CN114057201B - Device and method for preparing powdered silicon monoxide - Google Patents
Device and method for preparing powdered silicon monoxide Download PDFInfo
- Publication number
- CN114057201B CN114057201B CN202111395605.1A CN202111395605A CN114057201B CN 114057201 B CN114057201 B CN 114057201B CN 202111395605 A CN202111395605 A CN 202111395605A CN 114057201 B CN114057201 B CN 114057201B
- Authority
- CN
- China
- Prior art keywords
- silicon monoxide
- cooling
- silicon
- cooling section
- rotating
- 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.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
- C01B33/182—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by reduction of a siliceous material, e.g. with a carbonaceous reducing agent and subsequent oxidation of the silicon monoxide formed
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a device and a method for preparing powdered silicon monoxide. The device comprises a heating furnace and a tank body; a reaction section and a cooling section are arranged in the length direction of the tank body; the heating furnace provides a heat source for the reaction section; a rotating piece is erected in the cooling section and electrically connected with the motor, and when the motor works, the rotating piece rotates in the horizontal direction in the cooling section; the outer wall of the cooling section is sleeved with a cooling sleeve, and the cooling sleeve is communicated with a circulating water system; the cooling section is also provided with a vacuumizing pipeline for being externally connected with a vacuumizing device. The method comprises the steps of mixing high-purity silicon and silicon dioxide, placing the mixture in a reaction section, heating the mixture to 1150-1400 ℃ under a vacuum condition, preserving heat for a period of time, allowing generated silicon monoxide gas to flow into a cooling section, and allowing the silicon monoxide gas to contact with a rotating sheet under the action of the rotating speed of the rotating sheet, then cooling the silicon monoxide gas at the highest speed to micron-sized silicon monoxide powder and allowing the silicon monoxide powder to fall. The invention realizes the collection of the nano-scale silicon monoxide powder, saves the multi-stage crushing process, reduces the cost and improves the product purity and yield.
Description
Technical Field
The invention relates to a method and equipment for preparing powdered silicon monoxide.
Background
In recent years, lithium ion batteries are developed to large-scale application fields, indexes such as lithium ion energy density and the like need to be further improved, and in the aspect of negative electrode materials, the theoretical specific capacity of a traditional graphite negative electrode is 372mAh/g, so that the requirement of high-energy-density batteries is difficult to meet. The silicon-based material is concerned due to the theoretical specific capacity of 4200mAh/g, but the volume expansion of the silicon-based material is up to 300% in the charging and discharging processes, so that the reversible capacity of the silicon-based negative electrode material is low, and the cycle performance is poor.
At present, the prior domestic raw materials for preparing the silicon monoxide mainly comprise silicon powder and silicon dioxide powder which are mixed, vacuumized, heated and sublimated, and then rapidly cooled to prepare blocky and cylindrical silicon monoxide. Since the silicon monoxide needs to be crushed to micron-scale and nanometer-scale in the application of the later-stage lithium battery cathode material. The Mohs hardness of the silicon monoxide reaches about 7, the difficulty is great in the crushing process, and the multistage crushing is generally adopted to invisibly increase the energy consumption and the cost for manufacturing the silicon monoxide cathode material. Some studies have been made to produce a silica powder.
Through search, the patent application documents of the Chinese patent application number 201410056450.2 and the application publication date 2014, 7 and 2 disclose a method and an apparatus for manufacturing SiO powder. The method of this patent comprises the steps of: mixing silicon powder and silicon dioxide powder, and heating until gaseous SiO is sublimated; gaseous SiO is separated out on the outer surface of the separation matrix under the protection of inert gas; after cooling, the precipitated SiO is stripped to obtain SiO powder; the precipitation substrate rotates in the gaseous SiO precipitation process; the manufacturing device comprises a gas flow direction control assembly, a raw material chamber and a precipitation chamber are horizontally arranged relatively, and a rotary precipitation matrix is arranged in the precipitation chamber. The manufacturing device has the advantages that the specific precipitation surface area is larger, the heat conduction efficiency is higher, the zone temperature control is more accurate, and the precipitation capacity and the quality are higher; meanwhile, the sublimation gas is subjected to inert gas flow impact and guide control, so that the consistency of the particle size distribution of the precipitated particles is improved. However, the rotary precipitation substrate of this apparatus is expensive, siO is likely to be agglomerated due to the SiO oxide adhered to the cylindrical surface of the rotary precipitation substrate, the particle size of the produced SiO is too large, and the SiO adhered to the surface of the substrate is not easily cleaned.
