CN102998320A - Far infrared material analysis and manufacturing method - Google Patents
Far infrared material analysis and manufacturing method Download PDFInfo
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- CN102998320A CN102998320A CN2012103290312A CN201210329031A CN102998320A CN 102998320 A CN102998320 A CN 102998320A CN 2012103290312 A CN2012103290312 A CN 2012103290312A CN 201210329031 A CN201210329031 A CN 201210329031A CN 102998320 A CN102998320 A CN 102998320A
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- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000004458 analytical method Methods 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052613 tourmaline Inorganic materials 0.000 claims abstract description 60
- 229940070527 tourmaline Drugs 0.000 claims abstract description 60
- 239000011032 tourmaline Substances 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims description 36
- 238000002425 crystallisation Methods 0.000 claims description 24
- 230000008025 crystallization Effects 0.000 claims description 21
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 claims description 14
- 238000002441 X-ray diffraction Methods 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 238000000441 X-ray spectroscopy Methods 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 229910052863 mullite Inorganic materials 0.000 abstract description 22
- 238000001228 spectrum Methods 0.000 abstract 1
- 238000007669 thermal treatment Methods 0.000 description 14
- 229910052500 inorganic mineral Inorganic materials 0.000 description 13
- 239000011707 mineral Substances 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 description 5
- 208000035126 Facies Diseases 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910002552 Fe K Inorganic materials 0.000 description 3
- 229910003110 Mg K Inorganic materials 0.000 description 3
- 229910003251 Na K Inorganic materials 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 229910002703 Al K Inorganic materials 0.000 description 2
- -1 AlO2 Inorganic materials 0.000 description 2
- 229910002794 Si K Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910000144 sodium(I) superoxide Inorganic materials 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Analysing Materials By The Use Of Radiation (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a method for analyzing and manufacturing a far infrared material, which comprises the following steps: A. heating tourmaline to the working temperature at which mullite crystal phase appears; B. obtaining an observation section on the tourmaline; C. separating a mullite structure region from a non-mullite structure region on the observation section; D. detecting the X-ray energy spectrum of the non-mullite structural region to confirm the content of the components in the non-mullite structural region; E. carrying out crystal phase analysis on the observation section to obtain crystal phase information of a non-mullite structure region; F. according to the obtained information of the components and the crystal phase of the non-mullite structural region, the information is used as reference information for preparing the far infrared material; the manufacturing method comprises selecting the corresponding components, and heating the components to the crystal phase corresponding to step E to obtain a far infrared material.
Description
Technical field
The invention relates to a kind of far-infrared ray material analysis and manufacture method, particularly pointer is analyzed tourmaline thermal property and crystalline phase, just can understand the mineral composition that can improve far infrared irradiation efficient in the tourmaline, make a far-infrared ray material so as to utilizing these mineral compositions.
Background technology
The present manufacture method of general common far-infrared composition, such as No. 200844066 " manufacture method of far-infrared composition and goods thereof " Patent Case of TaiWan, China disclosed invention on November 16 in 2008, its exposure: with the high temperature sintering far-infrared ray material, and grind to form little/how behind the prescription of meter level, make this prescription be attached to a base material, make goods.Include SiO2, AlO2, NaO2, K2O, the MgO that cooperates this product-use to determine ratio owing to this far-infrared ray material, therefore, the difference that can cooperate various base materials, make vessel, fabric, film, paint, ceramic tile, fuel (gasoline, diesel oil, gas ... etc.), the exciting device of water ... wait goods, make this particular product utilize aforementioned formula characteristic and little/how riceization is active (little/Mi Xiaoying how, be that specific surface area increases), significantly promote releasing far infrared and effect negative ion.
Far-infrared composition manufacture method and the goods thereof of case before this patent, can can radiate at normal temperatures high-quality far infrared effective energy, but it does not disclose the far-infrared ray material that can utilize the tourmaline natural minerals to prepare high emissivity, and tourmaline is of a great variety, at present also without can accurately testing out the method that can radiate the far infrared composition, therefore, still have in the use many shortcomings.
