CVD DIAMOND AND RELATED MATERIALS AT INSTITUTE FOR SPACE RESEARCH AND INDUSTRY: RESEARCH, DEVELOPMENT AND INNOVATION.

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1 CVD DIAMOND AND RELATED MATERIALS AT INSTITUTE FOR SPACE RESEARCH AND INDUSTRY: RESEARCH, DEVELOPMENT AND INNOVATION. VLADIMIR JESUS TRAVA-AIROLDI Instituto Nacional de Pesquisas Espaciais-INPE São José dos Campos - S.P., Brazil Outline of Talk The conception of our Project Few Comments State of the Art of CVD-Diamond Application in Brazil Research, Development, and Industrialization Technology Transfer: examples of Industrialization Perspective of these Carbon Materials Final Comments LAWPP 2011_AITP2011, Mar Del Plata - Argentina, Nov

2 Space Application From the development of diamond and DLC for space application in our Institute comes a great novelty for space and spinspin-off Industries Employee, 400 Researcher Spin off Application

3 Multi disciplinar Project created in 1992 at INPE DIMARE RESEARCH DEVELOPMENT INDUSTRIALIZATION ADHERENCE AND STRESS IN SITU DIAGNOSTIC SURFACE PREPARATION COLUMNAR STRUCTURE TRIBOLOGY AND SOLID LUBRICANT MECHANISM STUDIES DRILLING TOOLS CUTTING TOOLS ODONTOLOGICAL AND MEDICAL BURR BIOLOGIC IMPLANT INJECTION TUBES MECHANICAL DEVICES CHOOSING FOR APPLICATIONS LOOKING FOR INDUSTRIAL INTEREST FINAL PRODUCT CHARACTERIZATION INDUSTRIAL ESCALING UP INDUSTRIAL PRODUCTION MARKETING AND SELLING 1 Industry was created and three others are in progress 12 Patents >200 papers DIAMOND AND DLC DOPING HIGH GROWTH RATES TECHNIQUES NEW TECHNIQUES NANO TUBES NANO STRUTURES MIXING MATERIALS CHEMICAL ELECTRODES AND FUEL CEL SPACE AND INDUSTRIAL DEVICES OF SOLID LUBRICANT

4 # of Publishe ed papers (a.u.) State of the Art Metals Carbon CVD Diamond, DLC, Fullerenes, Nanotubes

5 State of the Art in Brazil CVD diamond, DLC and nano tubes potential applications in some areas according to deposited patents Drilling 17% Cuttilng Tools 17% Other 17% Electrochemical 15% Abrading 34%% CVD diamond, DLC and nano tubes interest according to published papers Drilling and Cutting 8% Optical 12% Tribology 5% Abradding 12% Eletrodes 10% Other 9% Basic 36% Elect Devices 8%

6 Carbon The Biggest C is present in more than 10 million substances (it is in all medicines and all poison) It has 4 allotropic forms besides amorphous forms: Graphite, Diamond, Fullerenes and Nanotubes and more recently, (2004) a new allotropic form was announced the a kind of nano foam. Carbon has confirmed application areas ten times more than all metals and their alloys together. Carbon, alone, form the most fragile material, the graphite (the most largely applied), and also the hardest material, the diamond (the most desired).

7 CVD Diamond

8 2.45 GHz Microwave Plasma Reactor Diamond Wafer

9 In situ Diagnostic Laser System Nd:YAG/die, Microwave Reactor and Mass Spectrometry

10 Laser based gas phase diagnostics Previous work: CH 3 REMPI in HFCVD %CF

11 Study of halogen based diamond growth CF 4 addition to H 2 CH 4 mixtures -Better film quality -Growth on a larger area around the filament -Higher nucleation density -Growth at lower temperatures

12 CVD Diamond Micro-drills: Cooperation with NASA for Mart Surface exploration CVD Diamond Tubes (up to 100mm long and 3 mm diameter) for High pressure water cutting machine

13 Boron doped diamond Electrodes Large effective area electrodes Water treatment Fuel cell electrodes

14 CVD Diamond Ultra-sound Tips for Dentistry: CVDentus (small devices) Conventional Diamond Burr with galvanic welding CVD Diamond burr as a rough surface unique stone

15 Dentistry Burrs for Ultrasound System Conventional CVD Diamond After Using 10 min 800 µ 800 µ After Using 200 min

16 CVD Diamond Ultra-sound Tips for Dentistry: CVDentus (small devices) World Patent Ultrasound System The First Spin off

17 Examples of cavity preparation

18 CVD Diamond Drills for wells perforations (very big devices) Unused Unused 4 inches diameter annular drills Used 4 inches annular drills 2.5 more durable 30% faster and more stable than conventional one 8.5 inches diameter drill for deep water pre-salt wells Tested by Petrobras in deep water pre-salt wells, TUPI Petroleum Field (Brazil) The second Spin off Used

19 1 Kg of CVD Diamond rods ( 2 mm diameter and 10, 15 and 20 mm long)

20 New concept of Perforation Drills Abradding Face Face de ataque Conventional Abradding Face Diamond grain are lost during the perforation action. In these cases there are not the diamond wear Abradding Face New concept by using CVD Diamond rods: Pending Patent The wear of the CVD diamond is enforced during the perforation

21 New concept with diamond dowels Diamond powder impregnated in metal matrix Tool face Diamond dowel surface always flat and sharpened Metal matrix with diamond powder Metal matrix with diamond powder Action of diamond powder: CVD Diamond dowel surface sharpened Durability and efficiency of the bit.

22 New concept with diamond dowels CVD Diamond formed in radial, columnar structure Section cut Columnar polycrystalline growth structure Single stone that allows sharpening Flat surface can be self-sharpened during drilling

23 Attack surface roughness of pure diamond (1-3 mm diameter and 3-20 mm long rods) Attack surface features of pure diamond (columnar structure detail of 1.8 mm diameter rod)

24 CVD Diamonds O&G Bits Before By Using PCD Devices

25 CVD Diamonds O&G Bits After By Using PCD Devices

26 CVD Diamonds O&G Bits Before 100% CVD Dowels

27 CVD Diamonds O&G Bits After 100% CVD Dowels

28 DLC Sputtering System Ion Beam Assisted Deposition - IBAD RF Discharge, and Enhanced Pulsed DC Discharge Low cost Easy operation Better DLC films (HH, HA, LW, LF, HGR,15%<[H]<45%, etc.) Frequency from 10 to 50 KHz Duty cycle 5-90% DLC films hardness from 10 to 40 GPa Get better adherence Pulse Amplitude from -50 to -1500V Positive pulse from +10 to +80 V

29 Diamond-like Carbon (DLC) RF plasma and Pulsed DC 20 liters Chamber

30 Diamond-like Carbon (DLC) IBAD Ion Beam Assisted Deposition and Pulsed DC Chamber1000 liters Chamber Vacuum Chamber Ion Beam Inside

31 100 liters DLC chamber Modified cathode for scaling

32 MODEL - Substrate Surface Modification and DLC Film Same Material Two or more Carbon interface Hardness Thermal Expansion DLC Film > 30 GPa 1-3 x10-6 Modified Surface * ~ 8 GPa 5-8 x10-6 Substrate Stainless Steel ~ 2 GPa 10 x10-6 * By gas diffusion, subplantation processes, etc.

33 Thick DLC film Cross section analysis Stainless Steel Substrate ,723 µm Arb b. un carbon Fe Nitrogen X Cross section SEM micron EDX Linescan, low energy DLC film broke out of the interface line

34 Scratching, Friction Coefficient, Normal Force, and track profile on DLC film with very good adhesion on SS Cross section

35 High Resolution SEM Images Pending Patent Clusters Pure DLC DLC with NCD particles

36 Bactericidal Action

37 Some results of DLC deposition on metallic substrates The third spin off Satellite Solar panel pieces Automotive Oil & Gas Implants Drill for bone perforation Artificial heart parts Others applications studies are in progress in our lab Cutlery

38 Tubes Internal and External DLC Coatings D = 80mm L = 600mm High Adherence:>60N of crítical load High Hardness:>25 Gpa Low friction coeficient: 0,12 D = 120mm L = 450mm D = 140mm L = 280mm

39 Industrial Projects CVD Diamond DLC CVDentus Ultrassonic tips and Ultrassonic Equipment Perforation Drills for Petroleum wells DLC Coatings for medical, automobile, etc.. application DLC coatings for long tubes inside wall Instrumentation for DLC and CVD dia Project 1 Project 2 Project 3 Project 4 Project 5

40 INNOVATION Cycle in Progress Research Institute Small Business (CVD Vale) Central Gov Fapesp CNPq Capes Finep S o c i e t y Venture Capital Criatec/BNDES Reference

41 Thanks, FAPESP, Finep,C NPq and CAPES for Financial Support and all of You For your kindly attention