CN103305808A - Production device for silicon oxide film and production method thereof - Google Patents
Production device for silicon oxide film and production method thereof Download PDFInfo
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- CN103305808A CN103305808A CN2013102325179A CN201310232517A CN103305808A CN 103305808 A CN103305808 A CN 103305808A CN 2013102325179 A CN2013102325179 A CN 2013102325179A CN 201310232517 A CN201310232517 A CN 201310232517A CN 103305808 A CN103305808 A CN 103305808A
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Abstract
The invention provides a production method of silicon oxide, and the production method comprises the following steps of: warming a heating device, setting a to-be-filmed substrate, and introducing nitrogen to remove the impurity gas in the reaction chamber; bringing the reaction precursor ethyl silicate into the reaction chamber by the nitrogen carrier gas; conveying the oxygen in an oxygen source to an ozone generator, conveying the generated ozone into the reaction chamber; performing reactive deposition on the surface of the to-be-filmed substrate by the precursor ethyl silicate and the ozone in the reaction chamber, so as to prepare the silicon oxide film. In the production method of the silicon oxide film provided by the invention, a thermal reaction mode is used, plasma damage of the to-be-filmed substrate is avoided, and the production device of the silicon oxide film is simple, the technological process is easy to control, and the deposition temperature of the silicon oxide film is lowered effectively. Moreover, the silicon oxide film is deposited on the top layer of the Low-E glass, the properties, such as acid and alkali corrosion resistance, oxidation resistance, heat and humidity resistance and high temperature resistance, of the functional glass are improved greatly.
Description
Technical field
The present invention relates to the film deposition techniques field, relate in particular to a kind of production unit and production method thereof of silica membrane.
Background technology
The wearing and tearing of material, corrosion and environmental damage thereof are one of basic problems of facing of modern industry, and the effective way that addresses this problem is to come the surface of strengthening material by various process for treating surface.Surface treatment is chemical constitution, structure, microstructure and the stressed condition of using various technology change material surfaces, to improve the ability that material is resisted the environmental disruption effect.These sufacings, types such as the deposition that can atomize, particle deposition, whole deposition and surface modification.
Chemical vapor deposition (CVD) belongs to the atomic deposition class.The CVD technology has obtained to develop rapidly in the material surface modifying Application for Field.It is at the composition that does not change body material and do not weaken under the performance conditions such as intensity of body material and give the material surface special performances.The CVD process refers to that at a certain temperature reactant gases and matrix surface interact, and some composition in the reactant gases is decomposed, and form required solid film or coating at matrix surface.Because these retes generally have good performance, so to wear resistance solidity to corrosion and the ornamental effect that improvement is arranged of material.And, can prepare the thin-film material of various materials with the CVD method.Can prepare the film of various compositions by the combination of reactant gases, also can prepare and have new fully structure and the thin-film material of composition, even and the high-melting-point material also can under very low temperature, prepare.Using the CVD technology can be at different substrate preparation silicon-containing compound film.Change that processing parameter can obtain to have special electricity, the rete of optics, chemical machinery characteristic, thereby be subject to people's attention.
But; existing CVD coating technique still is confined to the semiconductor integrated circuit production field, and mainly for the manufacture of epitaxial film and insulating protective film etc., the control process influence factor of its CVD is various; technology is still unstable, remains those skilled in the art further to further investigate and apply.
So at the problem that prior art exists, this case designer relies on the industry experience for many years of being engaged in, the active research improvement is so had production unit and the production method thereof of a kind of silica membrane of the present invention.
Summary of the invention
The present invention be directed in the prior art, the technology of traditional CVD method cvd silicon dioxide film still is confined to the semiconductor integrated circuit production field, and CVD equipment complexity, control process influence factor are various, and technology still defective such as instability provides a kind of production unit of silica membrane.
The present invention's another purpose is in the prior art, the technology of traditional CVD method cvd silicon dioxide film still is confined to the semiconductor integrated circuit production field, and the control process influence factor of CVD is various, and technology still defective such as instability provides a kind of production method of silica membrane.
