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NETZSCH LFA 447 Nanoflash, Operating Instructions Manual

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NETZSCH LFA 447 Nanoflash Operating Instructions Manual Download Page 37

System Components

LFA 447

TM

 

01/09     J:\LFA447\CHAPTER3.DOC 

 

11

 

 

•

 

Sample holder for liquids 

 

By using a special sample holder it is possible to analyze liquids with the LFA 447 instrument. 
When using the sample holder please pay attention to the following indications. 
 
 

lid

crucible

liquid sample

ring
of stainless steel

 

Figure 12: sample holder for liquids 

 

 
 
 

Preparing the sample holder  

 

 

The bottom side of the crucible and the indentation on the top side of the lid must be 
coated with graphite spray as shown in Figure 13. 

 
 

lid

(coating)

crucible

(bottom side, 
with coating)

ring of
stainless steel

 

 

Figure 13: coatings on the cover and crucible 

 

If the upper edge of the lid is soiled when applying the graphite spray, it must be 
cleaned with alcohol. 

 

Summary of Contents for LFA 447 Nanoflash

Page 1: ...447TM 01 09 J LFA447 Contents doc Operating Instructions LFA 447TM Nanoflash Contents Chapter I General Information Chapter II Installation Chapter III System Components Chapter IV Operating the Inst...

Page 2: ...01 09 J LFA447 CHAPTER1 DOC Chapter I General Information LFA 447TM...

Page 3: ...ution of these instructions All technical data instrument features and other information described in these operating instructions are presented to the best of our knowledge and in accordance with the...

Page 4: ...articularly important information apart from the rest of the text ATTENTION These instructions must be followed exactly to avoid injury to the user and damage to the instrument This symbol refers to m...

Page 5: ...erated and maintained by authorized trained and individually instructed personnel who have been informed of possible sources of danger Responsibility Responsibility for commissioning operation and mai...

Page 6: ...all protective devices are in place and operate properly Only then should the instrument be started Industry specific Accident Prevention Regulations The operator must observe the relevant regulation...

Page 7: ...equired for safe operation The operating instructions should be placed in a suitable location in the work place and complied with by the employees Gases Observe the relevant regulations and protective...

Page 8: ...at an equilibrium pressure less than 1 5 bars absolute if the vessels are either not lagged or are lagged with a porous cellular type insulator The liquid air produced can result in oxygen enrichment...

Page 9: ...ries considerably The minimum oxygen content of breathing atmosphere should be 18 by volume at normal atmospheric pressure but to ensure a wider margin of operational safety it is recommended that per...

Page 10: ...Shock may also occur if the frostbite is at all extensive Effects of cold on lungs Prolonged breathing of extremely cold atmospheres may damage the lungs Hypothermia Low environmental temperatures can...

Page 11: ...e oxygen analyzer calibrated before use to ensure that the oxygen lies between 20 and 22 by volume The use of a safety work permit system is strongly recommended Note The latter two recommendations ne...

Page 12: ...NOT ATTEMPT TO ENTER AN OXYGEN DEFICIENT ATMOSPHERE WITHOUT USING SUITABLE SELF CONTAINED BREATHING APPARATUS OTHERWISE HE MAY HIMSELF BE OVERCOME Many double fatalities have occurred in industry as a...

Page 13: ...phine or some other potent analgesic is required to control the pain during thawing and should be administered under professional medical supervision e If the frozen part of the body has thawed by the...

Page 14: ...nts Ascertain the identity of the gas before using it Know and understand the properties and hazards associated with each gas before using it Establish and implement plans to cover any emergency situa...

Page 15: ...ectrical heating devices to raise the pressure of a container Containers should not be subjected to temperatures above 45 C Never re compress a gas or a gas mixture from a container without consulting...

Page 16: ...to prevent toppling or rolling Vertical storage is recommended where the container is so designed Container valves should be tightly closed and where appropriate valve outlets should be capped or plug...

Page 17: ...rials Unlike a liquid nitrogen tank a vaccum jacketed dewar flask is essentially a non pressurized container Recommendations for handling and storage are as follows The protective caps on dewar flask...

