Nano-diamond/Ni复合电刷镀层的组织形貌的研究

以45#钢为基体,制备了普通镍镀层和nano-diamond/Ni复合刷镀层,采用扫描电镜、能谱仪、X射线衍射仪和金相显微镜等设备对比研究了两种镀层的组织形貌。金相显微镜和扫描电镜分析结果表明,与普通镍镀层相比,nano-diamond/Ni复合刷镀层的表面更加平整、致密,组织更加细化;nano-dia-mond/Ni复合刷镀层表面呈典型的"菜花头"形状,弥散分布的纳米金刚石被镍包裹。能谱仪分析结果表明,nano-diamond/Ni复合刷镀层中纳米颗粒特征元素C的质量分数为7.37%。X射线衍射分析结果表明,随着纳米金刚石加入量的增加,镀层表面晶粒尺寸逐渐减小。

Influence of nano-diamond content on the microstructure,mechanical and thermal properties of the ZK60 composites

The effect of nano diamond(ND)content on the microstructure,mechanical properties,and thermal conductivity of ZK60+x(x=0,0.05,0.1,0.15,0.2 wt.%)ND composites were investigated.The microstructures of ND/ZK60 composites were observed,which indicated that the nanoscale MgZn_(2) and ND particles distributed evenly in theα-Mg matrix.The tensile yield strength(TYS)and compressive yield strength(CYS)of the composites first increased remarkably and then decreased with further increasing the ND content.Due to the surface area of the matrix-diamond interface increased and the grains sizes of composites decreased with the amount of ND increase,which cause the coefficient of thermal expansion(CTE)of the composites reduced significantly.Meanwhile,the thermal conductivity of the composite material decreases from 129 W·m^(−1)·K^(−1) to 116 W·m^(−1)·K^(−1) with the content of ND increasing from 0.05%to 2.0%.The thermal conductivity of the composites increases to the maximum and then decrease with the increase of temperature(in temperature range of 273-573 K).The ZK60+0.05 ND showed superior mechanical and thermal conductivity property,TYS of 343.97 MPa,CYS of 341.74 MPa,elongation of 15.71%,CTE of 7.3×10^(−6)K^(−1),and thermal conductivity of 129 W·m^(−1)·K^(−1) at room temperature.It is demonstrated that the ND content has an obvious influence on the microstructure,mechanical properties,and thermal conductivity of ND/ZK60 composites.

Preparation and characterization of nano-crystalline diamond films on glass substrate

Adherent nano diamond films were successfully deposited on glass substrate bymicrowave plasma assisted CVD method in H_2-CH_4 and Ar-CH_4 environment. Raman, AFM (Atomic ForceMicroscope), TEM (Transmission Electron Microscope), FTIR, and Nano Indentation techniques were usedfor characterization of the obtained nano diamond films. It was found that the average grain sizewas less than 100 nm with a surface roughness value as low as 2 nm. The nano diamond films werefound to have excellent transparency in visible and IR spectrum range, and were as hard as naturaldiamond. Experimental results were presented. Mechanisms for nano diamond film deposition werediscussed.

High temperature tribological behaviors of nano-diamond as oil additive

The tribological behaviors of the nano-diamond particles including the nano- diamond and the nano-diamond modified were studied at high temperature using SRV multifunctional test system. The worn steel surfaces were analyzed by means of X-ray photoelectron spectroscopy (XPS). The results show that nano-diamond particles can obviously improve the antiwear and friction reducing properties of the base oil at high temperature and the high load. The friction coefficient of the nano-diamond is very low at 200 ℃ when the test load is not more than 20 N. This tribological behaviors should attributed to the similarly to “ball bearing” lubrication action of the nano-diamond particles, so the movement between tribological pairs become sliding/rolling. The nano-diamond modified by dimer ester possesses excellent antiwear and friction reducing performance at 500 ℃ and load 500 N. The tribochemical reaction film between the nano-diamond particles and the renascent wear surface plays dominating lubrication role and the presence of the dimer ester on the rubbing surface can be propitious to form lubrication film containing nano- diamond on the worn surface at high temperature and high load.

Effect of Gas Sources on the Deposition of Nano-Crystalline Diamond Films Prepared by Microwave Plasma Enhanced Chemical Vapor Deposition

Nano-crystalline diamond （NCD） films were deposited on silicon substrates by a microwave plasma enhanced chemical vapor deposition （MPCVD） reactor in C2H5OH/H2 and CH4/H2/O2 systems, respectively, with a constant ratio of carbon/hydrogen/oxygen. By means of atomic force microscopy （AFM） and X-ray diffraction （XRD）, it was shown that the NCD films deposited in the C2H5OH/H2 system possesses more uniform surface than that deposited in the CH4/H2/O2 system. Results from micro-Raman spectroscopy revealed that the quality of the NCD films was different even though the plasmas in the two systems contain exactly the same proportion of elements. In order to explain this phenomenon, the bond energy of forming OH groups, energy distraction in plasma and the deposition process of NCD films were studied. The experimental results and discussion indicate that for a same ratio of carbon/hydrogen/oxygen, the C2H5OH/H2 plasma was beneficial to deposit high quality NCD films with smaller average grain size and lower surface roughness.

Micro/nano Indentation and Single Grit Diamond Grinding Mechanism on Ultra Pure Fused Silica

The existing research about ductile grinding of fused silica glass was mainly focused on how to carry out ductile regime material removal for generating very ＂smoothed＂ surface and investigate the machining-induced damage in the grinding in order to reduce or eliminate the subsurface damage.The brittle/ductile transition behavior of optical glass materials and the wear of diamond wheel are the most important factors for ductile grinding of optical glass.In this paper,the critical brittle/ductile depth,the influence factors on brittle/ductile transition behavior,the wear of diamond grits in diamond grinding of ultra pure fused silica（UPFS） are investigated by means of micro/nano indentation technique,as well as single grit diamond grinding on an ultra-stiff machine tool,Tetraform ＂C＂.The single grit grinding processes are in-process monitored using acoustic emission（AE） and force dynamometer simultaneously.The wear of diamond grits,morphology and subsurface integrity of the machined groves are examined with atomic force microscope（AFM） and scanning electron microscope（SEM）.The critical brittle/ductile depth of more than 0.5 μm is achieved.When compared to the using roof-like grits,by using pyramidal diamonds leads to higher critical depths of scratch with identical grinding parameters.However,the influence of grit shapes on the critical depth is not significant as supposed.The grinding force increased linearly with depth of cut in the ductile removal regime,but in brittle removal regime,there are large fluctuations instead of forces increase.The SEM photographs of the cross-section profile show that the median cracks dominate the crack patterns beneath the single grooves.Furthermore,The SEM photographs show multi worn patterns of diamond grits,indicating an inhomogeneous wear mechanism of diamond grits in grinding of fused silica with diamond grinding wheels.The proposed research provides the basal technical theory for improving the ultra-precision grinding of UPFS.

Deformation Analysis of Micro/Nano Indentation and Diamond Grinding on Optical Glasses

The previous research of precision grinding optical glasses with electrolytic in process dressing （ELID） technology mainly concentrated on the action of ELID and machining parameters when grinding, which aim at generating very ＂smoothed＂ surfaces and reducing the subsurface damage. However, when grinding spectrosil 2000 and BK7 glass assisted with ELID technology, a deeply comparative study on material removal mechanism and the wheel wear behaviors have not been given yet. In this paper, the micro/nano indentation technique is initially applied for investigating the mechanical properties of optical glasses, whose results are then refereed to evaluate the machinability. In single grit diamond scratching on glasses, the scratching traces display four kinds of scratch characteristics according to different material removal modes. In normal grinding experiments, the result shows BK7 glass has a better machinability than that of spectrosil 2000, corresponding to what the micro/nano indentation vent revealed. Under the same grinding depth parameters, the smaller amplitude of acoustic emission （AE） raw signals, grinding force and grinding force ratio correspond to a better surface quality. While for these two kinds of glasses, with the increasing of grinding depth, the variation trends of the surface roughness, the force ratio, and the AE raw signals are contrary, which should be attributed to different material removal modes. Moreover, the SEM micrographs of used wheels surface indicate that diamond grains on the wheel surface after grinding BK7 glass are worn more severely than that of spectrosil 2000. The proposed research analyzes what happened in the grinding process with different material removal patterns, which can provide a basis for producing high-quality optical glasses and comprehensively evaluate the surface and subsurface integrity of optical glasses.

Preparation of Nano-Crystalline Diamond Films on Poly-Crystalline Diamond Thick Films by Microwave Plasma Enhanced Chemical Vapor Deposition

Nano-crystalline diamond （NCD） films were prepared on poly-crystalline diamond （PCD） thick flims by the microwave plasma enhanced chemical vapor deposition （MPCVD） method. Free standing PCD thick film （50 mm in diameter） with a thickness of 413 μm was deposited in CHn/H2 plasma. It was then abraded for 2 hours and finally cut into pieces in a size of 10×10 mm^2 by pulse laser. NCD fihns were deposited on the thick film substrates by introducing a micro-crystalline diamond （MCD） interlayer. Results showed that a higher carbon concentration （5%） and a lower substrate temperature （650℃） were feasible to obtain a highly smooth interlayer, and the appropriate addition of oxygen （2%） into the gas mixture was conducive to obtaining a smooth nano-crystalline diamond film with a tiny grain size.

Preparation Nano-Diamond Film by Sol-Gelled Coating Method for Field Emission Display

The mixture of Nano-graphite and organic vehicles doped to Nano-diamond paste. The suitable paste proportion was found. Nano-diamond film (NDF) was prepared by sol-gel coating method on ITO glass at 3000/min. The field emission characteristics of luminance-current, luminance-voltage and luminance-power of Nano-diamond film were analyzed and tested. Comparing these tested curves, the luminance was well proportional to current was got. Theoretic, the inner resistance of NDF field emission display (FED) consumes electric energy and real voltage change between the cathode and the anode of NDF-FED was very small after electrons emit. So the characteristic of NDF-FED was preferable to describe by luminance-current linear relationship, which was advantageous to device tested and designed.

Ellipsometric analysis and optical absorption characterization of nano-crystalline diamond film

A nano-crystalline diamond (NCD) film with a smooth surface was successfully deposited on silicon by a hot filament chemical vapor deposition (HFCVD) method. Scanning electron microscopy (SEM), atomic force microscopy (AFM), RAMAN scattering spectra, as well as spectroscopic ellipsometry were employed to characterize the as-grown film. By fitting the spectroscopic ellipsometric data in the energy range of 0.75?1.50 eV with a three-layer model, Si|diamond+non-diamond|diamond+ non-diamond+void|air, the optical constants are obtained. The refractive index of the NCD film varies little from 2.361 to 2.366 and the extinction coefficient is of the order of 10?2. According to the optical transmittance and absorption coefficient in the wavelength range from 200 to 1 100 nm, the optical gap of the film is estimated to be 4.3 eV by a direct optical transition mechanics.

Application of printed nanocrystalline diamond film for electron emission cathode

The low-cost and large area screen-printed nano-diamond film (NDF) for electronic emission was fabricated. The edges and corners of nanocrystalline diamond are natural field-emitters. The nano-diamond paste for screen-printing was fabricated of mixing nano-graphite and other inorganic or organic vehicles. Through enough disperse in isopropyl alcohol by ultrasonic nano-diamond paste was screen-printed on the substrates to form NDF. SEM images showed that the surface morphology of NDF was improved, and the nano-diamond emitters were exposed from NDF through the special thermal-sintering technique and post-treatment process. The field emission characteristics of NDF were measured under -6 all conditions with 10 Pa pressure. The results indicated that the field emission stability and emission uniformity of NDF were improved through hydrogen plasma post-treatment process. The turn-on field decreased from 1.60 V/ μm to 1.25 V/ μm . The screen-printed NDF can be applied to the displays electronic emission cathode for low-cost outdoor in large area.

Application of rare-earth and nano elements on diamond cup wheels

Diamond cup wheel is used widely as an important tool for machining ceramic tile.In this paper,nano rare-earth oxide and nano carbide were added in the segments of seven kinds of diamond cup wheels.The performance of diamond cup wheels were tested on a special designed test machine by grinding two kinds of ceramic tiles.The surface morphology of the segments was examined by Scanning Election Microscopy(SEM) and the micro-hardness of segments was measured.The results showed that nano rare-earth oxide and nano carbide can fine segment micro structure,make grain boundary clear and increase grasping of diamond grits.They can increase also the wear resistance of diamond cup wheels as well as the grinding ratio.

金刚石/纳米氧化铝陶瓷复合材料高温高压合成物相结构分析

以正硅酸乙酯(TEOS)为反应前驱体,采用溶胶-凝胶法在金刚石微粉(粒度0.1~4μm)表面包覆一层非晶纳米氧化硅膜层,同时在覆膜层中加入纳米Si粉和纳米Al_(2)O_(3)粉,制备出金刚石/纳米SiO_(2)/纳米Al_(2)O_(3)复合包覆体。采用高温高压(HTHP)技术,将复合包覆材料置于六面顶压机中,以压力5 GPa、温度1100℃~1700℃、保温20 min的条件制备了金刚石-氧化铝陶瓷烧结体。在高温高压合成过程中,纳米SiO_(2)从非晶态转变为晶态,原料纳米Al_(2)O_(3)中的γ-相、θ-相转变为稳定的α-相,同时,SiO_(2)和Al_(2)O_(3)之间形成了Al_(2)SiO_(5)(莫来石)相,由此,通过高温高压下反应原料的结构转变与复合,可以获得致密度良好的金刚石-氧化铝复合材料。

Si_3N_4/Ni nanocomposite formed by electroplating: Effect of average size of nanoparticulates

Properties of Si3N4/Ni electroplated nanocomposite such as corrosion current density after long time immersion,roughness of obtained layer and distribution of nanometric particulates were studied.Other effective factors for fabrication of nanocomposite coatings were fixed for better studying the effect of the average size of nanoparticulates.The effects of the different average size of nanometric particulates(ASNP)from submicron scale(less than 1μm)to nanometric scale(less than 10 nm)were studied.The nanostructures of surfaces were examined by scanning electron microscopy(SEM),transmission electron microscopy(TEM)and atomic force microscopy(AFM).Corrosion rates of the coatings were determined using the Tafel polarization test.It is seen that decreasing the ASNP will lead to lower corrosion current densities;however,in some cases,pitting phenomena are observed.The roughness illustrates a minimum level while the distribution of nanometric particulates is more uniform by decreasing the ASNP.The effects of pulsed current on electrodeposition(frequency,duty cycle)and concentration of nanoparticulates in electrodeposition bath on trend of obtained curves have been discussed.Response surface methodology was applied for optimizing the effective operating conditions of coatings.The levels studied were frequency range between 1 000 and 9 000 Hz,duty cycle between 10%and 90%and concentration of nanoparticulates of 10-90 g/L.

Characterization of diamond MWCNTs composite fiber synthesized under high pressure and high temperature

A regrown composite fiber was synthesized during the sintering of diamond under high pressure 5.8 GPa and high temperature 1500℃for 1 min,using 3wt%MWCNTs as additive.SEM observation of the fiber after alkali and acid treatment revealed that the outer layer of the fiber is composed of nano-polycrystalline diamond.EDS,XPS,XRD and Raman spectrum analysis further identified that the fiber is composed of MWCNTs in the inner part and nano-polycrystalline diamond in the out layer.It is proposed that the untransformed MWCNTs may act as a template for the regrown outer layer of nano diamond fiber under high pressure and high temperature.

MICRO/NANO-MACHINING ON SILICON SURFACE WITH A MODIFIED ATOMIC FORCE MICROSCOPE

To understand the deformation and removal mechanism of material on nano-scale at ultralow loads,a systemic study on AFM micro/nano-machining on single crystal ailicon is conducted. The results indicate that AFM nano- machining has a precisely dimensional controllability and a good surface quality on nanometer scale.A SEM is adopted to observe nano-machined region and chips,the results indicate that the material removal mechanisms change with the applied normal load. An XPS is used to analyze the changes of chemical composition inside and outside the nano-machined region respectively.The nano-indentation which is conducted with the same AFM diamond tip on the machined region shows a big discrepancy compared with that on the macro-scale. The calculated results show higher nano-hardness and elastic modulus than normal values .This phenomenon on be regarded as the indentation size effect(ISE).

Characterization of the Diamond-like Carbon Based Functionally Gradient Film

Diamond-like carbon coatings have been used as solid lubricating coatings in vacuum technology for their good physical and chemical properties. In this paper, the hybrid technique of unbalanced magnetron sputtering and plasma immersion ion implantation (Plll) was adopted to fabricate diamond-like carbon-based functionally gradient film, N/TiN/Ti(N,C)/DLC, on the 304 stainless steel substrate. The film was characterized by using Raman spectroscopy and glancing X-ray diffraction (GXRD), and the topography and surface roughness of the film was observed using AFM. The mechanical properties of the film were evaluated by nano-indentation. The results showed that the surface roughness of the film was approximately 0.732 nm. The hardness and elastic modulus, fracture toughness and interfacial fracture toughness of N/TiN/Ti(N,C)/DLC functionally gradient film were about 19.84 GPa, 190.03 GPa, 3.75 MRa.m1/2 and 5.68 MPa.m1/2, respectively. Compared with that of DLC monolayer and C/TiC/DLC multilayer, this DLC gradient film has better qualities as a solid lubricating coating.

纳米金刚石浆体3D打印机单螺杆挤出装置的优化及分析

针对纳米金刚石薄膜在光学、电学和医学等方面的广泛应用,设计了一款新型单螺杆挤出型3D打印机,用于制备纳米金刚石薄膜。为了保证纳米金刚石浆体流速和提升打印质量,首先利用Polyflow软件仿真3种不同的单螺杆挤出装置。对比分析了挤出过程中的压力场、剪切速率场以及速度场。结果表明在相同转速下,恒定螺距的最大建压能力为3.571×10^(7)Pa,局部剪切速率最高为10 m/s,且轴向速度较为稳定,说明恒定螺距单螺杆能够提升浆体在输送过程的有效停留时间及混合度;然后使用最小二乘法对恒定螺距的螺杆转速与螺杆挤出口平均流速进行数据拟合,得到转速与挤出口平均流速的数学方程为y=0.00185x+0.000131,表明恒定螺距螺杆挤出装置的转速能够规律性地调节挤出口平均流速;最后通过恒定螺距螺杆挤出装置进行打印验证。实验结果表明,该挤出装置在满足打印效率以及精度的前提下,成功制备了纳米金刚石薄膜。

Microstructure and properties of the sintered diamond reinforced by diamond-MWCNTs composite fibers

A new type of sintered diamond reinforced by diamond MWCNTs composite fibers which were randomly orientated and even distributed in the diamond matrix was synthesized by using 3wt%mullti-walled carbon nanotubes（MWCNTs） as starting additive under high pressure of 5.8 GPa at temperature of 1500℃for 1 min.A special polycrystalline diamond structure of direct bonding of both diamond to diamond and diamond to diamond-MWCNTs composite fiber was observed.The testing results show that it possesses not only high hardness（49～52 GPa） and Young’s modulus（878 GPa） but also high bending strength（1320～1540 GPa） and fracture toughness(9.0～9.2 MPa·m1/2) as it was theoretically predicted.The high performances of the composite were contributed by the fiber strengthening effect and the special structure which can offer more extensive diamond to diamond bonding.

Novel Pretreatment of Hard Metal Substrate for Better Performance of Diamond Coated Cutting Tools

A surface engineering approach for a novel pre-treatment of hard metal tool substrate for optimum adhesion of diamond coatings is presented. Firsfly, an alkaline solution was used to etch the WC grains to generate a rough surface for better mechanical interlocking. Subsequently, surface Co was removed by etching in acid solution. Then the hard metal substrate was boronized to form a compound interlayer which acted as an efficient diffusion barrier to prevent the outward diffusion of Co. Novel nano-microcrystalline composite diamond film coatings with a very smooth surface was deposited on the surface engineering pre-treated hard metal surface. Promising results of measurement in adhesion strength as well as field cutting tests have been obtained.