CN116553482A - Nitrogen-free high-concentration ozone generating device and preparation method thereof - Google Patents
Nitrogen-free high-concentration ozone generating device and preparation method thereof Download PDFInfo
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- CN116553482A CN116553482A CN202310581939.0A CN202310581939A CN116553482A CN 116553482 A CN116553482 A CN 116553482A CN 202310581939 A CN202310581939 A CN 202310581939A CN 116553482 A CN116553482 A CN 116553482A
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- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000010410 layer Substances 0.000 claims abstract description 104
- 230000003197 catalytic effect Effects 0.000 claims abstract description 61
- 239000011241 protective layer Substances 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims description 69
- 239000000758 substrate Substances 0.000 claims description 54
- 229910001220 stainless steel Inorganic materials 0.000 claims description 47
- 239000010935 stainless steel Substances 0.000 claims description 47
- 239000000843 powder Substances 0.000 claims description 35
- 239000000919 ceramic Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 12
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 238000007650 screen-printing Methods 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- 238000007639 printing Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000011810 insulating material Substances 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000004513 sizing Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000005524 ceramic coating Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims 2
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 15
- 239000007789 gas Substances 0.000 abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 229910021645 metal ion Inorganic materials 0.000 abstract description 4
- 230000017525 heat dissipation Effects 0.000 abstract description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/10—Preparation of ozone
- C01B13/11—Preparation of ozone by electric discharge
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2201/00—Preparation of ozone by electrical discharge
- C01B2201/10—Dischargers used for production of ozone
- C01B2201/12—Plate-type dischargers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2201/00—Preparation of ozone by electrical discharge
- C01B2201/20—Electrodes used for obtaining electrical discharge
- C01B2201/22—Constructional details of the electrodes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2201/00—Preparation of ozone by electrical discharge
- C01B2201/20—Electrodes used for obtaining electrical discharge
- C01B2201/24—Composition of the electrodes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2201/00—Preparation of ozone by electrical discharge
- C01B2201/30—Dielectrics used in the electrical dischargers
- C01B2201/34—Composition of the dielectrics
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
Abstract
The invention provides a nitrogen-free added high-concentration ozone generating device and a preparation method thereof, wherein a catalytic protective layer is arranged on the surface of a ground electrode plate, which is close to a high-voltage electrode plate, so that the efficiency of generating ozone gas can be ensured under the condition that nitrogen is not added, the surface of the ground electrode plate is protected, the exceeding standard of metal ions is avoided, the purity of the generated ozone gas is ensured, meanwhile, only the high-voltage electrode plate uses a dielectric layer, the ground electrode plate does not use the dielectric layer, the production process steps are saved, the connecting layer between the dielectric layer and the ground electrode plate is reduced, the heat dissipation effect is improved, the flatness of the ground electrode plate is effectively improved, and the discharge uniformity is improved, thereby improving the device performance.
Description
Technical Field
The invention relates to the technical field of ozone production, in particular to a nitrogen-free high-concentration ozone generating device and a preparation method thereof.
Background
The ozone generator is used for preparing ozone gas (O) 3 ) The device is easy to decompose and can not be stored, and the device is required to be used in the field, so that an ozone generator is required in all places where ozone can be used. The high-purity ozone generator is necessary equipment for surface treatment of crystalline silicon, is widely applied to the industries of semiconductors, photovoltaics and the like, and the ozone purity directly influences the quality of semiconductor devices. At present, high purityAnd the high-concentration ozone generator adopts a DBD discharge technology, and the structure is a plate structure. The high-concentration ozone generator is added with a trace amount of nitrogen to catalyze the generation of high-concentration ozone, but the addition of nitrogen generally generates byproducts such as nitrogen oxides, and trace amounts of water vapor in the nitrogen oxides and the oxygen are combined to form nitric acid, so that an ozone pipeline is corroded, impurity metals such as Fe, cr, mn, ni are separated out, the metal content exceeds the production requirement of semiconductor devices, the yield and the performance of the semiconductor devices are negatively influenced, and the purity of ozone gas is influenced. The advanced nitrogen-free high-concentration ozone generating device can be produced by only few companies in Germany and Japan basically only by import, has high manufacturing cost and high price, and has high equipment maintenance cost, and even the imported high-concentration ozone generating device has the service cycle of only two years, needs to be maintained once every two years and has high use cost.