For another example, a chinese patent application No. 202010745425.0, published as 2020, 11/6, discloses a production apparatus for producing SiO powder. The device comprises a heating furnace, a cooling recovery device and a heat recovery device, wherein the heating furnace is connected with the cooling recovery device through a first heat-insulation connecting pipe, and the cooling recovery device is connected with the heat recovery device through a second heat-insulation connecting pipe; compared with the traditional SiO production equipment, the continuous SiO production can be carried out, the production efficiency is improved, and the production cost is reduced. However, only one spiral feeding rod is arranged in the cooling device of the device, and the cooled silica powder has a high caking risk and is easy to block the spiral device; in addition, the device has a relatively complex structure and high cost.
Therefore, in order to optimally control the particle size of the silica powder, an apparatus and a method for preparing the silica powder are needed.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems in the existing preparation process of the silicon monoxide, the invention provides a device and a method for preparing the powder silicon monoxide.
2. Technical scheme
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a device for preparing powdered silicon monoxide comprises a heating furnace and a tank body; a reaction section and a cooling section are arranged in the length direction of the tank body; the heating furnace provides a heat source for the reaction section, and the cooling section is exposed out of the heating furnace, so that the charging, the material taking and the slag cleaning are facilitated; a rotating piece is erected in the cooling section and electrically connected with a motor, and when the motor works, the rotating piece rotates in the horizontal direction in the cooling section; the outer wall of the cooling section is sleeved with a cooling sleeve, the cooling sleeve is communicated with a circulating water system, and circulating room temperature water is introduced into the cooling sleeve by the circulating water system; the cooling section is also provided with a vacuumizing pipeline for connecting an external vacuumizing device, and the cooling section is provided with a sealing cover which is opened in opposite directions.
Further, the support of having set up the rotor can be the pivot, and the cooling zone is run through in the pivot, and is connected with the motor, drives the rotor and rotates, and at this moment, pivot and cooling zone kneck adopt the rubber circle sealed.
Furthermore, the support for erecting the rotating piece can be hollow, the rotating piece and the motor are connected through wiring in the support, and at the moment, the rotating piece can be coated with a cooling jacket to accelerate cooling.
Furthermore, the rotating sheet is a metal molybdenum sheet or a stainless steel sheet, and the two metals have high melting points and good heat conductivity.
Further, in order to avoid the aggregation of excessive powder adhered to the rotating plate and influence the particle size of the generated powder, namely the production efficiency, the cooling tank is matched with a tank body with the total length of two meters, the length of the cooling tank is 65cm, the diameter of the cooling tank is 40cm, the thickness of the rotating plate is 0.3-1 cm, the length of the rotating plate is 25cm, and the width of the rotating plate is 6cm.
Further, the bottom of the inner wall of the cooling section is movably sleeved with a collector, the depth of the collector is larger than or equal to the height of the rotating piece which is erected, the rotating piece is cooled to room temperature after the preparation method is finished, and the collector is taken out to obtain the silicon monoxide powder.
Further, the collector is a high temperature resistant material.
The method for preparing the powdered silicon monoxide by adopting the device comprises the following steps: mixing high-purity silicon and silicon dioxide, placing the mixture in a reaction section, heating the mixture to 1150-1400 ℃ under a vacuum condition, preserving heat for a period of time, allowing the generated silicon monoxide gas to flow into a cooling section, allowing the silicon monoxide gas to contact with a rotating sheet and then rapidly cooling micron-sized silicon monoxide powder to fall down under the action of the rotating speed of the rotating sheet, introducing room-temperature circulating water into a cooling sleeve of the cooling section, and allowing the temperature of the cooling section to be below 900 ℃ due to the temperature difference between the reaction section and the cooling section, so that the silicon monoxide gas flows into the cooling section.
Further, the rotating speed of the rotating piece is 10-100r/min, and the D50 of the obtained silicon monoxide powder is 40-70 μm.
Further, the mixing mass ratio of the high-purity silicon and the silicon dioxide is 1:1.
Further, the purity of both the high purity silicon and the silica is greater than 99.5% wt.
Further, in order to ensure that the raw materials are fully sublimated, the heating rate of the reaction section is 1-6 ℃ for min, and the heat preservation time is 5-40h.
