CN203333758U - Production equipment of silicon dioxide film - Google Patents
Production equipment of silicon dioxide film Download PDFInfo
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- CN203333758U CN203333758U CN2013203362946U CN201320336294U CN203333758U CN 203333758 U CN203333758 U CN 203333758U CN 2013203362946 U CN2013203362946 U CN 2013203362946U CN 201320336294 U CN201320336294 U CN 201320336294U CN 203333758 U CN203333758 U CN 203333758U
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- gas piping
- reaction chamber
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Abstract
The utility model provides production equipment of a silicon dioxide film. The production equipment of the silicon dioxide film comprises a reaction chamber, heating devices, a bubbler, a first gas pipeline with a first splitter, a second gas pipeline with a second splitter, a third gas pipeline with a second gas flow meter, an ozone generator and a drying device, wherein the heating devices are arranged at the two sides of the reaction chamber; a reaction precursor ethyl silicate is arranged in the bubbler; one end of the first gas pipeline is connected with nitrogen carrier gas and the other end of the first gas pipeline is immersed under the liquid level of the reaction precursor ethyl silicate; one end of the second gas pipeline is arranged above the liquid level of the reaction precursor ethyl silicate and the other end of the second gas pipeline is communicated with the reaction chamber; the two ends of the third gas pipeline are communicated with the first splitter and the second splitter respectively; one end of the ozone generator is communicated with the reaction chamber and the other end of the ozone generator is communicated with an oxygen source; and the drying device is communicated with the reaction chamber. The production equipment of the silicon dioxide film is simple; the technical process is easy to control; the deposition temperature of the silicon dioxide film is effectively reduced; and plasma damage to a substrate on which a film is to be formed is avoided.
Description
Technical field
The utility model relates to the film deposition techniques field, relates in particular to a kind of production unit 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 addressed 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, the ability of to improve material, resisting the environmental disruption effect.These sufacings, the 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 application of CVD technology in the material surface modifying field obtained and developed rapidly.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 material surface special performance.The CVD process refers to that at a certain temperature reactant gases and matrix surface interaction are decomposed some composition in reactant gases, and formed 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 be improved of material.And, can prepare the thin-film material of various materials by the CVD method.The film that can prepare various compositions by the combination of reactant gases, also can prepare the thin-film material with fully new structure and composition, even and high-melting-point substances also can at very low temperature, prepare.Application CVD technology can prepare the silicon-containing compound film in different substrates.Change processing parameter can obtain there is 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; technique is still unstable, remains those skilled in the art further further investigate and apply.
Therefore the problem existed for prior art, this case designer relies on the industry experience for many years of being engaged in, and the active research improvement, so had production unit and the production method thereof of a kind of silica membrane of the utility model.
The utility model content
The utility model is in 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 is complicated, the control process influence factor is various, the technique still defect such as unstable provides a kind of production unit of silica membrane.
In order to address the above problem, the utility model provides a kind of production unit of silicon-dioxide, and described equipment comprises: reaction chamber, shown in reaction chamber for 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 is arranged on described reaction chamber both sides; Bubbler, arrange the pre-reaction material tetraethyl silicate in described bubbler; The first gas piping with first splitter, on described the first gas piping, the first gas meter is set, and one of described first gas piping end is connected with described nitrogen carrier gas, the other end of described the first gas piping immerses under the liquid level that is arranged on the pre-reaction material tetraethyl silicate in described bubbler; The second gas piping with second splitter, one of described second gas piping end is arranged in 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 the 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 the first splitter of described the first gas piping, and the other end of described the 3rd gas piping is communicated with the second splitter of described the second gas piping; Ozonizer, described ozonizer one end is communicated with described reaction chamber by described the 4th gas piping, the other end of described ozonizer by being arranged on the 3rd gas meter on described the 4th gas piping and for generating described ozone (O
3) source of oxygen (O
2) be communicated with; And drying installation, described drying installation is communicated with described reaction chamber.
Alternatively, the temperature deviation of described heating unit be controlled at ± 2 ℃ in.
Alternatively, described substrate to be filmed is monolithic float glass, Low-E glass, or one of them of solar thermal control glass.
In sum, the production unit of silica membrane described in the utility model is simple, and technological process is easily controlled, and effectively reduces the depositing temperature of silica membrane, and has avoided the plasma damage of described substrate to be filmed.
The accompanying drawing explanation
Figure 1 shows that the skeleton construction schematic diagram of the production unit of the utility model silica membrane;
Figure 2 shows that the schema of the production method of the utility model silica membrane.
Embodiment
By describing technology contents, structural attitude that the utility model creates in detail, being reached purpose and effect, below in conjunction with embodiment and coordinate accompanying drawing to be described in detail.
