Precision Modification of a Two-Stage Pressure Boosting System on a Domestic Cubic Press and Synthesized of Nano-Polycrystalline Diamond
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摘要: 传统国产铰链式六面顶压机采用限位开关定位、全开式快速充液和高速率升降压的工作模式，其六缸定位精度和充液同步性差，升降压速率无法满足超高压二级增压对偏载控制和力学平稳性的苛刻要求。为此，对国产650 mm缸径六面顶压机开展了系统性改造升级：设计安装了自锁式销轴，并对机架的高压形变进行了预补偿，以抑制或消除超压工况下机架的浮动及变形；搭建了双泵-多模式液压回路和油缸等体积进油充液流程，并创造性地提出了三阶段分段进给，结合独立位移的动作方式，提高了压机对中精度与充液同步性；编译了一套全新的闭环控制程序并与压机自身系统并联，实现了压机动作状态、油压、加热等数据组的实时采集、同步监控和闭环调节；提出了比例-积分-微分精密（proportional-integral-derivative，PID）复合控制结合精密控压模块构件的策略，实现了超慢速升降压速率控制。标定了合成腔压力-油压和加热温度-功率关系曲线，并进行了厘米尺寸纳米聚晶金刚石块材的高温高压合成。结果表明，优化升级后的国产650 mm缸径六面顶压机能够实现压力15 GPa、温度
2000 ℃以上条件下大体积样品的制备，极大地拓宽了国产六面顶压机的应用领域。Abstract: The traditional domestic hinge-type cubic presses are typically operated using limit switch for positioning, fully-open rapid hydraulic oil filling, and fixed-rate pressurization/depressurization modes. Such configurations are limited by poor six-cylinders positioning accuracy and hydraulic filling synchronization, and the pressurization and depressurization rates fail to meet the stringent requirements of ultra-high two-stage pressurization for eccentric load control and mechanical stability. In this study, systematic modification and upgrade were implemented on a domestic cubic press with 650 mm cylinders. To suppress or eliminate the floating and deformation of the frame under overpressure conditions, self-locking pin shaft was designed and assembled, and pre-compensation for frame deformation under high pressure was performed. In addition, aim at improving alignment accuracy and hydraulic filling synchronization, a dual-pump multi-mode hydraulic circuit and an equal-volume cylinder oil-filling process were built. Furthermore, a three-stage feeding method combined with an independent displacement action mode was innovatively proposed. A closed-loop control program was developed to operate in parallel with the original press control system, enabling the real-time acquisition, synchronous monitoring, and closed-loop adjustment of data sets including press operational status, oil pressure, and heating temperature. Additionally, a strategy combining proportional-integral-derivative (PID) control with precision pressure-control module components was proposed to achieve ultra-slow pressurization and depressurization. The correlation between synthesis chamber pressure and oil pressure, and the correlation between heating temperature and power were experimentally calibrated. Furthermore, the high-temperature and high-pressure (HTHP) synthesis of centimeter-sized nano-polycrystalline diamond bulk specimen was conducted. The results indicate that the optimized and upgraded domestic 650 mm cubic press is capable of synthesis large-volume samples at 15 GPa and over2000 ℃, which significantly expands the application area of domestic cubic presses. -
图 2 油路示意图：(a) 液压油路，(b) 同步缸，(c) 比例阀
Figure 2. Schematic diagram of the oil circuit: (a) hydraulic oil circuit; (b) synchronizing cylinder; (c) proportional valve
图 3 650压机的数据采集监控程序
Figure 3. Data acquisition and monitoring program for the 650 mm cubic press
图 4 合成压力与油压的关系：(a) 金属Bi，(b) ZnTe，(c) ZnS，(d) 合成压力-油压曲线（插图为标压组件局部示意图和局部标压曲线）
Figure 4. Relationship between synthesis pressure and oil pressure: (a) Bi; (b) ZnTe; (c) ZnS; (d) synthesis pressure-oil pressure curve (Inset: local schematic of the pressure calibration assembly and partial pressure calibration curve.)
图 5 合成腔中心温度-加热功率关系曲线（插图为组装示意图）
Figure 5. Temperature at the center of the synthesis chamber as a function of heating power (Inset illustrates the assembly geometry.)
图 6 前驱体与纳米聚晶金刚石样品的XRD谱
Figure 6. XRD patterns of the precursor and nano-polycrystalline diamond
图 7 纳米聚晶金刚石的TEM形貌及SEAD图像（插图）
Figure 7. TEM and SEAD images (insert) of the nano-polycrystalline diamond
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