In order to address the above problem, the invention provides a kind of production unit of silicon-dioxide, described equipment comprises: reaction chamber, shown in be used in the reaction chamber described substrate to be filmed is set, and on described substrate to be filmed cvd silicon dioxide film; Heating unit, described heating unit correspondence respectively are arranged on described reaction chamber both sides; Bubbler arranges the pre-reaction material tetraethyl silicate in the described bubbler; First gas piping with first splitter, on described first gas piping first gas meter is set, and one of described first gas piping end links to each other with described nitrogen carrier gas, and the other end of described first gas piping immerses under the liquid level that is arranged on the pre-reaction material tetraethyl silicate in the described bubbler; Second gas piping with second splitter, one of described second gas piping end is arranged in the described bubbler and is positioned on the liquid level of pre-reaction material tetraethyl silicate (TEOS) of described bubbler, and the other end of described second gas piping is communicated with described reaction chamber; The 3rd gas piping with second gas meter, one of described the 3rd gas piping end is communicated with first splitter of described first gas piping, and the other end of described the 3rd gas piping is communicated with second splitter of described second gas piping; Ozonizer, described ozonizer one end are communicated with described reaction chamber by described the 4th gas piping, the other end of described ozonizer and by be arranged on described the 4th gas piping the 3rd gas meter with for the described ozone (O of generation
3) source of oxygen (O
2) be communicated with; And drying installation, described drying installation is communicated with described reaction chamber.
Alternatively, the control of the temperature deviation of described heating unit is in ± 2 ℃.
For solving the present invention's another purpose, the invention provides a kind of method of utilizing the production unit production silica membrane of described silicon-dioxide, described method comprises:
Step S1: described heating unit is warming up to preset temp, and described substrate to be filmed is arranged in the described reaction chamber, and feed nitrogen, to get rid of the foreign gas in the reaction chamber;
Step S2: the nitrogen in the nitrogen carrier gas is brought the pre-reaction material tetraethyl silicate in the described bubbler into described reaction chamber;
Step S3: the oxygen in the described source of oxygen transfers to described ozonizer via described the 3rd gas meter, and the ozone that produces also enters described reaction chamber by described the 4th gas piping;
Step S4: the pre-reaction material tetraethyl silicate and the ozone that enter described reaction chamber carry out reactive deposition on the surface of described substrate to be filmed, to prepare described silica membrane.
Alternatively, described pre-reaction material tetraethyl silicate is arranged in the described bubbler, and described pre-reaction material tetraethyl silicate is carried out heating in water bath, and the temperature of described heating in water bath is 65 ℃ of constant temperature.
Alternatively, described production method further comprises described second gas piping is heated.
Alternatively, the preset temperature range of described heating unit is 300～500 ℃.
Alternatively, described reactive deposition temperature is 400 ℃.
Alternatively, described O
2/ TEOS ratio is more than or equal to 4:1.
Alternatively, the time of described reactive deposition is 30～360s.
Alternatively, described substrate to be filmed is monolithic float glass, Low-E glass, perhaps one of them of solar thermal control glass.
In sum, the production method of silica membrane of the present invention adopts the thermal response mode, not only avoided the plasma damage of described substrate to be filmed, and the production unit of described silica membrane is simple, technological process is controlled easily, has effectively reduced the depositing temperature of silica membrane.In addition, at the described silica membrane of Low-E glass top layer deposition, improve acid-alkali-corrosive-resisting, oxidation-resistance, humid, high thermal resistance of described functional glass etc. greatly.
Description of drawings
Figure 1 shows that the skeleton construction synoptic diagram of the production unit of silica membrane of the present invention;
Figure 2 shows that the schema of the production method of silica membrane of the present invention.
Embodiment
By the technology contents, the structural attitude that describe the invention in detail, reached purpose and effect, described in detail below in conjunction with embodiment and conjunction with figs..
