CN104400619B - Processing method for chemically and mechanically polishing tantalum by employing fixed abrasive - Google Patents

Processing method for chemically and mechanically polishing tantalum by employing fixed abrasive Download PDF

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Publication number
CN104400619B
CN104400619B CN201410556164.2A CN201410556164A CN104400619B CN 104400619 B CN104400619 B CN 104400619B CN 201410556164 A CN201410556164 A CN 201410556164A CN 104400619 B CN104400619 B CN 104400619B
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polishing
tantalum
processing method
abrasive
polishing fluid
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CN104400619A (en
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李军
宋龙龙
朱永伟
左敦稳
黄建东
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/04Lapping machines or devices; Accessories designed for working plane surfaces
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/11Lapping tools
    • B24B37/20Lapping pads for working plane surfaces
    • B24B37/24Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
    • B24B37/245Pads with fixed abrasives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/04Aqueous dispersions

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The invention discloses a processing method for chemically and mechanically polishing tantalum (Ta) by employing a fixed abrasive. The method is characterized by comprising the following steps: carrying out polishing on tantalum or a tantalum film by adopting a cerium oxide fixed abrasive polishing pad, controlling the polishing pressure to be 10-100kpa in the machining process, and controlling the rotating speed of a polishing disk to be 50-150rpm, wherein the polishing solution is composed of deionized water free of an abrasive, a surfactant, a complexing agent and a pH modifier; adjusting the pH value of the polishing solution to be 8 to 11; controlling the temperature of the polishing solution within a range of 20-30 DEG C, wherein the flow rate of the polishing solution is 80-150ml/min, so that the nano-precision surface roughness can be obtained, and the surface quality is excellent. According to the processing method disclosed by the invention, the processing efficiency and the surface quality of tantalum are improved; the qualified rate of the finished product is high; no environmental pollution is caused; the cleaning is easy and the cost is low.

