WO2013185511A1 - Method for manufacturing polycrystalline diamond compact enhanced by cvd diamond - Google Patents

Method for manufacturing polycrystalline diamond compact enhanced by cvd diamond Download PDF

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WO2013185511A1
WO2013185511A1 PCT/CN2013/075193 CN2013075193W WO2013185511A1 WO 2013185511 A1 WO2013185511 A1 WO 2013185511A1 CN 2013075193 W CN2013075193 W CN 2013075193W WO 2013185511 A1 WO2013185511 A1 WO 2013185511A1
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cvd
diamond
polycrystalline diamond
furnace
temperature
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PCT/CN2013/075193
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French (fr)
Chinese (zh)
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李成明
刘盛
刘金龙
陈良贤
魏俊俊
黑立富
吕反修
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北京科技大学
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Publication of WO2013185511A1 publication Critical patent/WO2013185511A1/en

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    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
    • C23C16/272—Diamond only using DC, AC or RF discharges

Definitions

  • the invention relates to a novel polycrystalline diamond composite sheet obtained by using a CVD diamond strip as a reinforcing relative to a conventional polycrystalline diamond composite sheet and a preparation method thereof, and is a novel method for sintering synthetic enhanced polycrystalline diamond composite sheet. It belongs to the fields of materials, machinery and tools.
  • Polycrystalline Diamond Compact (PDC composite sheet) is a composite material consisting of a polycrystalline diamond layer coated on the surface of a cemented carbide substrate. It combines the high wear resistance of polycrystalline diamond layer with the toughness and weldability of cemented carbide. It is therefore an efficient cutting tool material and excellent wear-resistant material, and is widely used in petroleum and geological drilling and machinery. Processing and other fields.
  • the basic preparation process of the PDC composite sheet is to adopt a special structure and method to form a tight bond between the polycrystalline diamond layer and the cemented carbide.
  • Direct synthesis means that the polycrystalline diamond layer and the cemented carbide substrate are synthesized at one time, that is, the diamond powder of the synthetic polycrystalline diamond layer is directly sintered at a high temperature and high pressure on the substrate and closely combined with the matrix, so that the obtained polycrystalline diamond layer is also called It is a growth type polycrystalline diamond.
  • the catalysis of components such as Ni, Co and W in the cemented carbide also promotes the bonding and bonding between the diamond powders and between the cemented carbides.
  • the polycrystalline diamond layer is first sintered separately, and the polycrystalline diamond layer is tightly bonded to the cemented carbide substrate by welding.
  • PDC composite sheets have better performance than natural diamonds and various hard alloys, tool steels, etc.
  • the rapid development of modern petroleum industry and machinery manufacturing industry continues to put forward the performance and quality of PDC composite sheets.
  • Higher requirements In practical applications, for example, PDC composite drill bits or tools are subjected to large shear stress due to high-speed rotation and cutting during operation, so the interface of the polycrystalline diamond layer, the cemented carbide substrate and the PDC composite sheet fails. The situation has always happened.
  • the failure condition of the PDC composite sheet the shedding of the polycrystalline diamond layer accounts for a large proportion. According to the statistical analysis of the US oil department, in deep well drilling operations, 33% of drill bit failures are caused by the shedding of the polycrystalline diamond layer.
  • U.S. Patent No. 5,662,720 describes a method for enhancing the interfacial adhesion and properties of a PDC composite by modifying the morphology of the cemented carbide substrate bonding surface prior to direct synthesis of the polycrystalline diamond layer.
  • the method in this patent is to machine a plurality of channels on the bonding surface of the cemented carbide substrate or to process the entire bonding surface into pits and protrusions which are "egg-carton shaped" undulations, thereby increasing the sintering.
  • the combined area of the polycrystalline diamond layer and the cemented carbide substrate not only improves the interfacial adhesion, but also leverages the "bite" relationship of the particular shape to enhance the ability of the PDC composite to withstand the shear stress experienced during operation.
  • the Chinese patent CN201110148812.7 mentions a method for reinforcing a PDC composite sheet by using a fiber-reinforced effect of carbon nanotubes, and the specific scheme is to incorporate carbon nanotubes into the diamond powder of the sintered polycrystalline diamond, thereby increasing the sintering.
  • the overall toughness and impact resistance of the PDC composite sheet mentions a method for reinforcing a PDC composite sheet by using a fiber-reinforced effect of carbon nanotubes, and the specific scheme is to incorporate carbon nanotubes into the diamond powder of the sintered polycrystalline diamond, thereby increasing the sintering.
  • the overall toughness and impact resistance of the PDC composite sheet mentions a method for reinforcing a PDC composite sheet by using a fiber-reinforced effect of carbon nanotubes
  • the object of the present invention is to further improve the bonding strength of a polycrystalline diamond layer and a cemented carbide substrate in a PDC composite sheet and the strength of the substrate.
  • the invention provides a CVD diamond reinforced polycrystalline diamond composite sheet, which is composed of a polycrystalline diamond layer, a cemented carbide substrate and a CVD diamond strip, wherein the CVD diamond strip is embedded in the composite sheet in an orderly manner, and the surface processed CVD diamond The upper end surface of the strip is exposed on the surface of the polycrystalline diamond layer, and the lower end surface penetrates into the cemented carbide substrate.
  • CVD diamond-reinforced polycrystalline diamond compact sheet is a CVD diamond strip having a special shape which is integrated into a contact interface between a through-polycrystalline diamond layer and a cemented carbide substrate in a polycrystalline diamond compact sheet;
  • Diamond strips are available in four types: "I” shape, "L” shape, "T” shape, and "work” shape. They are prepared by DC arc plasma CVD, microwave CVD or hot wire CVD, and are laser cut.