Refer to Fig. 1, Figure 1 shows that the skeleton construction schematic diagram of the production unit of the utility model silica membrane.Shown in the production unit 1 of silica membrane comprise reaction chamber 10, shown in reaction chamber 10 for described substrate to be filmed 2 is set, and on described substrate 2 to be filmed cvd silicon dioxide film (not shown); Heating unit 11, described heating unit 11 correspondence respectively is arranged on described reaction chamber 10 both sides; Bubbler 12, the interior pre-reaction material tetraethyl silicate 121 that arranges of described bubbler 12; The first gas piping 13 with first splitter 131, on described the first gas piping 13, the first gas meter 132 is set, and one of described first gas piping 13 end is connected with described nitrogen carrier gas 14, the other end of described the first gas piping 13 immerses under the liquid level that is arranged on the pre-reaction material tetraethyl silicate 121 in described bubbler 12; The second gas piping 15 with second splitter 151, one of described second gas piping 15 end is arranged in 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 the 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 the first splitter 131 of described the first gas piping 13, and the other end of described the 3rd gas piping 16 is communicated with the second splitter 151 of described the 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 the source of oxygen (O2) 171 for generating described ozone (O3) by the 3rd gas meter 181 be 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 utility model, 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 temperature control of described heating unit 11 is in ± 2 ℃.As those skilled in the art, hold intelligibly, described heating unit 11 can be arranged on described reaction chamber 10 1 sides, with described reaction chamber 10 temperature-stable in the deposition process of described silica membrane, is advisable.Described pre-reaction material tetraethyl silicate 121 is arranged in described bubbler 12, and described pre-reaction material tetraethyl silicate 121 is carried out to heating in water bath, and the temperature of described heating in water bath is 65 ℃ of constant temperature.Described the first gas piping 13 is for delivery of the nitrogen in described nitrogen carrier gas 14, and the pre-reaction material tetraethyl silicate 121 in described bubbler 12 are transferred in described reaction chamber 10 by described the second gas piping 15.Described the 3rd gas piping 16 is communicated with the first splitter 131 of described the first gas piping 13 and the second splitter 151 of described the second gas piping 15 respectively, carry out nitrogen dilution in order to the pre-reaction material tetraethyl silicate 121 that will be brought in described the second gas piping 15 from described bubbler 10, be easy to control the sedimentation rate of the silica membrane in described reaction chamber 10.Described drying installation 19 enters in described reaction chamber 10 for preventing extraneous steam.
Without limitation, the substrates to be filmed 2 that are arranged in described reaction chamber 10 include but not limited to monolithic float glass, Low-E glass, or one of them of solar thermal control glass.As those skilled in the art, hold intelligibly, the production unit 1 of described silica membrane can be connected with described floatation glass production line, to directly be transferred to by the float glass of described floatation glass production line production described silica membrane production line 1, to complete described silica membrane deposition, and can, according to user's purpose, to the described float glass with silica membrane, carry out further deep processing technology.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; magnetic-controlled sputtering coating equipment etc.; and the described Low-E glass with infrared reflecting layer is transferred to described silica membrane production unit 1, to complete the deposition of top layer silicon dioxide thinfilm protective coating.
Refer to Fig. 2, Figure 2 shows that the schema of the production method of the utility model silica membrane.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 described reaction chamber 10, and pass into nitrogen, to get rid of the foreign gas in reaction chamber 10;
Step S2: the nitrogen in nitrogen carrier gas 14 is brought the pre-reaction material tetraethyl silicate 121 in described bubbler 12 into described reaction chamber 10;
Step S3: the oxygen in described source of oxygen 171 transfers to described ozonizer 17 via described the 3rd gas meter 181, and the ozone produced 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 described in the utility model, in order to prevent that described pre-reaction material tetraethyl silicate 121 is in the interior condensation of described the second gas piping 15, preferably, described the 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 silica membrane of the utility model, out of the ordinaryly enumerate concrete processing parameter as embodiment, but cited parameter should not be considered as the utility model is created the restriction of technical scheme.Table 1 is depicted as the processing parameter that the utility model prepares silica membrane.After described substrate 2 to be filmed completes described silica membrane deposition, be positioned over standing 1min in the HF solution of 10:1, then take out 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, the depositing time of take is set forth as 5min as example.
From the 1-9 sample of table 1, from 300 ℃ to 400 ℃, sedimentation rate raises and raises along with temperature; From 400 ℃ to 500 ℃, sedimentation rate starts to descend.When temperature reaches 400 ℃, sedimentation rate reaches as high as 28nm/min.On the other hand, erosion rate is from the 22nm/min of 80nm/min to 500 ℃ of 300 ℃.Erosion rate reduces along with the rising of depositing temperature always, and along with temperature, after 400 ℃, continues to raise again, and the decline degree of erosion rate tends towards stability.The variation that described erosion rate descends can illustrate, along with the rising of temperature, the compactness of the silica membrane formed on described substrate 2 to be filmed improves gradually.
Table 1 is depicted as the processing parameter that the utility model prepares silica membrane
From the 10-15 sample of table 1, while for the temperature of reaction chamber 10, being 390 ℃, described sedimentation rate is along with the TEOS flow increases 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 compactness that the variation of erosion rate shows to be formed on the silica membrane on described substrate to be filmed 2 is along with the rising of TEOS flow descends on the contrary.
