CN118165702B - Preparation method of ceramic corundum abrasive - Google Patents

Preparation method of ceramic corundum abrasive Download PDF

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Publication number
CN118165702B
CN118165702B CN202410591872.3A CN202410591872A CN118165702B CN 118165702 B CN118165702 B CN 118165702B CN 202410591872 A CN202410591872 A CN 202410591872A CN 118165702 B CN118165702 B CN 118165702B
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Prior art keywords
particles
filter cake
corundum abrasive
ceramic corundum
drying
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CN118165702A (en
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翟涵
翟晨曦
孙明秀
王梦瑶
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Sisha Taililai Qingdao Grinding Co ltd
Zibo Sisha Taiyi Grinding Co ltd
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Sisha Taililai Qingdao Grinding Co ltd
Zibo Sisha Taiyi Grinding Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/021After-treatment of oxides or hydroxides
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1409Abrasive particles per se

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Polishing Bodies And Polishing Tools (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention belongs to the technical field of abrasive materials, and particularly relates to a preparation method of a ceramic corundum abrasive material, which is characterized by comprising the following steps: preparing a high-viscosity pseudo-boehmite wet product into a filter cake with solid content of more than 40% by means of extrusion and filtration; and (3) drying, crushing, calcining, impregnating with modifier, secondary drying, secondary calcining and sintering the filter cake to obtain the ceramic corundum abrasive. The invention has the advantages of simple process, low cost, safety and environmental protection. The high-viscosity pseudo-boehmite wet product does not need to be made into colloid, simplifies the manufacturing process, does not use nitric acid, solves the potential hazard in transportation and use, does not need to use expensive 304 stainless steel for manufacturing processing equipment in the subsequent working procedure, does not decompose to produce nitrogen oxide gas in the first calcination working procedure, does not need to treat the waste gas by an SCR reduction method, does not cause environmental pollution, and reduces the cost.

