CN102404886B - Full infrared radiation ceramic heater and manufacturing method thereof - Google Patents
Full infrared radiation ceramic heater and manufacturing method thereof Download PDFInfo
- Publication number
- CN102404886B CN102404886B CN201110373573.5A CN201110373573A CN102404886B CN 102404886 B CN102404886 B CN 102404886B CN 201110373573 A CN201110373573 A CN 201110373573A CN 102404886 B CN102404886 B CN 102404886B
- Authority
- CN
- China
- Prior art keywords
- sio
- heating core
- ceramic heating
- sic ceramic
- sic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 100
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 230000005855 radiation Effects 0.000 title claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 79
- 229910016006 MoSi Inorganic materials 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000005507 spraying Methods 0.000 claims abstract description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 63
- 239000013078 crystal Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 238000003723 Smelting Methods 0.000 claims description 12
- 239000011214 refractory ceramic Substances 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 14
- 229910052681 coesite Inorganic materials 0.000 abstract 7
- 229910052906 cristobalite Inorganic materials 0.000 abstract 7
- 239000000377 silicon dioxide Substances 0.000 abstract 7
- 235000012239 silicon dioxide Nutrition 0.000 abstract 7
- 229910052682 stishovite Inorganic materials 0.000 abstract 7
- 229910052905 tridymite Inorganic materials 0.000 abstract 7
- 241001062472 Stokellia anisodon Species 0.000 abstract 1
- 230000002950 deficient Effects 0.000 abstract 1
- 230000001678 irradiating effect Effects 0.000 abstract 1
- 230000000630 rising effect Effects 0.000 abstract 1
- 230000007547 defect Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Landscapes
- Resistance Heating (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a full infrared radiation ceramic heater and a manufacturing method thereof. The full infrared radiation ceramic heater comprises a SiC ceramic heating core; and a SiO2 glass layer with the thickness of 200 to 600 micrometers is attached to the inner surface as well as the outer surface of the SiC ceramic heating core. The manufacturing method comprises the steps as follows: irradiating the inner and the outer surfaces of the SiC ceramic heating core with laser beams; spraying a MoSi layer on the inner surface as well as the outer surface of the SiC ceramic heating core; placing the SiC ceramic heating core in a drying oven for drying; powering on and heating to form SiO2 substrate; immersing the SiC ceramic heating core in SiO2 smelt and then taking out to form rudiment of the SiO2 glass layers; and reducing the temperature to ordinary temperature. The invention has the advantages that the thicknesses of the SiO2 glass layers in the ceramic heater can be reduced effectively, the temperature rising speed of the ceramic heater can be improved, the manufacturing process is simple and convenient and is easy to operate, the production efficiency is high, the bonding strength of the SiO2 glass layers and the ceramic heating core is strong, so that the SiO2 glass layers can not drop off, the service life is long, the defective percentage is low during production, and the manufacturing cost can be reduced for enterprises advantageously.
Description
Technical field
The present invention relates to ceramic heater, specifically a kind of full infrared radiation ceramic heater and preparation method thereof.
Background technology
People, need be at SiC plane of crystal growth SiO when using SiC crystal to make heater at present
2siC crystal is protected, improved the oxidation resistance of heater, increase the service life.The manufacture method of existing ceramic heater is that the heating core that SiC crystal is made is encapsulated in double-deck SiO
2in glass tube, and by welding manner, the two is fixedly connected with.The ceramic heater that the method is made can be realized water power isolation effect, and the infrared radiation that SiC crystal produces can pass SiO smoothly
2glass.The heat that SiC crystal sends needs elder generation and SiO
2glass tube carries out heat exchange, then by SiO
2glass tube by dissipation of heat out, so SiO
2the thickness of glass tube has determined the speed that ceramic heater heats up, due to double-deck SiO
2glass tube at least needs SiO while making under prior art condition
2glassy layer has the thickness of 1mm, and therefore current existing ceramic heater all exists the fast not shortcoming of programming rate.In addition, in the manufacture method of existing ceramic heater, the encapsulation of heating core and welding process complex steps, operation easier is larger, and production efficiency is lower, SiO
2the bonding strength of glassy layer and ceramic heating core is lower, SiO after long-time use
2glassy layer easily comes off, and useful life is shorter, and defect rate during production is more than 5%, and the production cost of enterprise is higher.