Summary of the invention
Hence this has above-mentioned shortcoming because test at present the far infrared compositions, method, so the invention provides a kind of far-infrared ray material analysis and manufacture method, include: A. is heated to the working temperature that the Mullite-Crystallization phase occurs to a tourmaline; B. obtain one at this tourmaline and observe section; C. separate out mullite structure zone and non-mullite structure zone at this observation section; D. detect the x-ray spectroscopy in this non-mullite structure zone, to confirm the contained composition content in this non-mullite structure zone; E. this observation section is carried out the crystallization phase analysis, obtain the crystallization phase information in non-mullite structure zone; F. the non-mullite structure zone that is obtained according to step D and step e composition and crystallization phase information, as the reference information of allotment far-infrared ray material.
The working temperature system of above-mentioned steps A is between 1000 ℃ to 1600 ℃.
Above-mentioned steps B obtains this observation section to tourmaline execution cutting or/and lapping mode after this heating.
Above-mentioned steps C sees through an electron microscope, separates out mullite structure zone and non-mullite structure zone according to crystal form on the observation section of this tourmaline.
Above-mentioned steps D sees through the contained composition content that an energy dispersive spectroscopy instrument (EDS) is confirmed non-mullite structure zone.
Above-mentioned steps E sees through the crystallization phase that an X-ray diffraction analysis method (XRD) is confirmed this non-mullite structure zone.
The present invention also can be a kind of far-infrared ray material manufacture method, is to select the composition that is consistent according to the step D of above-mentioned far-infrared ray material analytical approach, again this composition is heated to the crystallization phase that meets step e, to make a far-infrared ray material.
The advantage that the present invention can reach is to analyze in the base material in non-mullite structure zone fast and simply for different tourmaline, has composition and the crystallization of high emissivity far infrared, so as to can be used as the usefulness of making high emissivity far-infrared ray material.
Description of drawings
Fig. 1 is operation steps process flow diagram of the present invention,
Fig. 2 is that tourmaline thermal property of the present invention is analyzed synoptic diagram,
Fig. 3 be tourmaline of the present invention through the far infrared irradiation rate of heat treatments at different,
Fig. 4 be tourmaline of the present invention with the XRD analysis synoptic diagram of heat treatments at different,
Fig. 5 is the microstructure metallograph of the former observation section of tourmaline of the present invention,
Fig. 6 is tourmaline of the present invention is observed section after 850 ℃ of thermal treatment microstructure metallograph,
Fig. 7 is tourmaline of the present invention is observed section after 950 ℃ of thermal treatment microstructure metallograph,
Fig. 8 is tourmaline of the present invention is observed section after 1000 ℃ of thermal treatment microstructure metallograph,
Fig. 9 is the local clump shape mat gold phasor that tourmaline of the present invention produces in the microstructure of observing section after 1450 ℃ of thermal treatment,
Figure 10 is the hole metallograph that tourmaline of the present invention produces in the microstructure of observing section after 1450 ℃ of thermal treatment,
Figure 11 is the complete acicular mullite metallograph that tourmaline of the present invention produces in the microstructure of observing section after 1450 ℃ of thermal treatment,
Figure 12 be tourmaline of the present invention after 1450 ℃ of thermal treatment, acicular mullite is carried out the analysis of components metallograph of EDS,
Figure 13 is the EDS analysis of components metallograph of mullite periphery base material in the tourmaline of the present invention,
Figure 14 is that the XRD mineral facies of base material in the tourmaline of the present invention are analyzed synoptic diagram,
Table one for tourmaline of the present invention through EDS analysis of components data,
Table two is the data of tourmaline of the present invention EDS analysis of components of acicular mullite after 1450 ℃ of thermal treatment,
Table three is the base material constituent data of tourmaline of the present invention after 1450 ° of C thermal treatment.