Description

Preparation method of ceramic corundum abrasive
Technical Field
The invention belongs to the technical field of abrasives, and particularly relates to a preparation method of a ceramic corundum abrasive.
Background
In the last twenty years, ceramic corundum abrasive materials are taken as new generation novel efficient abrasive materials, are developed in China, the market scale and export are continuously increased, and the ceramic corundum abrasive materials are more and more favored and paid attention to users at home and abroad. The prior art ceramic corundum abrasive is relatively complex in production process, for example, the technology disclosed by China patent office on 3 and 4 months, with publication number CN103013442A, the technology disclosed by the invention on 3 and 4 months, with publication number CN103013443A, the technology disclosed by the invention on 3 and 4 months, with publication number CN, the technology disclosed by the invention on 4 months, with publication number CN103013443A, the technology disclosed by the invention on 4 months, with a lozenge-like structure, is that the ceramic corundum abrasive is prepared by using a sol-gel technology, which firstly takes high-viscosity pseudo-boehmite (Bao Mdan semi-finished product) as a raw material, adds purified water to mix into suspension, adds a peptizing agent to prepare sol and gel, dries the colloid, crushes, screens out useful particles, calcines at low temperature, introduces modifier, calcines at low temperature for the second time, sinters, screens out abrasive products with various particle sizes.
As the first step of the above preparation method: the colloid is prepared by using a peptizing agent, and the peptizing agent with the best effect is nitric acid. Nitric acid is an oxidant and also a strong acid, belongs to dangerous chemicals, has a plurality of dangers in transportation and use, and can cause certain harm to operators and environment due to improper use. The colloid is acidic due to the nitric acid, the processing equipment in each subsequent process must be made of expensive 304 stainless steel to prevent corrosion and rust, the colloid is decomposed into nitrogen oxide waste gas in the first calcination process, the waste gas needs to be treated by SCR reduction method to avoid environmental pollution, and all the processes bring operational risks due to the addition of the nitric acid, so that the manufacturing cost is increased.
Disclosure of Invention
The invention aims to provide a preparation process of ceramic corundum abrasive materials, which simplifies the manufacturing process, does not need to use peptizers such as nitric acid and the like, presses and filters high-viscosity pseudo-boehmite wet products with large water content difference to obtain filter cakes with stable water content, does not need to prepare colloid, directly dries, breaks and calcines to prepare the ceramic corundum abrasive materials with good quality, reduces cost and risk, and reduces the generation and pollution of nitrogen oxides.
The invention is realized by the following technical scheme:
Namely a preparation process of ceramic corundum abrasive, which is characterized by comprising the following steps:
1) Preparing a high-viscosity pseudo-boehmite wet product into a filter cake with solid content of more than 40% by means of extrusion and filtration;
2) Drying the filter cake at 80-140 ℃, and naturally breaking the filter cake into fragments after drying;
3) Crushing the fragments, and screening particles between a 16-mesh screen and a 100-mesh screen after crushing;
4) Calcining the sieved particles at 550-750 ℃;
5) The calcined particles are introduced with modifier by an impregnation method to prepare an aqueous solution containing neodymium nitrate, lanthanum nitrate, yttrium nitrate, magnesium nitrate and cobalt nitrate, and the weight ratio of the calcined particles to the aqueous solution is 1:0.8, uniformly mixing the aqueous solution and the calcined particles;
6) Drying the immersed particles, removing the contained adsorbed water, wherein the drying temperature is 60-100 ℃;
7) Carrying out secondary calcination on the dried particles, wherein the calcination temperature is 550-750 ℃;
8) The calcined particles are further sintered for 5-30 minutes at 1420-1440 ℃.
The sintered particles are the ceramic corundum abrasive, and abrasive finished products with various granularity numbers are sieved out.
When the filter cake is manufactured in the step 1), a steel round die is preferably manufactured, industrial filter cloth is paved in the steel die, the high-viscosity pseudo-boehmite wet product is put into the industrial filter cloth, the industrial filter cloth is wrapped, pressure is added, part of water is extruded, and the size of the die is matched with the pressurizing pressure.
The method can not remove the water in the high-viscosity pseudo-boehmite wet product by adopting the modes of drying, airing or vacuumizing and the like. By adopting the mode to remove the moisture, a compact block filter cake cannot be obtained.
The step 2) does not evaporate water in the filter cake too fast when the filter cake is dried, otherwise air holes are generated, the air holes can cause insufficient compactness of the sintered abrasive, the strength of the abrasive is affected, the filter cake is naturally broken into fragments of several millimeters to more than ten millimeters after being dried, the cracked surfaces of the fragments are smooth and compact, and the fragments slightly reflect light, so that the fragments are compact and have no air holes.