3. Advantageous effects
(1) The method is different from the defects that the existing silicon monoxide is prepared into a block shape and a cylindrical shape and is difficult to crush, realizes the collection of product powder, saves multi-stage crushing procedures, reduces the cost, improves the product purity and the yield, and solves the difficulty of difficult crushing of the existing silicon monoxide, thereby better meeting the raw material utilization rate of the silicon monoxide and realizing the industrial production and quality requirements;
(2) The key point of the invention is that the synthesis equipment of the silicon monoxide is improved, the rotating piece is added in the cooling section, the rotating speed of the rotating piece is set to be 10-100r/min, the silicon monoxide gas generated in the reaction section flows into the cooling section through the temperature difference of the two sections, and when contacting the rotating piece, the strong cooling condition of the rotating speed action of the rotating piece is applied, the strong cooling condition is that the silicon monoxide gas is subjected to the instant impact force given by the rotation of the rotating piece, and the gaseous silicon monoxide is extremely rapidly cooled and converted into micron-sized powder, so that the collection of the silicon monoxide powder is realized, the crushing process is saved, and the production cost is reduced; meanwhile, the collected silica powder falls off by the rotation of the rotating piece, and is not easy to agglomerate;
(3) The invention provides a method for preparing powdered silicon oxide by vacuum heating of silicon powder and silicon dioxide powder, which can prepare powdered silicon oxide by a method of vacuumizing, heating, ceaseless rotation of a collector and a rotating sheet by using equipment and enabling gas evaporated from the silicon oxide to encounter a rotating paddle with lower temperature to be cooled at the highest speed;
(4) The invention has simple structure and low cost, and can control the D50 of the silicon monoxide powder to be 40-70 μm by adjusting the rotating speed to be 10-100 r/min.
Drawings
FIG. 1 is an XRD pattern for the preparation of the silica powder of example 1;
FIG. 2 is a schematic structural view of the present invention;
in the figure:
1. a heating furnace; 2. a tank body; 21. a reaction section; 22. a cooling section; 221. a rotating sheet; 222. a collector; 223. cooling the sleeve; 224. a vacuum pipeline is pumped; 225. and (7) sealing the cover.
Detailed Description
The invention is further described with reference to specific examples.
As shown in FIG. 1, the apparatus for preparing powdered silica of the present invention comprises a heating furnace 1 and a two-meter tank 2; a reaction section 21 and a cooling section 22 are arranged in the length direction of the tank body 2, and the length of the cooling section 22 is 65cm, and the diameter of the cooling section is 40cm; the reaction section 21 is arranged in the heating furnace 1 and provides a heat source for the heating furnace; the cooling section 22 is exposed out of the heating furnace 1, so that feeding, material taking and slag cleaning are facilitated; a rotating shaft penetrates through the cooling section 22, a rotating piece 221 is fixed at one end extending into the cooling section 22, one end extending out of the cooling section 22 is electrically connected with the motor, a connecting port of the rotating shaft and the cooling section is sealed by a rubber ring, the motor works, the rotating shaft drives the rotating piece 221 to rotate, and the rotating piece 221 rotates in the horizontal direction in the cooling section 22; wherein, the thickness of the rotating piece is 0.8mm, the length is 25cm, the width is 6cm, the rotating piece is a metal molybdenum piece or a stainless steel piece, and the metal molybdenum piece is taken as an example in the specific implementation mode; the outer wall of the cooling section 22 is sleeved with a cooling sleeve 223, the cooling sleeve 223 is communicated with a circulating water system, the circulating water system feeds circulating room temperature water into the cooling sleeve, and when the reaction section 21 is heated to 1150-1400 ℃, the room temperature water can control the temperature of the cooling section 22 to be lower than 900 ℃; the cooling section 22 is further provided with a vacuum pipe 224 for connecting a vacuum device to create a vacuum environment inside the tank 2. The cooling section is provided with a seal cover 225 which is opened in half for convenient operation.
In order to collect the silica powder, the collector 222 is movably sleeved at the bottom of the inner wall of the cooling section 22, the depth of the collector 222 is greater than or equal to the height of the rotating piece 221 which is erected, the container is cooled to room temperature after the preparation method is finished, and the collector 222 is taken out to obtain the silica powder, wherein the collector 222 is made of a high-temperature-resistant material, such as a crucible material or an iron sheet.
