技术领域technical field
本发明属于复杂岩层、高硬度岩层钻进工具技术领域，具体涉及油气勘探及采矿用金刚石钻齿。The invention belongs to the technical field of drilling tools for complex rock formations and high hardness rock formations, in particular to diamond drill teeth for oil and gas exploration and mining.
背景技术Background technique
聚（多）晶金刚石钻齿（Polycrystalline Diamond Cutter, PDC）是油气地质钻探的关键工作部件，油气钻头通常采用PDC对岩石进行切削与刮削钻进，因而，PDC的耐磨性、热稳定性及抗冲击性等性能是影响钻探效率、成本、安全性的关键要素，特别是在2000米以上深井钻探中，对PDC的各项性能要求则更严格。目前，油气钻探用高性能PDC的研发制备已经成为一项高技术含量的系统工程，相关技术也已成为油气地质钻探的核心技术之一。Polycrystalline Diamond Cutter (PDC) is a key working part of oil and gas geological drilling. Oil and gas drill bits usually use PDC to cut and scrape rocks. Therefore, the wear resistance, thermal stability and Performance such as impact resistance is a key factor that affects drilling efficiency, cost, and safety. Especially in deep well drilling above 2,000 meters, the performance requirements for PDC are more stringent. At present, the development and preparation of high-performance PDC for oil and gas drilling has become a high-tech system engineering, and related technologies have also become one of the core technologies of oil and gas geological drilling.
PDC一般由作为工作层的多晶金刚石层与ＷＣ硬质合金基体在在5～8万大气压、1400℃左右的高温高压条件下烧结复合而成。然而，目前工业合成聚（多）晶金刚石（Polycrystalline Diamond,PCD）材料过程中通常要加入超过1wt%的非碳成分作为粘结剂或烧结助剂，如：钴等金属材料，或碳化硅、碳化硼、碳化钛等非金属材料，采用粘结剂可以促进金刚石间D-D键的键合，从而相对降低烧结合成聚（多）晶金刚石过程中的高温高压条件，提升合成金刚石的成功率。但是，合成后PDC中残留的粘结剂会导致其耐磨性、硬度及热稳定性等相对较低。上述差别的理化原因在于：传统多晶金刚石材料中的非碳成分粘结剂如钴等，其热膨胀系数及弹性系数与金刚石差别大，在油气钻探过程中，随着持续不断的钻进，钻头与钻井间因摩擦产生大量热量，使得深井中不能及时散发出去的热量越积越多，从而使金刚石钻齿受热膨胀，其中残留的粘结剂也发生热膨胀，而粘结剂与金刚石间具有不同的热膨胀系数，这会导致金刚石钻齿在热膨胀的同时受到同样发生热膨胀的粘结剂的挤压，从而产生裂纹，致使其寿命减短；另一方面，粘结剂有高温下促进金刚石的石墨化，影响其性能。因此，商业钻探用多晶金刚石材料通常需要通过物理或化学方法去除内部所含的部分非碳成分粘结剂或烧结助剂，以提高其性能。但因为粘结剂是散落分布在金刚石晶界处，一方面难以完全去除，另一方面，即使部分去除粘结剂的工作也大大增加了金刚石钻齿的成本。PDC is generally composed of a polycrystalline diamond layer as a working layer and a WC cemented carbide substrate under high temperature and high pressure conditions of 50,000 to 80,000 atmospheres and 1400°C. However, at present, during the industrial synthesis of polycrystalline diamond (Polycrystalline Diamond, PCD) materials, more than 1wt% of non-carbon components are usually added as binders or sintering aids, such as metal materials such as cobalt, or silicon carbide, For non-metallic materials such as boron carbide and titanium carbide, the use of binders can promote the bonding of D-D bonds between diamonds, thereby relatively reducing the high temperature and high pressure conditions in the process of sintering and synthesizing poly(poly)crystalline diamonds, and improving the success rate of synthesizing diamonds. However, the residual binder in PDC after synthesis will lead to relatively low wear resistance, hardness and thermal stability. The physical and chemical reasons for the above differences are: the non-carbon binders in traditional polycrystalline diamond materials, such as cobalt, have a large difference in thermal expansion coefficient and elastic coefficient from diamond. In the process of oil and gas drilling, with continuous drilling, the drill bit A large amount of heat is generated due to friction with the drilling, so that the heat that cannot be dissipated in time in the deep well accumulates more and more, so that the diamond drill teeth are heated and expanded, and the residual binder also undergoes thermal expansion, and the binder and diamond have different properties. The coefficient of thermal expansion, which will cause the diamond drill teeth to be squeezed by the same thermally expanding binder while thermally expanding, resulting in cracks and shortening its life; on the other hand, the binder has graphite that promotes diamond at high temperature , affecting its performance. Therefore, polycrystalline diamond materials for commercial drilling usually need to remove part of the non-carbon component binder or sintering aid contained in the interior by physical or chemical methods to improve its performance. However, because the binder is scattered and distributed at the diamond grain boundary, it is difficult to completely remove it on the one hand, and on the other hand, even the work of partially removing the binder will greatly increase the cost of the diamond drill.