  • the CVD diamond-reinforced polycrystalline diamond compact sheet of the present invention is prepared by sequentially performing a CVD diamond film by a plasma jet CVD method, a microwave CVD method or a hot filament CVD method. Cutting and molding, CVD diamond strips are embedded in hard order The alloy and the polycrystalline diamond powder are then pressed into a billet, sintered at a high temperature, and annealed to eliminate residual stress and thermal stress, and finally processed.
  • a CVD diamond self-supporting film with a diameter of 60-120 mm and a thickness of 2-3 mm is prepared by DC arc plasma CVD.
  • the CVD diamond self-supporting film is separately cut into a plurality of "I”, “L”, “T”, and “work” shaped strips using a laser cutter.
  • the method for preparing a CVD diamond-reinforced polycrystalline diamond compact sheet is characterized in that a CVD diamond strip is embedded in a cemented carbide powder and a polycrystalline diamond layer powder, and then pressed into a billet, and then reduced in hydrogen. The film is hot pressed under an atmosphere and annealed to eliminate residual stress and thermal stress.
  • the specific operation process is as follows: 1
  • the compacted diamond micropowder, CVD diamond strip and cemented carbide substrate are compacted and assembled in a pyrophyllite synthesis mold, and then placed in a six-sided diamond press at a pressure of 5-7 GPa.
  • the temperature is 1350-1650 ° C, the synthesis is 2-5 minutes, the sample is taken out after the pressure is released to make the blank; 2 the formed blank is sealed into the graphite furnace, and the graphite furnace is placed in the pressure sintering furnace;
  • the flowing hydrogen gas is used to create a reducing atmosphere, and then the furnace temperature is raised from room temperature to 650-800 °C at a temperature increase rate of 10-30 ° C/min under the condition of maintaining a pressure of P 80 kN, and the temperature is maintained for 25-40 min;
  • the heating rate of 5-15 ° C / min is raised from 650-80 CTC to the final sintering temperature of 900-980 ° C, and maintained for 3-7 min; 5 continue to maintain pressure and hydrogen reduction atmosphere, to 5-15 ° C / min
  • the cooling rate is reduced to 450-550 ° C, and the temperature is kept for 5-15 min.
  • the preparation method comprises: burying a CVD diamond strip into a cemented carbide powder and a polycrystalline diamond layer powder, pressing it into a billet, performing hot press sintering under a hydrogen reduction atmosphere, and annealing to eliminate residual stress and Thermal stress;
  • the specific operation process is as follows: 1 Place the mixed powder containing CVD diamond strip in a stainless steel mold, pressurize it to 30 MPa with a hydraulic press to make a blank; 2 Seal the cold-formed blank into a graphite furnace, and graphite The furnace is placed in a pressure sintering furnace; 3 a flowing hydrogen gas is introduced into the furnace to create a reducing atmosphere, and then the furnace temperature is raised from room temperature to a temperature rising rate of 20 ° C/min under a condition of maintaining a pressure of P 80 kN.
  • the cooling rate of min is reduced to 500 ° C, and the temperature is kept lOmin; 6 the pressure load is removed, and the furnace is cooled to room temperature;
  • the CVD diamond strip is homogenous to the diamond powder of the sintered polycrystalline diamond layer, a tight bond is formed between the sintered polycrystalline diamond layer and the CVD diamond strip implanted therein, and the density of the CVD diamond strip is much larger than that of the polycrystal.
  • the diamond layer will firstly greatly improve the strength and impact resistance of the polycrystalline diamond layer.
  • the CVD diamond strip as a reinforcing phase as a whole penetrates through the polycrystalline diamond layer and the cemented carbide substrate of the PDC composite sheet, which are closely related to the two parts.
  • the combination is equivalent to increasing the bonding area and bonding strength of the two parts; again, the CVD diamond strip is located at the key position of the interface, playing a "bite" role, and its own high strength will be more favorable for the PDC composite sheet to resist the working condition. Large shear stress; In addition, a portion of the CVD diamond strip extending into the substrate also enhances the cemented carbide matrix, which greatly increases the useful life of the matrix, thereby increasing the utilization of the polycrystalline diamond layer and the overall PDC The use time of the composite sheet.
  • the mechanical properties such as strength and impact resistance of the PDC composite sheet are greatly improved, and the failure caused by the falling of the polycrystalline diamond layer in the use of the PDC composite sheet is effectively prevented, and the service life of the PDC composite sheet is improved.
  • Fig. 1 is a schematic view showing the basic structure of a conventional PDC composite sheet.
  • 1 is a polycrystalline diamond layer
  • 2 is a cemented carbide substrate
  • 3, 4, 5, and 6 are "I", “L”, “T”, and “work” CVD diamond bars, respectively.
  • an "I" shaped CVD diamond strip reinforced polycrystalline diamond compact is prepared as follows:
  • CVD diamond self-supporting film is laser cut into "I" strips, embedded in cemented carbide powder and polycrystalline gold
  • the corundum layer powder After being compacted into a billet, it is hot pressed and sintered under a hydrogen reducing atmosphere, and annealed to eliminate residual stress and thermal stress; the specific operation process is: 1 mixing the fine diamond powder, CVD diamond strip and hard
  • the alloy substrate is compacted and assembled in a pyrophyllite synthesis mold, placed in a six-sided diamond press, and subjected to a pressure of 5.7 GPa at a temperature of 1,450 ° C for 3 minutes.