Summary of the invention
The object of this invention is to provide a kind of full infrared radiation ceramic heater and preparation method thereof, it can effectively reduce SiO in ceramic heater
2the thickness of glassy layer, the programming rate of raising ceramic heater, and the course of processing is easy, easy operating, and production efficiency is high, SiO
2the bonding strength of glassy layer and ceramic heating core is high, SiO
2glassy layer can not come off, long service life, and defect rate during production is low, is conducive to enterprise and reduces production costs.
The present invention for achieving the above object, is achieved through the following technical solutions: comprise SiC ceramic heating core, SiC ceramic heating core surfaces externally and internally is all attached with SiO
2glassy layer, SiO
2the thickness of glassy layer is 200-600 μ m.
The manufacture method of full infrared radiation ceramic heater, comprises the steps:
1. with SiC crystal, make ceramic heating core;
2. with power, be 1-1.3KW, power density is 35-45 * 10
5w/cm
3laser beam with the process velocity of 30mm/ second, irradiate SiC ceramic heating core surfaces externally and internally, make that SiC ceramic heating core surfaces externally and internally is smooth, uniformity;
3. the SiC ceramic heating core surfaces externally and internally after laser cleaning sprays the thick MoSi layer of 50-100 μ m;
4. by step 3. in the SiC ceramic heating core of spraying MoSi layer be placed in drying oven, in the temperature of 180-200 ℃, dry 1.9-2.1 hour, obtain the SiC ceramic heating core with MoSi layer;
5. the SiC ceramic heating core with MoSi layer is switched under normal temperature in air, make SiC crystal heating to 1680-1750 ℃, and keep energising 5 minutes, make MoSi and the airborne O of SiC ceramic heating core surfaces externally and internally
2reaction generates SiO
2, SiO
2be grown in SiC ceramic heating core surfaces externally and internally, form SiO
2compact film, obtains SiO at SiC ceramic heating core surfaces externally and internally
2substrate;
6. by surfaces externally and internally with SiO
2the SiC ceramic heating core of substrate is inserted SiO
2in smelting furnace, SiO
2the neon of logical 0.01MPa in smelting furnace, SiO
2in smelting furnace and the SiO of 1600 ℃ is housed
2fused mass, will be with SiO
2the SiC ceramic heating core of substrate immerses the SiO of 1600 ℃
2in fused mass, keep taking out after 5 minutes, be cooled to 1460 ℃, make SiO
2siO in smelting furnace
2molecular link gathers in substrate, forms SiO
2glassy layer blank;
7. by 1460 ℃ with SiO
2the SiC ceramic heating core of glassy layer blank moves in deshydroxy stove, is progressively cooled to normal temperature, obtains the SiO that thickness is 200-600 μ m on SiC ceramic heating core surfaces externally and internally
2glassy layer.
Before 3. step sprays MoSi material powder, in the position of SiC ceramic heating core connecting electrode, refractory ceramics sleeve pipe is installed.
The invention has the advantages that: SiO
2the thickness of glassy layer reduces for comparing with existing product significantly, can effectively improve the programming rate of ceramic heater, and it is only existing SiO on the market that temperature rises to the peak time used
2/ 3rd of a full infrared radiation ceramic heater product of glassy layer the thinnest (being about 1mm); During making, do not need heating core and SiO
2glass encapsulates and welds, but allows SiO
2glassy layer is grown directly upon SiC ceramic heating core surfaces externally and internally, can effectively reduce SiO in ceramic heater
2the thickness of glassy layer has been simplified production method simultaneously, and the more existing technique of production efficiency has improved 5 times of left and right, has reduced operation easier, SiO
2the bonding strength of glassy layer and ceramic heating core is high, SiO
2glassy layer can not come off, and experiment shows than prior art, to extend 1.9 times of left and right its useful life, and in production, the defect rate of product, lower than 1 ‰, is conducive to enterprise and reduces production costs.
Accompanying drawing explanation
Fig. 1 is the structural representation of ceramic heater of the present invention.
