CN104630730A - Surface modification method of NiTi alloy martensitic root canal file - Google Patents
Surface modification method of NiTi alloy martensitic root canal file Download PDFInfo
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- CN104630730A CN104630730A CN201510086536.4A CN201510086536A CN104630730A CN 104630730 A CN104630730 A CN 104630730A CN 201510086536 A CN201510086536 A CN 201510086536A CN 104630730 A CN104630730 A CN 104630730A
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- root canal
- canal file
- niti alloy
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- martensite
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- 210000004262 dental pulp cavity Anatomy 0.000 title claims abstract description 69
- 229910001000 nickel titanium Inorganic materials 0.000 title claims abstract description 35
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 32
- 239000000956 alloy Substances 0.000 title claims abstract description 32
- 229910000734 martensite Inorganic materials 0.000 title claims abstract description 32
- 238000002715 modification method Methods 0.000 title abstract 5
- 238000000576 coating method Methods 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 17
- 238000004544 sputter deposition Methods 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 8
- 238000005477 sputtering target Methods 0.000 claims description 8
- 239000013077 target material Substances 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000000137 annealing Methods 0.000 abstract description 6
- 239000010410 layer Substances 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000005275 alloying Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910001080 W alloy Inorganic materials 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a surface modification method of a NiTi alloy martensitic root canal file. According to the method, a metal coating is deposited on the surface of the root canal file by use of a magnetic sputtering process; annealing treatment is performed under the conditions that a vacuum degree is not lower than 10<-3>Pa and the temperature is 600-900 DEG C, so that the metal elements of the coating are diffused to enter a martensitic root canal file substrate, the surface of the root canal file is a parent phase at the operating temperature, and martensite is formed inside the root canal file. The surface modification method is provided mainly for solving the problems of low strength and non-ideal cutting efficiency of the NiTi alloy martensitic root canal file. The surface modification method is also used for solving the problem of low bonding strength between the coating and the substrate of the root canal file. The surface modification method is simple in process, and low in requirements on equipment; the prepared root canal file has the advantages of high cutting efficiency, high fatigue resistance and the like.
Description
Technical field
The present invention relates to a kind of surface modifying method of NiTi alloy.
Background technology
Root canal file uses one of apparatus the most frequently in clinical oral, is mainly used in preparation and the shaping of tooth root pipe, significant for guarantee root canal success.In recent years, owing to having the advantages such as snappiness is good, elasticity is large, NiTi alloy root canal file is subject to the favor of oral cavity doctor gradually.According to the state of NiTi alloy when using, NiTi alloy root canal file can be divided into super-elasticity root canal file and martensite root canal file.NiTi alloy super-elasticity root canal file has the features such as snappiness is good, but its anti-fatigue performance is poor, and in use easily meeting accident fractures, and thisly fractures when often occurring in without any omen.For this reason, software engineering researchers invent martensite root canal file, this kind of apparatus has lower Young's modulus, very excellent snappiness and anti-cyclic fatigue performance, the super-elastic NiTi alloy root canal file that its cyclic fatigue drag is more traditional improves 3 ~ 5 times.But NiTi alloy in the martensitic state intensity is lower, is only 70-140MPa, this causes its stock-removing efficiency very undesirable.
There is no the effective ways improving NiTi alloy martensite root canal file at present.Existing method is mainly used in improving super-elastic NiTi alloy root canal file.Number of patent application is in the patent document of 200810064359.X, disclose a kind of method of direct current electrode position that adopts and the surperficial technique manufactured again is carried out to root canal appliance, successively at NiTi root canal file electroplating surface layer of Ni-W alloy coating and Zn coating, improve the surface quality of root canal appliance.The techniques such as ion implantation, tropical resources process, metal organic chemical vapor deposition are also used to the wear resistance and the stock-removing efficiency that improve NiTi root canal appliance.Coating prepared by above-mentioned technology can improve the surface property of root canal file to a certain extent, but the mechanical property of coating itself and the bonding strength between coating and matrix unsatisfactory, especially for the situation that NiTi root canal file deflection in crooked root tube preliminary procedure is larger, the toughness of the combination between coatings and substrate and coating self can not effectively be ensured.
Summary of the invention
The object of the present invention is to provide a kind of can improve NiTi alloy martensite root canal file intensity, improve stock-removing efficiency, combine the surface modifying method of firmly NiTi alloy martensite root canal file between coating and matrix.
The object of the present invention is achieved like this:
Utilize magnetron sputtering technique in root canal file surface deposition layer of metal coating, be not less than 10 in vacuum tightness
-3pa, temperature are carry out anneal under the condition of 600 ~ 900 DEG C, and coating metal Elements Diffusion enters martensite root canal file matrix, make root canal file surface at service temperatures for parent phase, inside are martensite.
The present invention can also comprise:
1, the described magnetron sputtering technique that utilizes specifically comprises in root canal file surface deposition layer of metal coating:
(1) using coating metal element as sputtering target material, sputtering target material is arranged on the corresponding target position of magnetron sputtering equipment;
(2) NiTi alloy martensite root canal file is placed in vacuum chamber sample table, is evacuated to 1 × 10
-4~ 1 × 10
-5pa, being filled with argon gas to vacuum tightness is 0.1 ~ 0.5Pa, is 50 ~ 600W at sputtering power, and between sputtering target material and substrate, spacing is sputtering sedimentation metallic coating under the condition of 20 ~ 200mm.
2, described coating metal element is Ni, Fe, V, Cr or Al.
3, described sample table is while rotating around vacuum chamber central axis, again can around root canal file axial-rotation.
The present invention is, problem that stock-removing efficiency undesirable low for NiTi alloy martensite root canal file intensity mainly, and a kind of surface modifying method proposed.Present invention addresses the problem that between root canal file coating and matrix, bonding strength is not high.
The present invention utilizes the NiTi alloy root canal file of this process of surface treatment modification, and top layer is rich Ni layer or contains Cr, V, Fe, the alloying elements such as Al, these alloying elements effectively can reduce the martensitic transformation temperature of NiTi alloy, thus cause this top layer to be parent phase at service temperatures.Compare with martensitic phase, the parent phase of NiTi alloy shows excellent super-elasticity and high rigidity, therefore can improve the stock-removing efficiency of root canal file.After this process, root canal file inside is still martensitic phase, which ensure that root canal file has high cycles fatigue drag.In addition, root canal file handled by this technique is integrated, and there is not the problem that coating is combined with matrix, therefore, efficiently solve the problem that bonding strength between coating and matrix is undesirable, so avoid deflection larger time coating on matrix, peel off the problem that patient is damaged.Technique of the present invention is simple, low for equipment requirements, can be adjusted the ratio of parent phase layer and Malpighian layer easily, obtain the root canal file being applicable to different occasion by control sputtering parameter or parameter and annealing.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the NiTi alloy root canal file cross section of process of the present invention.
Fig. 2 is the hardness of NiTi alloy root canal file after utilizing process of the present invention and untreated front comparing.
Embodiment
Illustrate below and the present invention is described in more detail.Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one:
(1) using coating metal element as sputtering target material, be arranged on the corresponding target position of magnetron sputtering equipment; (2) NiTi alloy martensite root canal file is placed in vacuum chamber sample table, is evacuated to 1 × 10
-4~ 1 × 10
-5pa, being filled with argon gas to vacuum tightness is 0.1 ~ 0.5Pa, is 50 ~ 600W at sputtering power, and between target and substrate, spacing is sputtering sedimentation metallic coating under the condition of 20 ~ 200mm; (3) root canal file depositing metallic coating is not less than 10 in vacuum tightness
-3carry out anneal under Pa condition, annealing temperature is 600 ~ 900 DEG C; (4) utilize pickling to remove the metallic coating of remained on surface, can obtain top layer is parent phase, and inside is martensitic NiTi alloy root canal file.
Embodiment two:
(1) choice for use high pure metal Ni is as sputtering target material, is arranged on the corresponding target position of magnetron sputtering equipment.(2) NiTi alloy martensite root canal file is placed in vacuum chamber sample table, is evacuated to 1 × 10
-4~ 1 × 10
-5pa, being filled with argon gas to vacuum tightness is 0.1 ~ 0.5Pa, is 50 ~ 600W at sputtering power, and target and substrate spacing are sputtering sedimentation metallic coating under the condition of 20 ~ 200mm; In sputter procedure, sample table around vacuum chamber central axis rotate while, around root canal file axial-rotation.(3) root canal file depositing W metal coating is not less than 10 in vacuum tightness
-3carry out anneal under Pa condition, annealing temperature is 600 ~ 900 DEG C, and annealing time is 15min ~ 120min.(4) root canal file after anneal is placed in dilute nitric acid solution, the Ni coating of etching away top layer remnants.Can obtain top layer is parent phase, and inside is martensitic NiTi alloy root canal file.
Figure 1 shows that the schematic diagram of root canal file cross section after above-mentioned process.The composition radially distribution gradient of outer 2, is parent phase at service temperatures, has high rigidity and hyperelastic feature; Internal layer 1 is martensitic phase, has higher fatigue resistance.Without obvious boundary line between two-layer.Utilize HVS-100 type digital display microhardness instrument to test hardness that is untreated and the rear root canal file of process, load is 100g, and the loading time is 10s.Get the mean value of 7 some impression hardness values as net result, as shown in Figure 2, as seen after above-mentioned process, the hardness of root canal file is greatly improved result, this means that, when reality uses, the stock-removing efficiency of root canal file also can be improved.
Embodiment three:
The difference of present embodiment and embodiment two is, adopts high pure metal V as target in present embodiment step (1).
Embodiment four:
The difference of present embodiment and embodiment two is, adopts high pure metal Fe as target in present embodiment step (1).
Embodiment five:
The difference of present embodiment and embodiment two is, adopts high pure metal Cr as target in present embodiment step (1).Hydrochloric acid is used to remove the Cr coating of surface residual in step (4).
Embodiment six:
The difference of present embodiment and embodiment two is, adopts high pure metal Al as target in present embodiment step (1).In step (3), annealing temperature is no more than 650 DEG C.Hydrochloric acid is used to remove the Al coating of surface residual in step (4).
Claims (5)
1. a surface modifying method for NiTi alloy martensite root canal file, is characterized in that: utilize magnetron sputtering technique in root canal file surface deposition layer of metal coating, be not less than 10 in vacuum tightness
-3pa, temperature are carry out anneal under the condition of 600 ~ 900 DEG C, and coating metal Elements Diffusion enters martensite root canal file matrix, make root canal file surface at service temperatures for parent phase, inside are martensite.
2. the surface modifying method of NiTi alloy martensite root canal file according to claim 1, is characterized in that the described magnetron sputtering technique that utilizes specifically comprises in root canal file surface deposition layer of metal coating:
(1) using coating metal element as sputtering target material, sputtering target material is arranged on the corresponding target position of magnetron sputtering equipment;
(2) NiTi alloy martensite root canal file is placed in vacuum chamber sample table, is evacuated to 1 × 10
-4~ 1 × 10
-5pa, being filled with argon gas to vacuum tightness is 0.1 ~ 0.5Pa, is 50 ~ 600W at sputtering power, and between sputtering target material and substrate, spacing is sputtering sedimentation metallic coating under the condition of 20 ~ 200mm.
3. the surface modifying method of NiTi alloy martensite root canal file according to claim 1 and 2, is characterized in that: described coating metal element is Ni, Fe, V, Cr or Al.
4. the surface modifying method of NiTi alloy martensite root canal file according to claim 1 and 2, is characterized in that: described sample table around vacuum chamber central axis rotate while, again around root canal file axial-rotation.
5. the surface modifying method of NiTi alloy martensite root canal file according to claim 3, is characterized in that: described sample table around vacuum chamber central axis rotate while, again around root canal file axial-rotation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510086536.4A CN104630730B (en) | 2015-02-17 | 2015-02-17 | Surface modification method of NiTi alloy martensitic root canal file |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510086536.4A CN104630730B (en) | 2015-02-17 | 2015-02-17 | Surface modification method of NiTi alloy martensitic root canal file |
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| Publication Number | Publication Date |
|---|---|
| CN104630730A true CN104630730A (en) | 2015-05-20 |
| CN104630730B CN104630730B (en) | 2017-04-12 |
Family
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|---|---|---|---|
| CN201510086536.4A Expired - Fee Related CN104630730B (en) | 2015-02-17 | 2015-02-17 | Surface modification method of NiTi alloy martensitic root canal file |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105908136A (en) * | 2016-06-12 | 2016-08-31 | 沈阳大学 | Preparation method for modified metallic nitrogen-oxygen titanium-zirconium composite film on surface of nickel-titanium root canal file |
| CN108788644A (en) * | 2018-06-21 | 2018-11-13 | 深圳市葆丰医疗器械有限公司 | A kind of preparation method of the flexible root canal file of Nitinol |
| CN114617651A (en) * | 2021-12-16 | 2022-06-14 | 广东工业大学 | Nickel-titanium radial gradient root canal file and manufacturing method thereof based on 3D printing |
| CN114734207A (en) * | 2022-04-14 | 2022-07-12 | 山东大学 | NiTi alloy surface cutting process and roughness adjusting method |
| CN115091126A (en) * | 2022-06-20 | 2022-09-23 | 成都市萨尼医疗器械有限公司 | Processing technology of low internal stress root canal file |
| CN116752099A (en) * | 2023-08-15 | 2023-09-15 | 北京航空航天大学宁波创新研究院 | NiTiAl-X multi-element alloy coating and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04183835A (en) * | 1990-11-16 | 1992-06-30 | Furukawa Electric Co Ltd:The | Manufacture of ni-ti alloy member |
| US20030131915A1 (en) * | 2002-01-17 | 2003-07-17 | Johnson A. David | Methods of fabricating high transition temperature SMA, and SMA materials made by the methods |
| CN2894649Y (en) * | 2006-03-16 | 2007-05-02 | 沈阳天贺新材料开发有限公司 | Root canal file |
| CN101497988A (en) * | 2009-01-24 | 2009-08-05 | 哈尔滨工业大学 | Method for plating tantalum on TiNi alloy surface |
-
2015
- 2015-02-17 CN CN201510086536.4A patent/CN104630730B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04183835A (en) * | 1990-11-16 | 1992-06-30 | Furukawa Electric Co Ltd:The | Manufacture of ni-ti alloy member |
| US20030131915A1 (en) * | 2002-01-17 | 2003-07-17 | Johnson A. David | Methods of fabricating high transition temperature SMA, and SMA materials made by the methods |
| CN2894649Y (en) * | 2006-03-16 | 2007-05-02 | 沈阳天贺新材料开发有限公司 | Root canal file |
| CN101497988A (en) * | 2009-01-24 | 2009-08-05 | 哈尔滨工业大学 | Method for plating tantalum on TiNi alloy surface |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105908136A (en) * | 2016-06-12 | 2016-08-31 | 沈阳大学 | Preparation method for modified metallic nitrogen-oxygen titanium-zirconium composite film on surface of nickel-titanium root canal file |
| CN108788644A (en) * | 2018-06-21 | 2018-11-13 | 深圳市葆丰医疗器械有限公司 | A kind of preparation method of the flexible root canal file of Nitinol |
| CN114617651A (en) * | 2021-12-16 | 2022-06-14 | 广东工业大学 | Nickel-titanium radial gradient root canal file and manufacturing method thereof based on 3D printing |
| CN114734207A (en) * | 2022-04-14 | 2022-07-12 | 山东大学 | NiTi alloy surface cutting process and roughness adjusting method |
| US11964337B2 (en) | 2022-04-14 | 2024-04-23 | Shandong University | NiTi alloy surface cutting process and roughness adjustment method |
| CN115091126A (en) * | 2022-06-20 | 2022-09-23 | 成都市萨尼医疗器械有限公司 | Processing technology of low internal stress root canal file |
| CN115091126B (en) * | 2022-06-20 | 2024-03-01 | 成都市萨尼医疗器械有限公司 | Processing technology of low internal stress root canal file |
| CN116752099A (en) * | 2023-08-15 | 2023-09-15 | 北京航空航天大学宁波创新研究院 | NiTiAl-X multi-element alloy coating and preparation method and application thereof |
| CN116752099B (en) * | 2023-08-15 | 2023-10-24 | 北京航空航天大学宁波创新研究院 | NiTiAl-X multi-element alloy coating and preparation method and application thereof |
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| Publication number | Publication date |
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| CN104630730B (en) | 2017-04-12 |
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Granted publication date: 20170412 |