  • the sample is taken out to form a blank;
  • the formed blank is sealed into the graphite furnace, and the graphite furnace is placed in the pressure sintering furnace; 3 flowing hydrogen gas into the furnace to create a reducing atmosphere, and then the furnace temperature is 20° under the condition of maintaining the pressure P 80kN
  • the heating rate of C/min is raised from room temperature to 700 °C, and kept for 30 minutes; 4 is further increased from 700 °C to the final sintering temperature of 950 °C at a heating rate of 10 °C/min for 5 min; Pressure and hydrogen reduction atmosphere, to 10 ° C / min cooling rate down to 500 ° C, insulation lOmin; 6 remove the pressure load, with the furnace cooled to room temperature; 7 processing molding.
  • an "L"-shaped CVD diamond strip reinforced polycrystalline diamond compact is prepared as follows:
  • the CVD diamond self-supporting film is laser-cut into "L"-shaped strips, embedded in the mixed powder, pressed into a billet, and sintered.
  • a "T" shaped CVD diamond strip reinforced polycrystalline diamond compact is prepared as follows:
  • the CVD diamond self-supporting film is laser cut into "T" shaped strips, embedded in the mixed powder, pressed into a billet, and sintered.
  • a method for preparing a "work" shaped CVD diamond strip reinforced polycrystalline diamond compact is as follows:
  • the CVD diamond self-supporting film is laser cut into "work” shaped strips, embedded in the mixed powder, pressed into a billet, and sintered.

Abstract

Disclosed are a polycrystalline diamond compact enhanced by CVD diamond and a method for manufacturing same. A CVD diamond strip is embedded into polycrystalline diamond and hard alloy powder and used as an enhancement phase, and after a blank is formed by pressing, a novel polycrystalline diamond compact enhanced by the CVD diamond is obtained by sintering the blank through a high-temperature and high-pressure sintering process and a proper thermal treatment process.

Description

CVD金刚石增强聚晶金刚石复合片的制备方法 技术领域  Method for preparing CVD diamond reinforced polycrystalline diamond composite sheet
本发明涉及一种使用 CVD金刚石条作为增强相对普通聚晶金刚石复合片加 以增强后得到的新型聚晶金刚石复合片及其制备方法，是一种烧结合成增强型聚 晶金刚石复合片的新方法， 属于材料、 机械以及工具领域。  The invention relates to a novel polycrystalline diamond composite sheet obtained by using a CVD diamond strip as a reinforcing relative to a conventional polycrystalline diamond composite sheet and a preparation method thereof, and is a novel method for sintering synthetic enhanced polycrystalline diamond composite sheet. It belongs to the fields of materials, machinery and tools.
背景技术 Background technique
聚晶金刚石复合片 （Polycrystalline Diamond Compact,下简称 PDC复合片） 是一种由聚晶金刚石层覆盖在硬质合金基体表面所组成的复合材料。它兼具了聚 晶金刚石层的高耐磨性和硬质合金的韧性、可焊性等优点， 因此成为高效的切削 工具材料和优良的耐磨材料， 并广泛应用于石油与地质钻探和机械加工等领域。  Polycrystalline Diamond Compact (PDC composite sheet) is a composite material consisting of a polycrystalline diamond layer coated on the surface of a cemented carbide substrate. It combines the high wear resistance of polycrystalline diamond layer with the toughness and weldability of cemented carbide. It is therefore an efficient cutting tool material and excellent wear-resistant material, and is widely used in petroleum and geological drilling and machinery. Processing and other fields.
PDC 复合片的基本制备过程是采用特殊的结构和方法使聚晶金刚石层和硬 质合金之间形成紧密的结合。合成的方法主要有两种： 直接合成与间接合成。直 接合成是指聚晶金刚石层与硬质合金基体一次性合成，即合成聚晶金刚石层的金 刚石粉体直接在基体上高温高压烧结并与基体形成紧密结合，因此得到的聚晶金 刚石层又称为生长型聚晶金刚石。 另外， 在烧结过程中， 硬质合金中的 Ni、 Co 和 W等成分的催化作用亦促进了金刚石粉体之间以及与硬质合金之间的粘结和 键合。间接合成则是先单独将聚晶金刚石层烧结成型， 再用焊接的方法使聚晶金 刚石层紧密结合到硬质合金基体上。  The basic preparation process of the PDC composite sheet is to adopt a special structure and method to form a tight bond between the polycrystalline diamond layer and the cemented carbide. There are two main methods of synthesis: direct synthesis and indirect synthesis. Direct synthesis means that the polycrystalline diamond layer and the cemented carbide substrate are synthesized at one time, that is, the diamond powder of the synthetic polycrystalline diamond layer is directly sintered at a high temperature and high pressure on the substrate and closely combined with the matrix, so that the obtained polycrystalline diamond layer is also called It is a growth type polycrystalline diamond. In addition, during the sintering process, the catalysis of components such as Ni, Co and W in the cemented carbide also promotes the bonding and bonding between the diamond powders and between the cemented carbides. For indirect synthesis, the polycrystalline diamond layer is first sintered separately, and the polycrystalline diamond layer is tightly bonded to the cemented carbide substrate by welding.
尽管 PDC复合片与天然金刚石以及各种硬质合金、 工具钢等相比具有更加 优良的性能， 但现代石油工业和机械制造加工业的不断迅猛发展仍然不断地对 PDC复合片的性能和质量提出更高要求。 在实际应用中例如 PDC复合片钻头或 刀具在工作时， 由于高速旋转和切削而受到巨大的剪应力作用， 因此 PDC复合 片的聚晶金刚石层、 硬质合金基体以及两者的界面结合处失效的情况都时有发 生。 在 PDC复合片的失效情况中， 聚晶金刚石层的脱落占了很大比重。 据美国 石油部门的统计分析， 在深井钻孔作业中， 33%的钻头失效是由聚晶金刚石层脱 落造成的。 另外基体的强度、硬度及抗冲击性的局限也容易造成钻头损坏， 或者 造成聚晶金刚石层的利用率不高而降低钻头的使用时效。 由此可见，改善界面应力、优化界面结构从而获得更好的界面结合以及强化、 硬化基体都可以更进一步提高 PDC复合片的性能和质量。 美国专利 US5662720 描述了一种通过在直接合成聚晶金刚石层之前改变硬质合金基体结合面的形貌 的方案来增强 PDC复合片的界面结合力和性能的方法。 该专利中的方法是在硬 质合金基体的结合面上加工出若干槽道或将整个结合面加工至呈 "蛋形" (egg-carton shaped) 起伏的凹坑和凸起， 从而增加烧结后聚晶金刚石层和硬质 合金基体的结合面积， 这样一来不仅提高了界面结合力， 而且充分利用了特殊形 状的 "咬合"关系来增强 PDC复合片对抗工作中经受的剪应力的能力。 另外， 中国专利 CN201110148812.7提到一种用碳纳米管的纤维增强效果增强 PDC复合 片的方法， 具体方案是将碳纳米管掺入到烧结聚晶金刚石的金刚石粉体中， 从而 增加烧结后 PDC复合片整体的韧性和抗冲击性能。 Although PDC composite sheets have better performance than natural diamonds and various hard alloys, tool steels, etc., the rapid development of modern petroleum industry and machinery manufacturing industry continues to put forward the performance and quality of PDC composite sheets. Higher requirements. In practical applications, for example, PDC composite drill bits or tools are subjected to large shear stress due to high-speed rotation and cutting during operation, so the interface of the polycrystalline diamond layer, the cemented carbide substrate and the PDC composite sheet fails. The situation has always happened. In the failure condition of the PDC composite sheet, the shedding of the polycrystalline diamond layer accounts for a large proportion. According to the statistical analysis of the US oil department, in deep well drilling operations, 33% of drill bit failures are caused by the shedding of the polycrystalline diamond layer. In addition, the strength, hardness and impact resistance of the substrate are also likely to cause damage to the drill bit, or the utilization rate of the polycrystalline diamond layer is not high and the use time of the drill bit is lowered. It can be seen that improving the interface stress, optimizing the interface structure to obtain better interface bonding, and strengthening and hardening the matrix can further improve the performance and quality of the PDC composite sheet. U.S. Patent No. 5,662,720 describes a method for enhancing the interfacial adhesion and properties of a PDC composite by modifying the morphology of the cemented carbide substrate bonding surface prior to direct synthesis of the polycrystalline diamond layer. The method in this patent is to machine a plurality of channels on the bonding surface of the cemented carbide substrate or to process the entire bonding surface into pits and protrusions which are "egg-carton shaped" undulations, thereby increasing the sintering. The combined area of the polycrystalline diamond layer and the cemented carbide substrate not only improves the interfacial adhesion, but also leverages the "bite" relationship of the particular shape to enhance the ability of the PDC composite to withstand the shear stress experienced during operation. In addition, the Chinese patent CN201110148812.7 mentions a method for reinforcing a PDC composite sheet by using a fiber-reinforced effect of carbon nanotubes, and the specific scheme is to incorporate carbon nanotubes into the diamond powder of the sintered polycrystalline diamond, thereby increasing the sintering. The overall toughness and impact resistance of the PDC composite sheet.
这些专利中提到的方法都在一定程度上增加了 PDC 复合片的强度和抗冲 击性， 也为新的 PDC复合片增强方案打开了思路。  The methods mentioned in these patents have increased the strength and impact resistance of PDC composites to a certain extent, and opened up new ideas for the new PDC composite reinforcement solution.
发明内容 Summary of the invention
本发明目的是为了进一步提高 PDC复合片中聚晶金刚石层和硬质合金基体 的结合强度以及基体的强度。 本发明提供一种 CVD金刚石增强的聚晶金刚石复合片，是由聚晶金刚石层、 硬质合金基体和 CVD金刚石条组成， 其中， CVD金刚石条有序埋入复合片中， 表面加工后 CVD金刚石条上端面在聚晶金刚石层表面露出， 下端面深入到硬质 合金基体中。  SUMMARY OF THE INVENTION The object of the present invention is to further improve the bonding strength of a polycrystalline diamond layer and a cemented carbide substrate in a PDC composite sheet and the strength of the substrate. The invention provides a CVD diamond reinforced polycrystalline diamond composite sheet, which is composed of a polycrystalline diamond layer, a cemented carbide substrate and a CVD diamond strip, wherein the CVD diamond strip is embedded in the composite sheet in an orderly manner, and the surface processed CVD diamond The upper end surface of the strip is exposed on the surface of the polycrystalline diamond layer, and the lower end surface penetrates into the cemented carbide substrate.
本发明提供的另一种 CVD金刚石增强的聚晶金刚石复合片， 是聚晶金刚石 复合片中复合进了贯通聚晶金刚石层和硬质合金基体接触界面的、具有特殊形状 的 CVD金刚石条； CVD金刚石条有 "I"形、 "L"形、 "T"形以及 "工"形四 种， 由直流电弧等离子体 CVD、 微波 CVD或热丝 CVD技术制备， 并经激光切 割成型。  Another CVD diamond-reinforced polycrystalline diamond compact sheet provided by the present invention is a CVD diamond strip having a special shape which is integrated into a contact interface between a through-polycrystalline diamond layer and a cemented carbide substrate in a polycrystalline diamond compact sheet; Diamond strips are available in four types: "I" shape, "L" shape, "T" shape, and "work" shape. They are prepared by DC arc plasma CVD, microwave CVD or hot wire CVD, and are laser cut.