Disclosure of Invention
The invention aims to provide a high-concentration ozone generating device without nitrogen addition and a preparation method thereof on the premise of remarkably reducing the manufacturing cost, so that the defect that the purity of ozone gas is influenced by adding trace nitrogen into a high-concentration ozone generator can be avoided, the preparation process is simplified, and the cost of the ozone generating device is remarkably reduced to replace high-cost imported equipment.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the nitrogen-free high-concentration ozone generating device is characterized by comprising a ground polar plate and a high-voltage polar plate, wherein the ground polar plate and the high-voltage polar plate are oppositely arranged, a catalytic protection layer is arranged on the surface, opposite to the high-voltage polar plate, of the ground polar plate, a first dielectric layer is arranged on the surface, opposite to the ground polar plate, of the high-voltage polar plate, and a discharge gap is formed between the catalytic protection layer and the first dielectric layer.
Preferably, the catalytic protective layer is made of any one of a first oxide catalyst group and/or any one of a second oxide catalyst group, the first oxide catalyst group including TiO 2 、WO 3 、MoO 3 ZnO and Fe 2 O 3 The second oxide catalyst group includes Nb 2 O 5 、Nb 2 O 3 、V 2 O 5 、Ta 2 O 5 And Cr (V) 2 O 3 。
Still preferably, in the nitrogen-free high-concentration ozone generating device, the ground electrode plate is a stainless steel plate, and at this time, the catalytic protective layer is made of any one of the first oxide catalyst group and/or any one of the second oxide catalyst group through a metal meltallizing process, and the meltallizing thickness is 10-1000 μm.
Still preferably, the ground electrode plate is composed of a stainless steel sheet substrate and a ceramic coating, and at this time, the catalytic protective layer is prepared by screen printing and baking metal powder slurry of any one of the first oxide catalyst group and/or any one of the second oxide catalyst group, and the thickness of the slurry is 1-100 μm.
Still preferably, the ozone generating device further includes an air gap forming layer located between the catalytic protective layer and the first dielectric layer.
Still preferably, the air gap forming layer is made of an insulating material.
Still preferably, the first dielectric layer is Al 2 O 3 And a ceramic layer.
According to another object of the present invention, the present invention also provides a method for preparing a nitrogen-free high concentration ozone generating device, the ozone generating device includes a ground electrode plate and a high voltage electrode plate disposed opposite to the ground electrode plate, a catalytic protection layer is disposed on a surface of the ground electrode plate facing the high voltage electrode plate, a first dielectric layer is disposed on a surface of the high voltage electrode plate facing the ground electrode plate, and a discharge gap is formed between the catalytic protection layer and the first dielectric layer; the catalytic protective layer is made of any one of a first oxide catalyst group and/or any one of a second oxide catalyst group, and the first oxide catalyst group comprises TiO 2 、WO 3 、MoO 3 ZnO and Fe 2 O 3 The second step ofThe oxide catalyst group comprises Nb 2 O 5 、Nb 2 O 3 、V 2 O 5 、Ta 2 O 5 And Cr (V) 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The preparation method comprises the following steps:
s1, processing a pair of stainless steel substrates according to a designed size, wherein one stainless steel substrate is used as a ground polar plate, and the other stainless steel substrate is used as a substrate of a high-voltage polar plate;
s2, preparing oxide catalyst powder;
s3, preparing a catalytic protective layer on one side surface of the stainless steel substrate of the ground polar plate through a meltallizing process;
s4, plating Al on one side surface of the stainless steel substrate of the high-voltage polar plate 2 O 3 The ceramic layer serves as a first dielectric layer;
s5, arranging the ground electrode plate and the high-voltage electrode plate oppositely, arranging the catalytic protection layer opposite to the first dielectric body layer, and forming a discharge gap between the catalytic protection layer and the first dielectric body layer.
Preferably, in step S3, the uniform powder is fused to the stainless steel substrate surface of the ground plate to a thickness of 10-1000 μm.