Example 1
(1) Mixing raw materials: mixing high purity silicon having a purity of greater than 99.5% wt and silica having a purity of greater than 99.5% wt in an amount of 1:1.
(2) Vacuum heating: putting the mixed materials into a reaction section 21, heating to 1200 ℃ under a vacuum condition, and preserving heat for 20h at the heating rate of 3 ℃/min. The rotation speed of the molybdenum sheet is adjusted to be 15r/min, the sublimation gas of silicon and silicon dioxide is rapidly cooled into a solid state when meeting the rotating molybdenum sheet in the cooling section, and the sublimation gas of silicon and silicon dioxide falls onto the collector 222 in a powdery state under the action of centrifugal force, the particle size detection D50 of the obtained silicon monoxide powder is 63 microns, as shown in figure 2, the XRD spectrum shows that the obtained powder silicon monoxide is in an amorphous state, and the performance of the subsequent processing into a battery is facilitated.
Example 2
(1) Mixing raw materials: mixing high purity silicon having a purity of greater than 99.5% wt and silica having a purity of greater than 99.5% wt according to 1:1.
(2) Vacuum heating: heating the mixed materials in the reaction section 21 to 1400 ℃ under a vacuum condition, and preserving heat for 20 hours at a heating rate of 3 ℃/min. The rotating speed of the molybdenum sheet is adjusted to be 20r/min, and the D50 of the obtained powder for detecting the particle size of the silicon oxide is 56 mu m.
Example 3
(1) Mixing raw materials: mixing high purity silicon having a purity of greater than 99.5% wt and silica having a purity of greater than 99.5% wt according to 1:1.
(2) Vacuum heating: the mixed materials are put into a reaction section 21, heated to 1400 ℃ under the vacuum condition, and kept for 30 hours, wherein the heating rate is 3 ℃/min. The rotating speed of the molybdenum sheet is adjusted to be 30r/min, and the D50 of the obtained powder for detecting the particle size of the silicon oxide is 50 mu m.
In the invention, the SiO powder with different particle sizes can be obtained by adjusting the rotation speed of the Mo piece, and the yield of different parameters is also changed, which is detailed in Table 1.
TABLE 1 measurement of Properties of products prepared under different conditions
As can be seen from Table 1, when the rotation speed of the molybdenum sheet is 10-100r/min, the D50 of the powdered silicon monoxide is distributed between 40-70 μm, and the preparation of micron-sized silicon monoxide powder is realized. However, when the rotation speed exceeds 100r/min, the particle diameter increases.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (8)
1. A method for preparing powdered silicon monoxide is characterized in that: the device for preparing the powdered silicon monoxide is adopted, and comprises a heating furnace (1) and a tank body (2);
a reaction section (21) and a cooling section (22) are arranged in the length direction of the tank body (2);
the heating furnace (1) provides a heat source for the reaction section (21);
a rotating piece (221) is erected in the cooling section (22), the rotating piece (221) is electrically connected with a motor, and when the motor works, the rotating piece (221) rotates in the horizontal direction in the cooling section (22);
a cooling sleeve (223) is sleeved on the outer wall of the cooling section (22), and the cooling sleeve (223) is communicated with a circulating water system;
the cooling section (22) is also provided with a vacuumizing pipeline (224) for connecting a vacuumizing device externally;
the preparation method comprises the following steps: mixing high-purity silicon and silicon dioxide, placing the mixture in a reaction section (21), heating the mixture to 1150-1400 ℃ under a vacuum condition, preserving heat for a period of time, allowing the generated silicon monoxide gas to flow into a cooling section (22), allowing the silicon monoxide gas to contact a rotating sheet (221) under the action of the rotating speed of the rotating sheet (221), cooling the silicon monoxide gas at a high speed to micron-sized silicon monoxide powder, and allowing the silicon monoxide powder to fall, wherein the rotating speed of the rotating sheet (221) is 10-100r/min, and the D50 of the obtained silicon monoxide powder is 40-70 mu m.
2. The method for preparing powdered silica according to claim 1, wherein: the rotating sheet (221) is a metal molybdenum sheet or a stainless steel sheet.
3. The method for preparing powdered silica according to claim 2, wherein: the thickness of the rotating sheet (221) is 0.3-1 cm, the length is 25cm, and the width is 6cm.