Page 18: ...01 09 J LFA447 CHAPTER2 DOC Chapter II Installation LFA 447TM...

Page 19: ...allation LFA 447TM 01 09 J LFA447 CHAPTER2 DOC Contents INSTALLATION 1 PACKING AND DELIVERY 1 LOCATION REQUIREMENTS 2 INSTALLATION SCHEMATICS 3 CONNECTING THE COMPUTER SYSTEM 4 CONNECTING THE THERMOST...

Page 20: ...acked in form molded foam to protect against damage during transport We recommend keeping the original cartons Should repairs or an extension of the system become necessary the cartons can be reused t...

Page 21: ...to the extent possible measuring system A stable shock absorbent table with a working surface of approx 2 m x 1 m is required for the measuring part measuring part computer printer thermostat The the...

Page 22: ...computer weight 10 5 Kg 310 depth 420 thermostat 230 V 115 V 10 A printer weight 12 Kg wide range power pack 100 240 V 6 A Option or provided by the customer monitor weight 3 5 Kg 460 640 470 500 tabl...

Page 23: ...onnecting the computer system WATER INLET WATER OUTLET serial port PC LFA 447 rear sensor connection computer connection serial port power supply Figure 2 connecting the computer system For connecting...

Page 24: ...ting the thermostat thermostat rear LFA 447 rear water filter ALARM power supply outlet inlet WATER INLET WATER OUTLET water inlet water outlet Figure 3 connecting the thermostat Adjust the temperatur...

Page 25: ...01 09 J LFA447 CHAPTER3 DOC Chapter III System Components LFA 447TM...

Page 26: ...T PANEL 3 BACK PANEL 4 EXTRACTOR TOOL 5 SAMPLE HOLDER 6 STANDARD SAMPLE HOLDERS 7 ROUND SAMPLES 7 SQUARE SAMPLES 7 SPECIAL SAMPLE HOLDERS 8 SAMPLE HOLDER FOR LAMINATED SAMPLES 8 IN PLANE SAMPLE HOLDER...

Page 27: ...System Components LFA 447TM 01 09 J LFA447 CHAPTER3 DOC 1 Measuring unit height 460 610 560 depth width Figure 1 LFA 447 measuring unit...

Page 28: ...able of operation from room temperature to 300 C The system is equipped with a software controlled automatic sample changer allowing measurement of up to 4 samples at the same time The temperature ris...

Page 29: ...easuring unit label function online green LED lights up instrument is switched on status start the software click on the Nanoflash icon the status light on the front panel lights up in a red yellow gr...

Page 30: ...el function 1 6A 240 V mains fuses 2 power switch power switch instrument on off 3 AC input power connection 230 115 V 4 fan 5 detector amplifier signal connection to the detector 9 6 thermostat outle...

Page 31: ...nd of the extractor tool in the respective part of the sample holder e g furnace lid the two fixing bolts on the lower part of the extractor tool must be clamped into the holes of the furnace lid The...

Page 32: ...der is moved via the software in a horizontally stable and therefore defined position Once the detector has been moved to the center position this is done by clicking on the corresponding button in th...

Page 33: ...sk sample holder plate sample holder plate with mask size 1 edge length 8 0 mm 5 0 mm mask sample holder plate sample holder plate with mask size 2 sample diameter 12 7 mm 9 8 mm mask sample holder pl...

Page 34: ...les The sample must be cut into single sample strips A strips length 12 7 mm placed into the sample holder plate B affixed by the two fixing screws C and covered by the corresponding mask D see Figure...

Page 35: ...rned by 90 on their side F so that the sample can be measured in a horizontal direction The sample strips must be placed into the sample holder plate G affixed by the two fixing screws H and covered b...

Page 36: ...easured temperature increase of the sample shows the thermal diffusivity in a horizontal direction in plane Please note that the application is limited to thin samples with a high conductivity Therefo...

Page 37: ...rucible liquid sample ring of stainless steel Figure 12 sample holder for liquids Preparing the sample holder The bottom side of the crucible and the indentation on the top side of the lid must be coa...

Page 38: ...thickness of the crucible bottom hcrucible and the lid bottom hlid can be measured with a micrometer screw The liquid level hsample is the difference between the total height of the sample holder hto...

