CN103787288B - A kind of preparation method of boron nitride alkene nanometer sheet - Google Patents
A kind of preparation method of boron nitride alkene nanometer sheet Download PDFInfo
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- CN103787288B CN103787288B CN201410029564.8A CN201410029564A CN103787288B CN 103787288 B CN103787288 B CN 103787288B CN 201410029564 A CN201410029564 A CN 201410029564A CN 103787288 B CN103787288 B CN 103787288B
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Abstract
The invention discloses a kind of preparation method of boron nitride alkene nanometer sheet, take sodium borohydride as boron source, ammonium sulfate is nitrogenous source, graphene nanometer sheet is template, step is as follows: (1) takes ammonium sulfate, sodium borohydride and graphene nanometer sheet respectively; Ammonium sulfate, sodium borohydride and graphene nanometer sheet are 1.5 ~ 1.67:1:0.13 ~ 0.33 in mass ratio; (2) three kinds of raw materials are mixed in loading reactor, be tamping reactor, put in crucible oven and be heated to 500 ~ 600 DEG C, insulation 10 ~ 16h, stop heating making it cool to room temperature with the furnace; (3) by products therefrom hydrochloric acid cleaning 3 ~ 5 times, then use washed with de-ionized water 3 ~ 5 times, suction filtration is till filtrate is neutrality; (4) by products therefrom at 60 ~ 90 DEG C of dry 5 ~ 8h in loft drier; (5) then dried product is heated to 700 ~ 800 DEG C of oxide treatment in muffle furnace, namely obtains linen boron nitride alkene nanometer sheet.The equipment that the present invention uses is simple and security good, and cost is lower, stable preparation process, and manipulation is simple, and production efficiency is high.
Description
Technical field
The present invention relates to a kind of machine non-metallic material preparation method for material, especially a kind of boron nitride alkene nanometer sheet preparation method.
Background technology
From 2004, the people such as Novoselov and Geim successfully prepared the Graphene only having one deck carbon atom, successfully opened the prelude of the research of two-dimensional material thus.H-BN and graphite have similar structure, and the single-layer silicon nitride boron nanometer sheet therefore equally with two-dirnentional structure also more and more receives the concern of investigator.
Similar to Graphene, single-layer silicon nitride boron nanometer sheet (boron nitride alkene) also has excellent physical properties, good mechanical property, high chemical stability and oxidation-resistance, thermal conductivity is about 2000W/ (m × K), high-clarity (visible region is substantially without absorption).In addition, its band gap width reaches 5.97eV.Research for single-layer silicon nitride boron nanometer sheet performance is at the early-stage, and a lot of performance is also tested.
Boron nitride alkene nanometer sheet is formed by single-layer silicon nitride boron alkene two dimensional structure stacking, and thickness is two dimension nano materials of nanoscale.
At present, the method preparing boron nitride alkene nanometer sheet comprises: mechanically peel method, ultrasonic wave added solvent stripping method, chemical Vapor deposition process, SiC epitaxial growth method etc.Boron nitride alkene nanometer sheet defect prepared by mechanically peel method (such as ball milled) is many, and boron nitride alkene nanometer sheet output prepared by additive method is very little, and the transfer process of boron nitride alkene nanometer sheet is complicated.
Summary of the invention
The object of the invention is for overcoming above-mentioned the deficiencies in the prior art, provide a kind of preparation method of boron nitride alkene nanometer sheet, the method does not use catalyzer, and cost is lower, and manipulation is simple, and raw amount is high, good product performance.
For achieving the above object, the present invention adopts following technical proposals:
A preparation method for boron nitride alkene nanometer sheet, it take sodium borohydride as boron source, ammonium sulfate is nitrogenous source, graphene nanometer sheet is template, and concrete steps are as follows:
(1) ammonium sulfate, sodium borohydride and graphene nanometer sheet is taken respectively; Wherein, ammonium sulfate, sodium borohydride and graphene nanometer sheet are 1.5 ~ 1.67:1:0.13 ~ 0.33 in mass ratio;
(2) three kinds of raw materials in step (1) are mixed in loading reactor, be tamping reactor, put in crucible oven and be heated to 500 ~ 600 ° of C, insulation 10 ~ 16h, stop heating making it cool to room temperature with the furnace;
(3) step (2) is reacted products therefrom hydrochloric acid cleaning 3 ~ 5 times, then use washed with de-ionized water 3 ~ 5 times, suction filtration is till filtrate is neutrality;
(4) by step (3) products therefrom at 60 ~ 90 ° of C dry 5 ~ 8h in loft drier;
(5) then dried product in step (4) is heated to 700 ~ 800 ° of C oxide treatment in muffle furnace, namely obtains linen boron nitride alkene nanometer sheet.
Described step (1) is adopted and is weighed with scale.
The thickness of described graphene nanometer sheet is 1 ~ 20nm.
Concentration of hydrochloric acid in described step (3) is 37.5%.
Gained linen boron nitride alkene nanometer sheet obtains finished product through grinding, carries out other sign and test.
Beneficial effect of the present invention is:
(1) equipment of the present invention's use is simple.The present invention mainly uses stainless steel autoclave, and chemical gas-phase reaction method and SiC epitaxial growth method use tube furnace, harsh to requirement for experiment condition.Need higher vacuum tightness, general use hazardous gas ammonia.
(2) cost is lower, and desired raw material is all conventional industrial chemicals.The raw material used in the present invention such as ammonium sulfate, sodium borohydride are all common agents.And chemical gas-phase reaction method needs to use tinsel, SiC epitaxial growth method uses SiC wafer etc., and price is more expensive.
(3) stable preparation process, manipulation is simple, and production efficiency is high.The amount of the boron nitride alkene nanometer sheet adopting mechanically peel method and ultrasonic solvent stripping method to prepare is considerably less, and the magnitude that the nanometer sheet of one time to produce of the present invention can reach at most gram.In addition, boron nitride alkene nanometer sheet prepared by chemical gas-phase reaction method and SiC epitaxial growth method all needs transfer, and this process operation is complicated and have infringement to quality product.
(4) excellent product performance.The boron nitride alkene nanometer sheet prepared by the method and graphene nanometer sheet have similar excellent properties, can be used as matrix material wild phase, sensor, semiconductor diode, field emission device etc.
Accompanying drawing explanation
Fig. 1 is the x-ray diffraction pattern of the boron nitride alkene nanometer sheet of embodiment 1;
Fig. 2 is the scanning electron microscope shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 1;
Fig. 3 is the transmission electron microscope shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 1;
Fig. 4 is the high-resolution electron microscopy shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 1;
Fig. 5 is the SEM shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 2;
Fig. 6 is the SEM shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 3;
Fig. 7 is the HRTEM figure of the boron nitride alkene nanometer sheet of embodiment 4;
Fig. 8 is the SEM shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 5;
Fig. 9 is the HRTEM figure of the boron nitride alkene nanometer sheet of embodiment 6.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
Embodiment 1:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet is Template preparation boron nitride alkene nanometer sheet.Weigh in the balance and get 1.5g sodium borohydride, 2.4g ammonium sulfate and 0.2g graphene nanometer sheet, load in reactor, be tamping reactor, put in crucible oven and be heated to 600 ° of C, insulation 12h, stop heating making it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, then use washed with de-ionized water 3 times, suction filtration is till filtrate is neutrality; Then by it at 80 ° of C dry 6h in loft drier; Dried product is heated in muffle furnace 750 ° of C and carries out oxide treatment, namely obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 1 uses 1.5g sodium borohydride, 2.4g ammonium sulfate and 0.2g graphene nanometer sheet, is heated to 600 ° of C, and insulation 12h, 750 ° of C oxide treatment obtain the x-ray diffraction pattern of canescence boron nitride alkene nanometer sheet.Diffraction peak in figure is all characteristic diffraction peaks of h-BN, and diffraction peak is obvious, does not have other other material to be detected, illustrates that the product purity after process is high, well-crystallized.
Fig. 2 uses 1.5g sodium borohydride, 2.4g ammonium sulfate and 0.2g graphene nanometer sheet, is heated to 600 ° of C, and insulation 12h, 750 ° of C oxide treatment obtain the SEM shape appearance figure of linen boron nitride alkene nanometer sheet.Can find out that boron nitride alkene nanometer sheet is energy printing opacity, show the very thin thickness of boron nitride alkene nanometer sheet.And the area of boron nitride alkene nanometer sheet reaches micron order.
Fig. 3 and Fig. 4 uses 1.5g sodium borohydride, 2.4g ammonium sulfate and 0.2g graphene nanometer sheet, is heated to 600 ° of C, insulation 12h, and 750 ° of C oxide treatment obtain TEM shape appearance figure and the HRTEM figure of linen boron nitride alkene nanometer sheet.As can be seen from the figure, the thinner thickness of boron nitride alkene nanometer sheet, thickness is about 5nm.
Embodiment 2:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet is Template preparation boron nitride nanosheet.Weigh in the balance and get 1.5g sodium borohydride, 2.45g ammonium sulfate and 0.3g graphene nanometer sheet, load in reactor, be tamping reactor, put in crucible oven and be heated to 550 ° of C, insulation 15h, stop heating making it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, then use washed with de-ionized water 5 times, suction filtration is till filtrate is neutrality; Then by it at 70 ° of C dry 5.5h in loft drier; Dried product is heated in muffle furnace 730 ° of C and carries out oxide treatment, namely obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 5 uses 1.5g sodium borohydride, 2.45g ammonium sulfate and 0.3g graphene nanometer sheet, is heated to 550 ° of C, and insulation 15h, 730 ° of C oxide treatment obtain the SEM shape appearance figure of linen boron nitride alkene nanometer sheet.Can find out that the amount of boron nitride alkene nanometer sheet is larger, but have certain curling.
Embodiment 3:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet is Template preparation boron nitride nanosheet.Weigh in the balance and get 1.45g sodium borohydride, 2.5g ammonium sulfate and 0.4g graphene nanometer sheet, load in reactor, be tamping reactor, put in crucible oven and be heated to 580 ° of C, insulation 14h, stop heating making it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, then use washed with de-ionized water 4 times, suction filtration is till filtrate is neutrality; Then by it at 65 ° of C dry 8h in loft drier; Dried product is heated in muffle furnace 770 ° of C and carries out oxide treatment, namely obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 6 uses 1.45g sodium borohydride, 2.5g ammonium sulfate and 0.4g graphene nanometer sheet, is heated to 580 ° of C, and insulation 8h, 770 ° of C oxide treatment obtain the SEM shape appearance figure of linen boron nitride alkene nanometer sheet.Can find out that the area of boron nitride alkene nanometer sheet also reaches micron order, but also there are some particles around boron nitride alkene nanometer sheet, this may cause because soaking time is slightly short.
Embodiment 4:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet is Template preparation boron nitride nanosheet.Weigh in the balance and get 1.55g sodium borohydride, 2.46g ammonium sulfate and 0.3g graphene nanometer sheet, load in reactor, be tamping reactor, put in crucible oven and be heated to 520 ° of C, insulation 16h, stop heating making it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, then use washed with de-ionized water 4 times, suction filtration is till filtrate is neutrality; Then by it at 75 ° of C dry 7.5h in loft drier; Dried product is heated in muffle furnace 720 ° of C and carries out oxide treatment, namely obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 7 uses 1.55g sodium borohydride, 2.46g ammonium sulfate and 0.3g graphene nanometer sheet, is heated to 520 ° of C, insulation 16h, and 720 ° of C oxide treatment obtain the HRTEM figure of linen boron nitride alkene nanometer sheet.As can be seen from the figure, also there are some unformed BN particles near boron nitride alkene nanometer sheet, this is because temperature of reaction is lower slightly.
Embodiment 5: in order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet is Template preparation boron nitride alkene nanometer sheet.Weigh in the balance and get 1.5g sodium borohydride, 2.25g ammonium sulfate and 0.2g graphene nanometer sheet, load in reactor, be tamping reactor, put in crucible oven and be heated to 500 ° of C, insulation 10h, stop heating making it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, then use washed with de-ionized water 3 times, suction filtration is till filtrate is neutrality; Then by it at 60 ° of C dry 5h in loft drier; Dried product is heated in muffle furnace 700 ° of C and carries out oxide treatment, namely obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 8 uses 1.5g sodium borohydride, 2.25g ammonium sulfate and 0.2g graphene nanometer sheet, is heated to 500 ° of C, insulation 10h, and 700 ° of C oxide treatment obtain the HRTEM figure of linen boron nitride alkene nanometer sheet.As can be seen from the figure, boron nitride alkene nanometer sheet pattern is poor, and thickness is also larger.This is because ammonium sulfate addition is less, and the required nitrogenous source of reaction is not enough, and in addition, temperature of reaction is also lower slightly.