From the 10-15 sample of table 1, O
2/ TEOS ratio is to described silica membrane compactness important.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, 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 utility model, as concrete embodiment, the Low-E glass of described substrate 2 to be filmed for thering is the infrared external reflection functional layer.Preparation method by silica membrane described in the utility model 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 using routine without silica membrane as the Low-E glass of top layer protective layer as reference.The preparation method of the Low-E glass that described top layer is silica membrane comprises:
Step 1: described heating unit 121 is warming up to 400 ℃, and the described Low-E glass with infrared external reflection functional layer is arranged in described reaction chamber 10, and pass into nitrogen, to get rid of the foreign gas in reaction chamber 10;
Step 2: the nitrogen in nitrogen carrier gas 14 is brought the pre-reaction material tetraethyl silicate 121 in described bubbler 12 into described reaction chamber 10;
Step 3: the oxygen in described source of oxygen 171 transfers to described ozonizer 17 via described the 3rd gas meter 181, and the ozone produced 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 the described surface with Low-E glass of infrared external reflection functional layer, take and prepare the Low-E glass that top layer is silica membrane.
Low-E glass described in the utility model is: the production method by silica membrane described in the utility model 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: routine is the Low-E glass as the top layer protective layer without silica membrane.
Table 2 is contrasted for transmitance (Tr's) before and after grinding
As shown in Table 2, the Low-E glass that manufacture method by Low-E described in the utility model obtains is before and after grinding, it is less that its printing opacity Tr changes, and characterizes the Low-E glass that the manufacture method of Low-E described in the utility model obtains and have 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) | |
| The utility model Low-e glass | 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 described in the utility model obtains has resistance of oxidation, is difficult for the characteristic of oxidation.
In sum, the production method of silica membrane described in the utility model 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 easily controlled, and effectively reduces the depositing temperature of silica membrane.In addition, at the described silica membrane of Low-E glass top layer deposition, improve greatly acid-alkali-corrosive-resisting, oxidation-resistance, humid, high thermal resistance of described functional glass etc.
Those skilled in the art all should be appreciated that, in the situation that do not break away from spirit or scope of the present utility model, can carry out various modifications and variations to the utility model.Thereby, if when any modification or modification fall in the protection domain of appended claims and equivalent, think that the utility model contains these modifications and modification.
Claims (3)
1. the production unit of a silica membrane, is characterized in that, described equipment comprises:
Reaction chamber, shown in reaction chamber for substrate to be filmed is set, and on described substrate to be filmed cvd silicon dioxide film;
Heating unit, described heating unit correspondence respectively is arranged on described reaction chamber both sides;
Bubbler, arrange the pre-reaction material tetraethyl silicate in described bubbler;
The first gas piping with first splitter, on described the first gas piping, the first gas meter is set, and one of described the first gas piping end is connected with the nitrogen carrier gas, the other end of described the first gas piping immerses under the liquid level that is arranged on the pre-reaction material tetraethyl silicate in described bubbler;
The second gas piping with second splitter, one of described second gas piping end is arranged in 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 the 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 the first splitter of described the first gas piping, and the other end of described the 3rd gas piping is communicated with the second splitter of described the second gas piping;
Ozonizer, described ozonizer one end is communicated with described reaction chamber by the 4th gas piping, the other end of described ozonizer by being arranged on the 3rd gas meter on described the 4th gas piping and for generating described ozone (O
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 silica membrane as claimed in claim 1, is characterized in that, the temperature deviation of described heating unit is controlled at ± 2 ℃ in.
3. the production unit of silica membrane as claimed in claim 1, is characterized in that, described substrate to be filmed is monolithic float glass, Low-E glass, or one of them of solar thermal control glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013203362946U CN203333758U (en) | 2013-06-13 | 2013-06-13 | Production equipment of silicon dioxide film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013203362946U CN203333758U (en) | 2013-06-13 | 2013-06-13 | Production equipment of silicon dioxide film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN203333758U true CN203333758U (en) | 2013-12-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013203362946U Expired - Lifetime CN203333758U (en) | 2013-06-13 | 2013-06-13 | Production equipment of silicon dioxide film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305808A (en) * | 2013-06-13 | 2013-09-18 | 林嘉佑 | Production device for silicon oxide film and production method thereof |
| CN108485030A (en) * | 2018-03-28 | 2018-09-04 | 浙江达因包装材料有限公司 | A kind of processing technology of the special shrink film of bowl face |
-
2013
- 2013-06-13 CN CN2013203362946U patent/CN203333758U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305808A (en) * | 2013-06-13 | 2013-09-18 | 林嘉佑 | Production device for silicon oxide film and production method thereof |
| CN108485030A (en) * | 2018-03-28 | 2018-09-04 | 浙江达因包装材料有限公司 | A kind of processing technology of the special shrink film of bowl face |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170628 Address after: 12 building, International Building, Kunshan Development Zone, Jiangsu, 215321 Patentee after: CHANGJIANG GLASS Co.,Ltd. TAIBO Address before: Taicang Shenjiang port economic and Technological Development Zone, Road No. 9 Patentee before: Lin Jiayou |
|
| TR01 | Transfer of patent right | ||
| CX01 | Expiry of patent term |
Granted publication date: 20131211 |
|
| CX01 | Expiry of patent term |