Embodiment
Full infrared radiation ceramic heater of the present invention, comprises SiC ceramic heating core 1, and SiC ceramic heating core 1 surfaces externally and internally is all attached with SiO
2 glassy layer 2, SiO
2the thickness of glassy layer 2 is 200-600 μ m.Ceramic heater of the present invention is compared with existing product, SiO
2the thickness of glassy layer significantly reduces, and can effectively improve the programming rate of ceramic heater.It is only existing SiO on the market that full infrared radiation ceramic heater temperature of the present invention rises to the peak time used
2/ 3rd of a full infrared radiation ceramic heater product of glassy layer the thinnest (being about 1mm).
The manufacture method of full infrared radiation ceramic heater of the present invention comprises the steps:
1. with SiC crystal, make ceramic heating core;
2. with power, be 1-1.3KW, power density is 35-45 * 10
5w/cm
3laser beam with the process velocity of 30mm/ second, irradiate SiC ceramic heating core surfaces externally and internally, make that SiC ceramic heating core surfaces externally and internally is smooth, uniformity;
3. the SiC ceramic heating core surfaces externally and internally after laser cleaning sprays the thick MoSi layer of 50-100 μ m;
4. by step 3. in the SiC ceramic heating core of spraying MoSi layer be placed in drying oven, in the temperature of 180-200 ℃, dry 1.9-2.1 hour, obtain the SiC ceramic heating core with MoSi layer;
5. the SiC ceramic heating core with MoSi layer is switched under normal temperature in air, make SiC crystal heating to 1680-1750 ℃, and keep energising 5 minutes, make MoSi and the airborne O of SiC ceramic heating core surfaces externally and internally
2reaction generates SiO
2, SiO
2be grown in SiC ceramic heating core surfaces externally and internally, form SiO
2compact film, obtains SiO at SiC ceramic heating core surfaces externally and internally
2substrate;
6. by surfaces externally and internally with SiO
2the SiC ceramic heating core of substrate is inserted SiO
2in smelting furnace, SiO
2the neon of logical 0.01MPa in smelting furnace, SiO
2in smelting furnace and the SiO of 1600 ℃ is housed
2fused mass, will be with SiO
2the SiC ceramic heating core of substrate immerses the SiO of 1600 ℃
2in fused mass, keep taking out after 5 minutes, be cooled to 1460 ℃, make SiO
2siO in smelting furnace
2molecular link gathers in substrate, forms SiO
2glassy layer blank;
7. by 1460 ℃ with SiO
2the SiC ceramic heating core of glassy layer blank moves in deshydroxy stove, is progressively cooled to normal temperature, obtains the SiO that thickness is 200-600 μ m on SiC ceramic heating core surfaces externally and internally
2glassy layer.
The laser power of step in is 2. preferably 1.2KW, and power density is preferably 40 * 10
5w/cm
3, SiC ceramic heating core surfaces externally and internally is heated to the temperature that just can make SiC crystal melting, cooling immediately after SiC crystal melting, make SiC ceramic heating core smooth surface, uniformity.Step 3. in the thickness of MoSi layer can follow according to actual conditions and adjust within the scope of 50-100 μ m, the thickness of MoSi layer can be guaranteed when MoSi layer is dried can not come off within the scope of this time, wherein the preferred thickness of MoSi layer is 75 μ m.The bake out temperature of step in is 4. preferably 190 ℃, drying time is preferably 2 hours, and the actual effect during according to oven dry can suitably be adjusted bake out temperature within the scope of 180-200 ℃, and drying time is 1.9-2.1 hour, if exceed this scope, can to cause MoSi layer to adhere to insecure, easily comes off.The step SiO that 5. middle SiC crystal heating to 1680 ℃ can make SiC ceramic heating core surfaces externally and internally generate above
2melting, the uniform SiO of cooling rear formation
2compact film, but SiC crystal heating temperature should be higher than 1750 ℃, if higher than this temperature, SiO
2the mobility of compact film is too high, causes SiO
2compact film uneven thickness, affects SiO
2the quality of substrate, wherein the preferred temperature of SiC crystal heating is 1710 ℃, SiO at this temperature
2the state of fused mass can form the SiO that the uniformity is the highest
2compact film.1460 ℃ described in 6. of step are SiO
2the critical temperature that glass is started to solidify by liquid state, i.e. SiO
2after glass starts to solidify, then will be with SiO
2the SiC ceramic heating core of glassy layer moves to deshydroxy descent of temperature.Step 7. will be with SiO
2the SiC ceramic heating core of glassy layer blank moves in deshydroxy stove progressively lowers the temperature and can eliminate residual stress.This manufacture method does not need heating core and SiO
2glass encapsulates and welds, but allows SiO
2glassy layer is grown directly upon SiC ceramic heating core surfaces externally and internally, can effectively reduce SiO in ceramic heater
2the thickness of glassy layer, makes SiO
2the thickness of glassy layer is only 200-600 μ m, can improve the programming rate of ceramic heater, has simplified production method simultaneously, and production efficiency has improved 5 times of left and right than existing methods, has reduced operation easier, SiO
2the bonding strength of glassy layer and ceramic heating core is high, SiO
2glassy layer can not come off, and experiment shows than prior art, to extend 1.9 times of left and right its useful life, and in production, the defect rate of product, lower than 1 ‰, is conducive to enterprise and reduces production costs.