进一步的， 本发明所述的 CVD金刚石增强的聚晶金刚石复合片的制备方法 为， 制备过程顺序依次为利用等离子体喷射 CVD法、 微波 CVD法或热丝 CVD 法进行 CVD金刚石膜制备， 将激光切割成型， 把 CVD金刚石条有序埋入硬质 合金和聚晶金刚石粉体中， 然后压制成坯， 进行高温烧结， 再进行退火处理以消 除残余应力和热应力， 最后加工成型。 Further, the CVD diamond-reinforced polycrystalline diamond compact sheet of the present invention is prepared by sequentially performing a CVD diamond film by a plasma jet CVD method, a microwave CVD method or a hot filament CVD method. Cutting and molding, CVD diamond strips are embedded in hard order The alloy and the polycrystalline diamond powder are then pressed into a billet, sintered at a high temperature, and annealed to eliminate residual stress and thermal stress, and finally processed.
所述金刚石条制备方法具体步骤为：  The specific steps of the diamond strip preparation method are as follows:
( 1 ) 使用直流电弧等离子体 CVD技术制备直径 60— 120mm、 厚度为 2— 3mm的 CVD金刚石自支撑膜。  (1) A CVD diamond self-supporting film with a diameter of 60-120 mm and a thickness of 2-3 mm is prepared by DC arc plasma CVD.
(2)使用激光切割机将 CVD金刚石自支撑膜分别切割成若干 "I"形、 "L" 形、 "T"形以及 "工"形的长条。 进一步的， 所述的 CVD金刚石增强聚晶金刚石复合片的制备方法， 其特征 在于：将 CVD金刚石条埋入硬质合金粉体和聚晶金刚石层粉体中，压制成坯后， 在氢还原气氛下热压烧结， 并退火处理以消除残余应力和热应力。具体操作过程 是： ①将混合好的金刚石微粉、 CVD 金刚石条与硬质合金基体置于叶蜡石合成 模中压实组装后，放入六面顶金刚石压机中，在压力 5-7GPa，温度 1350-1650°C， 合成 2-5分钟， 卸压后取出样品制成毛坯； ②将成型的毛坯密封进石墨炉胆， 并 将石墨炉胆放入压力烧结炉中；③向炉内通入流动氢气营造还原气氛，然后在保 持压力 P 80kN 的条件下使炉内温度以 10-30°C/min 的升温速度从室温升到 650-800 °C , 保温 25-40min; ④再以 5-15°C/min的升温速度从 650-80CTC升至最 终的烧结温度 900-980°C， 并保持 3-7min; ⑤继续保持压力和氢还原气氛， 以 5-15°C/min的降温速度降至 450-550°C， 保温 5-15min; ⑥撤去压力载荷， 随炉 冷却至室温； ⑦经机械抛磨后获得新型的聚晶金刚石复合片。 优选的， 所述制备方法是将 CVD金刚石条埋入硬质合金粉体和聚晶金刚石 层粉体中， 压制成坯后， 在氢还原气氛下热压烧结， 并退火处理以消除残余应力 和热应力； 具体操作过程是： ①将含有 CVD金刚石条的混合粉料置于不锈钢模 具中， 用油压机加压至 30MPa制成毛坯； ②将冷压成型的毛坯密封进石墨炉胆， 并将石墨炉胆放入压力烧结炉中；③向炉内通入流动氢气营造还原气氛，然后在 保持压力 P 80kN 的条件下使炉内温度以 20 °C/min 的升温速度从室温升到 700 °C , 保温 30min; ④再以 10°C/min的升温速度从 700°C升至最终的烧结温度 950°C， 并保持 5min; ⑤继续保持压力和氢还原气氛， 以 10°C/min的降温速度 降至 500°C， 保温 lOmin; ⑥撤去压力载荷， 随炉冷却至室温； ⑦加工成型。 (2) The CVD diamond self-supporting film is separately cut into a plurality of "I", "L", "T", and "work" shaped strips using a laser cutter. Further, the method for preparing a CVD diamond-reinforced polycrystalline diamond compact sheet is characterized in that a CVD diamond strip is embedded in a cemented carbide powder and a polycrystalline diamond layer powder, and then pressed into a billet, and then reduced in hydrogen. The film is hot pressed under an atmosphere and annealed to eliminate residual stress and thermal stress. The specific operation process is as follows: 1 The compacted diamond micropowder, CVD diamond strip and cemented carbide substrate are compacted and assembled in a pyrophyllite synthesis mold, and then placed in a six-sided diamond press at a pressure of 5-7 GPa. The temperature is 1350-1650 ° C, the synthesis is 2-5 minutes, the sample is taken out after the pressure is released to make the blank; 2 the formed blank is sealed into the graphite furnace, and the graphite furnace is placed in the pressure sintering furnace; The flowing hydrogen gas is used to create a reducing atmosphere, and then the furnace temperature is raised from room temperature to 650-800 °C at a temperature increase rate of 10-30 ° C/min under the condition of maintaining a pressure of P 80 kN, and the temperature is maintained for 25-40 min; The heating rate of 5-15 ° C / min is raised from 650-80 CTC to the final sintering temperature of 900-980 ° C, and maintained for 3-7 min; 5 continue to maintain pressure and hydrogen reduction atmosphere, to 5-15 ° C / min The cooling rate is reduced to 450-550 ° C, and the temperature is kept for 5-15 min. 6 The pressure load is removed, and the furnace is cooled to room temperature. 7 After the mechanical polishing, a new polycrystalline diamond composite sheet is obtained. Preferably, the preparation method comprises: burying a CVD diamond strip into a cemented carbide powder and a polycrystalline diamond layer powder, pressing it into a billet, performing hot press sintering under a hydrogen reduction atmosphere, and annealing to eliminate residual stress and Thermal stress; The specific operation process is as follows: 1 Place the mixed powder containing CVD diamond strip in a stainless steel mold, pressurize it to 30 MPa with a hydraulic press to make a blank; 2 Seal the cold-formed blank into a graphite furnace, and graphite The furnace is placed in a pressure sintering furnace; 3 a flowing hydrogen gas is introduced into the furnace to create a reducing atmosphere, and then the furnace temperature is raised from room temperature to a temperature rising rate of 20 ° C/min under a condition of maintaining a pressure of P 80 kN. 700 ° C, heat preservation for 30 min; 4 and then increase from 700 ° C at a temperature increase rate of 10 ° C / min to a final sintering temperature of 950 ° C for 5 min; 5 continue to maintain pressure and hydrogen reduction atmosphere, at 10 ° C / The cooling rate of min is reduced to 500 ° C, and the temperature is kept lOmin; 6 the pressure load is removed, and the furnace is cooled to room temperature;
由于 CVD金刚石条与烧结聚晶金刚石层的金刚石粉同质， 因此烧结后的聚 晶金刚石层和植入其中的 CVD金刚石条间会形成紧密结合， 同时 CVD金刚石 条的致密度远远大于聚晶金刚石层，首先将大大提高聚晶金刚石层的强度和抗冲 击性； 其次， CVD金刚石条作为增强相整体贯穿于 PDC复合片的聚晶金刚石层 和硬质合金基体两部分， 与两部分分别紧密结合，相当于增加了两部分的结合面 积和结合强度； 再次， CVD 金刚石条位于界面关键位置， 起到 "咬合"作用， 同时其自身的高强度将更有利于 PDC复合片抵御在工作状态下承受的巨大剪应 力； 另外， 伸入基体中的 CVD金刚石条的一部分也对硬质合金基体起到增强作 用，这将大大提高基体的使用寿命，从而提高聚晶金刚石层的利用率和整个 PDC 复合片的使用时效。 Since the CVD diamond strip is homogenous to the diamond powder of the sintered polycrystalline diamond layer, a tight bond is formed between the sintered polycrystalline diamond layer and the CVD diamond strip implanted therein, and the density of the CVD diamond strip is much larger than that of the polycrystal. The diamond layer will firstly greatly improve the strength and impact resistance of the polycrystalline diamond layer. Secondly, the CVD diamond strip as a reinforcing phase as a whole penetrates through the polycrystalline diamond layer and the cemented carbide substrate of the PDC composite sheet, which are closely related to the two parts. The combination is equivalent to increasing the bonding area and bonding strength of the two parts; again, the CVD diamond strip is located at the key position of the interface, playing a "bite" role, and its own high strength will be more favorable for the PDC composite sheet to resist the working condition. Large shear stress; In addition, a portion of the CVD diamond strip extending into the substrate also enhances the cemented carbide matrix, which greatly increases the useful life of the matrix, thereby increasing the utilization of the polycrystalline diamond layer and the overall PDC The use time of the composite sheet.
本发明的有益效果：  The beneficial effects of the invention:
大大提高 PDC复合片的强度、抗冲击性等力学性能， 有效防止在 PDC复合 片使用中聚晶金刚石层脱落造成的失效， 并提高 PDC复合片的使用寿命。  The mechanical properties such as strength and impact resistance of the PDC composite sheet are greatly improved, and the failure caused by the falling of the polycrystalline diamond layer in the use of the PDC composite sheet is effectively prevented, and the service life of the PDC composite sheet is improved.
附图说明 DRAWINGS
下面结合附图和实施例对本发明进一步说明。  The invention will now be further described with reference to the drawings and embodiments.
图 1是普通 PDC复合片的基本结构示意图。  Fig. 1 is a schematic view showing the basic structure of a conventional PDC composite sheet.
图 2、 图 3、 图 4和图 5分别是本发明的 4个实施例的结构示意图。  2, 3, 4 and 5 are schematic views of the structure of four embodiments of the present invention, respectively.
各图中， 1为聚晶金刚石层， 2为硬质合金基体， 3、 4、 5、 6分别为 "I" 形、 "L"形、 "T"形以及 "工"形 CVD金刚石条。  In each figure, 1 is a polycrystalline diamond layer, 2 is a cemented carbide substrate, and 3, 4, 5, and 6 are "I", "L", "T", and "work" CVD diamond bars, respectively.