Page 39: ...e of the sample holder plate shallow margin 1 6 mm must show to the top Insert the sample holder plate 12 7 mm into the sample tray such that the shallow margin 1 6 mm faces upwards see figure crucibl...

Page 40: ...or the filling level ideal liquid level ok excessive Oil or hydrocarbons are often difficult to be placed inside a crucible They form no pearl but creep along he crucible walls This will cause higher...

Page 41: ...st measurement with water should yield the following result a 0 146 mm 2 s at room temperature Example of a measurement Liquid sample holder 304 V Long 3500ms Signal Ratio empty water 1 7 3 shots calc...

Page 42: ...all measurements with the sample holder for liquids due to the heat spreading in the container which influences the detector signal above 2000 ms In dependence on the thermophysical properties of the...

Page 43: ...t plate lid pan upper support plate Figure 14 sample holder for powdery and pasty samples Sample preparation for non transparent samples pan bottom side graphite spary cover plate schematic pan bottom...

Page 44: ...ottom side Coat the bottom side with graphite spray so that only the edge of the lid bottom side is coated NOTE Only the transparent edge of the lid must be coated with graphite spray in order to prev...

Page 45: ...m the upper edge of the pan powder sample pan lid Place the lid onto the pan upper support plate Place the upper support plate as shown in the figure and fix it by means of the phillips screws Check t...

Page 46: ...pan must always be coated with graphite spray in order to make sure that the energy will be absorbed on the inner side of the pan lid bottom side schematic lid bottom side coat here Turn the lid and c...

Page 47: ...side coated pan inside Wait some minutes until the coating is dried powder sample transparent Insert the coated pan into the lower support plate ATTENTION The powdery sample should exceed slightly fro...

Page 48: ...the thickness The inner distance between pan and lid is approx 1 5 mm If the sample is not compressible a higher sample thickness could result Compare the thickness with and without sample Additional...

Page 49: ...rmostatic control of instrument components relevant to the measurement and cooling of the furnace system The thermostat is connected to the thermostat inlet outlet connections on the back panel of the...

Page 50: ...01 09 J LFA447 CHAPTER4 doc Chapter IV Operating the Instrument LFA 447TM...

Page 51: ...NIT 4 SAMPLE PREPARATION 5 SAMPLE THICKNESS 5 SAMPLE COATING 6 TRANSPARENT MATERIAL 6 GRAPHITE COATING 6 SAMPLE MASS 7 SAMPLE DENSITY 7 CALIBRATION MATERIALS 8 INSERT A SAMPLE 9 STARING A MEASUREMENT...

Page 52: ...ed hardware and simple menu driven software to provide fast accurate and safe measurements The Nanoflash works to the flash method according international standards ASTM E 1461 DIM EN 821 and DIN 3090...

Page 53: ...here a temperature diffusivity in cm 2 s l thickness of the test piece in cm t50 time at 50 of the temperature increase measured a t the rear of the test piece in s The above described method replaces...

Page 54: ...01 09 J LFA447 CHAPTER4 doc 3 Preparing the IR detector sensor cover Remove the detector cover from the top of the detector casing plug Remove the plug from the top of the detector casing funnel Inser...

Page 55: ...r should be completely filled The detector cooling stabilizes after 5 minutes Open and close the measuring unit Press the interlock button and move the hood to the rear end position in order to open t...

Page 56: ...e test The optimum sample thickness depends on the diffusivity of the material The selected measurement period should correspond to 10 12 half times and be between 10 and 200000 ms The thermal diffusi...

Page 57: ...phite it is also necessary if a thin sputtered metal film is already existing in order to enhance the absorption of laser energy and the emission of IR radiation to the detector The graphite coating g...

Page 58: ...ly sweep across the row of samples several times while maintaining a constant distance applying one thin coat 4 Wait approximately 2 minutes for the coat to be dry 5 Repeat steps 2 4 three more times...

Page 59: ...ting no graphite PocoAXM graphite 2000 C graphite Pyroceram ceramics 900 C graphite Alumina ceramics 2000 C graphite The reference samples are also used in laser flash apparatus up to 2000 C A graphit...

