Study on growth of coarse grains of diamond with high quality under HPHT

The growth of coarse grains of diamond was observed with graphite as carbon source and Fe₈₀Ni₂₀ alloy powder as catalyst at HPHT in a China-type SPD 6×1670T cubic high-pressure apparatus with highly exact control system. To synthesize coarse grains of diamond crystal with high quality, advanced indirect heat assembly, powder catalyst technology and catalyst with optimal granularity were used. Especially the nucleation of diamond and the growth rate were strictly controlled by the optimized synthesis craft. At last, diamond crystals (about 0.85 mm) in the perfect hex-octahedron shape were successfully synthesized at ~5.4 GPa and ~1360℃ in 60 min. The characteristic of crystal growth with powder catalyst technology under HPHT was discussed. The results and techniques might be useful for production of coarse grains of diamond.     

Synthesis of high quality type-Ib diamond crystals in carats grade

High quality type-Ib tower-shape gem-diamond crystals in carats grade were synthesized in cubic anvil high pressure apparatus (SPD-6×1200) at 5.4 GPa and 1250-1450°C. The relationship between the growth time and the weight of growth diamond has been gained. The faces of {110} and {113} were found in the synthetic diamond crystals frequently. We found that the relative growth rate of {113} face was descending with the increase of growth temperature, and that of {110} face had no obvious change with the incre...     

Effects of carbon diffusing field in alloy solvent on the growth of tower-shape diamond single crystal

High-quality type-Ib tower-shape diamond single crystals were synthesized in cubic anvil high pressure apparatus (SPD-6×1200) at 5.4 GPa and 1250-1450°C. The (100) face of seed crystal was used as the growth face, and FeNiMnCo alloy was used as the solvent/catalyst. Two kinds of carbon diffusing fields (type-B and type-G) were simulated by finite element method (FEM). Using the two kinds of carbon diffusing fields, many diamond single crystals were synthesized. The effects of carbon diffusing fields on the ...     

Fe-Ni-C粉末触媒体系金刚石的合成与表征

利用FeNi粉末触媒在六面顶压机上进行工业金刚石单晶的合成与表征. 结果表明: 在Fe-Ni-C体系合成了优质的六面体、 六-八面体及八面体金刚石单晶; 金刚石{111}晶面的生长属于二维层状生长机制; 金刚石中的包裹体主要由FeNi合金组成.     

金刚石压砧径向X射线衍射技术的评述

与金刚石压砧传统轴向X射线衍射技术相比,采用金刚石压砧径向X射线衍射技术更方便,且实验压力更高（大于100Gea）,获取的信息更多．以c-BC2N样品的高压原位同步辐射径向X射线衍射实验为例,说明了金刚石压砧径向X射线衍射技术的优越性．     

金刚石薄膜/立方氮化硼异质结的制备

利用高温高压合成的立方氮化硼单晶材料,采用恒浓度高温扩散方法制备n型立方氮化硼半导体材料。通过化学气相沉积方法在n型立方氮化硼上外延生长p型金刚石薄膜。在此基础上,通过欧姆接触电极的制作,制备出金刚石薄膜／立方氮化硼异质pn结,并给出pn结的伏安特性曲线。     

Mechanism of diamond-to-graphite transformation at diamond-stable conditions

The diamond-to-graphite transformation at diamond-stable conditions is studied by temperature gradient method （TGM） under high pressure and high temperature （HPHT）, although it is unreasonable from the view of thermodynamic considerations. It is found that, at diamond-stable conditions, for example, at 5.5 GPa and 1550 K, with fine diamond grits as carbon source and NiMnCo alloy as metal solvent assisted, not only large diamond crystals, but metastable regrown graphite crystals would be grown by layer growth mechanism, and the abundance of carbon source in the higher temperature region is indispensable for the presence of metastable regrown graphite crystals. From this transformation, it is concluded that, with metal solvent assisted, although the mechanism of crystal growth could be understood by the macro-mechanism of solubility difference between diamond and graphite in metal solvents, from the point of micro-mechanism, the minimum growth units for diamond or graphite crystals should be at atomic level and unrelated to the kinds of carbon source （diamond or graphite）, which could be accumulated free-selectively on the graphite with Sp2Tr or diamond crystals with sp3 bond structure.     

铁基粉末触媒合成金刚石

本文利用六种铁基粉末触媒（FeNiNa,n=0,1,2,3,d,5X。代表Fe在触媒中的含量,Xn〉xn-1）在国产六面顶压机上进行了金刚石单晶的合成实验,研究了高温高压条件下（～6GPa,～1600℃）,铁基粉末触媒随铁含量的改变,石墨碳—铁基触媒体系合成金刚石条件的变化规律以及金刚石单晶的生长特性,利用穆斯堡尔谱对金刚石中铁元素形成的包裹体进行了检测．结果表明,随着铁基粉末触媒中铁含量的增加,合成金刚石的压力和温度条件逐渐增高,金刚石生长的“V形区”上移,同时得出了铁基粉末触媒适合高温区（110）和（111）面生长以及金刚石中铁元素以FeNi和FeyC形式存在的结论．     

Effects of Ti additive on HPHT diamond synthesis in Fe-Ni-C system

Diamond crystals with low nitrogen concentration were synthesized from the Fe-Ni-C system with Ti additive at high pressure and high temperature （HPHT） in a china-type cubic high pressure apparatus （CHPA）. The synthesis pressure range was 4.8-5.2 GPa, and the temperature range was 1420-1600 K. The lowest synthesis pressure for diamond fell first and then rose with the increase of Ti additive. The color, shape, surface morphology and nitrogen impurity concentration of the synthesized diamond crystals were characterized using optical microscopy （OM）, scanning electron microscopy （SEM） and micro Fourier transform infrared （FTIR） spectrometry. The results show that the Ti additive has significant effects on color, growth rate, crystal shape, surface morphology and nitrogen impurity con- centration of the synthesized diamond crystals. The color of diamond crystals synthesized without Ti additive is yellow, while that with Ti additive becomes light and nearly colorless. The growth rate without Ti additive is higher than that with Ti additive. The crystal shapes of as-grown diamond crystals vary with the increase of Ti additive. The {111} crystal faces become dominant and some {311} crystal faces appear with the increase of Ti additive. The concentration of nitrogen impurity in diamond crystals without Ti additive is higher than that with Ti additive.     

电镀晶种法合成金刚石单晶实验研究

目的寻求一种合成金刚石大单晶的有效方法。方法采用在金刚石单晶上面电镀一层金属镍膜作为触媒,镀有镍膜的金刚石晶种被规则地放在石墨片上预先刻好的洞中,每两个洞之间保持相等的间距,然后与其他石墨片交替组装在高温高压下进行实验合成。结果实验结果表明,在合成压力、温度和时间分别~5.8 GPa、~1 460℃和14 min的条件下,合成后的单晶尺寸约是原晶种的3倍。与传统的合成工艺相比较,合成后的金刚石单晶具有较好的形貌与质量。结论采用电镀晶种法合成对高品级金刚石大单晶的合成具有一定参考意义。     

低量浓度掺杂La~(3+)对KDP晶体生长质量的影响

在低浓度掺杂下,利用溶液降温法生长了KDP晶体和掺杂不同量浓度三价La3+的KDP晶体。通过对未掺杂KDP晶体和掺杂La3+生长的KDP晶体对比研究发现,随着La3+离子掺杂量浓度的增加,抑制了柱面的扩展,减慢了KDP晶体生长速度,但是提高了生长溶液的稳定性,同时减少了晶体中缺陷的产生。对晶体柱区进行显微硬度的测量发现,随La3+离子掺杂量浓度的增加,晶体的致密度降低;用紫外/可见分光光度计在200~800 nm波段对样品柱区做了透过率测定,发现低量浓度(La3+≤4×10-3mol/L)的La3+掺杂可以提高KDP晶体在紫外波段的透过率,改善晶体的质量。     

Effect of additive boron on type-Ib gem diamond single crystals synthesized under HPHT

The boron-doped type-Ib gem diamond crystals were synthesized successfully by adding amorphous boron into a system of graphite and Kovar catalyst under high pressure and high temperature (HPHT).The effect of additive boron on type-Ib gem diamond was extensively studied including the growth characteristic,morphology and nitrogen concentration.The synthesized boron-doped type-Ib gem diamond crystals were characterized by optical microscope (OM),scanning electron microscope (SEM) and infrared spectrometer (IR)...     

Diamond synthesis from a system of chromium-carbide and Ni70Mn25Co5 alloy

In order to ascertain the mechanism of interaction between carbide and metallic catalyst and formation of diamond under high pressure and high temperature, and find a new method to synthesize diamond with special properties, it is necessary to investigate the reaction behavior of different carbides and metallic solvent_catalysts under high pressure and high temperature. A system of Cr-3C-2 powder and Ni 70Mn 25Co 5 alloy in weight ratio of 1∶6 was treated under 6 0 GPa and 1 500℃ for 20, 30 or 60 min respectively. X_ray diffraction of the samples indicated the Cr 3C 2 decomposed partially after high pressure and temperature treatment, and Cr 7C 3, Cr and diamond formed respectively. There was not any trace of graphite in the samples. The result suggested that the separated carbon atoms could form diamond directly without conversion process of graphite into diamond. The observation of SEI, WDX and EDX also showed that diamond crystals were synthesized in the system, which have perfect surfaces and shapes, with the average grain size of about 40 μm. The properties of the crystals are being investigated.     

Cu基块状非晶合金微观结构的特点及组织演化

采用水冷铜坩埚-铜模吸铸法成功制备了底部直径10 mm、长度80 mm的Cu50Zr42Al8圆锥形块体非晶试样.利用X射线衍射,光学显微镜和SEM、TEM等测试手段对圆锥形试样轴向和径向微观结构的特点和微观组织的演变进行了研究.结果表明,由于冷却速率的不同,圆锥形试样的显微组织由表面非晶区、中心等轴晶区及介于两区之间的过渡区组成.过渡区由非晶和晶体相组成,晶体的尺寸和体积分数由表面向中心逐渐增加,具有梯度变化的特征.     

掺Mn钾钠铌酸锶钡晶体光折变研究

实验中，生长、极化、制备出了掺０．０２％和０．０４％Ｍｎ钾钠铌酸锶钡晶体样品，并对其二波耦合、二波耦合响应时间及自泵浦相位共轭进行了测量．研究发现：掺Ｍｎ可以有效地增加钾钠铌酸锶钡晶体的吸收，在波长６３２．８ｎｍ，０．０２％Ｍｎ晶体样品的二波耦合增益系数大于７ｃｍ－１而０．０４％Ｍｎ晶体样品的二波耦合增益系数大于９ｃｍ－１，０．０４％Ｍｎ晶体样品二波耦合增益时间响应比０．０２％Ｍｎ晶体样品二波耦合增益时间响应快近４倍；０．０４％Ｍｎ晶体样品有很高自泵浦相位共轭反射率，高达７０％．实验研究表明：掺Ｍｎ可以提高钾钠铌酸锶钡晶体在长光波段的光折变性能     

静态破碎剂的轴向膨胀力学性能实验研究

针对静态破碎剂轴向膨胀力学行为进行了深入研究,提出了测量静态破碎剂膨胀压的轴向输出法,设计了测试系统及核心钢筒组件.分别采用轴向输出法和外管法对静态破碎剂膨胀压进行了测试.通过对比在不同孔径条件下两种方法测得的膨胀压,分析了孔径大小对静态破碎剂轴向膨胀压及其输出率的影响.结果表明:轴向输出法能够可靠准确测得静态破碎剂膨胀压;在固定的高径比条件下,静态破碎剂轴向膨胀压随孔径尺寸增大而增加;孔径小于50 mm时,自封孔效应导致静态破碎剂输出轴向膨胀压的能力减弱;孔径大于150 mm时,轴向膨胀压与径向膨胀压趋于一致,轴压输出率达100%.     

The tectonic uplift of the Hua Shan in the Cenozoic

Six granite samples were collected from six difference elevation locations at the Hua Shan in a main ridge of the Qinling Mountain. Apatite and zircon separated from these six samples were dated by the fission track technique. An assessment of the Cenozoic uplift or exhumation rate was obtained from the altitude difference of sampling samples dated by fission track, and from the difference of fission track dates of both apatite and zircon for a sample. The preliminary results suggest that the beginning of uplift of the Hua Shan was as early as 68.2 MaBP and the uplift rates for different periods are 0.02–0.19 mm/a (from the elevation difference) or 0.12–0.16 mm/a (from two mineral fission track dates). The average uplift rate is 0.12 mm/a (from the elevation difference) or 0.14 mm/a (from two mineral fission track dates). The uplift of the Hua Shan might accelerate since (17.8±2.0) MaBP, and the average uplift rate is about 0.19 mm/a.     

Ferroelectric and piezoelectric properties of novel relaxor ferroelectric single crystals PMNT

Relaxor ferroelectric single crystals PMNT with the size of 40 mm×80 mm have been grown by a modified Bridgman method and their ferroelectric and piezoelectric properties have been characterized.The properties varied with the compositions and cut types.On the (001) cut,PMNT76/24 single crystals exhibited a dielectric constant of about 3 400,a dielectric loss of tan＜0.7%,a piezoelectric constant d33 of 980 pC/N,an electromechanical coupling factor kt of 0.55 and Tc of about 110℃.Whereas the properties of PMNT67/33 single crystals on (001) cut were better: ε of about 5 300,tanδ＜0.6%,d33 up to 3 000 pC/N,kt 0.64,k33 0.93 and Tc of about 150℃.The piezoelectric properties on other cuts such as (110) and (111) were much lower than those on the (001) cut.The rhombohedral PMNT crystals grown by this method showed more excellent piezoelectric properties than those grown by high temperature solution method and higher value of kt than the rhombohedral PZNT single crystals.It has also been found that the fluctuation in ferroelectric and piezoelectric properties was related to such factors as composition uniformity and poling degree.     

Optical characterization of single-crystal diamond grown by DC arc plasma jet CVD

Optical centers of single-crystal diamond grown by DC arc plasma jet chemical vapor deposition (CVD) were examined using a low-temperature photoluminescence (PL) technique. The results show that most of the nitrogen-vacancy (NV) complexes are present as NV-centers, although some H2 and H3 centers and B-aggregates are also present in the single-crystal diamond because of nitrogen aggregation resulting from high N₂ incorporation and the high mobility of vacancies under growth temperatures of 950-1000℃. Furthermore, emissions of radiation-induced defects were also detected at 389, 467.5, 550, and 588.6 nm in the PL spectra. The reason for the formation of these radiation-induced defects is not clear. Although a Ni-based alloy was used during the diamond growth, Ni-related emissions were not detected in the PL spectra. In addition, the silicon-vacancy (Si-V)-related emission line at 737 nm, which has been observed in the spectra of many previously reported microwave plasma chemical vapor deposition (MPCVD) synthetic diamonds, was absent in the PL spectra of the single-crystal diamond prepared in this work. The high density of NV- centers, along with the absence of Ni-related defects and Si-V centers, makes the single-crystal diamond grown by DC arc plasma jet CVD a promising material for applications in quantum computing.     

基于围压增量的损伤砂岩三轴蠕变试验

为研究岩石峰后轴向与径向蠕变特性,采用MTS815岩石力学试验系统,进行了三轴压缩下红砂岩峰后蠕变试验,获取了不同性态的峰后轴向与径向蠕变曲线,探讨了岩石峰后轴向与径向蠕变特征,研究了损伤程度、围压增量对峰后轴向与径向蠕变特性的影响规律.试验结果表明:岩石峰后轴向与径向蠕变曲线主要由等速蠕变阶段和加速蠕变阶段组成,峰后径向蠕变特征相比轴向蠕变特征更显著;轴向和径向蠕变量与损伤程度呈正相关,径向蠕变相比轴向蠕变对损伤程度的敏感性更高,损伤程度的变化对径向蠕变的影响程度更强;施加围压增量,轴向与径向蠕变速率大大降低,蠕变失稳时间延长;围压增量对径向蠕变的影响明显强于轴向蠕变,工程实践中应重点控制围岩的径向变形.