4. The method for producing powdered silica according to any one of claims 1 to 3, wherein: the bottom of the inner wall of the cooling section (22) is movably sleeved with a collector (222), and the depth of the collector (222) is larger than or equal to the height of the rotating piece (221) which is erected.
5. The method for preparing powdered silica according to claim 4, wherein: the collector (222) is a high temperature resistant material.
6. The method for preparing powdered silica according to claim 1, wherein: the mixing mass ratio of the high-purity silicon to the silicon dioxide is 1:1.
7. The method for preparing powdered silica according to claim 6, wherein: the purity of both the high purity silicon and the silica is greater than 99.5% wt.
8. The method for preparing powdered silica according to claim 7, wherein: the heating rate of the reaction section (21) is 1-6 ℃ for min, and the heat preservation time is 5-40h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111395605.1A CN114057201B (en) | 2021-11-23 | 2021-11-23 | Device and method for preparing powdered silicon monoxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111395605.1A CN114057201B (en) | 2021-11-23 | 2021-11-23 | Device and method for preparing powdered silicon monoxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114057201A CN114057201A (en) | 2022-02-18 |
| CN114057201B true CN114057201B (en) | 2023-02-28 |
Family
ID=80275461
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111395605.1A Active CN114057201B (en) | 2021-11-23 | 2021-11-23 | Device and method for preparing powdered silicon monoxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114057201B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115140739B (en) * | 2022-07-19 | 2023-05-16 | 新疆晶硕新材料有限公司 | Production equipment and method of silicon oxide |
| CN116161667A (en) * | 2022-09-08 | 2023-05-26 | 安徽科达新材料有限公司 | Method for preparing silicon monoxide by adding fluxing agent |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109956478A (en) * | 2017-12-25 | 2019-07-02 | 新特能源股份有限公司 | The method that gaseous phase deposition stove and production aoxidize sub- silicon |
-
2021
- 2021-11-23 CN CN202111395605.1A patent/CN114057201B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN114057201A (en) | 2022-02-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114057201B (en) | Device and method for preparing powdered silicon monoxide | |
| CN102703160B (en) | Preparation method of graphite-bi-selenylation niobium nanocomposite | |
| CN111747416B (en) | Production of SiOxApparatus and method of | |
| CN105935620A (en) | Preparation device for nano material | |
| CN110818432A (en) | Superfine high-entropy boride nano powder and preparation method thereof | |
| US7625543B2 (en) | Production process for carbonized product and carbonized product obtained by the same process | |
| CN106903322B (en) | The rotary continuous preparation method of dynamic of copper rhodium-tellurium intermetallic compound powder | |
| CN110655084A (en) | Solid pure object side collecting device of horizontal electric heating equipment | |
| CN110655085A (en) | Single-side collecting method for solid purified object horizontal electric heating equipment | |
| CN112209390B (en) | High-temperature device for preparing lithium ion battery cathode material and preparation method thereof | |
| CN113636559A (en) | Preparation device and preparation method of silicon-based electrode material | |
| CN103011252A (en) | Method for producing high-purity low-chlorine electroplating-grade cupric oxide continuously from basic copper carbonate | |
| CN106981645A (en) | Modified phosphate iron lithium anode material and preparation method thereof | |
| CN113528859A (en) | Preparation method and preparation equipment of ultrathin metal lithium foil | |
| CN108823409B (en) | System and method for recovering waste heat of liquid magnesium chloride generated in titanium sponge preparation process | |
| CN110657671A (en) | Side collecting device for horizontal electric heating equipment | |
| CN110745802A (en) | Method for preparing lithium iron phosphate by electromagnetic induction self-heating | |
| CN212476140U (en) | Cyclone separation production device for gallium oxide micro powder | |
| CN210480876U (en) | System for preparing graphene powder by redox method | |
| CN110668448A (en) | Single-side lateral horizontal collecting device of solid pure object electric heating equipment | |
| CN203495241U (en) | Novel powder metallurgy pulverizing device | |
| CN218976868U (en) | Cover temperature control device is collected to horizontal electrical heating equipment side | |
| CN212283991U (en) | Reaction system for thermal dehydration into anhydride | |
| CN110657669A (en) | Horizontal collecting device for two-side surfaces of solid pure object electric heating equipment | |
| CN110671933A (en) | Method for collecting solid-state purified matter on two lateral sides of horizontal electric heating equipment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |