CN215004841U - Measure device of diaphragm infiltration nature - Google Patents
Measure device of diaphragm infiltration nature Download PDFInfo
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- CN215004841U CN215004841U CN202120235223.1U CN202120235223U CN215004841U CN 215004841 U CN215004841 U CN 215004841U CN 202120235223 U CN202120235223 U CN 202120235223U CN 215004841 U CN215004841 U CN 215004841U
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- 230000008595 infiltration Effects 0.000 title abstract description 16
- 238000001764 infiltration Methods 0.000 title abstract description 16
- 238000012360 testing method Methods 0.000 claims abstract description 42
- 239000003792 electrolyte Substances 0.000 claims abstract description 31
- 239000012528 membrane Substances 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 abstract description 11
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 13
- 238000007689 inspection Methods 0.000 description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 206010066054 Dysmorphism Diseases 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The utility model provides a device for measuring the wettability of a diaphragm, which comprises a power supply, a test groove and a voltage and time measuring part; the test slot comprises a clamping assembly and electrolyte; the clamping assembly is internally provided with a tension area acting on the diaphragm, and the diaphragm is clamped in the clamping assembly; when the wettability of the diaphragm is measured, the clamping assembly clamped with the diaphragm is immersed in electrolyte; and the voltage and time measuring part is connected to two ends of the test groove, is electrically connected with the power supply and is used for measuring and recording the real-time voltage of the diaphragm and the corresponding time of the real-time voltage. Compared with the prior art, the testing groove of the device simulates the stress condition of the diaphragm in the battery cell by simulating the arrangement of the diaphragm in the battery cell, and then the real-time voltage and the corresponding time of the measuring piece testing the diaphragm reflect the change of the infiltration of the diaphragm along with the time, so that the liquid absorption speed of the diaphragm is reflected, and the infiltration problem of the diaphragm is quantitatively measured.
Description
Technical Field
The utility model relates to a lithium cell field, concretely relates to measure device of diaphragm infiltration nature.
Background
The lithium ion battery has the advantages of high specific energy, no memory effect, excellent cycle life and the like, is widely applied to various electronic devices such as digital cameras, mobile phones, tablet computers, unmanned aerial vehicles and the like, is continuously developed to the field of new energy automobiles, and is an important driving force for the development of electrochemical energy storage devices. Meanwhile, the requirement of higher energy density and higher current quick-charging performance becomes one of the important technical challenges in the development of the current lithium ion battery.
The lithium battery comprises a positive electrode, a negative electrode, electrolyte and a diaphragm, wherein the diaphragm is positioned between the positive electrode and the negative electrode, the diaphragm has electronic insulation, and the diaphragm is used for separating the positive electrode from the negative electrode, preventing active substances from migrating, avoiding self-discharge and prolonging the service life. The infiltration capacity of the pole piece and the diaphragm of the lithium battery to the electrolyte can affect the capacity and the cycle life of the battery, and particularly under the condition of high-rate charging, the long-term cycle performance of the battery can be greatly affected if the diaphragm cannot be well infiltrated by the electrolyte.
The current method for judging the wettability of the diaphragm mainly comprises three methods:
1) and (3) dropping a typical electrolyte on the surface of the diaphragm, and checking whether the electrolyte disappears rapidly, if so, explaining that the wettability basically meets the requirement. However, this method can only qualitatively compare the wettability of the diaphragm and is greatly influenced by human factors.
2) The contact angle between the separator and the electrolyte is measured by dropping the electrolyte on the separator, and the smaller the contact angle, the better the wettability of the separator is. However, this method requires accurate measurement of the contact angle, and the separator has a high wetting rate with the electrolyte, which makes it difficult to accurately measure the contact angle.
3) And recording the process from the contact of the electrolyte with the diaphragm to the disappearance of the electrolyte by using a super-high resolution camera, and comparing the wettability of different diaphragms by time. Although the method has high accuracy, the method needs large cost investment and is complex to operate, and the method is not beneficial to operation in actual production of enterprises.
In view of the above, it is necessary to provide a technical solution to the above problems.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a: the utility model provides a measure device of diaphragm wettability, solves present diaphragm wettability testing arrangement operation complicacy, the unable problem of comparatively accurate reaction diaphragm wettability.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
an apparatus for measuring wettability of a diaphragm, comprising:
a power source;
a test slot comprising a clamping assembly and electrolyte; a tension area acting on the diaphragm is arranged in the clamping assembly, and the diaphragm is clamped in the clamping assembly; when the wettability of the diaphragm is measured, the clamping assembly clamped with the diaphragm is immersed in the electrolyte;
and the voltage and time measuring pieces are connected to two ends of the test groove, electrically connected with the power supply and used for measuring and recording the real-time voltage of the diaphragm and the corresponding time of the real-time voltage.
Preferably, the voltage and time measuring element is a polling device.
Preferably, the clamping assembly comprises at least two clamping pieces, two adjacent clamping pieces are respectively provided with an opening area, the opening areas are arranged oppositely, and the diaphragm covers the opening areas so as to simulate the stress of the diaphragm in the battery core.
Preferably, the opening area is located in the middle of the clamping piece, and the two opening areas are the same in size.
Preferably, a plurality of diaphragms are clamped between two adjacent clamping pieces.
Preferably, the test slot is further provided with heating members for providing different ambient temperatures for the membrane.
Preferably, the groove body of the test groove is provided with at least two positions by adopting metal connecting plates. The metal connecting plate can be a platinum plate and/or a silver plate, and the metal connecting plate should be free from reaction with electrolyte and conductive, so that the voltage and time measuring part can be connected to two ends of the test slot, the real-time voltage of the diaphragm can be detected, and a test result can be guaranteed. Preferably, the metal connecting plate may be a platinum plate. Of course, the metal connecting plate may be made of other materials which do not react with the electrolyte and can conduct electricity.
Compared with the prior art, the beneficial effects of the utility model reside in that: the utility model provides a testing arrangement, the test groove of this device is through simulating the setting of diaphragm in electric core, and the atress condition of tensile district simulation in electric core, then through the real-time voltage of measuring test diaphragm and its corresponding time, reflects the change of the infiltration of diaphragm along with time, and then reflects the diaphragmatic imbibition speed, and the diaphragm's infiltration nature problem is measurationally measured.
Drawings
Fig. 1 is a circuit diagram of the testing device of the present invention.
Fig. 2 is a schematic structural diagram of the measuring device of the present invention.
FIG. 3 is a graph of voltage and resistance over time for a single layer diaphragm test.
FIG. 4 is a graph of voltage and resistance over time for a three-layer diaphragm test.
In the figure: 1-a test slot; 11-a clamp; 111-open area; 12-a metal connecting plate; 13-a heating element; 2-voltage and time measurement.
Detailed Description
In order to make the technical solutions and advantages of the present invention clearer, the present invention and its advantageous effects will be described in further detail below with reference to the accompanying drawings of the detailed description and the specification, but the present invention is not limited thereto.
In the description of the present invention, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "fixed" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The utility model discloses the standard part that uses all can purchase from the market, and dysmorphism piece all can be customized according to the description with the record of drawing of description, and the concrete connection mode of each part all adopts conventional means such as ripe bolt, rivet, welding among the prior art, and machinery, part and equipment all adopt prior art, and conventional model, including circuit connection adopts conventional connection mode among the prior art, does not detailed here again.
As shown in fig. 1 to 4, a device for measuring membrane wettability comprises a power supply, a test slot 1 and a voltage and time measuring part 2; the test slot 1 comprises a clamping assembly and electrolyte; the clamping assembly is internally provided with a tension area acting on the diaphragm, and the diaphragm is clamped in the clamping assembly; when the wettability of the diaphragm is measured, the clamping assembly clamped with the diaphragm is immersed in electrolyte; the voltage and time measuring part 2 is connected to two ends of the test slot 1, is electrically connected with the power supply, and is used for measuring and recording the real-time voltage of the diaphragm and the corresponding time of the diaphragm. Wherein, the power supply is a stabilized voltage power supply as a current source of the whole device.
Further, the voltage and time measuring part 2 is a patrol instrument. After the voltage is measured by the inspection instrument, the change curve of the voltage can be displayed according to time, the liquid absorption speed of the diaphragm can be reflected through the curve, and then the wettability of the diaphragm is quantitatively measured. Wherein the inspection instrument is a voltage-stabilizing inspection instrument.
Further, the clamping assembly comprises at least two clamping pieces 11, two adjacent clamping pieces 11 are respectively provided with an opening area 111, the opening areas 111 are arranged oppositely, and the membrane covers the opening areas 111 so as to simulate the stress of the membrane in the battery core. The aperture of the open region 111 is 40 to 60 mm. Preferably, the opening region 111 is located in the middle of the clamping member 11, and the two opening regions 111 have the same size. During testing, the two clamping pieces 11 need to clamp the diaphragm to ensure that the diaphragm is in close contact with each other, and then the stress condition of the diaphragm in an actual electric core can be simulated by utilizing the arrangement of the opening area 111. Meanwhile, because the clamping pieces 11 clamp the diaphragm and need to be in contact with the electrolyte, the clamping pieces are made of high polymer which does not react with the electrolyte, and the two clamping pieces 11 can be tightly connected.
Further, a plurality of diaphragms are clamped between two adjacent clamping members 11. The multilayer diaphragm is placed at one time, so that the problem that the single-layer diaphragm cannot be accurately measured due to too high infiltration rate can be effectively solved, and meanwhile, the error value caused by uneven distribution of the diaphragm pores is effectively eliminated. As shown in fig. 3 to 4, in the test of one layer of the diaphragm, the voltage drop time is fast, and as the number of layers of the diaphragm increases, the voltage drop time is shifted backward, and the complete infiltration time is increased, so that the experimenter can better record the change condition, and the voltage change condition is more convenient for comparing the difference of the infiltration rates of different diaphragms. Wherein, the test result of FIGS. 3-4 is 1.3g/cm3The aqueous potassium hydroxide solution of (a) was used as a test solution.
Furthermore, the test slot 1 is provided with heating elements 13 for providing different ambient temperatures for the membrane. The real-time voltage of the diaphragm at different temperatures is measured by adjusting the environmental temperature of the diaphragm, so that the real-time voltage of the diaphragm can be recorded more accurately, a plurality of groups of temperatures are set for testing, and the infiltration condition of the diaphragm can be judged more comprehensively.
Further, the groove body of the test groove 1 is provided with at least two metal connecting plates 12. The metal connecting plate 12 may be a platinum plate and/or a silver plate, and the metal connecting plate 12 should be free from reaction with the electrolyte and conductive, so that the voltage and time measuring part 2 may be connected to both ends of the test slot 1 to detect the real-time voltage of the membrane, thereby ensuring the test result. Preferably, the metal connecting plate 12 may be a platinum plate. Of course, the metal connecting plate 12 may be made of other materials that do not react with the electrolyte and are conductive. Specifically, the left end and the right end of the groove body of the test groove 1 are made of platinum plates, and the rest of the groove body is made of inorganic glass.
With the testing device, the specific testing method comprises the following steps:
s1, connecting a circuit according to the diagram shown in FIG. 1, wherein the indication of the inspection instrument is the voltage brought by the constant voltage and electrolyte fixed by the inspection instrument, adjusting the inspection instrument to a blank voltage, specifically, tightly connecting the clamping components, inserting the clamping components into the test slot 1, the indication of the inspection instrument is the voltage brought by the clamping components, recording the voltage as the blank voltage, and taking out the clamping components for drying for later use; the blank voltage is adjusted mainly for adjusting the constant voltage fixed by the measuring instrument and the voltage brought by the test slot 1, so that the influence of the voltages on the test result is avoided, and the measurement error is reduced;
s2, after the voltage is stabilized, putting the dried diaphragm into a clamping assembly, ensuring that the diaphragm can completely cover the opening region 111, and ensuring that the diaphragm in the opening region 111 is flat and has certain tension so as to simulate the stress condition of the diaphragm in the battery cell;
and S3, rapidly and completely immersing the assembled clamping assembly in electrolyte, and recording the voltage change condition of the diaphragm with time by a patrol instrument in real time. When the diaphragm is not soaked, the diaphragm is an insulator, the resistance is large, the circuit is basically completely cut off, and the testing device is not communicated; when the diaphragm is in contact with the electrolyte, the circuit is conducted, the voltage rapidly reaches a maximum value, the resistance of the diaphragm is gradually reduced along with the wetting of the diaphragm, the voltage at two ends of the diaphragm is gradually reduced, the voltage is not changed after the diaphragm is completely wetted, and the diaphragm is restored to a stable state. At the moment, the liquid absorption speed of the diaphragm can be reflected by a voltage change curve displayed on the polling instrument, so that the wettability of the diaphragm can be quantitatively measured, and the voltage reduction rate is higher as the wetting speed of the diaphragm is higher.
The principle of the method is as follows: according to WasThe hburn equation reflects the change of the infiltration of the diaphragm along with time by monitoring the change of voltage and resistance along with time in the infiltration process of the diaphragm, so that the problem of the infiltration of the diaphragm is accurately reflected. The Washburn equation is: h ═ k × t1/2(ii) a h is the diffusion height in the capillary, which is indirectly characterized by the voltage of the membrane; k is the diffusion rate of the electrolyte in the separator; t is the diffusion time.
Specifically, the derivation formula of the Washburn equation is as follows: dh/dt ═ r2/8ηh)*[(2γcosθ/r)-Δρgh]When r is small, the two sides are integrated to obtain h ═ k × (t)1/2And k is (r γ cos θ/2 η)1/2(ii) a Where r is the capillary radius, η is the interfacial surface tension, γ is the liquid viscosity (electrolyte viscosity), θ is the contact angle, and Δ ρ is the change in liquid-solid areal density.
Compared with the existing measuring method, the measuring method is simpler and more convenient, and can quickly and accurately measure the infiltration condition of the diaphragm in the electrolyte. In the Washburn equation, because the diaphragm is a non-uniform porous material and is difficult to directly and accurately measure the h value, the voltage of the diaphragm is used for indirectly representing the test, the diaphragm is soaked in the electrolyte at the beginning, because the diaphragm is basically in an insulating state and has larger resistance, a circuit is basically and completely cut off, the voltage quickly reaches a maximum value, the resistance of the diaphragm is gradually reduced along with the gradual soaking of the diaphragm, the voltage at two ends of the diaphragm is gradually reduced, the voltage is not changed after the diaphragm is completely soaked and is recovered to a stable state, and the liquid suction speed of the diaphragm can be reflected by the change of the real-time voltage along with the time, so the wettability of the diaphragm can be quantitatively measured by the method.
Variations and modifications to the above-described embodiments may become apparent to those skilled in the art from the disclosure and teachings of the above description. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious modifications, replacements or variations made by those skilled in the art on the basis of the present invention belong to the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (8)
1. An apparatus for measuring wettability of a diaphragm, comprising:
a power source;
a test slot (1) comprising a clamping assembly and electrolyte; a tension area acting on the diaphragm is arranged in the clamping assembly, and the diaphragm is clamped in the clamping assembly; when the wettability of the diaphragm is measured, the clamping assembly clamped with the diaphragm is immersed in the electrolyte;
and the voltage and time measuring part (2) is connected to two ends of the test slot (1), is electrically connected with the power supply and is used for measuring and recording the real-time voltage of the diaphragm and the corresponding time of the real-time voltage.
2. Device for measuring the wettability of a membrane according to claim 1, wherein said voltage and time measuring element (2) is a polling device.
3. The device for measuring membrane wettability according to claim 1, wherein the clamping assembly comprises at least two clamping pieces (11), each of two adjacent clamping pieces (11) is provided with an open area (111), the open areas (111) are arranged oppositely, and the membrane covers the open areas (111) so as to simulate the stress of the membrane in the cell.
4. Device for measuring membrane wettability according to claim 3, wherein said perforated region (111) is located in the middle of said clamping member (11), and the two perforated regions (111) are of the same size.
5. Device for measuring membrane wettability according to claim 4, wherein several membranes are clamped between two adjacent clamping members (11).
6. Device for measuring the wettability of membranes according to any one of claims 1 to 5, wherein heating elements (13) are also arranged in the test slot (1) for providing different ambient temperatures to the membranes.
7. Device for measuring the wettability of membranes according to claim 1, wherein the housing of the test slot (1) has at least two places arranged by means of metal connecting plates (12).
8. Device for measuring the wettability of a membrane according to claim 7, wherein said metal connecting plate (12) is a platinum and/or silver plate.
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CN112834393A (en) * | 2021-01-28 | 2021-05-25 | 惠州锂威新能源科技有限公司 | A method and device for measuring diaphragm wettability |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112834393A (en) * | 2021-01-28 | 2021-05-25 | 惠州锂威新能源科技有限公司 | A method and device for measuring diaphragm wettability |
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