%Al that palladium is modified in metal ion-modified device2O3+
60%SiO2, load capacity 0.5%), ratio of height to diameter 7:1；The intensity of metal ion electrostatic adsorption device is 500 volts/rice, negative electrode
The specification of plate is 0.2 meter * 1 meter.
The flow velocity of ethyl orthosilicate crude product is preferably 3 meter per seconds.
The temperature of destilling tower, secondary distillation tower and three-stage distillation tower is 170 DEG C.
The condensing unit, the second condensing unit and third condensing unit are passed through into 25 DEG C of cooling water circulating condensings.
Impurity composition and content in ethyl orthosilicate crude product used in embodiment 1 are shown in Table 1；To being obtained in embodiment 1
High-purity ethyl orthosilicate detected, obtain the results are shown in Table 2.
The impurity composition and content of 1 embodiment of table, 1 ethyl orthosilicate crude product
The testing result of 2 embodiment of table, 1 electronic pure ethyl orthosilicate
Embodiment 2
Preparation flow is with embodiment 1, the difference is that the intensity of metal ion electrostatic adsorption device is 400 volts/rice.
High-purity grade of ethyl orthosilicate product obtained in embodiment 2 is detected, testing result meets with embodiment 1
It is required that.
Embodiment 3
Preparation flow is with embodiment 1, the difference is that solidifying filled with the modified sial of platinum in metal ion-modified device
Glue (40%Al2O3+ 60%SiO2, load capacity 1%), ratio of height to diameter 10:1；The intensity of metal ion electrostatic adsorption device is 500
Volt/rice, the specification of negative electrode plate are 0.3 meter * 1 meter.
High-purity grade of ethyl orthosilicate product obtained in embodiment 3 is detected, testing result meets with embodiment 1
It is required that.
Claims (10)
1. a kind of production method of high-purity ethyl orthosilicate characterized by comprising
S1) by ethyl orthosilicate crude product after moisture adsorbent is adsorbed, the ethyl orthosilicate for the moisture that is removed；
S2) by the dewatered ethyl orthosilicate after metal ion-modified materials are handled, the positive silicic acid that obtains that treated
Ethyl ester；
S3) treated that ethyl orthosilicate is distilled by described, obtains high-purity ethyl orthosilicate.
2. production method according to claim 1, which is characterized in that the moisture adsorbent is selected from 3A molecular sieve.
3. production method according to claim 1, which is characterized in that the metal ion-modified materials are selected as your gold loaded
Belong to modified silica-alumina gel.
4. production method according to claim 1, which is characterized in that the S3) specifically:
Treated by described in, and ethyl orthosilicate carries out first time distillation, the ethyl orthosilicate after condensation, after obtaining single flash；
Ethyl orthosilicate after the single flash is carried out second to distill, the positive silicic acid after condensation, after obtaining second distillation
Ethyl ester；
Ethyl orthosilicate after the second distillation is subjected to third time distillation, after condensation, obtains high-purity ethyl orthosilicate.
5. production method according to claim 4, which is characterized in that after distillation, condensation after Electrostatic Absorption is handled, is obtained
To high-purity ethyl orthosilicate.
6. a kind of production system of high-purity ethyl orthosilicate characterized by comprising
Water adsorption device；The water adsorption device includes ethyl orthosilicate crude product entrance and outlet；
Metal ion-modified device；The outlet of the moisture absorbing device is connected with the metal ion-modified device；
Destilling tower；The destilling tower is connected with metal ion-modified device.
7. production system according to claim 6, which is characterized in that further include condensing unit；The condensing unit and steaming
The tower top for evaporating tower is connected.
8. production system according to claim 7, which is characterized in that further include secondary distillation tower and the second condensing unit；
The secondary distillation tower is connected with the condensing unit；The tower top of the secondary distillation tower is connected with the second condensing unit.
9. production system according to claim 8, which is characterized in that further include three-stage distillation tower and third condensing unit；
The three-stage distillation tower is connected with second condensing unit；The tower top of the three-stage distillation tower is connected with third condensing unit
It is logical.
10. production system according to claim 9, which is characterized in that it further include metal ion electrostatic adsorption device, it is described
Metal ion electrostatic adsorption device is connected with the third condensing unit.
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| CN109400637A (en) * | 2018-09-29 | 2019-03-01 | 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 |
| CN109734742A (en) * | 2019-03-12 | 2019-05-10 | 大连恒坤新材料有限公司 | A kind of method of purification of ethyl orthosilicate |
| CN112592717A (en) * | 2020-12-18 | 2021-04-02 | 湖南工业大学 | Nano fluorescent carbon dots and preparation method thereof |
| CN114507250A (en) * | 2022-01-12 | 2022-05-17 | 湖北江瀚新材料股份有限公司 | Synthesis process of electronic-grade ethyl orthosilicate and electronic-grade ethyl polysilicate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109400637A (en) * | 2018-09-29 | 2019-03-01 | 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 |
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| CN109438495B (en) | 2023-05-26 |
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