super hard diamond-like carbon coatings

super hard diamond-like carbon coatings

INTRODUCTION TO MODERNTECHNOLOGIES IN BELARUS –PHYSICAL-TECHNICAL INSTITUTEPart 2Prof. Dr. Anatoli GordienkoDirector10 Kuprevich St.220141 Minsk, BELARUSPhone/ fax: (+375 17) 263 76 93e-mail:

VACUUM INSTALLATION VU1000 «ALMAZ» Is intended for a wide range ofcoatings deposition andequipped with differentplasma and ion sources. Specifications: conductive anddielectric coatings can bedeposited Automatic control system Coating temperature and colormonitoring are available Half-automatic loading system Oil-free pumps Chamber dimensions: 1000×1000 mm2

SUPER HARD DIAMOND-LIKE CARBONCOATINGS (DLC)The carbon plasma is formed by ashort-time electrical arc dischargeowing to thermal erosion of graphitecathode. The plasma is acceleratedby a Hall-type plasma accelerator anddirected towards the substrate. In theplasma source, the discharge ignitionis realized by a discharge betweenspecial electrodes placed aroundcathode. The electrodes have acontact through thin carbon film thatdeposits periodically during previousdischarge. Control thyristor is used to switch discharge of the ignition capacitor of 2 ... 10μF. The pulse arc discharge releases owing to energy of main capacitors battery having acapacity of some thousand of microfarads. The ignition system has a localized electricalcontact of thin film conductor, deposited on the surface of the insulator. The localisedcontact moves from pulse to pulse along ring-shaped ignition electrode around thecathode. Such technique provides a high discharge ignition probability and practicallyavoid the erosion of an insulator, providing a long service life of the ignition system3

SUPER HARD DIAMOND-LIKE CARBON COATINGSPulsed plasma source& power supply/control systemTECHNICAL SPECIFICATIONS:The graphite cathode diameter, mm 33Main discharge voltage, V 200...400Auxiliary discharge voltage , V 200...400Ignition discharge voltage , V 600Discharge impulse repetition rate, Hz 1...10Maximal power, W 1000Maximal deposition rate, μm/min 0.12Range of discharge impulse setting 1 to 99999Weight, kg 15Control of graphite cathode feeding4

SUPER HARD DIAMOND-LIKE CARBON COATINGSEquipmentCarbonplasmasourceArgonplasmasourceTitaniumplasmasourcePlastic moldparts coatedby DLC filmVacuum machine of UVNIIPA -1001 and its vacuum chamber containing arc DLCcoated parts of a plastic mold

SUPER HARD DIAMOND-LIKE CARBON COATINGSVacuum machine VU-700DL for arc DLC films and coatings deposition equippedwith laser ignition system and large graphite rotated cathodeSPECIFICATIONSDiameter of vacuum chamber, mm 700Height of vacuum chamber, mm 700High-vacuum pumping, l/s 3200Low-vacuum pumping, l/s 80Time to achieve pressure 10 -3 Pa, min 25Speed of deposition DLC usingdouble planetary rotation, nm/min 4Area occupied by machine, m 2 15Height of machine, cm 240Dimensions of graphite cathode, mm Ø140x330Gydraulic system SMC, JapanPneumosystemSMC, JapanControl system PLC, Omron

SUPER HARD DIAMOND-LIKE CARBON COATINGSVacuum Machine VU-700-001 for arc DLC films and coatings deposition equippedwith two pulsed arc carbon plasma sources and magnetic separatorsSPECIFICATIONSVacuum chamber dimensions, mm 500x600x650Vacuum pump set: turbopump (1500 l/s), rotaryvane (16 l/s)Gas flow control system: 5 channels (Ar, N 2, O 2,CH 4,C 2H 6)Rotary drive: planetary rotation with variable andmonitoring rotary speed is up to 10 rpm.Coating area, cm 2 400Discharge impulse repetition, Hz 1…20Max deposition rate, μm/h 0.3Process control: Fully automated process controlby PLC (with color touch panel) having computerinterface. Up to 20 coating programs for differentapplications can be stored.Power connection: 400 V ±10%, zero, four wires,protective earth , 50 Hz, approx. 45 kW