Description

The processing method that a kind of concretion abrasive chemically-mechanicapolish polishes tantalum
Technical field
The present invention relates to the processing method of a kind of functional material tantalum (ta) or tantalum film, especially in integrated circuit, contain tantalum material The chemically mechanical polishing processing method of material, the processing method that specifically a kind of concretion abrasive chemically-mechanicapolish polishes tantalum.
Background technology
With the development of the high-tech industries such as network, communication, the requirement more and more higher to integrated circuit, inside integrated circuit Being planarized into of full wafer is located for core.In modern integrated circuits, characteristic size constantly reduces, in the multilayer wiring of copper, Mainly using tantalum as barrier layer, and every layer of etching will ensure that full wafer planarizes, and flattening effect directly affects entirely integrated The performance of circuit;Meanwhile, it is desirable to polishing fluid has selectivity so that copper and tantalum have suitable removal rate in the course of processing, Ensure global planarizartion.Chemically mechanical polishing (chemical mechanical polishing, abbreviation cmp) can reduce table Surface roughness, improves surface quality, realizes global planarizartion.Ta is a kind of hard metal material, Mohs' hardness 6 ~ 6.5, and It is inert material, fusing point is 2996 DEG C, there is high corrosion resistance, Precision Machining is difficult.
The processing of tantalum at present is substantially free abrasive chemically mechanical polishing.Chinese patent 102093817 discloses one kind Stop the chemical mechanical polishing liquid of polishing for tantalum.This polishing fluid comprise abrasive grains, organic acid, polyacrylic, metal delay Erosion agent, quaternary amine alkali, oxidant and water, this polishing fluid is directed to the removal rate improving barrier layer (ta or tan), prevents medal polish During produce local and general corrosion, this polishing fluid be acid polishing slurry, to equipment, there are corrosivity.Chinese patent 102010660 disclose a kind of preparation method of tantalum chemical mechanical polishing liquid.The preparation of this polishing fluid needs ultra-clean process, needs With using 18m ω ultra-pure deionized water, and it is stirred using negative pressure vortex, operating process is loaded down with trivial details it is desirable to condition is harsh.In State's patent 102782066 discloses a kind of chemical mechanical planarization method of the base material of cupric, ruthenium and tantalum layer.The main pin of the method To the base material containing copper, ruthenium and tantalum, take into account the polishing of three, be not directed to tantalum and chemically-mechanicapolish polished.Chinese patent 1312843 and 101535442 individually disclose free abrasive polishing fluid, are all containing copper, ruthenium and tantalum for chemically mechanical polishing Base material, the chemically mechanical polishing for tantalum do not have specific aim.It mostly is free abrasive chemically mechanical polishing above, technique is multiple Miscellaneous, high processing costs, working (machining) efficiency are low, and contain abrasive hardcoat particle in lapping liquid, and the surface tear after processing is serious, clearly Wash high cost.
Content of the invention
The purpose of the present invention is uncontrollable for surfacing clearance during existing free abrasive chemically mechanical polishing tantalum, Global planarizartion effect is poor, the tantalum piece complex process of free abrasive polishing simultaneously, in a large number using polishing fluid, high processing costs;Clear afterwards Wash difficulty, in polishing waste liquid and cleaning process a series of problems, such as a large amount of hazardous chemicals pollution environment, a kind of processing of invention Efficiency high, process is simple, the good finishing method of surface quality;Polishing fluid does not contain abrasive material, cleans simple, low the consolidating of processing cost afterwards The processing method that knot abrasive chemical mechanically polishes tantalum.And in polishing process, alkalescence polishing liquid is little to equipment damage, polishing fluid In phosphate radical can effectively suppress ta2o5Generation, cerium oxide concretion abrasive polishing pad can occur in the environment of alkalescence polishing liquid Chemical reaction, improves polishing speed.
The technical scheme is that
The processing method that a kind of concretion abrasive chemically-mechanicapolish polishes tantalum, is characterized in that: using concretion abrasive polishing pad to tantalum It is polished processing, control polish pressure in the course of processing between 10 ~ 100 kpa, the rotating speed of polishing pad controls 50 ~ Between 150rpm, the ph value of polishing fluid adjusts between 8 ~ 11, the temperature control of polishing fluid in the range of 20 ~ 30 DEG C, polishing fluid Flow velocity, between 80 ~ 150 ml/min, meets sets requirement up to surface quality.
Described consolidation polishing pad is cerium oxide concretion abrasive polishing pad, and the granularity of concretion abrasive is not more than 5 microns.
Described polishing fluid is deionized water without abrasive material, surfactant, chelating agent and ph regulator composition, surface The volume fraction of activating agent is 0.1%-1.0%, and the mass fraction of chelating agent is 0.5%-5.0%, and balance of deionized water and ph adjust Section agent.
The surfactant of described polishing fluid is that alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether or nonyl phenol gather One of oxygen vinyl Ether or more than one combination.
The chelating agent of described polishing fluid is one of ethylenediamine tetraacetic methene sodium phosphate, tartaric acid or triethanolamine or one Plant above combination.
The ph value regulator of described polishing fluid is phosphoric acid, acetic acid, citric acid, ammonia, hydroxylamine, Tetramethylammonium hydroxide Or one of ethylenediamine or more than one combination.
The invention has the beneficial effects as follows:
The concretion abrasive chemical Mechanical Polishing Technique of the present invention combines non-abrasive polishing solution and concretion abrasive polishing pad, polishing Do not contain hard abrasive material in liquid, surface will not be caused to scratch, improve polishing speed and workpiece surface quality, equipment and workpiece Cleaning is also relatively simple.Effectively solve a difficult problem for polishing tantalum surface planarization, while improve polishing speed, effectively Ensure surface quality.Meanwhile, concretion abrasive cmp tantalum, does not have abrasive material in polishing fluid, the chemical action of polishing fluid plays main work With being aided with mechanical grinding, high in machining efficiency, surface clearance is high, and reaction is easily controlled.
Meanwhile, the concretion abrasive chemical Mechanical Polishing Technique of the present invention can be widely applied to quasiconductor, hard metal, easily oxygen The polishing of the materials such as the metal material changed, the surface damage after processing is little, surface quality is high, and flattening effect is good.
The concretion abrasive polishing of the present invention, compared with traditional free abrasive polishing, abrasive material is fixedly arranged on polishing pad, is difficult Produce cut, pit equivalent damage, no sub-surface damage, surface quality is high, flattening effect is good.And tradition free abrasive polishing tantalum Piece, surface clearance is difficult to control to, and surface planarisation effect is poor.Meanwhile, the polishing fluid of selection and concretion abrasive polishing pad base Body occurs appropriate chemical reaction to realize the self-correction of polishing pad in the course of processing, improves working (machining) efficiency.
The abrasive material of the present invention is fixedly arranged on polishing pad, and abrasive material utilization rate is high;Meanwhile, also greatly reduce post processing workload With cost, decrease a large amount of pollutions to environment for the hazardous chemicals in polishing waste liquid and cleaning process.And free abrasive polishing During, abrasive material utilization rate is low, and working (machining) efficiency is not high, abrasive material random distribution, and distribution density is uneven, causes surface of the work to planarize Effect is poor, and workpiece face shape is difficult to control to;A large amount of hazardous chemicals pollution environment in polishing waste liquid and cleaning process, post processing is multiple Miscellaneous and high cost.
Specific embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment one.
The processing method that a kind of concretion abrasive chemically-mechanicapolish polishes tantalum:
First prepare polishing fluid, using 0.1kg fatty alcohol-polyoxyethylene ether, 0.05kg tartaric acid taking 10kg as a example, go from Sub- water 9.84kg, then with appropriate Tetramethylammonium hydroxide (or citric acid, phosphoric acid, ammonia, ethylenediamine, acetic acid, citric acid, ammonia Water, hydroxylamine or ethylenediamine) adjust polishing fluid ph value be 8.5, obtain the polishing fluid of about 10kg;
Secondly, tantalum piece is polished process for 3 μm of cerium oxide concretion abrasive polishing pads using granularity, controls in the course of processing Polish pressure processed is 21kpa, and the speed setting of polishing disk is 80rpm, and the solute component of polishing fluid is that the temperature of polishing fluid sets For 25 DEG C, polishing fluid flow rate set is 100 ml/min.Tantalum is polished using this polishing fluid and technological parameter, obtains surface roughness For 2.56nm, tantalum metal polishing rate height, surface no abrasive particle scratches, and flattening effect is good, and surface quality is excellent.
Embodiment two.
The processing method that a kind of concretion abrasive chemically-mechanicapolish polishes tantalum:
First, prepare polishing fluid, using 0.01kg alkylphenol polyoxyethylene, 0.2kg ethylenediamine tetramethyl taking 10kg as a example Fork sodium phosphate, deionized water 9.79kg, then with appropriate phosphoric acid (or citric acid, ammonia, ethylenediamine, acetic acid, citric acid, ammonia, Hydroxylamine, Tetramethylammonium hydroxide or ethylenediamine) adjust polishing fluid ph value be 10 polishing fluids obtaining about 10kg;
Secondly, substrate tantalum film is polished process for 1 μm of cerium oxide concretion abrasive polishing pad with granularity, in the course of processing Control polish pressure is 28kpa, and the speed setting of polishing disk is 100rpm, and the temperature of polishing fluid is set as 25 DEG C, polishes liquor stream Speed is set as 120ml/min.Tantalum is polished using this polishing fluid and technological parameter, acquisition surface roughness is 1.32nm, tantalum metal Polishing speed is high, and surface no abrasive particle scratches, and flattening effect is good, and surface quality is excellent.
Embodiment three.
The processing method that a kind of concretion abrasive chemically-mechanicapolish polishes tantalum:
Prepare polishing fluid first, using 0.5kg alkylphenol polyoxyethylene, 0.5kg ethylenediamine tetraacetic methene taking 10kg as a example Sodium phosphate, deionized water 9.44kg, then with appropriate citric acid (or phosphoric acid, ammonia, ethylenediamine, acetic acid, citric acid, ammonia, hydroxyl Base amine, Tetramethylammonium hydroxide or ethylenediamine) adjust polishing fluid ph value be 11 polishing fluids obtaining about 10kg;
Secondly, tantalum piece is polished process for 5 μm of cerium oxide concretion abrasive polishing pads with granularity, controls in the course of processing Polish pressure is 34kpa, and the speed setting of polishing disk is 120rpm, and the temperature of polishing fluid is set as 25 DEG C, and polishing flow velocity sets It is set to 100ml/min.Tantalum is polished using this polishing fluid and technological parameter, acquisition surface roughness is 3.57nm, tantalum medal polish Speed is high, and surface no abrasive particle scratches, and flattening effect is good, and surface quality is excellent.
Example IV.
The processing method that a kind of concretion abrasive chemically-mechanicapolish polishes tantalum:
First, prepare polishing fluid, using 0.08kg NPE, 0.1kg triethanolamine taking 10kg as a example, Deionized water 9.81kg, then with appropriate hydroxylamine (or phosphoric acid, citric acid, ammonia, ethylenediamine, acetic acid, citric acid, ammonia, four Ammonium hydroxide or ethylenediamine) adjust polishing fluid ph value be 8, the polishing fluid obtaining about 10kg is standby;
Secondly, tantalum film is polished process for 2 μm of cerium oxide concretion abrasive polishing pads with granularity, controls in the course of processing Polish pressure is 10kpa, and the speed setting of polishing disk is 50rpm, and the temperature of polishing fluid is set as 30 DEG C, polishing fluid flow rate set For 150 ml/min.Tantalum is polished using this polishing fluid and technological parameter, acquisition surface roughness is 1.18nm, tantalum medal polish speed Rate is high, and surface no abrasive particle scratches, and flattening effect is good, and surface quality is excellent.
Embodiment five.
The processing method that a kind of concretion abrasive chemically-mechanicapolish polishes tantalum:
First, prepare polishing fluid, using 0.1kg NPE, 0.5kg tartaric acid taking 10kg as a example, go from Sub- water 9.39kg, then with appropriate acetic acid (or hydroxylamine, phosphoric acid, citric acid, ammonia, ethylenediamine, citric acid, ammonia, tetramethyl Ammonium hydroxide or ethylenediamine) adjust polishing fluid ph value be 9, the polishing fluid obtaining about 10kg is standby;
Secondly, tantalum film is polished process for 4 μm of cerium oxide concretion abrasive polishing pads with granularity, controls in the course of processing Polish pressure is 100kpa, and the speed setting of polishing disk is 150rpm, and the temperature of polishing fluid is set as 20 DEG C, and polishing flow velocity sets It is set to 80 ml/min.Tantalum is polished using this polishing fluid and technological parameter, acquisition surface roughness is 1.25nm, tantalum medal polish Speed is high, and surface no abrasive particle scratches, and flattening effect is good, and surface quality is excellent.
The formula of cerium oxide concretion abrasive polishing pad of the present invention can adopt the Application No. of applicant's earlier application Slightly do change on the basis of the formula of 201010145260.x to be achieved, its preparation method can refer to the phase of applicant's earlier application Close the preparation method of concretion abrasive polishing pad.
Part that the present invention does not relate to is all same as the prior art or can be realized using prior art.

Claims (5)

1. the processing method that a kind of concretion abrasive chemically-mechanicapolish polishes tantalum, is polished to tantalum adding using concretion abrasive polishing pad Work, controls polish pressure between 10 ~ 100 kpa in the course of processing, the rotating speed of polishing pad controls between 50 ~ 150rpm, throws The ph value of light liquid adjusts between 8 ~ 11, and, in the range of 20 ~ 30 DEG C, polishing flow velocity is 80 ~ 150 for the temperature control of polishing fluid Between ml/min, until surface quality meets sets requirement, it is characterized in that: described polishing fluid is the deionization without abrasive material Water, surfactant, chelating agent and ph regulator composition, the volume fraction of surfactant is 0.1%-1.0%, the matter of chelating agent Amount fraction is 0.5%-5.0%, balance of deionized water and ph regulator.
2. processing method according to claim 1 is it is characterised in that described concretion abrasive polishing pad consolidates for cerium oxide Abrasive polishing pad, the granularity of concretion abrasive is not more than 5 microns.
3. processing method according to claim 1 is it is characterised in that the surfactant of described polishing fluid is alkyl phenol One of polyoxyethylene ether, fatty alcohol-polyoxyethylene ether or NPE or more than one combination.
4. processing method according to claim 1 is it is characterised in that the chelating agent of described polishing fluid is ethylenediamine tetramethyl One of fork sodium phosphate, tartaric acid or triethanolamine or more than one combination.
5. processing method according to claim 1 is it is characterised in that the ph value regulator of described polishing fluid is phosphoric acid, second One of acid, citric acid, ammonia, hydroxylamine, Tetramethylammonium hydroxide or ethylenediamine or more than one combination.
CN201410556164.2A 2014-10-20 2014-10-20 Processing method for chemically and mechanically polishing tantalum by employing fixed abrasive Active CN104400619B (en)

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CN106078487A (en) * 2016-06-07 2016-11-09 大连理工常州研究院有限公司 Nickel-base alloy solidified abrasive grinding and cmp method

Citations (4)

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Publication number Priority date Publication date Assignee Title
CN101468448A (en) * 2007-12-28 2009-07-01 安集微电子(上海)有限公司 Chemical mechanical polishing technological process
CN102172879A (en) * 2011-02-23 2011-09-07 南京航空航天大学 Method for processing soft and crisp LBO crystals based on consolidated abrasive polishing pad
CN103252708A (en) * 2013-05-29 2013-08-21 南京航空航天大学 Sapphire substrate ultraprecision machining method based on fixed abrasive pad
CN103921205A (en) * 2014-04-04 2014-07-16 德清晶辉光电科技有限公司 Production process of 6-inch lithium niobate or lithium tantalite chips

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Publication number Priority date Publication date Assignee Title
US6419553B2 (en) * 2000-01-04 2002-07-16 Rodel Holdings, Inc. Methods for break-in and conditioning a fixed abrasive polishing pad

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101468448A (en) * 2007-12-28 2009-07-01 安集微电子(上海)有限公司 Chemical mechanical polishing technological process
CN102172879A (en) * 2011-02-23 2011-09-07 南京航空航天大学 Method for processing soft and crisp LBO crystals based on consolidated abrasive polishing pad
CN103252708A (en) * 2013-05-29 2013-08-21 南京航空航天大学 Sapphire substrate ultraprecision machining method based on fixed abrasive pad
CN103921205A (en) * 2014-04-04 2014-07-16 德清晶辉光电科技有限公司 Production process of 6-inch lithium niobate or lithium tantalite chips

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