See also Fig. 1, Figure 1 shows that the skeleton construction synoptic diagram of the production unit of silica membrane of the present invention.Shown in the production unit 1 of silica membrane comprise reaction chamber 10, shown in be used for described substrate to be filmed 2 is set in the reaction chamber 10, and on described substrate 2 to be filmed cvd silicon dioxide film (not shown); Heating unit 11, described heating unit 11 correspondence respectively are arranged on described reaction chamber 10 both sides; Bubbler 12 arranges pre-reaction material tetraethyl silicate 121 in the described bubbler 12; First gas piping 13 with first splitter 131, on described first gas piping 13 first gas meter 132 is set, and one of described first gas piping 13 end links to each other with described nitrogen carrier gas 14, and the other end of described first gas piping 13 immerses under the liquid level that is arranged on the pre-reaction material tetraethyl silicate 121 in the described bubbler 12; Second gas piping 15 with second splitter 151, one of described second gas piping 15 end is arranged in the described bubbler 12 and is positioned on the liquid level of pre-reaction material tetraethyl silicate (TEOS) 121 of described bubbler 12, and the other end of described second gas piping 15 is communicated with described reaction chamber 10; The 3rd gas piping 16 with second gas meter 161, one of described the 3rd gas piping 16 end is communicated with first splitter 131 of described first gas piping 13, and the other end of described the 3rd gas piping 16 is communicated with second splitter 151 of described second gas piping 15; Ozonizer 17, described ozonizer 17 1 ends are communicated with described reaction chamber 10 by described the 4th gas piping 18, and the other end of described ozonizer 17 also is communicated with source of oxygen (O2) 171 for the described ozone of generation (O3) by the 3rd gas meter 181 that is arranged on described the 4th gas piping 18; And drying installation 19, described drying installation 19 is communicated with described reaction chamber 10.
In the present invention, for the temperature of reaction of controlling described reaction chamber 10 is constant, preferably in the both sides of described reaction chamber 10 correspondence heating unit 11 is set.The Controllable Temperature of described heating unit 11 is in ± 2 ℃.As those skilled in the art, understand ground easily, described heating unit 11 can be arranged on described reaction chamber 10 1 sides, is advisable with described reaction chamber 10 temperature-stable in the deposition process of described silica membrane.Described pre-reaction material tetraethyl silicate 121 is arranged in the described bubbler 12, and described pre-reaction material tetraethyl silicate 121 is carried out heating in water bath, and the temperature of described heating in water bath is 65 ℃ of constant temperature.Described first gas piping 13 is for delivery of the nitrogen in the described nitrogen carrier gas 14, and the pre-reaction material tetraethyl silicate 121 in the described bubbler 12 are transferred in the described reaction chamber 10 by described second gas piping 15.Described the 3rd gas piping 16 is communicated with first splitter 131 of described first gas piping 13 and second splitter 151 of described second gas piping 15 respectively, in order to carrying out nitrogen dilution from the pre-reaction material tetraethyl silicate 121 that described bubbler 10 is brought in described second gas piping 15, be easy to control the sedimentation rate of the silica membrane in the described reaction chamber 10.Described drying installation 19 is used for preventing that extraneous steam from entering in the described reaction chamber 10.
Without limitation, the substrate to be filmed 2 that is arranged in the described reaction chamber 10 includes but not limited to monolithic float glass, Low-E glass, perhaps one of them of solar thermal control glass.As those skilled in the art, understand ground easily, the production unit 1 of described silica membrane can be connected with described floatation glass production line, to directly be transferred to described silica membrane production line 1 by the float glass of described floatation glass production line production, to finish described silica membrane deposition, and can carry out further deep processing technology to described float glass with silica membrane according to user's purpose.On the other hand; the production unit 1 of described silica membrane also can be connected with existing off-line Low-E production line; for example; magnetron sputtering film device etc.; and described Low-E glass with infrared reflecting layer transferred to described silica membrane production unit 1, to finish the deposition of top layer silicon dioxide thinfilm protective coating.