Embodiment 6:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet is Template preparation boron nitride alkene nanometer sheet.Weigh in the balance and get 1.5g sodium borohydride, 2.55g ammonium sulfate and 0.5g graphene nanometer sheet, load in reactor, be tamping reactor, put in crucible oven and be heated to 600 ° of C, insulation 16h, stop heating making it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 5 times, then use washed with de-ionized water 5 times, suction filtration is till filtrate is neutrality; Then by it at 90 ° of C dry 8h in loft drier; Dried product is heated in muffle furnace 800 ° of C and carries out oxide treatment, namely obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 9 uses 1.5g sodium borohydride, 2.55g ammonium sulfate and 0.5g graphene nanometer sheet, is heated to 600 ° of C, insulation 16h, and 800 ° of C oxide treatment obtain the HRTEM figure of linen boron nitride alkene nanometer sheet.As can be seen from the figure, boron nitride alkene nanometer sheet reaches micron order, but the fold on surface is slightly many.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (3)
1. a preparation method for boron nitride alkene nanometer sheet, is characterized in that, it take sodium borohydride as boron source, ammonium sulfate is nitrogenous source, graphene nanometer sheet is template, and concrete steps are as follows:
(1) ammonium sulfate, sodium borohydride and graphene nanometer sheet is taken respectively; Wherein, ammonium sulfate, sodium borohydride and graphene nanometer sheet are 1.5 ~ 1.67:1:0.13 ~ 0.33 in mass ratio;
(2) three kinds of raw materials in step (1) are mixed in loading reactor, be tamping reactor, put in crucible oven and be heated to 500 ~ 600 DEG C, insulation 10 ~ 16h, stop heating making it cool to room temperature with the furnace;
(3) step (2) is reacted products therefrom hydrochloric acid cleaning 3 ~ 5 times, then use washed with de-ionized water 3 ~ 5 times, suction filtration is till filtrate is neutrality;
(4) by step (3) products therefrom at 60 ~ 90 DEG C of dry 5 ~ 8h in loft drier;
(5) then dried product in step (4) is heated to 700 ~ 800 DEG C of oxide treatment in muffle furnace, namely obtains linen boron nitride alkene nanometer sheet, gained linen boron nitride alkene nanometer sheet obtains finished product through grinding;
The thickness of described graphene nanometer sheet is 1 ~ 20nm.
2. the preparation method of boron nitride alkene nanometer sheet as claimed in claim 1, it is characterized in that, described step (1) is adopted and is weighed with scale.
3. the preparation method of boron nitride alkene nanometer sheet as claimed in claim 1, it is characterized in that, the concentration of hydrochloric acid in described step (3) is 37.5%.
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| CN104637898B (en) * | 2014-12-08 | 2019-01-11 | 上海大学 | The heat-conductive composite material layer and electronic device conductive structure packaging method of integrated circuit device |
| CN105293453B (en) * | 2015-11-20 | 2018-05-11 | 汕头大学 | It is a kind of to adulterate hexagonal boron nitride nanosheet and preparation method thereof and using its catalyst and application as carrier |
| CN111433156B (en) * | 2018-02-07 | 2023-12-19 | 国立大学法人东京工业大学 | Boron atomic layer sheet, laminated sheet, method for producing same, and liquid crystal |
| CN108328585A (en) * | 2018-05-03 | 2018-07-27 | 河北工业大学 | A kind of preparation method of boron nitride coated graphite alkene nanometer sheet |
| CN110655048A (en) * | 2019-11-09 | 2020-01-07 | 徐少晨 | Preparation method of silicon nitride nanosheet |
| CN112745132A (en) * | 2020-12-24 | 2021-05-04 | 徐州康纳高新材料科技有限公司 | High-compactness high-strength quartz ceramic matrix composite material and preparation method thereof |
| CN114293050B (en) * | 2021-12-13 | 2023-01-06 | 南京航空航天大学 | Two-dimensional boron-alkene reinforced metal matrix composite material and preparation method thereof |
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| US4714599A (en) * | 1982-04-15 | 1987-12-22 | National Institute For Researches In Inorganic Materials | Process for preparing rhombohedral system boron nitride using NaBH4 -and NH4 Cl |
| CN101259960A (en) * | 2008-03-28 | 2008-09-10 | 山东大学 | Method for preparing boron nitride coating carbon nano-tube/nano-wire and boron nitride nano-tube |
| CN103043634A (en) * | 2013-01-16 | 2013-04-17 | 华南农业大学 | Hexagonal boron nitride two-dimensional ultrathin nanometer sheet as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4714599A (en) * | 1982-04-15 | 1987-12-22 | National Institute For Researches In Inorganic Materials | Process for preparing rhombohedral system boron nitride using NaBH4 -and NH4 Cl |
| CN101259960A (en) * | 2008-03-28 | 2008-09-10 | 山东大学 | Method for preparing boron nitride coating carbon nano-tube/nano-wire and boron nitride nano-tube |
| CN103043634A (en) * | 2013-01-16 | 2013-04-17 | 华南农业大学 | Hexagonal boron nitride two-dimensional ultrathin nanometer sheet as well as preparation method and application thereof |
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Inventor after: Bi Zhenyu Inventor after: Chen Yafei Inventor after: Pei Bihong Inventor after: Bi Jianqiang Inventor after: Yin Chonglong Inventor after: You Guanglei Inventor after: Bai Yujun Inventor after: Zhao Qingqiang Inventor before: Bi Jianqiang Inventor before: Chen Yafei Inventor before: Yin Chonglong Inventor before: You Guanglei Inventor before: Bai Yujun Inventor before: Zhao Qingqiang |
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