In the manufacture method of full infrared radiation ceramic heater of the present invention, for reserved electrode link position on SiC ceramic heating core, can before 3. step sprays MoSi material powder, in the position of SiC ceramic heating core connecting electrode, refractory ceramics sleeve pipe be installed.Refractory ceramics sleeve pipe is by ZrO
2, Al
2o
3deng high temperature ceramic material, make, its fusing point is higher than 2000 ℃, can stop that MoSi material powder is attached to the ，Shi Gai position, position that refractory ceramics sleeve pipe is installed and can generate SiO during spraying MoSi material powder
2glassy layer, after 7. step lowers the temperature, takes off refractory ceramics sleeve pipe.
Claims (2)
1. the manufacture method of full infrared radiation ceramic heater, is characterized in that: comprise the steps:
1. with SiC crystal, make ceramic heating core;
2. with power, be 1-1.3KW, power density is 35-45 * 10
5w/cm
3laser beam with the process velocity of 30mm/ second, irradiate SiC ceramic heating core surfaces externally and internally, make that SiC ceramic heating core surfaces externally and internally is smooth, uniformity;
3. the SiC ceramic heating core surfaces externally and internally after laser cleaning sprays the thick MoSi layer of 50-100 μ m;
4. by step 3. in the SiC ceramic heating core of spraying MoSi layer be placed in drying oven, in the temperature of 180-200 ℃, dry 1.9-2.1 hour, obtain the SiC ceramic heating core with MoSi layer;
5. the SiC ceramic heating core with MoSi layer is switched under normal temperature in air, make SiC crystal heating to 1680-1750 ℃, and keep energising 5 minutes, make MoSi and the airborne O of SiC ceramic heating core surfaces externally and internally
2reaction generates SiO
2, SiO
2be wrapped in SiC ceramic heating core surfaces externally and internally, form SiO
2compact film, obtains SiO at SiC ceramic heating core surfaces externally and internally
2substrate;
6. by surfaces externally and internally with SiO
2the SiC ceramic heating core of substrate is inserted SiO
2in smelting furnace, SiO
2the neon of logical 0.01Mpa in smelting furnace, SiO
2in smelting furnace and the SiO of 1600 ℃ is housed
2fused mass, will be with SiO
2the SiC ceramic heating core of substrate immerses the SiO of 1600 ℃
2in fused mass, keep taking out after 5 minutes, be cooled to 1460 ℃, make SiO
2siO in smelting furnace
2molecular link gathers in substrate, forms SiO
2glassy layer blank;
7. by 1460 ℃ with SiO
2the SiC ceramic heating core of glassy layer blank moves in deshydroxy stove, is progressively cooled to normal temperature, obtains the SiO that thickness is 200-600 μ m on SiC ceramic heating core surfaces externally and internally
2glassy layer.