See also Fig. 2, Figure 2 shows that the schema of the production method of silica membrane of the present invention.The production method of described silica membrane comprises:
Step S1: described heating unit 121 is warming up to preset temp, and described substrate 2 to be filmed is arranged in the described reaction chamber 10, and feed nitrogen, to get rid of the foreign gas in the reaction chamber 10;
Step S2: the nitrogen in the nitrogen carrier gas 14 is brought the pre-reaction material tetraethyl silicate 121 in the described bubbler 12 into described reaction chamber 10;
Step S3: the oxygen in the described source of oxygen 171 transfer to described ozonizer 17 via described the 3rd gas meter 181, and the ozone that produces also enters described reaction chamber 10 by described the 4th gas piping 18;
Step S4: the pre-reaction material tetraethyl silicate 121 and the ozone that enter described reaction chamber 10 carry out reactive deposition on the surface of described substrate 2 to be filmed, to prepare described silica membrane.
When using the production method of silica membrane of the present invention, in order to prevent the condensation in described second gas piping 15 of described pre-reaction material tetraethyl silicate 121, preferably, described second gas piping 15 is heated.The preset temperature range of described heating unit 121 is 300～500 ℃.The time of described reactive deposition is 30～360s.
Be convenient to describe in detail the production method of the present invention's silica membrane, out of the ordinaryly enumerate concrete processing parameter as embodiment, but cited parameter should not be considered as the restriction to the invention technical scheme.Table 1 is depicted as the processing parameter that the present invention prepares silica membrane.After described substrate 2 to be filmed is finished described silica membrane deposition, be positioned in the HF solution of 10:1 and leave standstill 1min, take out then with alpha-step200 model step instrument and measure thickness.Can test the compactness of described silica membrane by described testing method.In the performance test contrast experiment, be that 5min is that example is set forth with the depositing time.
By the 1-9 sample of table 1 as can be known, from 300 ℃ to 400 ℃, sedimentation rate raises and raises along with temperature; From 400 ℃ to 500 ℃, sedimentation rate begins to descend.When temperature reached 400 ℃, sedimentation rate reached as high as 28nm/min.On the other hand, erosion rate is from 300 ℃ 80nm/min to 500 ℃ 22nm/min.Erosion rate reduces along with the rising of depositing temperature always, and along with temperature continues to raise after 400 ℃ again, the decline degree of erosion rate tends towards stability.The variation that described erosion rate descends can illustrate that along with the rising of temperature, the compactness of the silica membrane that forms on the described substrate 2 to be filmed improves gradually.
Table 1 is depicted as the processing parameter that the present invention prepares silica membrane
By the 10-15 sample of table 1 as can be known, when being 390 ℃ for the temperature of reaction chamber 10, described sedimentation rate increases along with the TEOS flow and raises.When described TEOS flow is 100 or during 110sccm, sedimentation rate reaches 29nm/min, the rising trend of sedimentation rate by fast to steady gradually.On the other hand, under 390 ℃, erosion rate is along with the rising of TEOS flow presents ascendant trend, and ascendant trend is accelerated.The variation of erosion rate shows that the compactness that is formed on the silica membrane on the described substrate to be filmed 2 is along with the rising of TEOS flow descends on the contrary.
By the 10-15 sample of table 1 as can be known, O
2/ TEOS ratio has material impact to described silica membrane compactness.Erosion rate is along with O
2The curve of/TEOS ratio presents the exponential form decay, works as O
2/ TEOS ratio tends towards stability when 4:1.
As those skilled in the art, from described simultaneous test as can be known, preferably, described reactive deposition temperature is 400 ℃.Described O
2/ TEOS ratio is more than or equal to 4:1.