The calcination in the above steps 4) and 7) is preferably performed by a rotary calciner, which can continuously calcine, has high productivity, and saves energy.
The calcined particles in the step 5) generate a large number of micro-pores in the particles due to the removal of crystal water, so that a space is provided for introducing the modifier, and neodymium nitrate, lanthanum nitrate, yttrium nitrate, magnesium nitrate and cobalt nitrate in the aqueous solution are all absorbed into the particles due to the micro-pore adsorption during impregnation.
The temperature of the particles impregnated in step 6) is not too high to avoid decomposition of nitrate.
And 7) performing secondary calcination on the particles in the step 7) to remove residual moisture and promote the decomposition of nitrate.
Further, after sintering, the particles of the invention have a particle size of 24# 180.
Further, the thickness of the filter cake is less than or equal to 10mm.
Further, in the sintered particles of the present invention, the sum of yttrium oxide, neodymium oxide, lanthanum oxide, magnesium oxide and cobalt oxide is 3.3% -6% based on the aluminum oxide.
The filter cake prepared by the method is preferably in a flake shape, the thickness of the filter cake is not more than 10mm, and the water content of each part of the filter cake is consistent. If the filter cake is too thick, the water content in the middle part is higher, and the filter cake with high water content has poor effect.
Further, the fragments of the present invention are crushed using a ball mill or a pulverizer or a twin roll or a disc crusher.
The crushing equipment is selected according to the final grinding object, and the shapes of the material particles crushed by the roller and the disc crusher are relatively sharp, so that the grinding device is suitable for low-pressure grinding; the particles crushed by the ball mill and the pulverizer are round, and are suitable for grinding under high pressure.
Any other known crusher may be used in the present invention, provided that the selected crusher is capable of crushing the pieces to a set size.
Furthermore, the invention adopts a muffle furnace or a microwave sintering furnace or a gas-fired kiln or a rotary kiln during sintering.
The sintering of the granules is not limited to the above kilns, but can be carried out by any kiln known in the art which can reach sintering temperatures.
The invention has the advantages of simple process, low cost, safety and environmental protection. The high-viscosity pseudo-boehmite wet product does not need to be made into colloid, simplifies the manufacturing process, does not use nitric acid, solves the potential hazard in transportation and use, does not need to use expensive 304 stainless steel for manufacturing processing equipment in the subsequent working procedure, does not decompose to produce nitrogen oxide gas in the first calcination working procedure, does not need to treat the waste gas by an SCR reduction method, does not cause environmental pollution, and reduces the cost.
Drawings
FIG. 1 is a schematic view of a cake extrusion die of example 1 of the present invention;
FIG. 2 is a graph showing the Vickers hardness test of the ceramic corundum abrasive material prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the ceramic corundum abrasive material produced in example 1 of the present invention;
FIG. 4 is a graph showing the Vickers hardness test of the ceramic corundum abrasive material produced in example 2 of the present invention;
FIG. 5 is a scanning electron microscope image of the ceramic corundum abrasive material produced in example 2 of the present invention;
FIG. 6 is a graph showing the Vickers hardness test of the ceramic corundum abrasive material prepared in example 3;
FIG. 7 is a scanning electron microscope image of the ceramic corundum abrasive material produced in example 3;
FIG. 8 is a scanning electron microscope image of the ceramic corundum abrasive material of comparative example 2 of the present invention.
As shown in the figure: 1. an upper plate; 2. a mold; 3. a bottom plate; 4. and (3) small holes.
Detailed Description
Example 1: as shown in figure 1, a cylindrical steel mold 2 with a diameter of 300mm and a height of 50mm is manufactured, the mold 2 is provided with an integrated bottom plate 3, a plurality of small holes 4 are arranged on the bottom plate 3, the upper end of the mold 2 is opened, an upper plate 1is arranged at the opening, 1000 g of a commercially available high-viscosity pseudo-boehmite wet product (the water content is about 65 percent and the solid content is about 35 percent) is put into the mold 2, flattened, the upper plate 1is put on an oil press to be pressurized, water is extruded out through the small holes 4 until the solid content reaches 43 percent, a newly manufactured filter cake (the thickness of 10 mm) is put into a enamel plate, and is put into a baking oven with the temperature of 100 ℃ for about 8 hours, the filter cake is broken into fragments of a few millimeters to a few millimeters, and is broken by a disc breaker, and particles between a 18-mesh screen and a 100-mesh screen are sieved.
Placing the sieved particles into a ceramic crucible, placing into a muffle furnace, heating to 650 ℃, preserving heat for 30 minutes, and naturally cooling.
1000 G of aqueous solution is prepared, and 32.5 g of neodymium nitrate hexahydrate, 42.4 g of yttrium nitrate hexahydrate, 33.3 g of lanthanum nitrate hexahydrate, 80.1 g of magnesium nitrate hexahydrate and 2.4 g of cobalt nitrate hexahydrate are contained.
Mixing the aqueous solution and the calcined particles according to the weight ratio of 0.8:1, after being uniformly mixed, nitrate in the aqueous solution is fully immersed into the calcined granule, and then the material is dried at the temperature of 80 ℃.
The soaked and dried material is put into a ceramic crucible again, placed into a muffle furnace, heated to 650 ℃, and kept for 30 minutes. And (5) naturally cooling.
Finally, sintering in a high-temperature furnace, wherein the furnace temperature is controlled to 1440 ℃, and the sintering time is 10 minutes.
The sintered particles were based on alumina, and the sum of yttria, neodymia, lanthana, magnesia, and cobalt oxide was 4%.
The sintered product was tested with a Memeroret Rajik AccuPyc II 1340 densitometer to a true density of 3.938 g/cm 3.
As shown in fig. 2, vickers hardness was measured with a home-made digital display micro vickers hardness tester under the following conditions: the diamond indenter, 200g load, dwell time 10 seconds, was tested at ten points and averaged to give a test result of 2151kgf/mm 2.
As shown in FIG. 3, the grain structure, including the sheet structure, was tested by scanning electron microscopy.
Example 2: the high viscosity Bao Shuishi product of this example was press-filtered to obtain a solid content of 40%, the cake drying temperature was 80 ℃, the 1000 g aqueous solution contained 26 g of neodymium nitrate hexahydrate, 33.9 g of yttrium nitrate hexahydrate, 26.6 g of lanthanum nitrate hexahydrate, 64.1 g of magnesium nitrate hexahydrate and 4.3 g of cobalt nitrate hexahydrate, respectively, the first calcination temperature and the second calcination temperature were 550 ℃, the post-impregnation drying temperature was 60 ℃, the sintering temperature was 1420 ℃, and the sintering time was 5 minutes, otherwise the same as in example 1.
The sintered particles were based on alumina, and the sum of yttria, neodymia, lanthana, magnesia, and cobalt oxide was 3.3%.
The ceramic corundum abrasive sintered in this example had a true density of 3.905 g/cm 3 and a View hardness of 2015kgf/mm 2.
FIG. 4 is a graph showing the Vickers hardness test of the ceramic corundum abrasive material prepared in this example.
Fig. 5 is a scanning electron microscope image of the ceramic corundum abrasive material prepared in this example, and the scanning electron microscope shows that the crystal structure contains a lamellar structure.
Example 3: the high viscosity Bao Shuishi product of this example was press-filtered to a solids content of 44%, the cake drying temperature was 140 ℃, the 1000 g aqueous solution contained 48.75 g neodymium nitrate hexahydrate, 63.6 g yttrium nitrate hexahydrate, 50.0 g lanthanum nitrate hexahydrate, 120.2 g magnesium nitrate hexahydrate and 3.4 g cobalt nitrate hexahydrate, respectively, the first and second calcination temperatures were 750 ℃, the post-impregnation drying temperature was 100 ℃, the sintering temperature was 1430 ℃, and the sintering time was 30 minutes, otherwise, as in example 1.
The sintered particles were based on alumina, and the sum of yttria, neodymia, lanthana, magnesia, and cobalt oxide was 6%.
The true density after sintering was 3.936 g/cm 3 and the View hardness was 2252kgf/mm 2.
FIG. 6 is a graph showing the Vickers hardness test of the ceramic corundum abrasive material produced in this example.
Fig. 7 is a scanning electron microscope image of the ceramic corundum abrasive material prepared in this example, and the scanning electron microscope shows that the crystal structure contains a lamellar structure.
Comparative example 1: the wet product high-viscosity pseudo-boehmite filter cake is obtained from Hunan Lishi new material Co., ltd, is a product produced normally, has a water content of 64% and a solid content of 36% detected, is not extruded to remove water, is directly dried, and is otherwise the same as in example 1.
The sintered product has a true density of 3.823 g/cm 3, which is too low to be used as an abrasive.
Comparative example 2: commercial ceramic corundum abrasive F46 produced by sol-gel method using nitric acid as a peptizing agent, a sample was taken from the company of grinding stock, tsingtaziy (Qingdao), and the true density was 3.916 g/cm 3, the Vickers hardness was 2100kgf/mm 2, and a scanning electron microscope picture was shown in FIG. 8 under the same conditions as in example 1.
By comparing fig. 3, 5, 7 and 8, the abrasives prepared in examples 1 to 3 are substantially the same as those of the abrasives prepared in comparative example 2, and the vickers hardness of examples 1 to 3 is also equivalent to that of comparative example 2. The quality of the ceramic corundum abrasive prepared by the preparation method is basically the same as that of the ceramic corundum abrasive produced by the traditional sol-gel method using nitric acid as a peptizing agent.