Embodiment
At first, see also shown in Figure 1ly, the present invention is a kind of far-infrared ray material analytical approach, includes the following step:
A. a tourmaline is heated to the working temperature that the Mullite-Crystallization phase occurs: it is the processing of heating for a tourmaline, make its working temperature system between 1000 ℃ to 1600 ℃, carry out the thermal property analysis after this tourmaline heating, as shown in Figure 2, about 900 ℃ to 1000 ℃, the obvious loss in weight and themopositive reaction are arranged, and also demonstrate for its analysis (as shown in Figure 3) of carrying out the far infrared irradiation rate, far infrared irradiation rate mean value is since 500 ℃ of phenomenons that enhancing is arranged, after slightly reducing to 0.955 to 950 ℃, along with the raising of heat treatment temperature, the far infrared irradiation rate can continue to improve; Because the phenomenon that its far infrared irradiation rate of tourmaline of process high temperature sintering is improved so can learn tourmaline transformation structurally, is the factor that far infrared radioactivity can strengthen; Therefore, analyze for thermal property and the crystalline phase of tourmaline especially, just can understand the transformation of tourmaline crystalline phase and the reason that radiological performance improves, again with reference to shown in Figure 4, tourmaline is after various temperature are heat-treated, when being warming up to 850 ° of C, the structure of tourmaline is without too large transformation, and after heat treatment temperature is increased to 1000 ° of C, then begins to produce the mullite mineral facies, raising along with heat treatment temperature, the phenomenon that the crystalline phase intensity of mullite is improved, and contrast far infrared irradiation rate shown in Figure 3, the higher person of heat treatment temperature, the emissivity of far infrared is higher, and therefore provable generation with mullite is relevant;
B. obtain one at this tourmaline and observe section: for the tourmaline after this heating, carry out a cutting or/with lapping mode, so as on this tourmaline, obtaining an observation section;
C. separate out mullite structure zone and non-mullite structure zone at this observation section: see through an electron microscope (SEM), observation section for this tourmaline is observed, exist the crystallization (as shown in Figure 5) that many sizes are about 0.5 μ m in the tourmaline, can grow into the crystallization (as shown in Figure 6) of the about 2 μ m of size via crystal grain after 850 ℃ of thermal treatments, tourmaline is after 950 ℃ of thermal treatment, it begins to crack for structure, broken-out section can also pick out the structure of mineral on the whole, and the crystal grain (as shown in Figure 7) that has a little, after 1000 ℃ of thermal treatments, crystal grain is complete obiteration, and there is serious lines to produce (as shown in Figure 8), tourmaline is after 1450 ℃ thermal treatment, can produce local clump shape crystallization (as shown in Figure 9) on the surface, then can obviously observe comparatively complete acicular mullite (such as Figure 10 and the shown in Figure 11) in the part of hole, on the observation section of this tourmaline, separate out mullite structure zone and non-mullite structure zone according to crystal form;
D. detect the x-ray spectroscopy in this non-mullite structure zone, to confirm the contained composition content in this non-mullite structure zone: elder generation is for the observation section of this tourmaline, see through an energy dispersive spectroscopy instrument (EDS) and confirm that this tourmaline has the contained composition content in mullite structure zone, as shown in table 1 is the EDS analysis of components of tourmaline, wherein the content of Al2O3 is 35.92%, the content of SiO2 is 39.17%, be illustrated in figure 9 as tourmaline after 1450 ° of C thermal treatment, with EDS the acicular crystal that tourmaline was produced is carried out analysis of components, the content of Al2O3 rises to 43.25 %, the SiO2 content is 30.07 % (as shown in table 2)
The variation ratio that Al2O3 and SiO2 produce in its composition changes 1:0.7 into from 1:1.09, and the typical case of mullite form in the ratio of Al2O3 and SiO2 be 1:0.6, after heat treatment, composition levels off to mullite (Mullite), therefore the deducibility tourmaline after heat treatment, its acicular crystal should be mullite, because mullite is not far-infrared emitter, infer that the far infrared irradiation source should be the base material beyond the mullite, the zone of non-mullite structure will have been separated out in the tourmaline, see through the contained composition content of base material (such as Figure 10 and shown in Figure 11) that this energy dispersive spectroscopy instrument (EDS) is confirmed non-mullite structure zone, found that in this base material composition to be without the composition (as shown in Table 3) of Al2O3 and SiO2.
| Element | Content (%) | Mineral composition |
| Na K | 1.73 | Na 2O |
| Mg K | 2.92 | MgO |
| Al K | 35.92 | Al 2O 3 |
| Si K | 39.17 | SiO 2 |
| Fe K | 16.72 | FeO |
| Cu K | 2.04 | CuO |
| Zn K | 1.49 | ZnO |
Table one
| Element | Content (%) | Mineral composition |
| Na K | 1.09 | Na 2O |
| Mg K | 3.03 | MgO |
| Al K | 43.25 | Al 2O 3 |
| Si K | 30.07 | SiO 2 |
| Fe K | 22.56 | FeO |
Table two
| Element | Content (%) | Mineral composition |
| Na K | 9.93 | Na 2O |
| Mg K | 35.89 | MgO |
| Fe K | 54.18 | FeO |
Table three
E. this observation section is carried out the crystallization phase analysis, obtain the crystallization phase information in non-mullite structure zone: see through again the crystallization phase that an X-ray diffraction analysis method (XRD) is confirmed this non-mullite structure zone, diffraction analysis via XRD, and with analyse and compare out the mineral facies magnesioferrite (Magnesioferrite) (such as Figure 12 and shown in Figure 13) of this base material of picture library, also show mullite phase (as shown in figure 14) in the analysis of the XRD of 1450 ° of C mineral facies, therefore the deducibility tourmaline after heat treatment, its acicular crystal should be mullite, because the temperature that tourmaline is heat-treated is higher, then the crystal grain of mullite and structure are more complete, relative Mg, Fe, the concentration of the oxide of Na also produces change because of separating out of mullite, because mullite is not the emitter of far infrared, therefore can learn the Mg in the tourmaline, the Na of Fe and trace is the main cause of far infrared irradiation rate raising, so as to the relevant information of crystallization phase that obtains non-mullite structure zone;
F. the non-mullite structure zone that obtains according to step D and step e composition and crystallization phase information, reference information as the allotment far-infrared ray material: determine via above-mentioned steps D and step e, the composition in non-mullite structure zone and crystallization are the Na of Mg, Fe and trace in the tourmaline, so can be for the experimental data analyzed of tourmaline after the heating, utilize Mg, Fe and micro-Na with these data, carry out the composition allotment of high emissivity far-infrared ray material.
The present invention also can be a kind of far-infrared ray material manufacture method, it is according to above-mentioned far-infrared ray material analytical approach, obtain to have the mineralogical composition data of high emissivity far-infrared ray material, the Na that namely includes Mg, Fe and trace, then select wherein this composition that is consistent of the mineral composition be consistent with it, comprise magnesium 31-41%, iron 49-59% and sodium 6-13%, again this mineral composition is heated to and meets the identical crystallization phase of base material that has high emissivity far-infrared ray material in the step e, so as to the material with far infrared radiation function that can complete.
Only; the above only is one of them most preferred embodiment of the present invention; when the patent protection scope that can not limit with this present invention; such as the simple equivalence of doing according to the present invention's claim and description changes and replaces, and all should still belong in the scope of the present patent application protection that claim is contained.
Claims (8)
1. a far-infrared ray material analytical approach comprises the following steps:
A. a tourmaline is heated to and Mullite-Crystallization phase working temperature occurs;
B. obtain one at this tourmaline and observe section;
C. separate out mullite structure zone and non-mullite structure zone at this observation section;
D. detect the x-ray spectroscopy in this non-mullite structure zone, to confirm the contained composition content in this non-mullite structure zone;
E. this observation section is carried out the crystallization phase analysis, obtain the crystallization phase information in non-mullite structure zone;
F. obtain composition and the crystallization phase information in non-mullite structure zone according to step D and step e, as the reference information of allotment far-infrared ray material.