For the superiority of the prepared silica membrane of the production method of the silica membrane of further setting forth the present invention, as concrete embodiment, the Low-E glass of described substrate 2 to be filmed for having the infrared external reflection functional layer.Preparation method by silica membrane of the present invention prepares the Low-E glass that top layer is silica membrane; and carry out the test of acid, alkali; the test of anti-measuring mechanical property and antioxidant property, and with routine do not have silica membrane as the Low-E glass of top layer protective layer as reference.Described top layer is the preparation method of the Low-E glass of silica membrane, comprising:
Step 1: described heating unit 121 is warming up to 400 ℃, and described Low-E glass with infrared external reflection functional layer is arranged in the described reaction chamber 10, and feed nitrogen, to get rid of the foreign gas in the reaction chamber 10;
Step 2: the nitrogen in the nitrogen carrier gas 14 is brought the pre-reaction material tetraethyl silicate 121 in the described bubbler 12 into described reaction chamber 10;
Step 3: the oxygen in the described source of oxygen 171 transfer to described ozonizer 17 via described the 3rd gas meter 181, and the ozone that produces also enters described reaction chamber 10 by described the 4th gas piping 18;
Step 4: the pre-reaction material tetraethyl silicate 121 and the ozone that enter described reaction chamber 10 carry out reactive deposition on described surface with Low-E glass of infrared external reflection functional layer, are the Low-E glass of silica membrane with the preparation top layer.
Low-E glass of the present invention is: the production method by silica membrane of the present invention is at the described described silica membrane of Low-E glass top layer deposition with infrared external reflection functional layer;
Reference Low-E glass is: conventional no silica membrane is as the Low-E glass of top layer protective layer.
Table 2 is contrasted for transmitance (Tr's) before and after grinding
As shown in Table 2, the Low-E glass that the manufacture method by Low-E of the present invention obtains is before and after grinding, and its printing opacity Tr changes less, characterizes the Low-E glass that the manufacture method of Low-E of the present invention obtains and has anti-abrasive characteristic well.
Table 3 is contrasted for the antioxidant property test
| Nakedly put test (natural oxidation time) | Humid heat test (damp and hot machine oxidization time) | |
| Low-e glass of the present invention | 6200 min | 490 min |
| Reference Low-e glass | 4560 min | 240 min |
| Time expand | 1640 min | 250 min |
As shown in Table 3, it is strong that the Low-E glass that the manufacture method by Low-E of the present invention obtains has resistance of oxidation, is difficult for the characteristic of oxidation.
In sum, the production method of silica membrane of the present invention adopts the thermal response mode, not only avoided the plasma damage of described substrate to be filmed, and the production unit of described silica membrane is simple, technological process is controlled easily, has effectively reduced the depositing temperature of silica membrane.In addition, at the described silica membrane of Low-E glass top layer deposition, improve acid-alkali-corrosive-resisting, oxidation-resistance, humid, high thermal resistance of described functional glass etc. greatly.
Those skilled in the art all should be appreciated that, under the situation that does not break away from the spirit or scope of the present invention, can carry out various modifications and variations to the present invention.Thereby, if when any modification or modification fall in the protection domain of appended claims and equivalent, think that the present invention contains these modifications and modification.
Claims (10)
1. the production unit of a silicon-dioxide is characterized in that, described equipment comprises:
Reaction chamber, shown in be used in the reaction chamber described substrate to be filmed is set, and on described substrate to be filmed cvd silicon dioxide film;
Heating unit, described heating unit correspondence respectively are arranged on described reaction chamber both sides;
Bubbler arranges the pre-reaction material tetraethyl silicate in the described bubbler;
First gas piping with first splitter, on described first gas piping first gas meter is set, and one of described first gas piping end links to each other with described nitrogen carrier gas, and the other end of described first gas piping immerses under the liquid level that is arranged on the pre-reaction material tetraethyl silicate in the described bubbler;
Second gas piping with second splitter, one of described second gas piping end is arranged in the described bubbler and is positioned on the liquid level of pre-reaction material tetraethyl silicate (TEOS) of described bubbler, and the other end of described second gas piping is communicated with described reaction chamber;
The 3rd gas piping with second gas meter, one of described the 3rd gas piping end is communicated with first splitter of described first gas piping, and the other end of described the 3rd gas piping is communicated with second splitter of described second gas piping;
Ozonizer, described ozonizer one end are communicated with described reaction chamber by described the 4th gas piping, the other end of described ozonizer and by be arranged on described the 4th gas piping the 3rd gas meter with for the described ozone (O of generation
3) source of oxygen (O
2) be communicated with; And,
Drying installation, described drying installation is communicated with described reaction chamber.