Claims (3)

1. The preparation process of the ceramic corundum abrasive is characterized by comprising the following steps:
1) Preparing a high-viscosity pseudo-boehmite wet product into a filter cake with the solid content of more than 40% in a squeezing and filtering mode, wherein the thickness of the filter cake is less than or equal to 10mm;
2) Drying the filter cake at 80-140 ℃, and naturally breaking the filter cake into fragments after drying;
3) Crushing the fragments, and screening particles between a 16-mesh screen and a 100-mesh screen after crushing;
4) Calcining the sieved particles at 550-750 ℃;
5) The calcined particles are introduced with modifier by an impregnation method to prepare an aqueous solution containing neodymium nitrate, lanthanum nitrate, yttrium nitrate, magnesium nitrate and cobalt nitrate, and the weight ratio of the calcined particles to the aqueous solution is 1:0.8, uniformly mixing the aqueous solution and the calcined particles;
6) Drying the immersed particles, removing the contained adsorbed water, wherein the drying temperature is 60-100 ℃;
7) Carrying out secondary calcination on the dried particles, wherein the calcination temperature is 550-750 ℃;
8) The calcined particles are further sintered for 5-30 minutes at 1420-1440 ℃.
2. A process for the preparation of a ceramic corundum abrasive material according to claim 1 characterized in that the fragments are crushed by means of a ball mill or a pulverizer or a twin-roll or a disc crusher.
3. The process for preparing a ceramic corundum abrasive according to claim 1 characterized in that the sintered particles are composed of 3.3% -6% of the sum of yttrium oxide, neodymium oxide, lanthanum oxide, magnesium oxide and cobalt oxide based on aluminum oxide.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109734427A (en) * 2019-02-18 2019-05-10 青岛瑞克尔新材料科技有限公司 A kind of carbide composite ceramic crystallite abrasive material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
ES2118161T3 (en) * 1993-04-30 1998-09-16 Hermes Schleifmittel Gmbh & Co CORINDON CERAMIC ABRASIVE MATERIAL.
CN1084314C (en) * 1995-04-05 2002-05-08 圣戈本陶瓷及塑料股份有限公司 Method for firing sol-gel alumina particles
CN104961446A (en) * 2015-06-16 2015-10-07 翟晨曦 Processing method for preparing boehmite for alpha-aluminum-oxide-based ceramic abrasive materials with sol gel technology
CN108675776A (en) * 2018-05-31 2018-10-19 青岛四砂泰益超硬研磨股份有限公司 Preparation method with laminated structure Ceramic corundum abrasive
CN110759719A (en) * 2019-07-09 2020-02-07 青岛汉兴环保科技有限公司 Diamond ceramic microcrystalline abrasive and preparation method thereof
RU2737169C1 (en) * 2020-03-10 2020-11-25 Федеральное государственное бюджетное учреждение науки Федеральный исследовательский центр "Кольский научный центр Российской академии наук" (ФИЦ КНЦ РАН) Method of producing corundum ceramics

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109734427A (en) * 2019-02-18 2019-05-10 青岛瑞克尔新材料科技有限公司 A kind of carbide composite ceramic crystallite abrasive material and preparation method thereof

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