According to another object of the present invention, the present invention also provides a method for preparing a nitrogen-free additive high-concentration ozone generating device, which is characterized in that the ozone generating device comprises a ground electrode plate and a high-voltage electrode plate arranged opposite to the ground electrode plate, a catalytic protection layer is arranged on the surface of the ground electrode plate facing the high-voltage electrode plate, a first dielectric layer is arranged on the surface of the high-voltage electrode plate facing the ground electrode plate, and a discharge gap is formed between the catalytic protection layer and the first dielectric layer; the catalytic protective layer is made of any one of a first oxide catalyst group and/or any one of a second oxide catalyst group, and the first oxide catalyst group comprises TiO 2 、WO 3 、MoO 3 ZnO and Fe 2 O 3 The second oxide catalyst group includes Nb 2 O 5 、Nb 2 O 3 、V 2 O 5 、Ta 2 O 5 And Cr (V) 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The preparation method comprises the following steps:
s1, processing a pair of stainless steel substrates according to a designed size, wherein one stainless steel substrate is used as a ground electrode plate substrate, and the other stainless steel substrate is used as a substrate of a high-voltage electrode plate;
s2, plating Al on one side surface of the stainless steel substrate of the ground polar plate and the stainless steel substrate of the high-voltage polar plate 2 O 3 A ceramic layer;
s3, preparing oxide catalyst powder, and preparing the powder into slurry;
s4, al of the ground polar plate is printed through a screen printing process 2 O 3 Printing sizing agent on the surface of the ceramic layer, and sintering and curing to obtain a catalytic protective layer;
s5, arranging the ground electrode plate and the high-voltage electrode plate oppositely, arranging the catalytic protection layer opposite to the first dielectric body layer, and forming a discharge gap between the catalytic protection layer and the first dielectric body layer.
Preferably, when the oxide catalyst powder is selected from a mixture of a first oxide catalyst and a second oxide catalyst, the powder preparation method thereof is as follows:
s1.1, mixing 2 oxide catalysts;
s1.2, calcining the mixture at a high temperature;
s1.3, ball milling the materials in the previous step;
s1.4, sieving the ball-milled substances to obtain uniform powder.
Still preferably, the sintering curing temperature in step S4 is not higher than 500 ℃.
Still preferably, in step S4, the paste is printed to a thickness of 1-100 μm.
Compared with the prior art, the invention has the beneficial effects that: the catalytic protective layer is arranged on the surface of the ground electrode plate, which is close to the high-voltage electrode plate, so that the efficiency of generating ozone gas can be ensured under the condition that nitrogen is not added, the surface of the ground electrode plate is protected, the exceeding of metal ions is avoided, the purity of the generated ozone gas is ensured, meanwhile, only the high-voltage electrode plate uses a dielectric layer, the ground electrode plate does not use the dielectric layer, the production process steps are saved, the connecting layer between the dielectric and the ground electrode plate is reduced, the heat dissipation effect is improved, the flatness of the ground electrode plate is effectively improved, the discharge uniformity is improved, and the device performance is improved; in addition, the ground plate and the high-voltage polar plate are both stainless steel substrates with lower cost, and compared with a ceramic substrate, the processing cost and the material cost of the stainless steel substrate are obviously reduced.
Drawings
FIG. 1 is a schematic diagram of a nitrogen-free high concentration ozone generating device according to an embodiment of the present invention;
fig. 2 is a schematic structural view of a nitrogen-free high-concentration ozone generating device according to another embodiment of the invention.
Description of the embodiments
For a further understanding of the objects, construction, features, and functions of the invention, reference should be made to the following detailed description of the preferred embodiments.
Referring to fig. 1, the nitrogen-free high-concentration ozone generating device of the present invention includes a ground electrode plate 1 and a high-voltage electrode plate 2, wherein the ground electrode plate 1 and the high-voltage electrode plate 2 are disposed opposite to each other, a catalytic protection layer 3 is disposed on a surface of the ground electrode plate 1 adjacent to the high-voltage electrode plate 2, a first dielectric layer 4 is disposed on a surface of the high-voltage electrode plate 2 adjacent to the ground electrode plate 1, and a discharge gap is formed between the catalytic protection layer 3 and the first dielectric layer 4.