发明内容Contents of the invention
本发明目的在于提供一种金刚石钻齿，以克服现有聚晶金刚石钻齿（PDC）在用于油气钻探中的不足。所述金刚石钻齿由多晶金刚石整体加工制成或由多晶金刚石与基体分体连接复合后加工而成，所述金刚石钻齿整体为圆柱、棱柱等柱状，其上多晶金刚石的底部是与钻头或基体连接的连接端，顶部是多晶金刚石工作层的工作面；基体与所述多晶金刚石连接的一面为与多晶金刚石连接端的形状相配合的连接面，所述多晶金刚石内含有的非碳成分小于多晶金刚石工作层总质量的1wt%。The object of the present invention is to provide a diamond drill tooth to overcome the shortcomings of existing polycrystalline diamond drill teeth (PDC) used in oil and gas drilling. The diamond drill tooth is made of polycrystalline diamond as a whole or is processed by connecting and compounding polycrystalline diamond and the matrix. The connection end connected with the drill bit or the substrate, the top is the working surface of the polycrystalline diamond working layer; the side connecting the substrate with the polycrystalline diamond is the connection surface matching the shape of the polycrystalline diamond connection end, and the inner surface of the polycrystalline diamond is The non-carbon component contained is less than 1wt% of the total mass of the polycrystalline diamond working layer.
本发明所述的用于整体加工或分体复合后加工制成金刚石钻齿的多晶金刚石是采用高纯碳作为原材料，在高温高压条件下烧结合成的。多晶金刚石与基体分体连接复合的方式为将高温高压烧结合成的多晶金刚石叠于基体的连接面上，通过高温高压烧结、真空焊接、激光焊接、微波焊接或者机械固定方式使之粘结在一起；还可以是将用于合成多晶金刚石的原材料均匀分布在基体的连接面上，在高温高压烧结合成多晶金刚石层的过程中使之粘结在一起。高纯碳原材料为石墨、石墨烯、富勒烯、纳米洋葱碳、C60、微米级金刚石、纳米级金刚石中的一种或多种，基体的主要成分可以是碳化钨、碳化钛、碳化硅、碳化铬中的一种或几种。高温高压条件范围为8～25GPa、1200～3000℃，其最优化烧结温压条件约为10～18GPa、1500～2500℃。本发明中的应用于油气钻探的多晶金刚石的高温高压烧结在基于六面顶压机的二级六-八型大腔体静高压装置中进行，目前商业钻探用多晶金刚石材料的高温高压烧结通常采用六面顶压机或两面顶压机的一级压腔进行。According to the present invention, the polycrystalline diamond used for integral processing or split composite processing to make diamond drill teeth is made of high-purity carbon as a raw material, and is sintered and synthesized under high temperature and high pressure conditions. The method of connecting and recombining the polycrystalline diamond and the substrate is to stack the polycrystalline diamond synthesized by high temperature and high pressure sintering on the connection surface of the substrate, and bond it by high temperature and high pressure sintering, vacuum welding, laser welding, microwave welding or mechanical fixing. together; it is also possible to evenly distribute the raw materials used for synthesizing polycrystalline diamond on the connection surface of the substrate, and bond them together during the process of high temperature and high pressure sintering to synthesize the polycrystalline diamond layer. High-purity carbon raw materials are one or more of graphite, graphene, fullerene, nano-onion carbon, C60 , micron-sized diamond, and nano-sized diamond. The main component of the matrix can be tungsten carbide, titanium carbide, and silicon carbide. , one or more of chromium carbide. The range of high temperature and high pressure conditions is 8-25GPa, 1200-3000°C, and the optimal sintering temperature and pressure conditions are about 10-18GPa, 1500-2500°C. The high-temperature and high-pressure sintering of polycrystalline diamond used in oil and gas drilling in the present invention is carried out in a two-stage six-eight large-cavity static high-pressure device based on a six-sided top press. At present, the high-temperature and high-pressure sintering of polycrystalline diamond materials for commercial drilling Sintering is usually carried out in the primary pressure chamber of a six-sided top press or a two-sided top press.
本发明提供的多晶金刚石钻齿顶部工作面与连接端的形状都可以加工成平面、弧面、锥面、波纹面、或者长城状凹凸面，其中平面形工作面钻齿即平顶齿最早问世，其应用也最广泛，而将金刚石钻齿制成球形、锥形、械形、勺形等更锐利的形状，可以达到更有效地研磨、刨削和冲击效果，同时延长钻齿的使用寿命，有着重要的实际意义。The shape of the top working surface and the connecting end of the polycrystalline diamond drill tooth provided by the present invention can be processed into a plane, an arc surface, a conical surface, a corrugated surface, or a Great Wall-like concave-convex surface, and the plane-shaped working surface drill teeth, namely flat-top teeth, came out the earliest , which is also the most widely used, and the diamond drill teeth are made into sharper shapes such as spherical, conical, mechanical, spoon-shaped, etc., which can achieve more effective grinding, planing and impact effects, and at the same time extend the service life of the drill teeth , has important practical significance.
本发明所述金刚石钻齿，是将在高温高压烧结合成的多晶金刚石直接加工或与基体连接复合后加工成为标准尺寸的钻齿，其多晶金刚石部分的晶粒尺寸为几纳米至几百微米，晶粒间具有强而多的金刚石-金刚石（D-D）键合，其耐磨性、硬度、热稳定性及抗冲击性等性能都远高于目前使用的采用粘结剂作为触媒而制成的PDC。The diamond drill tooth of the present invention is a drill tooth of a standard size after the polycrystalline diamond synthesized by sintering at high temperature and high pressure is directly processed or processed into a standard size, and the grain size of the polycrystalline diamond part is several nanometers to several hundred Micron, there are strong and many diamond-diamond (D-D) bonds between the grains, and its wear resistance, hardness, thermal stability and impact resistance are much higher than those currently used using binders as catalysts. into the PDC.
油气钻头一般包括钻头本体和连接在钻头本体上的金刚石钻齿，将本发明所述金刚石钻齿通过焊接或机械固定方式连接在钻头本体从而制成钻头，钻头本体冠部形状可以是鱼尾形、浅锥形、短抛物线形或抛物线形。Oil and gas drill bits generally include a drill body and diamond drill teeth connected to the drill body. The diamond drill teeth of the present invention are connected to the drill body by welding or mechanical fixing to make a drill bit. The crown shape of the drill body can be fishtail, Shallow conical, short parabolic or parabolic.
本发明提供的多晶金刚石钻齿与传统PDC相比具有更高的硬度、耐磨性、热稳定性、抗冲击性，本发明所述多晶金刚石钻齿在油气钻探中的使用寿命比合成过程中加入粘结剂得到的传统聚晶金刚石钻齿（PDC）的寿命增加了1倍以上，一次性钻进地下岩层可达2500米以上。Compared with the traditional PDC, the polycrystalline diamond drill provided by the present invention has higher hardness, wear resistance, thermal stability and impact resistance, and the service life of the polycrystalline diamond drill described in the present invention in oil and gas drilling is more The life of the traditional polycrystalline diamond drill bit (PDC) obtained by adding a binder in the process has more than doubled, and one-time drilling into the underground rock formation can reach more than 2,500 meters.
附图说明Description of drawings
图1为传统聚晶金刚石钻齿（PDC）金刚石工作层部分的XRD物相分析图谱；Figure 1 is the XRD phase analysis pattern of the diamond working layer of a traditional polycrystalline diamond drill tooth (PDC);
图2为本发明提供的多晶金刚石钻齿金刚石工作层部分的XRD物相分析图谱；Fig. 2 is the XRD phase analysis spectrum of polycrystalline diamond drill tooth diamond working layer part provided by the present invention;
图3为由多晶金刚石整体制成的平顶齿示意图；Fig. 3 is the schematic diagram of the flat-top tooth made of polycrystalline diamond as a whole;
图4为由多晶金刚石与硬质合金复合制成的平顶齿示意图；Fig. 4 is the schematic diagram of flat-top teeth made of polycrystalline diamond and cemented carbide composite;
图5 为复合齿工作面为长城状凹凸面示意图；Fig. 5 is a schematic diagram of a Great Wall-like concave-convex surface on the working surface of the compound tooth;
图6为复合齿工作面为弧形面示意图；Fig. 6 is a schematic diagram showing that the working surface of the compound tooth is an arc surface;
图7为复合平顶齿中金刚石层与硬质合金层连接面为长城状凹凸面示意图；Fig. 7 is a schematic diagram of a Great Wall-shaped concave-convex surface at the connection surface between the diamond layer and the cemented carbide layer in the composite flat-topped tooth;
图8为多晶金刚石与硬质合金复合制成的圆柱锥状复合齿示意图；Figure 8 is a schematic diagram of a cylindrical conical composite tooth made of polycrystalline diamond and cemented carbide;
实施例Example
实施例1Example 1
如图3、4所示，图3 所示金刚石钻齿由多晶金刚石1整体加工制成，图4所示金刚石钻齿是由多晶金刚石层1与WC硬质合金层2在5～10GPa、1300～1500℃的高温高压条件下烧结复合而成，多晶金刚石1是由将石墨在18～20GPa，1700～2000℃的条件下直接转变成金刚石并烧结复合而成，这两种钻齿的多晶金刚石工作层内含有少于1wt%的非粘结剂的非碳成分，钻齿整体为圆柱平顶齿，顶部金刚石部分为工作层。这两种钻齿金刚石部分的维氏硬度在100GPa以上，其在油气钻探中的使用寿命比合成过程中加入粘结剂得到的聚晶金刚石钻齿（PDC）的寿命增加了1倍以上，一次性钻进地下岩层可达2500米以上。As shown in Figures 3 and 4, the diamond drill tooth shown in Figure 3 is made of polycrystalline diamond 1 as a whole, and the diamond drill tooth shown in Figure 4 is made of polycrystalline diamond layer 1 and WC cemented carbide layer 2 at a temperature of 5-10GPa. , 1300 ~ 1500 ℃ high temperature and high pressure conditions sintering and compounding, polycrystalline diamond 1 is made by directly transforming graphite into diamond under the conditions of 18 ~ 20GPa, 1700 ~ 2000 ℃ and sintering compounding, these two kinds of drill teeth The polycrystalline diamond working layer contains less than 1wt% of non-bonding non-carbon components, the drill teeth are cylindrical flat-topped teeth as a whole, and the top diamond part is the working layer. The Vickers hardness of the diamond part of these two kinds of drill teeth is above 100GPa, and its service life in oil and gas drilling is more than double that of polycrystalline diamond drill teeth (PDC) obtained by adding a binder in the synthesis process. It can drill into the underground rock formation up to more than 2500 meters.
实施例2Example 2
如图5所示金刚石钻齿是由多晶金刚石层1与WC硬质合金层2通过微波焊接复合而成，多晶金刚石1是由将微米级金刚石粉末在15～20GPa，1800～2200℃的条件下烧结复合而成，这种钻齿的多晶金刚石工作层1内含有少于1wt%的非粘结剂的非碳成分，钻齿整体为圆柱状，其上多晶金刚石层1的工作面为长城状凹凸面。这种钻齿金刚石部分的维氏硬度在100GPa以上，其在油气钻探中的使用寿命比合成过程中加入粘结剂得到的聚晶金刚石钻齿（PDC）的寿命增加了1.5倍以上，一次性钻进地下岩层可达2550米以上。As shown in Figure 5, the diamond drill tooth is composed of polycrystalline diamond layer 1 and WC cemented carbide layer 2 through microwave welding. The polycrystalline diamond working layer 1 of this kind of drill tooth contains less than 1wt% of non-bonding non-carbon components. The overall drill tooth is cylindrical, and the working layer of polycrystalline diamond layer 1 on it The surface is a Great Wall-shaped concave-convex surface. The Vickers hardness of the diamond part of this drill tooth is above 100GPa, and its service life in oil and gas drilling is more than 1.5 times longer than that of the polycrystalline diamond drill tooth (PDC) obtained by adding a binder in the synthesis process. Drilling into the underground rock formation can reach more than 2550 meters.
实施例3Example 3
如图6所示金刚石钻齿是由多晶金刚石层1与WC硬质合金层2通过激光焊接复合而成，多晶金刚石1是由将微米级金刚石粉末在21～23GPa，2500～3000℃的条件下烧结复合而成，这种钻齿的多晶金刚石工作层1内含有少于1wt%的非粘结剂的非碳成分，钻齿整体为圆柱状，其上多晶金刚石层1的工作面为弧形面。这种钻齿在油气钻探中的使用寿命比合成过程中加入粘结剂得到的聚晶金刚石钻齿（PDC）的寿命增加了1.5倍以上，一次性钻进地下岩层可达2600米以上。As shown in Figure 6, the diamond drill tooth is composed of a polycrystalline diamond layer 1 and a WC cemented carbide layer 2 through laser welding. The polycrystalline diamond working layer 1 of this kind of drill tooth contains less than 1wt% of non-bonding non-carbon components. The overall drill tooth is cylindrical, and the working layer of polycrystalline diamond layer 1 on it The surface is curved. The service life of this drill tooth in oil and gas drilling is more than 1.5 times longer than that of the polycrystalline diamond drill tooth (PDC) obtained by adding a binder in the synthesis process, and it can drill more than 2,600 meters into the underground rock formation at one time.
实施例4Example 4
如图7所示金刚石钻齿是由多晶金刚石层1与WC硬质合金层2通过机械固定复合而成，多晶金刚石1是由将纳米级金刚石粉末在15～18GPa，2500～2800℃的条件下烧结复合而成，这种钻齿的多晶金刚石工作层1内含有少于1wt%的非粘结剂的非碳成分，钻齿整体为圆柱状，其上多晶金刚石层1的与WC硬质合金层连接的连接端为长城状凹凸面。这种钻齿金刚石部分的维氏硬度在100GPa以上，其在油气钻探中的使用寿命比合成过程中加入粘结剂得到的聚晶金刚石钻齿（PDC）的寿命增加了1.5倍以上，一次性钻进地下岩层可达2700米以上。As shown in Figure 7, the diamond drill tooth is composed of a polycrystalline diamond layer 1 and a WC cemented carbide layer 2 through mechanical fixation. The polycrystalline diamond working layer 1 of this kind of drill tooth contains less than 1wt% non-bonding non-carbon components. The overall drill tooth is cylindrical, and the polycrystalline diamond layer 1 and The connection end of the WC hard alloy layer connection is a Great Wall-shaped concave-convex surface. The Vickers hardness of the diamond part of this drill tooth is above 100GPa, and its service life in oil and gas drilling is more than 1.5 times longer than that of the polycrystalline diamond drill tooth (PDC) obtained by adding a binder in the synthesis process. Drilling into underground rock formations can reach more than 2,700 meters.
实施例5Example 5
如图8所示金刚石钻齿是由多晶金刚石层1与WC硬质合金层2通过机械固定复合而成，多晶金刚石1是由将微米晶金刚石粉末与纳米晶金刚石粉末的混合物在18～20GPa，2800～3000℃的条件下烧结复合而成，这种钻齿的多晶金刚石工作层1内含有少于1wt%的非粘结剂的非碳成分，钻齿整体为圆柱锥状。这种钻齿金刚石部分的维氏硬度在100GPa以上，其在油气钻探中的使用寿命比合成过程中加入粘结剂得到的聚晶金刚石钻齿（PDC）的寿命增加了1.5倍以上，一次性钻进地下岩层可达2700米以上。As shown in Figure 8, the diamond drill tooth is composed of a polycrystalline diamond layer 1 and a WC cemented carbide layer 2 through mechanical fixing. The polycrystalline diamond 1 is made of a mixture of microcrystalline diamond powder and nanocrystalline diamond powder at 18 ~ 20GPa, sintered and composited at 2800-3000°C, the polycrystalline diamond working layer 1 of this drill contains less than 1wt% of non-bonding non-carbon components, and the drill as a whole is cylindrical and conical. The Vickers hardness of the diamond part of this drill tooth is above 100GPa, and its service life in oil and gas drilling is more than 1.5 times longer than that of the polycrystalline diamond drill tooth (PDC) obtained by adding a binder in the synthesis process. Drilling into underground rock formations can reach more than 2,700 meters.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611115909.7ACN106761429A (en) | 2016-12-07 | 2016-12-07 | A kind of diamond drill machine tooth |
| Application Number | Priority Date | Filing Date | Title |
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| CN201611115909.7ACN106761429A (en) | 2016-12-07 | 2016-12-07 | A kind of diamond drill machine tooth |
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| CN106761429Atrue CN106761429A (en) | 2017-05-31 |
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| CN201611115909.7APendingCN106761429A (en) | 2016-12-07 | 2016-12-07 | A kind of diamond drill machine tooth |
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| CN112746814A (en)* | 2020-12-22 | 2021-05-04 | 吉林大学 | High-temperature-resistant wear-resistant polycrystalline diamond compact and preparation method thereof |
| CN115572878A (en)* | 2022-09-30 | 2023-01-06 | 蒋孟瑶 | Hard alloy material and preparation method and application thereof |
| CN116748658A (en)* | 2023-06-13 | 2023-09-15 | 四川大学 | Method for preparing pure-phase polycrystalline diamond drill teeth through high-pressure welding technology |
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| JPH11239977A (en)* | 1997-11-20 | 1999-09-07 | General Electric Co <Ge> | Polycrystalline diamond compact cutter reduced in damage when brazed |
| CN103752220A (en)* | 2008-02-06 | 2014-04-30 | 住友电气工业株式会社 | Polycrystalline diamond |
| CN103752833A (en)* | 2008-11-11 | 2014-04-30 | 山特维克知识产权股份有限公司 | Cemented carbide body and method |
| CN102459802A (en)* | 2009-05-20 | 2012-05-16 | 史密斯国际股份有限公司 | Cutting elements, methods for making such cutting elements, and tools incorporating such cutting elements |
| CN103028731A (en)* | 2011-09-30 | 2013-04-10 | 中国石油化工股份有限公司 | A hot-pressed impregnated diamond drill tooth and its manufacturing method and its application in strong abrasive formation |
| CN102794447A (en)* | 2012-06-13 | 2012-11-28 | 河南省亚龙金刚石制品有限公司 | Anti-impact diamond layer, diamond composite sheet and preparation method for diamond composite sheet |
| CN104047548A (en)* | 2013-03-13 | 2014-09-17 | 江雨明 | Diamond drill tooth with cobalt content gradient |
| CN104643425A (en)* | 2013-11-20 | 2015-05-27 | 青岛古宇石墨有限公司 | Preparation formula of high-purity diamond |
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| CN109778040A (en)* | 2019-04-04 | 2019-05-21 | 吉林大学 | A kind of graphene-reinforced pre-alloyed-based diamond composite material and preparation method thereof |
| CN111233476A (en)* | 2020-01-17 | 2020-06-05 | 成都东为科技有限公司 | Binder-free polycrystalline diamond material and preparation method thereof |
| CN111548165A (en)* | 2020-06-09 | 2020-08-18 | 欧阳晓平 | Polycrystalline SiC-diamond double-layer composite material and preparation method thereof |
| CN111592360A (en)* | 2020-06-09 | 2020-08-28 | 欧阳晓平 | Polycrystal B4C-diamond double-layer composite material and preparation method thereof |
| CN112746814A (en)* | 2020-12-22 | 2021-05-04 | 吉林大学 | High-temperature-resistant wear-resistant polycrystalline diamond compact and preparation method thereof |
| CN112746814B (en)* | 2020-12-22 | 2022-01-04 | 吉林大学 | A kind of high temperature resistant and wear resistant polycrystalline diamond composite sheet and preparation method thereof |
| CN115572878A (en)* | 2022-09-30 | 2023-01-06 | 蒋孟瑶 | Hard alloy material and preparation method and application thereof |
| CN116748658A (en)* | 2023-06-13 | 2023-09-15 | 四川大学 | Method for preparing pure-phase polycrystalline diamond drill teeth through high-pressure welding technology |
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| WD01 | Invention patent application deemed withdrawn after publication | Application publication date:20170531 | |
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