2. far-infrared ray material analytical approach as claimed in claim 1, it is characterized in that: the working temperature system of steps A is between 1000 ℃ to 1600 ℃.
3. far-infrared ray material analytical approach as claimed in claim 1 is characterized in that: step B carries out cutting or/and lapping mode obtains this observation section to the tourmaline after this heating.
4. far-infrared ray material analytical approach as claimed in claim 1, it is characterized in that: step C sees through an electron microscope, separates out mullite structure zone and non-mullite structure zone according to crystal form on the observation section of this tourmaline.
5. far-infrared ray material analytical approach as claimed in claim 1, it is characterized in that: step D sees through the contained composition content that an energy dispersive spectroscopy instrument (EDS) is confirmed non-mullite structure zone.
6. far-infrared ray material analytical approach as claimed in claim 1, it is characterized in that: step e is to see through the crystallization phase that an X-ray diffraction analysis method (XRD) is confirmed this non-mullite structure zone.
7. far-infrared ray material manufacture method is that the step D of according to claim 1 described far-infrared ray material analytical approach selects the composition that is consistent, again this composition is heated to the crystallization phase that meets step e, to make a far-infrared ray material.
8. far-infrared ray material manufacture method as claimed in claim 7, it is characterized in that: this composition that is consistent is to comprise magnesium 31-41%, iron 49-59% and sodium 6-13%.
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| TW100132570 | 2011-09-09 | ||
| TW100132570A TWI507686B (en) | 2011-09-09 | 2011-09-09 | Analysis and Manufacturing Method of Far Infrared Materials |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58151380A (en) * | 1982-03-05 | 1983-09-08 | 旭硝子株式会社 | Far infrared ray radiator and manufacture |
| JPH1046426A (en) * | 1996-07-26 | 1998-02-17 | Brother Ind Ltd | Fiber |
| CN1271758A (en) * | 2000-05-18 | 2000-11-01 | 上海维安热电材料有限公司 | Additive of efficient far infrared powder and its preparing process |
| CN101023793A (en) * | 2005-11-19 | 2007-08-29 | 丛繁滋 | Food, medicine preparation with far-infrared health-care function and assitant therapy functions and their preparing method |
-
2011
- 2011-09-09 TW TW100132570A patent/TWI507686B/en active
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2012
- 2012-09-07 CN CN2012103290312A patent/CN102998320A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58151380A (en) * | 1982-03-05 | 1983-09-08 | 旭硝子株式会社 | Far infrared ray radiator and manufacture |
| JPH1046426A (en) * | 1996-07-26 | 1998-02-17 | Brother Ind Ltd | Fiber |
| CN1271758A (en) * | 2000-05-18 | 2000-11-01 | 上海维安热电材料有限公司 | Additive of efficient far infrared powder and its preparing process |
| CN101023793A (en) * | 2005-11-19 | 2007-08-29 | 丛繁滋 | Food, medicine preparation with far-infrared health-care function and assitant therapy functions and their preparing method |
Non-Patent Citations (1)
| Title |
|---|
| 陈俊良 等: "电气石之相变化与热分解产物之远红外线放射率研究", 《远东学报》, vol. 27, no. 2, 30 June 2010 (2010-06-30), pages 183 - 191 * |
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| TWI507686B (en) | 2015-11-11 |
| TW201312111A (en) | 2013-03-16 |
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Inventor after: Chen Zhicheng Inventor after: Zhong Mingji Inventor after: Chen Junliang Inventor after: Liao Jianhong Inventor after: Huang Yafeng Inventor after: Yang Shixian Inventor before: Chen Zhicheng Inventor before: Liao Jianhong |
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Free format text: CORRECT: INVENTOR; FROM: CHEN ZHICHENG LIAO JIANHONG TO: CHEN ZHICHENG ZHONG MINGJI CHEN JUNLIANG LIAO JIANHONG HUANG YA YANG SHIXIAN |
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Application publication date: 20130327 |