2. the manufacture method of full infrared radiation ceramic heater according to claim 1, is characterized in that: before 3. step sprays MoSi material powder, in the position of SiC ceramic heating core connecting electrode, refractory ceramics sleeve pipe is installed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110373573.5A CN102404886B (en) | 2011-11-22 | 2011-11-22 | Full infrared radiation ceramic heater and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110373573.5A CN102404886B (en) | 2011-11-22 | 2011-11-22 | Full infrared radiation ceramic heater and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102404886A CN102404886A (en) | 2012-04-04 |
| CN102404886B true CN102404886B (en) | 2014-01-15 |
Family
ID=45886536
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110373573.5A Expired - Fee Related CN102404886B (en) | 2011-11-22 | 2011-11-22 | Full infrared radiation ceramic heater and manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102404886B (en) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19614676C2 (en) * | 1996-04-13 | 1998-09-03 | Choe Kum Chol | Process for refining SiC heating rods |
| JP4534620B2 (en) * | 2004-06-22 | 2010-09-01 | パナソニック電工株式会社 | Infrared radiation element |
| CN201352860Y (en) * | 2009-02-13 | 2009-11-25 | 周存文 | Infrared radiation ceramic heater |
-
2011
- 2011-11-22 CN CN201110373573.5A patent/CN102404886B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102404886A (en) | 2012-04-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5993514B2 (en) | Low pressure and vacuum glass that is hermetically sealed by frame and recess | |
| JP5137362B2 (en) | Structure comprising a metal substrate and an inorganic material surface layer | |
| TWI442810B (en) | Frit-sealed device | |
| US20090151848A1 (en) | Method for bonding components made of high silica material | |
| JP4426442B2 (en) | Method for producing a hermetic and heat-resistant bond of molded parts made of non-oxide ceramics using a laser | |
| US20060046075A1 (en) | Method for bonding components made of material with a high silicic acid content, and assembly composed of such components | |
| CN104838079A (en) | Low temperature hermetic sealing via laser | |
| JPH10321921A (en) | Thermoelectric conversion module and its manufacture | |
| CN108640522A (en) | A kind of devitrified glass solder and the method using solder welding porous silicon nitride and compact silicon nitride | |
| US20080012109A1 (en) | Method for the packaging of optical or optoelectronic components, and optical or optoelectronic package element producible according to the method | |
| CN105017936A (en) | Infrared reflection heat preservation coating for crystalline silicon furnace, preparation technology and application | |
| CN102404886B (en) | Full infrared radiation ceramic heater and manufacturing method thereof | |
| CN103936268B (en) | High temp glass cup weldprocedure | |
| JP2011088776A (en) | Composite crucible and method for manufacturing the same | |
| CN106271188A (en) | A kind of titanium cup Special vacuum solder and processing method thereof and soldering processes | |
| JP5467653B2 (en) | Glass polygonal tube, manufacturing method thereof and container | |
| CN102701743B (en) | Production process for heating ceramic cores of infrared-radiation heaters | |
| CN100549216C (en) | Crystal qualitative SiO 2-Al 2O 3The preparation method of mixed oxide deposition material | |
| CN109863826A (en) | Infrared radiator | |
| WO2015078088A1 (en) | Method and device for brazing glass and kovar combination with oxygen-free copper | |
| JP2007530409A (en) | Refractory materials and their uses, and methods of treating refractory materials. | |
| CN111484254B (en) | High-temperature sealing glass and preparation method and application thereof | |
| CN107621166A (en) | A kind of variable-frequency electromagnetic energy non-ferrous metal casting furnace | |
| CN208905560U (en) | On one side with reeded glass magnetic conducting and heating disk | |
| CN204216095U (en) | A kind of laser sintered equipment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: BEIJING DONGFANG QIJING NEW ENERGY TECHNOLOGY DEVE Free format text: FORMER OWNER: ZHOU CUNWEN Effective date: 20140117 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhou Cunwen Inventor after: Zhou Bing Inventor after: Ren Qiyong Inventor before: Zhou Cunwen Inventor before: Zhou Bing |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: ZHOU CUNWEN ZHOU BING TO: ZHOU CUNWEN ZHOU BING REN QIYONG Free format text: CORRECT: ADDRESS; FROM: 250013 JINAN, SHANDONG PROVINCE TO: 100044 HAIDIAN, BEIJING |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20140117 Address after: 100044, Beijing, Three Mile River Road, 11, housing department, South Building 101, Room 102 Patentee after: Beijing Dongfang Qijing New Energy Science & Technology Development Center Address before: 250013 Shandong Province, Lixia District of Ji'nan City No. 1 min Zi Qian Road No. 5 Building 3 unit 101 room Patentee before: Zhou Cunwen |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140115 Termination date: 20171122 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |