CN113270270B - Anti-oxidation nickel slurry and preparation method and application thereof - Google Patents
Anti-oxidation nickel slurry and preparation method and application thereof Download PDFInfo
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- CN113270270B CN113270270B CN202110606865.2A CN202110606865A CN113270270B CN 113270270 B CN113270270 B CN 113270270B CN 202110606865 A CN202110606865 A CN 202110606865A CN 113270270 B CN113270270 B CN 113270270B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/005—Electrodes
- H01G4/008—Selection of materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
Abstract
The invention discloses an antioxidant nickel slurry and a preparation method and application thereof. The oxidation resistant nickel slurry comprises nickel powder, ceramic powder, a binder, a dispersant and a solvent, wherein the nickel powder is nickel oxide. According to the invention, nickel metal in the MLCC internal electrode slurry is replaced by nickel oxide, so that on one hand, the problem of easy oxidation of base metal is not considered, the upper limit value of the binder removal temperature is widened, high-temperature binder removal is realized, and the decomposition of organic additives is promoted, so that the carbon residue rate after MLCC binder removal is reduced, the oxidation problem in the internal electrode binder removal process is reduced, the generation of internal defects is reduced, and the MLCC internal electrode slurry has obvious positive effects on the improvement of the subsequent sintering yield and the reliability, and on the other hand, the finally obtained MLCC product can still maintain good electrical property.
Description
Technical Field
The invention relates to the field of electronic materials and components, in particular to antioxidant nickel paste and a preparation method and application thereof.
Background
Chip multilayer ceramic capacitors (MLCCs) are one of the most widely used passive components in downstream electronic components. In recent years, with the continuous development of technologies such as 5G, Internet, vehicle-mounted and the like, higher requirements are put forward on the electrical performance reliability of the MLCC, and researches show that the reduction of the carbon residue rate after the glue removal of the MLCC has obvious positive effects on the improvement of the subsequent sintering yield and the improvement of the reliability. However, in the current MLCC preparation process using base metal as inner electrode slurry, because base metal is easy to oxidize, the highest glue discharging temperature needs to be strictly controlled, and is mostly less than 300 ℃, and sintering needs to be carried out in non-oxidizing atmosphere or reducing atmosphere, which brings great difficulty to further reduce the carbon residue rate of the final product.
In order to reduce the carbon residue rate of MLCC, the main method used at present is to properly prolong the highest temperature heat preservation time, but because of the crosslinking carbonization of the binder macromolecule, the effect of prolonging the time at low temperature on reducing the carbon residue rate is very limited. Therefore, it is desired to develop a method for significantly reducing the carbon residue rate after the MLCC binder removal and improving the yield and reliability of the subsequent sintering while maintaining the good electrical properties of the final MLCC product.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the oxidation-resistant nickel slurry as well as the preparation method and the application thereof.
In order to achieve the above object, in a first aspect, the present invention provides an oxidation-resistant nickel paste comprising nickel powder, ceramic powder, a binder, a dispersant and a solvent, wherein the nickel powder is an oxide of nickel.
Preferably, the total weight of the nickel powder and the ceramic powder is 40-70% of the weight of the oxidation-resistant nickel slurry, and the weight of the nickel powder is 3-6 times of the weight of the ceramic powder.
Preferably, the weight of the nickel powder is 4.5-5.5 times of that of the ceramic powder.
Preferably, the weight of the adhesive is 1-13% of the total weight of the nickel powder and the ceramic powder, the weight of the dispersant is 0.3-2.5% of the total weight of the nickel powder and the ceramic powder, and the balance is the solvent.
Preferably, the weight of the adhesive is 4-7% of the total weight of the nickel powder and the ceramic powder.
Preferably, the viscosity of the antioxidant nickel slurry is 15000-60000 cps.
Preferably, the nickel powder is at least one of nickel protoxide and nickel oxide; the ceramic powder is SrTixZr1- xO3、ZrO2、BaTiO3Wherein x is more than or equal to 0 and less than 1; the adhesive mainly comprises a main body resin and a plasticizer, wherein the main body resin is at least one of acrylic resin, ethyl cellulose and polyvinyl butyral, and the plasticizer is at least one of polypropylene glycol diacetate, polyethylene glycol diacetate, phthalate, fatty diacid ester, tributyl citrate, acetylated tributyl citrate and rosin polyol ester; the dispersant is a solvent dispersant; the solvent is ethylene glycol monoalkyl ether, ethylene glycol dialkyl ether, polyethylene glycol monoalkyl ether, polyethylene glycol dialkyl ether, propylene glycol monoalkyl ether, propylene glycol dialkyl ether, polypropylene glycol monoalkyl ether, polypropylene glycol dialkyl ether, ethylene glycol monoalkyl ether carboxylate, polyethylene glycol monoalkyl ether carboxylate, propylene glycol monoalkyl ether, propylene glycol dialkyl ether carboxylate, propylene glycol etherAt least one of monoalkyl ether carboxylate, polypropylene glycol monoalkyl ether carboxylate, terpineol, dihydroterpinyl acetate, turpentine, dimethyl sulfoxide, N-methylpyrrolidone, cyclohexyl acetate, 2-methylcyclohexyl acetate, and 4-tert-butylcyclohexyl acetate.
In a second aspect, the invention provides a preparation method of the antioxidant nickel paste, which comprises the following steps:
(1) dissolving a binder in a part of solvent to obtain a binder solution;
(2) mixing and dispersing the ceramic powder, the dispersing agent and the residual solvent, adding the binder solution, and dispersing until no agglomeration exists to obtain a first slurry;
(3) and adding nickel powder into the first slurry, and dispersing until no agglomeration exists to obtain the oxidation-resistant nickel slurry.
In a third aspect, the present invention provides the use of the above-described oxidation-resistant nickel paste as an internal electrode paste for a chip multilayer ceramic capacitor.
Preferably, when the anti-oxidation nickel paste is used as the inner electrode paste to prepare the chip type multilayer ceramic capacitor, the highest glue discharging temperature is 350-600 ℃; preferably, degreasing is carried out in air, and sintering is carried out in a protective gas atmosphere, wherein the protective gas contains hydrogen with the volume fraction of 0.1-3.5%.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, nickel metal in the MLCC internal electrode slurry is replaced by nickel oxide, so that on one hand, the problem of easy oxidation of base metal is not considered, the upper limit value of the binder removal temperature is widened, high-temperature binder removal is realized, and the decomposition of organic additives is promoted, so that the carbon residue rate after MLCC binder removal is reduced, the oxidation problem in the internal electrode binder removal process is reduced, the generation of internal defects is reduced, and the MLCC internal electrode slurry has obvious positive effects on the improvement of the subsequent sintering yield and the reliability, and on the other hand, the finally obtained MLCC product can still maintain good electrical property.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
In the prior art, in order to prevent the oxidation of the inner electrode slurry and strictly control the highest glue discharging temperature in a lower range in the process of preparing the MLCC by using the inner electrode slurry containing base metal, the carbon residue rate of a final product is higher, in order to reduce the carbon residue rate after the MLCC glue discharging and improve the yield and reliability of subsequent sintering, the invention uses nickel oxide to replace nickel metal in the MLCC inner electrode slurry, thus, the problem of easy oxidation of base metal is not considered, the upper limit value of the binder removal temperature can be widened, high-temperature binder removal is realized, the decomposition of organic additives is promoted, thereby reducing the carbon residue rate after the MLCC rubber discharge, reducing the oxidation problem in the rubber discharge process of the inner electrode, reducing the generation of internal defects, the method has obvious positive effects on the improvement of the subsequent sintering yield and the improvement of the reliability, and meanwhile, the electrical performance of the MLCC product prepared by the method is not obviously different from that of the MLCC product prepared by adopting the elemental nickel as the nickel powder in the internal electrode slurry. Specifically, the oxidation resistant nickel slurry comprises nickel powder, ceramic powder, a binder, a dispersant and a solvent, wherein the nickel powder is nickel oxide.
The total weight of the nickel powder and the ceramic powder is 40-70% of the weight of the oxidation-resistant nickel slurry, the weight of the nickel powder is 3-6 times of the weight of the ceramic powder, and the weight of the nickel powder is preferably 4.5-5.5 times of the weight of the ceramic powder.
The weight of the adhesive is 1-13% of the total weight of the nickel powder and the ceramic powder. The weight of the adhesive is preferably 4-7% of the total weight of the nickel powder and the ceramic powder.
The weight of the dispersing agent is usually 0.3-2.5% of the total weight of the nickel powder and the ceramic powder.
The solvent is usually added in an amount of 14.5-58.7 wt% (i.e. the weight of the solvent is 14.5-58.7% of the weight of the antioxidant nickel slurry) to adjust the viscosity of the antioxidant nickel slurry to 15000-60000 cps.
The oxidation resistant nickel slurry of the invention can only consist of nickel powder, ceramic powder, adhesive, dispersant and solvent, and can also be added with other auxiliary agents besides the components.
In some embodiments, the nickel powder is selected from nickel protoxide (NiO), nickel oxide high (Ni)2O3) One or two of them.
The ceramic powder can be selected according to the type of ceramic wafer container, for one type of ceramic wafer container, SrTi is selectedxZr1-xO3(0≤x＜1)、ZrO2Ceramic powder is prepared; for the two types of ceramic wafers, BaTiO is selected3Etc., but the selectable kinds of the ceramic powder are not limited thereto.
The selection of the binder is not particularly critical and is generally composed mainly of a host resin and a plasticizer. The host resin is preferably at least one of acrylic resin (ACR), Ethyl Cellulose (EC), and polyvinyl butyral (PVB). The plasticizer is preferably at least one of polypropylene glycol diacetate, polyethylene glycol diacetate, phthalate, fatty diacid ester, tributyl citrate, acetylated tributyl citrate and rosin polyol ester. However, the selection of the host resin and the plasticizer is not limited to the above. In some embodiments, the adhesive is comprised of a host resin and a plasticizer.
The dispersant is a solvent-based dispersant. In some embodiments, the dispersant is a commercially available solvent-based dispersant such as bekk byk110, byk163, byk190, etc., digo 700, tego674, tego630, etc., germany, rohm and haas acumer3100, usa. The dispersant may be one or more selected from the above-listed dispersants, but the selectable kinds of dispersants are not limited thereto.
In some embodiments, the solvent is at least one of ethylene glycol monoalkyl ether, ethylene glycol dialkyl ether, polyethylene glycol monoalkyl ether, polyethylene glycol dialkyl ether, propylene glycol monoalkyl ether, propylene glycol dialkyl ether, polypropylene glycol monoalkyl ether, polypropylene glycol dialkyl ether, ethylene glycol monoalkyl ether carboxylate, polyethylene glycol monoalkyl ether carboxylate, propylene glycol monoalkyl ether carboxylate, polypropylene glycol monoalkyl ether carboxylate, terpineol, dihydroterpinyl acetate, turpentine, dimethyl sulfoxide, N-methylpyrrolidone, cyclohexyl acetate, 2-methylcyclohexyl acetate, 4-tert-butylcyclohexyl acetate. But the selectable kind of the solvent is not limited thereto.
In some embodiments, a method of preparing an oxidation resistant nickel paste comprises the steps of:
(1) dissolving a binder in a part of solvent to obtain a binder solution;
(2) mixing ceramic powder, a dispersing agent and the rest solvent, uniformly stirring, grinding for 6-8 hours by using a sand mill, adding the binder solution obtained in the step (1), uniformly stirring, grinding for 2-4 hours by using the sand mill, and dispersing until no agglomeration exists to obtain a first slurry;
(3) adding nickel powder (nickel oxide) into the first slurry obtained in the step (2), stirring for 2-4 h by using a planetary stirrer, grinding for 6-10 times by using a three-roll mill, and dispersing until no agglomeration exists, thus obtaining the oxidation-resistant nickel slurry. It should be noted that the preparation method of the oxidation resistant nickel slurry of the present invention is not limited to this process.
When the antioxidant nickel paste is used as an inner electrode paste to prepare a chip multilayer ceramic capacitor, the highest glue discharging temperature is preferably 350-600 ℃; the degreasing sintering is generally performed in a protective gas atmosphere. Preferably, the protective gas contains 0.1-3.5% of hydrogen by volume fraction. The protective gas can be at least one of nitrogen and inert gas, and is preferably nitrogen. The inert gas can be selected from argon and the like.
The MLCC product obtained by the invention is subjected to performance test by adopting the following test method:
1) capacity (Cp) and loss (Df): the capacitance meter (KEYSIGHT model E4981A) is set with voltage 1V, X7R for testing frequency 1KHZ and C0G for testing frequency 1 MHZ. The capacity (Cp) and loss (Df) were measured at 25 ℃ at room temperature.
2) Breakdown voltage (BDV): and the withstand voltage tester (YD9811A) sets the boosting speed of 6000V/30s and records the voltage of the product during breakdown.
3) Insulation Resistance (IR): resistance meter (agilent model 4339B), test conditions 0603X7R104C and 0402C0G 101A: charging at 50V for 60s, and recording an IR value; 1206COG 102F: the 630V was charged for 30s and the IR value recorded.
4) High Accelerated Life Test (HALT): capacitor high-temperature aging reliability test system, 0603X7R 104C: setting the temperature at 140 ℃, and maintaining the pressure at 300V for 12 h; 0402C0G 101A: setting the temperature at 140 ℃, and maintaining the pressure at 350V for 168 h; 1206COG 102F: the temperature is set at 140 ℃, and the pressure is maintained at 630V for 168 h. And if the product leakage current is larger than 10mA, alarming to fail, judging to be NG, respectively recording the product failure number, and calculating the ratio of the failure number.
Examples 1 to 5 and comparative examples 1 to 2
Examples 1 to 5 and comparative examples 1 to 2 each provide a nickel paste, wherein the nickel paste comprises the following components and the weight contents thereof are shown in table 1, wherein the average particle diameter of a nickel source (i.e., nickel oxide powder or elemental nickel powder) used in the 1206 specification is 600nm, the average particle diameter of a nickel source (i.e., nickel oxide powder or elemental nickel powder) used in the 0402 and 0603 specifications is 400nm, the average particle diameters of ceramic powders used in all examples and comparative examples are 100nm, acrylic resin is b-66 produced by dow chemical, polyvinyl butyral is b30t produced by kohly, ethyl cellulose is dt-n-50 produced by guang city courser biotechnology limited, a dispersant is german birk byk110, german birk byk163, german di hight 700, german dit hight 674, or U.S. roha haus acumer 3100. The preparation method of each of the nickel pastes of examples and comparative examples includes the following steps:
(1) dissolving a binder in part of the mixed solvent to obtain a binder solution;
(2) mixing the ceramic powder, the dispersing agent and the residual mixed solvent, stirring at 2000rpm for 1h, grinding by a sand mill at 1200rpm (the diameter of a grinded zirconia ball is 0.3mm) for 8h, adding the binder solution obtained in the step (1), stirring at 800rpm for 30min, and then grinding by the sand mill for 3.5h to obtain a first slurry without agglomeration;
(3) adding a nickel source into the first slurry obtained in the step (2), stirring for 3 hours at 800rpm by using a planetary stirrer, then passing through a three-roll mill with the roll spacing of 0.3-0.8 mm, grinding for 8 times at 500rpm, filtering and discharging to obtain the antioxidant nickel slurry.
MLCC was prepared using the nickel pastes obtained in each example and comparative example as inner electrode pastes, respectively, and the respective conditions of draining and sintering are shown in Table 2, wherein comparative examples 1-1 and comparative examples 1-2 each use the nickel paste obtained in comparative example 1 as an inner electrode. The conditions for removing the gel are described in example 1, and "460 ℃ for 2 h" is defined asThe gel is discharged for 2h at the maximum temperature of 460 ℃, and the descriptions of other examples and comparative examples are similar; the sintering conditions are described in example 1, namely 3% H at 1280 deg.C22H' refers to sintering at 1280 ℃ for 2H under the atmosphere of protective gas, wherein the protective gas consists of 3 vol% of H2And 97 vol% N2The composition, other examples and comparative examples are described similarly.
TABLE 1
TABLE 2
The MLCC products obtained in each embodiment and comparative example are subjected to an accelerated life test, and partial test results are shown in tables 3-5.
TABLE 3
TABLE 4
TABLE 5
It can be seen from the data in the above table that the MLCC product of the same specification has no obvious difference in electrical properties due to the use of nickel oxide as a nickel source and the use of simple substance nickel as a nickel source in the conventional method, that is, the electrical properties equivalent to those of the conventional process can be achieved by using the formulation and the preparation method of the present invention. The method has the advantages that the oxide of nickel is used as a nickel source, so that the upper limit value of the binder removal temperature can be widened, the binder removal can be carried out at a higher temperature, the purpose of reducing the carbon residue rate can be achieved, the generation of internal defects is reduced, and the reliability of the MLCC product is improved; as can be seen from the accelerated life test data, for products with different specifications, the reject ratio of the product prepared by the invention is obviously lower than that of the product prepared by the traditional formula process, and the reliability is obviously improved.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (4)
1. The application of the oxidation-resistant nickel slurry as the inner electrode slurry of the chip multilayer ceramic capacitor is characterized in that the oxidation-resistant nickel slurry comprises nickel powder, ceramic powder, a binder, a dispersant and a solvent, wherein the nickel powder is nickel oxide; when the anti-oxidation nickel slurry is used as an inner electrode slurry to prepare a chip multilayer ceramic capacitor, carrying out glue removal in the air, wherein the highest glue removal temperature is 350-600 ℃, and sintering is carried out in a protective gas atmosphere, wherein the protective gas contains hydrogen with the volume fraction of 0.1-3.5%; the total weight of the nickel powder and the ceramic powder is 40-70% of the weight of the antioxidant nickel slurry, and the weight of the nickel powder is 4.5-5.5 times of the weight of the ceramic powder; the weight of the adhesive is 4-7% of the total weight of the nickel powder and the ceramic powder, the weight of the dispersing agent is 0.3-2.5% of the total weight of the nickel powder and the ceramic powder, and the balance is the solvent.
2. The use according to claim 1, wherein the viscosity of the antioxidant nickel paste is 15000 to 60000 cps.
3. The use according to claim 1, wherein the nickel powder is at least one of nickel protoxide and nickel oxide; the ceramic powder is SrTixZr1-xO3、ZrO2、BaTiO3Wherein x is more than or equal to 0 and less than 1; the adhesive mainly comprises a main body resin and a plasticizer, wherein the main body resin is at least one of acrylic resin, ethyl cellulose and polyvinyl butyral, and the plasticizer is at least one of polypropylene glycol diacetate, polyethylene glycol diacetate, phthalate, fatty diacid ester, tributyl citrate, acetylated tributyl citrate and rosin polyol ester; the dispersant is a solvent dispersant; the solvent is at least one of ethylene glycol monoalkyl ether, ethylene glycol dialkyl ether, polyethylene glycol monoalkyl ether, polyethylene glycol dialkyl ether, propylene glycol monoalkyl ether, propylene glycol dialkyl ether, polypropylene glycol monoalkyl ether, polypropylene glycol dialkyl ether, ethylene glycol monoalkyl ether carboxylate, polyethylene glycol monoalkyl ether carboxylate, propylene glycol monoalkyl ether carboxylate, polypropylene glycol monoalkyl ether carboxylate, terpineol, dihydroterpinyl acetate, turpentine, dimethyl sulfoxide, N-methylpyrrolidone, cyclohexyl acetate, 2-methylcyclohexyl acetate and 4-tert-butylcyclohexyl acetate.