Through setting up catalytic protection layer 3 on the surface that ground polar plate 1 is close to high-pressure polar plate 2, under the condition of not adding nitrogen gas, can guarantee to produce ozone gas's efficiency, protection ground polar plate surface avoids the metal ion to exceed standard, guarantees to produce ozone gas's purity, simultaneously, only high-pressure polar plate 2 uses the dielectric layer, ground polar plate 1 does not use the dielectric layer, save production process step, reduce the articulamentum between dielectric and the ground polar plate 1, improve the radiating effect, effectively improve ground polar plate 1 planarization, improve the homogeneity of discharging, thereby improve the device performance.
In a preferred embodiment, the catalytic protective layer 3 is made of any one of a first oxide catalyst group including TiO and/or any one of a second oxide catalyst group 2 、WO 3 、MoO 3 ZnO and Fe 2 O 3 The second oxide catalyst group includes Nb 2 O 5 、Nb 2 O 3 、V 2 O 5 、Ta 2 O 5 And Cr (V) 2 O 3 So that the catalytic protection layer 3 has both catalytic and protection functions.
Preferably, the first dielectric layer 4 is Al 2 O 3 And a ceramic layer.
Referring to fig. 2, fig. 2 is a schematic structural diagram of a nitrogen-free high-concentration ozone generating device according to another embodiment of the invention. In comparison with the embodiment in fig. 1, in the present embodiment, the ozone generating device further includes an air gap forming layer 5, and the air gap forming layer 5 is located between the catalytic protective layer 3 and the first dielectric layer 4 to be able to control the discharge gap.
Preferably, the air gap forming layer 5 is made of an insulating material.
The invention also provides a preparation method of the nitrogen-free high-concentration ozone generating device, which comprises the following steps:
s1, processing a pair of stainless steel substrates according to a designed size, wherein one stainless steel substrate is used as a ground polar plate, and the other stainless steel substrate is used as a substrate of a high-voltage polar plate;
s2, preparing oxide catalyst powder;
s3, preparing a catalytic protective layer on one side surface of the stainless steel substrate of the ground polar plate through a meltallizing process;
s4, plating Al on one side surface of the stainless steel substrate of the high-voltage polar plate 2 O 3 The ceramic layer serves as a first dielectric layer;
s5, arranging the ground electrode plate and the high-voltage electrode plate oppositely, arranging the catalytic protection layer opposite to the first dielectric body layer, and forming a discharge gap between the catalytic protection layer and the first dielectric body layer.
In the above step S2, if the first oxide catalyst group is selected to include TiO 2 、WO 3 、MoO 3 ZnO and Fe 2 O 3 Or the second oxide catalyst group comprises Nb 2 O 5 、Nb 2 O 3 、V 2 O 5 、Ta 2 O 5 And Cr (V) 2 O 3 Oxide catalyst of (a)The catalyst is prepared into powder and is sprayed to form a catalytic protection layer, and oxide powder prepared by fine grinding can be directly sprayed to form the catalytic protection layer on the surface of the stainless steel substrate. In a more preferred embodiment, one oxide catalyst may be selected from each of the first oxide catalyst group and the second oxide catalyst group, and the powder is prepared by mixing the oxide catalysts and then performing the meltallizing process, and the specific steps of the powder preparation are as follows:
s1.1, mixing two oxide catalyst powders;
s1.2, calcining the mixture at a high temperature;
s1.3, ball milling the calcined mixture in the previous step;
s1.4, sieving the ball-milled substances to obtain uniform powder.
The mixed oxide catalyst can form a catalyst with better performance after high-temperature calcination, and then a catalytic protection layer with better performance can be formed after the mixed oxide catalyst is fused and sprayed on the surface of the stainless steel substrate, so that the high purity of ozone gas is ensured.
With the selected oxide catalyst as TiO 2 And Nb (Nb) 2 O 5 For example, explanation will be given.
First, tiO is treated with 2 And Nb (Nb) 2 O 5 Mixing the powder according to a certain mass ratio (for example, 0.1-3) by a ball mill, sieving the mixed powder, and sintering at high temperature (for example, 1300 ℃) in a box-type resistance furnace to obtain yellow solid (Ti-Nb-O) with TiNb 2 O 7 Ti and 2 Nb 10 O 29 at least one crystal form of (a). Pulverizing Ti-Nb-O solid, putting into a ball milling tank together with a ball milling medium and pure water, and sieving the powder after ball milling to obtain powder (0.01-100 μm) with uniform particles.
In a preferred embodiment, in step S3, the uniform powder is fused to the stainless steel substrate surface of the ground plate to a thickness of 10-1000 μm.
In the above embodiment, the catalytic protection layer is formed by means of meltallizing, and in another embodiment of the present application, the catalytic protection layer may be formed by means of screen printing to prepare the ozone generating device, which specifically includes the following steps:
s1, processing a pair of stainless steel substrates according to a designed size, wherein one stainless steel substrate is used as a ground electrode plate substrate, and the other stainless steel substrate is used as a substrate of a high-voltage electrode plate;
s2, plating Al on one side surface of the stainless steel substrate of the ground polar plate and the stainless steel substrate of the high-voltage polar plate 2 O 3 A ceramic layer;
s3, preparing oxide catalyst powder, and preparing the powder into slurry;
s4, al of the ground polar plate is printed through a screen printing process 2 O 3 Printing sizing agent on the surface of the ceramic layer, and sintering and curing to obtain a catalytic protective layer;
s5, arranging the ground electrode plate and the high-voltage electrode plate oppositely, arranging the catalytic protection layer opposite to the first dielectric body layer, and forming a discharge gap between the catalytic protection layer and the first dielectric body layer.
In this embodiment, since the oxide catalyst slurry is required to be sintered and solidified to form the catalytic protection layer after screen printing, the sintering temperature is close to 500 ℃, and at this time, if the slurry is directly printed on the surface of the stainless steel substrate, the stainless steel is basically easy to deform, precipitate impurities and the like during high-temperature sintering, and the quality of the ozone generating device is affected, so that it is required to form Al on the surface of the stainless steel substrate 2 O 3 The ceramic layer is then printed and sintered with slurry, so that the quality and the use requirement of the ozone generating device can be ensured.
In addition, similarly, in the present embodiment, if the first oxide catalyst group is selected to include TiO 2 、WO 3 、MoO 3 ZnO and Fe 2 O 3 Or the second oxide catalyst group comprises Nb 2 O 5 、Nb 2 O 3 、V 2 O 5 、Ta 2 O 5 And Cr (V) 2 O 3 The oxide catalyst is made into a catalytic protective layer by pulping, printing and sintering, and can be directly processed into adhesive slurry by using oxide powder prepared by fine grinding, and Al on a stainless steel substrate 2 O 3 A catalytic protective layer is formed on the ceramic layer. In a more preferred embodiment of the present invention,the first oxide catalyst group and the second oxide catalyst group can be selected from an oxide catalyst, and then mixed to prepare powder, and then the powder is subjected to a meltallizing process, wherein the specific steps of the powder preparation are the same as above, and the detailed description is omitted.
Likewise, with TiO 2 And Nb (Nb) 2 O 5 Powder mixing is exemplified by processing the calcined, ball-milled and screened Ti-Nb-O powder into a slurry with viscosity, printing Al on a stainless steel substrate of a ground electrode plate 2 O 3 The surface of the ceramic layer is printed with the thickness of 1-100 mu m, and the sintering temperature is below 500 ℃.
In the preparation method, only the high-voltage polar plate uses the dielectric medium, the dielectric medium is not formed on the ground polar plate, the production process steps are saved, the connecting layer between the dielectric medium and the ground polar plate is reduced, and the connecting layer is generally made of insulating materials, so that the thermal resistance is large, and the radiating effect can be obviously improved; meanwhile, the flatness of the ground polar plate can be effectively improved, and the discharge uniformity is improved, so that the performance of the device is improved.
In actual production, the arrangement of the catalytic protective layer on the surface of the ground electrode plate and the arrangement of the first dielectric layer on the surface of the high-voltage electrode plate can be performed simultaneously, so that the preparation time is saved, and the preparation efficiency is improved.