SUPER HARD DIAMOND-LIKE CARBON COATINGSVacuum machine VDU-CI for pulsed arc DLC films and coatings depositionequipped with four arc carbon plasma sources and magnetic separatorsSPECIFICATIONSPower consumption, kW 60Vacuum chamber, mm 900×900Number of carbonplasma sources 4Number of gasion sources 2Graphite cathodediameter, mm 29Number of metalplasma sources 3Metal cathodediameter, mm 80Pulse repetition, Hz 10

SUPER HARD DIAMOND-LIKE CARBON COATINGSDLC film characterizationAFM image of the DLC filmon silicone waferRa = 0.19 nm, Rq = 0.34 nm,Rv-p = 15.96 nmRaman shiftD-peak position: 1379.1 cm-1G-peak position: 1574.1 cm-1I D /I G = 0.15DLC film specificationsHardness ( GPa)1009080706050403020100Analyst Project.xlsHardness vs Displacement Into SurfaceDLC_1.xls HardnessDLC_1.xls Modulus0 50 100 150 200Displacement Into Surface (nm)Hardness & Young’s modulus vs nanoindentationdepth for the 1200 nm DLC film on the WC substrateHV = 8500 (85 GPa), E = 950 GPa1400120010008006004002000Modulus (G Pa)Density, g/cm 3 2.8…3.0 Thickness, nm 50…2500Hardness, GPa 60…85 Roughness Ra, nm 0.2…0.5Young`s modulus, GPa 650…950 Friction coefficient 0.05…0.1Thermal stability, °C 300…350


SUPER HARD DIAMOND-LIKE CARBON COATINGSAdvantages of method High ionization rate of plasma plum up to 98% ⇒ high nucleation density ⇒ continuousfilms at small thickness ⇒ smooth film surface is provided. Quasi-neutrality of plasma flow on a substrate ⇒ 1) dielectric substrates may be used,2) no harmful micro discharges. High energies of carbon ion up to 60...70 ev ⇒ 1) high content of sp 3 carbon bonds up to85% ⇒ high density up 2.9…3.1 g/cm 3 ⇒ excellent barrier against metal ion diffusion,2) high hydrophoby ⇒ good biocompatibility, 3) good adhesion, 4) no bias voltage is needed ⇒uniform coating on a substrate of a complex geometry. A number of simultaneously existing cathode spots and their high velocity ⇒ lowcontamination of plasma plum by the graphite macroparticles ⇒ high film surface quality ⇒application of DLC films for precession technique and medicine using simple plasma filter set. Possibility to use high discharge current to guide plasma through magnetic filtereffective ⇒ no need for any additional high power current sources. Precession film thickness control by discharge impulse number set.

SUPER HARD DIAMOND-LIKE CARBON COATINGSDLC COATING PROPERTIES• Thickness, nm 10-1000• Density, g/cm 3 2.8-3.1• Young’s Modulus, GPa 650-700• Hardness, GPa 60-70• Friction coefficient 0.1-0.15• Wearing, μm 3 /N·m (1-3)·103• Thermo-stability, o C up to 400• Thrombocyte test Index > 4.5• Endotelization period, days 30ARTIFICIAL HEART VALVESCUTTING TOOLSMEASURINGINSTRUMENTMACHINE PARTS (a ballconnection, plungers)12

APPLICATION OF THE DLC COATINGS IN MEDICINEThe DLC coatings reduce the extent of valve-related thrombogenesis by surfacemodification making the surfaces more adherent to endothelial cells and albuminand less adherent to platelets, thus improving. About two thousand articles havebeen manufactured and used in medicine by nowBodies of the artificial heard valves made ofVT-16 Ti-alloy coated by the DLC thin filmsThe artificial heart valves assembled13

APPLICATION OF THE DLC COATINGS IN MEDICINEABView of DLC coated implants: fixing damaged backbone section set (A), and rotor of the blood pump (B)14

SUPER HARD DIAMOND-LIKE CARBON COATINGSWatch partsX20DLCArc DLC films deposed on very little watch pinion axis to decrease friction and to extendtheir survivability by several times as well as decorative coatings on watch bracelets whichchange interference color depending on their thicknesses

INDUSTRIAL APPLICATION OFTHE DLC COATINGS - flexible polymer bandAbrasive for procession polishing of surface is a DLC film on the textured surfaceof flexible polymer band. Patents of Belarus - N 809 (1995), USA - 5643343(1997), 5711773 (1998), Canada - 2177170 (1997), Russia - 2136485(1999),Europe - PST 0730513 (1999), Germany - 69416855.6 (1999), Italy -23128/BE/99 (1999), China - 1090552С (2002), Ukraine - 48123 (2002)The sample of DLC flexible abrasiveFields of using:• precision polishing of superhard materials;• silicon wafer polishing;• treatment of magnetic disks and heads;• finish treatment of optic lens and optic disksPolishing machine equipped withDLC flexible abrasive16(3M Corporation, USA)

INDUSTRIAL APPLICATION OFTHE DLC COATINGS - Diesel engines, ball pivotsAn appreciable life time increase have been achieved for plungers ofDiesel engines and ball pivots coated with DLC filmsPlungers forDieselenginescoated withDLC coatingBall pivots for MAZtrucks coated withDLC and TiN films asthe best combinationfor friction pairs17

INDUSTRIAL APPLICATION OFTHE DLC COATINGS - toolsSuper hard diamond-like carbon coatings on cutting tools increase their life time1.5…2 times as much. These coatings are especially effective in a case of woodcutting tool due to corrosion resistance and anti-sticking resin effect of the DLCcoatings. The good results of DLC coating application have been obtained forcutters assigned for nonferrous metal and reinforced plastics treatmentCuttersDrillsTaps18

SUPER HARD DIAMOND-LIKE CARBON COATINGSPunches for chain productionThe punches for chain fabrication coated with DLC filmsobtained using a new combined PVD/CVD arc technologyrevealed increasing of the life time by a factor of 2.5 - 3

SUPER HARD DIAMOND-LIKE CARBON COATINGSMeasuring toolsWear resistant carbon DLC deposited on a worksurface of measuring tools such as plain gagesplugs,thread gages, Johansson blocks, etc.repeatedly magnify their resistance to a wear,longevity and calibration interval periods.Measuring tools with DLC coatings have thefollowing technical characteristics: increase of in term service > 3 times increase of recalibration interval 5…10 times friction coefficient with steel < 0.15

SUPER HARD DIAMOND-LIKE CARBON COATINGSPlastic molds & diesBArc DLC is a chemically inert material in respect of all plastics we know. Thearc DLC coating prevents wear, corrosion and sticking of any plastic on workmolds and dies surfaces. They improve plastic articles surface smoothness.The positive combined effect achieved if the coatings are applied for frictionpart of mold due to a low dry friction coefficient of arc DLC coatings. It wasshown in short-run environment that arc DLC coatings extend survivability ofmolds by 3…5 times

SUPER HARD DIAMOND-LIKE CARBON COATINGSFine abrasive materialAbrasive material is a flexible polymer band havingspecial surface texture with deposited arc DLCFields of of Application• precise polishing of super hard materials• polishing of silicon plates for microelectronics• treatment of magnet disks and magnet heads• finish treatment of optical disks and lensesThe arc DLC abrasive material has been patented allover the world

Technology descriptionELECTROLYTE-PLASMA POLISHINGOF METAL ARTICLESTechnology of Electrolyte-Plasma Polishing isbased on physical-chemical processes takingplace in electrolyte region closed to surface ofelectrodes immersed into solutions of mineralsalts in the conditions of high electrical potentialleading to micro arc plasma etching just of atreatment surfaceThis technology excepts mechanical influenceson articles and charging abrasive particles intoa surfaceIt can be used to treatment of metal articles manufactured from copperand its alloys (brass, bronze, German silver), low-carbon and stainlesssteels and other electroconductive materials

ELECTROLYTE-PLASMA POLISHINGOF METAL ARTICLESProcessThe process realizes in electrolyte which constitutes a solution ofammonium salts (chloride, sulfate and nitrate) and a little domestic of theorganic dissolvine Z. (C 10H 16N 2O 8) Concentration of salts varies in a range1% to 10 % to provide electrolyte density of 1.02 g/cm 3 . Before carrying outof polishing the electrolyte is heated up to temperatures of 60...90 0 CThe positive potential of 150...200 V is applied to any article treatment. Thepotential is higher for articles made of steel comparing with those of copperalloys. Processing time is 30 s for deflashing, 5..8 and 10...15 mins forcopper- and steel polish, respectivelyAs a result of the polishing process, there is a deflashing and blunting ofsharp edges as well as pretreatment of article surface to be coated bygalvanic or vacuum films. The surface roughness decreases up to Ra =0.2...0.05 µm

ELECTROLYTE-PLASMA POLISHINGOF METAL ARTICLESEquipmentEIP-10 machine was designed andmanufactured to realize the technology.Specifications:Maximal consume power, kW 10Maximal polishing surface, cm 2 250Specific electrical energyconsumption, kW·h/m 2 30Anode current density, A/cm 2 0.2...0.6Efficiency, % 85Time of continuous work, h 8Sizes: length, cm 1400width, cm 710high, cm 2100Wight, kg 200

ELECTROLYTE-PLASMA POLISHINGOF METAL ARTICLESProductsA B C D ESamples of stainless steel (A), copper (C),before polishing and the same samplesafter polish (B) and (D), respectivelyFWares: (E) knifes for vegetables before(top) and after (down) polishing, (F) brassbracelets polished for watches

CROSS - WEDGE ROLLINGForming of various-shape parts iscarried out within one rolling cycle.Tool is easy in design,manufacturing, adjustment and repair.Tool is replaced in severalminutes.All constructional steels, someinstrumental steels and copper andtitanium alloys can be cross-wedgerolled.Metal loss is decreased by up to 40 %27

MANUFACTURING OF FEW-LEAF SPRINGS16 patents areobtained in Belarus,Russia, the USAand Great Britain.The license is soldand production ismastered at“Eaton” Company(USA)Multi-leaf springFew-leaf spring• The process productivity is increased by a factor of 4 to 5• Power requirement is decreased by 35 to 40 %• Spring life is increased by a factor of 1.5 to 2.0• Spring weight is decreased by 25 to 30 kgThe cost of technological equipment is decreased by a factor of 4 to 528

MAGNETIC PULSE STAMPINGStrength, thermal andelectrophysical effects ofinteraction between magneticfields and material• Multi-functionality• Flexibility• High quality• Minimum power requirementsand material and laborconsumptionDecrease of expenditures on• Power consumption is up to 3 times• Die tooling up to 10 times• Period of preparation for production up to 5 times29

OBTAINING of BULK NANOSTRUCTUREDMATERIALS by ECAPEqual-channel angular pressing (ECAP)was invented in 1972 at the PhysicalTechnical Institute.Multi-pass ECAP processing ofmaterials by plastic deformation toproduce a uniform nanostructuredmaterials down to the nanometer range.Any type of microstructure, fromequiaxed to any degree of grainelongation can be formed. Thecapability to control grain orientationhas great practical significance forcreation of anisotropic or isotropicproducts with various functionaldesignations: structural, magnetic,superconducting, etc.Pure metals such as Al, Mg,Ti, Cu, Ni, Fe, Nb, etc. and for anumber of their alloys30

MECHANICAL PROPERTIES OFNANOSTRUCTURED MATERIALSMaterial Structure HardnessHVUltimatetensilestrength, MPaElon-gationδ, %Redu-ctionof area ψ,%Pure FeNanopolycristal300909803506215570Pure CuNanopolycristal1555548024011196787Pure NiNanopolycristal31070920400822629018-10steelNanopolycristal640200155056027704169InvarN36Nanopolycristal3001208504601630748831

ITEMS FOR BIOMEDICAL USE(PELVIS-FEMUR JOINT ENDOPROTHESIS)Mechanical properties:• Tensile strength is 960 to 1100 MPa• Yield strength is 860 to 880 MPaEndoprothesis of the system SLPS (Self lockingPorous Systems) are manufactured jointly with“Altimed” Company.Standard requirements of ISO 5832/3 are observed.X-ray photograph afterimplantation ofendoprothesisDevelopment of the technology for production ofendoprothesis blanks of 12 sizes from the titanium VT6and Co-Cr-Mo alloys using the method of hot volumeforming. V-shape of shank ensures exclusive fixationand rotary stability in three planes.Economic efficiency is 1500 USDfor one endoprothesis32

Thank you!Physical - Technical InstituteNational Academy of Sciences of Belarus10 Kuprevich St., 220141Minsk, BELARUSE-mail: phti@belhost.by33

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