4. The use according to claim 1, wherein the preparation method of the oxidation-resistant nickel paste comprises the following steps:
(1) dissolving a binder in a part of solvent to obtain a binder solution;
(2) mixing and dispersing the ceramic powder, the dispersing agent and the residual solvent, adding the binder solution, and dispersing until no agglomeration exists to obtain a first slurry;
(3) and adding nickel powder into the first slurry, and dispersing until no agglomeration exists to obtain the oxidation-resistant nickel slurry.
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| CN114255904B (en) * | 2021-11-26 | 2023-07-14 | 中国电子产品可靠性与环境试验研究所（（工业和信息化部电子第五研究所）（中国赛宝实验室）） | Nickel electrode paste, resistor and preparation method of resistor |
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| JP2999304B2 (en) * | 1991-08-29 | 2000-01-17 | 第一工業製薬株式会社 | Conductor paste for ceramic capacitor electrodes |
| JP4986356B2 (en) * | 2000-02-18 | 2012-07-25 | カナディアン・エレクトロニクス・パウダーズ・コーポレーション | Method for producing nickel powder |
| JP4020764B2 (en) * | 2001-12-21 | 2007-12-12 | Ｊｆｅミネラル株式会社 | Super fine metal slurry with excellent dispersibility |
| JP3744427B2 (en) * | 2002-01-28 | 2006-02-08 | 株式会社村田製作所 | Manufacturing method of multilayer ceramic electronic component |
| JP2004183027A (en) * | 2002-12-02 | 2004-07-02 | Murata Mfg Co Ltd | Method for manufacturing nickel powder, nickel powder, electroconductive paste, and multilayered ceramic electronic component |
| JP4355169B2 (en) * | 2003-05-14 | 2009-10-28 | ナミックス株式会社 | Nickel oxide particle-containing electrode paste composition |
| KR101032344B1 (en) * | 2008-06-25 | 2011-05-02 | 삼화콘덴서공업주식회사 | Method for manufacturing paste for internal electrode of high multi layer ceramic capacitor |
| JP4968309B2 (en) * | 2009-10-06 | 2012-07-04 | Ｔｄｋ株式会社 | Paste composition, electronic component and method for producing multilayer ceramic capacitor |
| KR101565631B1 (en) * | 2012-06-04 | 2015-11-03 | 삼성전기주식회사 | Conductive paste composition for internal electrode, multilayer ceramic electronic capacitor and fabricating method thereof |
| CN103440982A (en) * | 2013-07-29 | 2013-12-11 | 无锡商业职业技术学院 | Preparation method for multilayer ceramic capacitor |
| CN103894623B (en) * | 2014-03-19 | 2016-08-17 | 深圳航天科技创新研究院 | A kind of preparation method of antioxidant ultrafine nickel powder |
| CN105304159B (en) * | 2014-07-08 | 2017-06-16 | 华中科技大学 | Electrode electrocondution slurry and its preparation method and application in multilayer sheet type ceramic component |
| KR102589697B1 (en) * | 2016-01-12 | 2023-10-16 | 도호 티타늄 가부시키가이샤 | nickel powder |
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Application publication date: 20210817 Assignee: CHAOZHOU THREE-CIRCLE (Group) Co.,Ltd. Assignor: Guangdong advanced ceramic material technology Co.,Ltd. Contract record no.: X2022980009887 Denomination of invention: An antioxidant nickel slurry and its preparation method and Application Granted publication date: 20220405 License type: Exclusive License Record date: 20220706 |