According to the nitrogen-free added high-concentration ozone generating device and the preparation method thereof, the catalytic protective layer is arranged on the surface of the ground electrode plate, which is close to the high-voltage electrode plate, so that the efficiency of generating ozone gas can be guaranteed under the condition that nitrogen is not added, the surface of the ground electrode plate is protected, the exceeding standard of metal ions is avoided, the purity of the generated ozone gas is guaranteed, meanwhile, only the high-voltage electrode plate uses a dielectric layer, the ground electrode plate does not use the dielectric layer, the production process steps are saved, the connecting layer between the dielectric and the ground electrode plate is reduced, the heat dissipation effect is improved, the flatness of the ground electrode plate is effectively improved, and the discharge uniformity is improved, so that the device performance is improved; the high-voltage polar plate and the ground plate both use stainless steel plates as substrate materials, and compared with other materials such as Al, the processing cost and the material cost 2 O 3 The ceramic is significantly reduced; the prepared ozone generating device can meet the preparation requirement of high-concentration ozone, can meet the service life requirement of common semiconductor equipment, and can replace expensive ozone generation devicesAnd port equipment promotes the localization of semiconductor equipment.
The invention has been described with respect to the above-described embodiments, however, the above-described embodiments are merely examples of practicing the invention. It should be noted that the disclosed embodiments do not limit the scope of the invention. On the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (13)
1. The nitrogen-free high-concentration ozone generating device is characterized by comprising a ground polar plate and a high-voltage polar plate, wherein the ground polar plate and the high-voltage polar plate are oppositely arranged, a catalytic protection layer is arranged on the surface, opposite to the high-voltage polar plate, of the ground polar plate, a first dielectric layer is arranged on the surface, opposite to the ground polar plate, of the high-voltage polar plate, and a discharge gap is formed between the catalytic protection layer and the first dielectric layer.
2. The nitrogen-free added high concentration ozone generating device as claimed in claim 1, wherein said catalytic shielding layer is made of any one of a first oxide catalyst group and/or any one of a second oxide catalyst group, said first oxide catalyst group comprising TiO 2 、WO 3 、MoO 3 ZnO and Fe 2 O 3 The second oxide catalyst group includes Nb 2 O 5 、Nb 2 O 3 、V 2 O 5 、Ta 2 O 5 And Cr (V) 2 O 3 。
3. The nitrogen-free high-concentration ozone generating device according to claim 2, wherein the ground plate is a stainless steel plate, and the catalytic shielding layer is made of any one of the first oxide catalyst group and/or any one of the second oxide catalyst group by a metal-spraying process, and the spraying thickness is 10-1000 μm.
4. The nitrogen-free high-concentration ozone generating device according to claim 2, wherein the ground electrode plate is composed of a stainless steel sheet substrate and a ceramic coating, and at this time, the catalytic protective layer is prepared by screen printing any one of the first oxide catalyst group and/or any one of the second oxide catalyst group through metal powder slurry and then baking, and the thickness of the slurry printed is 1-100 μm.
5. The nitrogen-free high concentration ozone generating device as recited in claim 1, further comprising an air gap forming layer located between said catalytic protective layer and said first dielectric layer.
6. The nitrogen-free high-concentration ozone generating device as recited in claim 3, wherein said air gap forming layer is made of an insulating material.
7. The nitrogen-free high-concentration ozone generating device according to claim 1, wherein said first dielectric layer is Al 2 O 3 And a ceramic layer.
8. The preparation method of the nitrogen-free added high-concentration ozone generating device is characterized in that the ozone generating device comprises a ground polar plate and a high-voltage polar plate arranged opposite to the ground polar plate, wherein a catalytic protective layer is arranged on the surface of the ground polar plate facing the high-voltage polar plate, a first dielectric layer is arranged on the surface of the high-voltage polar plate facing the ground polar plate, and a discharge gap is formed between the catalytic protective layer and the first dielectric layer; the catalytic protective layer is made of any one of a first oxide catalyst group and/or any one of a second oxide catalyst group, and the first oxide catalyst group comprises TiO 2 、WO 3 、MoO 3 ZnO and Fe 2 O 3 The second oxide catalyst group includes Nb 2 O 5 、Nb 2 O 3 、V 2 O 5 、Ta 2 O 5 And Cr (V) 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The preparation method comprises the following steps:
s1, processing a pair of stainless steel substrates according to a designed size, wherein one stainless steel substrate is used as a ground polar plate, and the other stainless steel substrate is used as a substrate of a high-voltage polar plate;
s2, preparing oxide catalyst powder;
s3, preparing a catalytic protective layer on one side surface of the stainless steel substrate of the ground polar plate through a meltallizing process;
s4, plating Al on one side surface of the stainless steel substrate of the high-voltage polar plate 2 O 3 The ceramic layer serves as a first dielectric layer;
s5, arranging the ground electrode plate and the high-voltage electrode plate oppositely, arranging the catalytic protection layer opposite to the first dielectric body layer, and forming a discharge gap between the catalytic protection layer and the first dielectric body layer.
9. The method for producing a nitrogen-free high-concentration ozone generating device according to claim 8, wherein in step S3, the uniform powder is fused to the stainless steel substrate surface of said ground plate to a thickness of 10 to 1000 μm.
10. The preparation method of the nitrogen-free added high-concentration ozone generating device is characterized in that the ozone generating device comprises a ground polar plate and a high-voltage polar plate arranged opposite to the ground polar plate, wherein a catalytic protective layer is arranged on the surface of the ground polar plate facing the high-voltage polar plate, a first dielectric layer is arranged on the surface of the high-voltage polar plate facing the ground polar plate, and a discharge gap is formed between the catalytic protective layer and the first dielectric layer; the catalytic protective layer is made of any one of a first oxide catalyst group and/or any one of a second oxide catalyst group, and the first oxide catalyst group comprises TiO 2 、WO 3 、MoO 3 ZnO and Fe 2 O 3 The second oxide catalyst group includes Nb 2 O 5 、Nb 2 O 3 、V 2 O 5 、Ta 2 O 5 And Cr (V) 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The preparation method comprises the following steps:
s1, processing a pair of stainless steel substrates according to a designed size, wherein one stainless steel substrate is used as a ground electrode plate substrate, and the other stainless steel substrate is used as a substrate of a high-voltage electrode plate;
s2, plating Al on one side surface of the stainless steel substrate of the ground polar plate and the stainless steel substrate of the high-voltage polar plate 2 O 3 A ceramic layer;
s3, preparing oxide catalyst powder, and preparing the powder into slurry;
s4, al of the ground polar plate is printed through a screen printing process 2 O 3 Printing sizing agent on the surface of the ceramic layer, and sintering and curing to obtain a catalytic protective layer;
s5, arranging the ground electrode plate and the high-voltage electrode plate oppositely, arranging the catalytic protection layer opposite to the first dielectric body layer, and forming a discharge gap between the catalytic protection layer and the first dielectric body layer.
11. The method for producing a nitrogen-free added high concentration ozone generating device as claimed in claim 8 or 10, wherein when the oxide catalyst powder is selected from the group consisting of a mixture of a first oxide catalyst and a second oxide catalyst, the powder production method thereof is as follows:
s1.1, mixing 2 oxide catalysts;
s1.2, calcining the mixture at a high temperature;
s1.3, ball milling the materials in the previous step;
s1.4, sieving the ball-milled substances to obtain uniform powder.
12. The method for producing a nitrogen-free high-concentration ozone generating device as claimed in claim 10, wherein the sintering solidification temperature in step S4 is not higher than 500 ℃.
13. The method for producing a nitrogen-free high-concentration ozone generating device as claimed in claim 10, wherein in step S4, the printing thickness of the paste is 1 to 100 μm.
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| CN1774394A (en) * | 2004-02-25 | 2006-05-17 | 东芝三菱电机产业***株式会社 | Ozone generator and ozone generating method |
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| CN107428529A (en) * | 2015-03-18 | 2017-12-01 | 住友精密工业株式会社 | The manufacture method of ozone gas generation device and ozone gas generation device |
| CN108712998A (en) * | 2016-03-25 | 2018-10-26 | 住友精密工业株式会社 | The manufacturing method of ozone gas generating means and ozone gas generating means |
| CN217921491U (en) * | 2022-08-29 | 2022-11-29 | 苏州中世太新能源科技有限公司 | Plate-type ozone generator discharge chamber |
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| CN1774394A (en) * | 2004-02-25 | 2006-05-17 | 东芝三菱电机产业***株式会社 | Ozone generator and ozone generating method |
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