2. the production unit of silicon-dioxide as claimed in claim 1 is characterized in that, the temperature deviation control of described heating unit is in ± 2 ℃.
3. method of utilizing claim 1 or 2 described silicon-dioxide production units to produce silica membranes is characterized in that described method comprises:
Step S1: described heating unit is warming up to preset temp, and described substrate to be filmed is arranged in the described reaction chamber, and feed nitrogen, to get rid of the foreign gas in the reaction chamber;
Step S2: the nitrogen in the nitrogen carrier gas is brought the pre-reaction material tetraethyl silicate in the described bubbler into described reaction chamber;
Step S3: the oxygen in the described source of oxygen transfers to described ozonizer via described the 3rd gas meter, and the ozone that produces also enters described reaction chamber by described the 4th gas piping;
Step S4: the pre-reaction material tetraethyl silicate and the ozone that enter described reaction chamber carry out reactive deposition on the surface of described substrate to be filmed, to prepare described silica membrane.
4. as the production method of silica membrane as described in the claim 3, it is characterized in that, described pre-reaction material tetraethyl silicate is arranged in the described bubbler, and described pre-reaction material tetraethyl silicate is carried out heating in water bath, and the temperature of described heating in water bath is 65 ℃ of constant temperature.
5. as the production method of silica membrane as described in the claim 3, it is characterized in that described production method further comprises described second gas piping is heated.
6. as the production method of silica membrane as described in the claim 3, it is characterized in that the preset temperature range of described heating unit is 300～500 ℃.
7. as the production method of silica membrane as described in the claim 6, it is characterized in that described reactive deposition temperature is 400 ℃.
8. as the production method of silica membrane as described in the claim 7, it is characterized in that described O
2/ TEOS ratio is more than or equal to 4:1.
9. as the production method of silica membrane as described in the claim 3, it is characterized in that the time of described reactive deposition is 30～360s.
10. as the production method of silica membrane as described in the claim 3, it is characterized in that described substrate to be filmed is monolithic float glass, Low-E glass, perhaps one of them of solar thermal control glass.
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| CN2013102325179A CN103305808A (en) | 2013-06-13 | 2013-06-13 | Production device for silicon oxide film and production method thereof |
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| CN2013102325179A CN103305808A (en) | 2013-06-13 | 2013-06-13 | Production device for silicon oxide film and production method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108018538A (en) * | 2017-11-24 | 2018-05-11 | 中航（重庆）微电子有限公司 | The method and apparatus of silica membrane is prepared using PE-TEOS techniques |
| CN109321896A (en) * | 2017-07-31 | 2019-02-12 | 北京北方华创微电子装备有限公司 | A kind of atomic layer deposition system |
| CN109750276A (en) * | 2019-01-28 | 2019-05-14 | 中国科学院电工研究所 | Based on inert gas/oxygen plasma membrane deposition method and device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109321896A (en) * | 2017-07-31 | 2019-02-12 | 北京北方华创微电子装备有限公司 | A kind of atomic layer deposition system |
| CN109321896B (en) * | 2017-07-31 | 2021-01-29 | 北京北方华创微电子装备有限公司 | Atomic layer deposition system |
| CN108018538A (en) * | 2017-11-24 | 2018-05-11 | 中航（重庆）微电子有限公司 | The method and apparatus of silica membrane is prepared using PE-TEOS techniques |
| CN109750276A (en) * | 2019-01-28 | 2019-05-14 | 中国科学院电工研究所 | Based on inert gas/oxygen plasma membrane deposition method and device |
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Application publication date: 20130918 |