具体实施方式 detailed description
实施例 1  Example 1
如图 2所示， 一种 "I"形 CVD金刚石条增强聚晶金刚石复合片制备方法， 步骤如下：  As shown in Figure 2, an "I" shaped CVD diamond strip reinforced polycrystalline diamond compact is prepared as follows:
CVD金刚石自支撑膜激光切割成 "I"形长条， 埋入硬质合金粉体和聚晶金 刚石层粉体中， 压制成坯后， 在氢还原气氛下热压烧结， 并退火处理以消除残余 应力和热应力； 具体操作过程是： ①将混合好的金刚石微粉、 CVD 金刚石条与 硬质合金基体置于叶蜡石合成模中压实组装后，放入六面顶金刚石压机中，在压 力 5.7GPa， 温度 1450°C， 合成 3分钟， 卸压后取出样品制成毛坯； ②将成型的 毛坯密封进石墨炉胆， 并将石墨炉胆放入压力烧结炉中；③向炉内通入流动氢气 营造还原气氛， 然后在保持压力 P 80kN的条件下使炉内温度以 20°C/min的升 温速度从室温升到 700 °C， 保温 30min; ④再以 10°C/min的升温速度从 700 °C升 至最终的烧结温度 950°C，并保持 5min;⑤继续保持压力和氢还原气氛， 以 10°C /min的降温速度降至 500°C， 保温 lOmin; ⑥撤去压力载荷， 随炉冷却至室温； ⑦加工成型。 CVD diamond self-supporting film is laser cut into "I" strips, embedded in cemented carbide powder and polycrystalline gold In the corundum layer powder, after being compacted into a billet, it is hot pressed and sintered under a hydrogen reducing atmosphere, and annealed to eliminate residual stress and thermal stress; the specific operation process is: 1 mixing the fine diamond powder, CVD diamond strip and hard The alloy substrate is compacted and assembled in a pyrophyllite synthesis mold, placed in a six-sided diamond press, and subjected to a pressure of 5.7 GPa at a temperature of 1,450 ° C for 3 minutes. After depressurization, the sample is taken out to form a blank; The formed blank is sealed into the graphite furnace, and the graphite furnace is placed in the pressure sintering furnace; 3 flowing hydrogen gas into the furnace to create a reducing atmosphere, and then the furnace temperature is 20° under the condition of maintaining the pressure P 80kN The heating rate of C/min is raised from room temperature to 700 °C, and kept for 30 minutes; 4 is further increased from 700 °C to the final sintering temperature of 950 °C at a heating rate of 10 °C/min for 5 min; Pressure and hydrogen reduction atmosphere, to 10 ° C / min cooling rate down to 500 ° C, insulation lOmin; 6 remove the pressure load, with the furnace cooled to room temperature; 7 processing molding.
实施例 2 Example 2
如图 3所示， 一种 "L"形 CVD金刚石条增强聚晶金刚石复合片制备方法， 步骤如下：  As shown in Figure 3, an "L"-shaped CVD diamond strip reinforced polycrystalline diamond compact is prepared as follows:
CVD金刚石自支撑膜激光切割成 "L"形长条， 埋入混合粉体中，压制成坯、 烧结成型。  The CVD diamond self-supporting film is laser-cut into "L"-shaped strips, embedded in the mixed powder, pressed into a billet, and sintered.
实施例 3 Example 3
如图 4所示， 一种 "T"形 CVD金刚石条增强聚晶金刚石复合片制备方法， 步骤如下：  As shown in Figure 4, a "T" shaped CVD diamond strip reinforced polycrystalline diamond compact is prepared as follows:
CVD金刚石自支撑膜激光切割成 "T"形长条， 埋入混合粉体中，压制成坯、 烧结成型。  The CVD diamond self-supporting film is laser cut into "T" shaped strips, embedded in the mixed powder, pressed into a billet, and sintered.
实施例 4 Example 4
如图 5所示， 一种 "工"形 CVD金刚石条增强聚晶金刚石复合片制备方法， 步骤如下：  As shown in FIG. 5, a method for preparing a "work" shaped CVD diamond strip reinforced polycrystalline diamond compact is as follows:
CVD 金刚石自支撑膜激光切割成 "工"形长条， 埋入混合粉体中， 压制成 坯、 烧结成型。  The CVD diamond self-supporting film is laser cut into "work" shaped strips, embedded in the mixed powder, pressed into a billet, and sintered.

Claims

1. 一种 CVD金刚石增强的聚晶金刚石复合片， 其特征在于： 由聚晶金刚石层、 硬质合金基体和 CVD金刚石条组成， 其中， CVD金刚石条有序埋入复合片 中， 表面加工后 CVD 金刚石条上端面在聚晶金刚石层表面露出， 下端面深 入到硬质合金基体中。 A CVD diamond-reinforced polycrystalline diamond compact sheet comprising: a polycrystalline diamond layer, a cemented carbide substrate and a CVD diamond strip, wherein the CVD diamond strip is embedded in the composite sheet in an orderly manner, after surface processing The upper end surface of the CVD diamond strip is exposed on the surface of the polycrystalline diamond layer, and the lower end surface penetrates into the cemented carbide substrate.
2. 一种 CVD 金刚石增强的聚晶金刚石复合片， 其特征在于： 聚晶金刚石复合 片中复合进了贯通聚晶金刚石层和硬质合金基体接触界面的、 具有特殊形状 的 CVD金刚石条； CVD金刚石条有 "I"形、 "L"形、 "T"形以及 "工"形 四种， 由直流电弧等离子体 CVD、微波 CVD或热丝 CVD技术制备， 并经激 光切割成型。  2. A CVD diamond-reinforced polycrystalline diamond compact sheet, characterized in that: a polycrystalline diamond compact sheet is compounded into a CVD diamond strip having a special shape that penetrates a contact interface between a polycrystalline diamond layer and a cemented carbide substrate; Diamond strips are available in four types: "I" shape, "L" shape, "T" shape, and "work" shape. They are prepared by DC arc plasma CVD, microwave CVD or hot wire CVD, and are laser cut.
3. 根据权利要求 1或 2所述的 CVD金刚石增强的聚晶金刚石复合片的制备方 法，其特征在于，制备过程顺序依次为利用等离子体喷射 CVD法、微波 CVD 法或热丝 CVD法进行 CVD金刚石膜制备， 将激光切割成型， 把 CVD金刚 石条有序埋入硬质合金和聚晶金刚石粉体中，然后压制成坯，进行高温烧结， 再进行退火处理， 最后加工成型。  The method for preparing a CVD diamond-reinforced polycrystalline diamond compact according to claim 1 or 2, wherein the preparation process is sequentially performed by plasma jet CVD, microwave CVD or hot filament CVD. The diamond film is prepared by laser cutting, and the CVD diamond strips are sequentially embedded in the cemented carbide and the polycrystalline diamond powder, and then pressed into a billet, sintered at a high temperature, annealed, and finally processed.
4. 根据权利要求 3所述的 CVD金刚石增强聚晶金刚石复合片的制备方法， 其 特征在于： 将 CVD 金刚石条埋入硬质合金粉体和聚晶金刚石层粉体中， 压 制成坯后，在氢还原气氛下热压烧结， 并退火处理以消除残余应力和热应力。 具体操作过程是： ①将混合好的金刚石微粉、 CVD金刚石条与硬质合金基体 置于叶蜡石合成模中压实组装后，放入六面顶金刚石压机中，在压力 5-7GPa， 温度 1350-1650°C， 合成 2-5分钟， 卸压后取出样品制成毛坯； ②将成型的毛 坯密封进石墨炉胆， 并将石墨炉胆放入压力烧结炉中； ③向炉内通入流动氢 气营造还原气氛， 然后在保持压力 P 80kN的条件下使炉内温度以 10-3CTC /min的升温速度从室温升到 650-800 °C， 保温 25-40min; ④再以 5-15°C/min 的升温速度从 650-800 °C升至最终的烧结温度 900-980°C， 并保持 3-7min; ⑤ 继续保持压力和氢还原气氛， 以 5-15°C/min的降温速度降至 450-550°C， 保 温 5-15min; ⑥撤去压力载荷， 随炉冷却至室温； ⑦经机械抛磨后获得新型 的聚晶金刚石复合片。 The method for preparing a CVD diamond-reinforced polycrystalline diamond compact according to claim 3, wherein: the CVD diamond strip is embedded in the cemented carbide powder and the polycrystalline diamond layer powder, and then pressed into a blank, It is hot pressed and sintered under a hydrogen reduction atmosphere and annealed to eliminate residual stress and thermal stress. The specific operation process is as follows: 1 The compacted diamond micropowder, CVD diamond strip and cemented carbide substrate are compacted and assembled in a pyrophyllite synthesis mold, and then placed in a six-sided diamond press at a pressure of 5-7 GPa. The temperature is 1350-1650 ° C, the synthesis is 2-5 minutes, the sample is taken out after the pressure is released to make the blank; 2 the formed blank is sealed into the graphite furnace, and the graphite furnace is placed in the pressure sintering furnace; Into the flowing hydrogen to create a reducing atmosphere, and then under the condition of maintaining the pressure P 80kN, the furnace temperature is raised from room temperature to 650-800 °C at a heating rate of 10-3 CTC / min, and the temperature is maintained for 25-40 min; The heating rate of 15 ° C / min is raised from 650-800 ° C to the final sintering temperature of 900-980 ° C, and maintained for 3-7 min; 5 continue to maintain the pressure and hydrogen reduction atmosphere, to 5-15 ° C / min The cooling rate is reduced to 450-550 ° C, and the temperature is kept for 5-15 min. 6 The pressure load is removed, and the furnace is cooled to room temperature. 7 After the mechanical polishing, a new type is obtained. Polycrystalline diamond composite sheet.
5. 根据权利要求 3所述的 CVD金刚石增强聚晶金刚石复合片的制备方法， 其特征在于： 将 CVD金刚石条埋入硬质合金粉体和聚晶金刚石层粉体中， 压制 成坯后， 在氢还原气氛下热压烧结， 并退火处理以消除残余应力和热应力； 具体 操作过程是： ①将含有 CVD金刚石条的混合粉料置于不锈钢模具中， 用油压机 加压至 30MPa制成毛坯； ②将冷压成型的毛坯密封进石墨炉胆， 并将石墨炉胆 放入压力烧结炉中； ③向炉内通入流动氢气营造还原气氛， 然后在保持压力！5^ 80kN 的条件下使炉内温度以 20°C/min 的升温速度从室温升到 700 °C， 保温 30min; ④再以 10°C/min的升温速度从 700°C升至最终的烧结温度 950°C， 并保 持 5min; ⑤继续保持压力和氢还原气氛， 以 lCTC/min的降温速度降至 500°C， 保温 lOmin; ⑥撤去压力载荷， 随炉冷却至室温； ⑦加工成型。 The method for preparing a CVD diamond-reinforced polycrystalline diamond compact according to claim 3, wherein: the CVD diamond strip is embedded in the cemented carbide powder and the polycrystalline diamond layer powder, and then pressed into a blank, Hot-pressed and sintered under hydrogen reduction atmosphere, and annealed to eliminate residual stress and thermal stress; the specific operation process is as follows: 1 The mixed powder containing CVD diamond strip is placed in a stainless steel mold, and pressed into a blank by a hydraulic press to 30 MPa. 2 Seal the cold-formed blank into the graphite furnace and place the graphite furnace into the pressure sintering furnace; 3 Pass the flowing hydrogen into the furnace to create a reducing atmosphere, and then maintain the pressure! Under the condition of 5 ^ 80kN, the temperature in the furnace was raised from room temperature to 700 °C at a heating rate of 20 °C/min, and kept at 30 minutes ; 4 was further increased from 700 °C to the final temperature at a heating rate of 10 °C/min. Sintering temperature 950 ° C, and maintained for 5 min; 5 continue to maintain pressure and hydrogen reduction atmosphere, to 1 °C / min cooling rate down to 500 ° C, insulation lOmin; 6 remove the pressure load, with the furnace cooled to room temperature; 7 processing.
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