Page 60: ...od to the rear end position see Figure 4 The sample holder is located below the detector housing hood sample holder device Figure 4 open the measuring unit Use the extractor tool as shown in Figure 5...

Page 61: ...Figure 6 and Figure 7 with corresponding mask The sample tray can also be moved removed or installed by means of the extractor tool sample holder plates round or square inserts sample tray Figure 6 p...

Page 62: ...sample tray with each individual sample position numbered 1 through 4 1 2 3 4 sample 1 sample 3 sample 2 sample 4 Figure 8 sample positions Reinstall the cover by means of the extractor tool and clos...

Page 63: ...rating the Instrument LFA 447TM 01 09 J LFA447 CHAPTER4 doc 12 Staring a measurement 1 After software installation please insert the sample s and check the hardware settings File Instrument Configurat...

Page 64: ...n to decrease the flash lamp power 270 V short pulse is e g a signal overflow at room temperature using a gain value of 1260 and lower especially at thin samples low mass or samples with a low specifi...

Page 65: ...vity of one unknown layer or to measure contact resistance between two layers thermal diffusivity of both layers should be known please enter data for each layer with the exception of the thickness al...

Page 66: ...shot enter the number of steps if you want to measure at different temperatures enter the temperature between two steps Inc enter the number of shots at each temperature usually 5 or 6 to increase the...

Page 67: ...an be used 25 C 5012 100 C 623 200 C 315 300 C 155 These values are only a rough estimation and can differ depending on the sample dimension and thermophysical properties above 10 Volts an overflow wi...

Page 68: ...Operating the Instrument LFA 447TM 01 09 J LFA447 CHAPTER4 doc 17 Duration time is too short Duration time is ok maximum at 2 5 of total x range...

Page 69: ...owing questions with yes the last measurement should now be visible in the database window with a double click on the measurement these will be loaded into the analysis Measurement Recalculate diffusi...

Page 70: ...Operating the Instrument LFA 447TM 01 09 J LFA447 CHAPTER4 doc 19...

Page 71: ...ns result if the thickness of the sample and reference is strong different But important is the distance between the surface of the sample and IR detector viz through balancing of the difference of le...

Page 72: ...n 1 0 Position 2 25 Position 3 50 Position 4 75 Position 5 100 Position 6 100 Position 7 100 Position 8 100 The choice of flash power depends mainly on the thickness or heat capacity product of mass a...

Page 73: ...01 09 J LFA447 CHAPTER5 DOC Chapter V Appendix LFA 447TM...

Page 74: ...Appendix LFA 447 TM 01 09 J LFA447 CHAPTER5 DOC Contents TECHNICAL DATA 1 MATRIX SAMPLE HOLDER 2 INDIVIDUAL PARTS 2 INSTALLATION 3 START A MEASUREMENT 13 LITERATURE 15...

Page 75: ...rix sample holder only room temperature Thermal Diffusivity Range 0 001 cm 2 s to 10 cm 2 s Flash lamp Illumination Xenon flash lamp Wavelength 150 nm 2000 nm Pulse Energy 10 J pulse adjustable power...

Page 76: ...ndividual parts sample holder plate A B C D E F G H coordinates plate adjusting plate casing aperture support apertures with fixing screws phillips screws allen key support plate Figure 1 Matrix sampl...

Page 77: ...ition to place the sample holder in the position for changing the sample holder 2 Close the measuring software on off switch 3 Switch off the LFA measuring unit on the rear of the instrument cap 4 Rem...

Page 78: ...s 6 Loosen the phillips screws hood 7 Remove the hood lift it upwards front cover front cover phillips screws plug connection 8 Loosen the phillips screws remove the front cover and disconnect the plu...

Page 79: ...J LFA447 CHAPTER5 DOC 5 slide unit 9 Move the slide unit in the rear position cover plate 10 Remove the cover plate sample tray 11 Remove the sample tray plug connection sensor 12 Disconnect the plug...

Page 80: ...rt and fix it with the phillips screws Apertures with different aperture diameter are available 1 mm 2 mm 3 5 mm 5 mm Apertures with a small aperture diameter allow a higher lateral resolution than ap...

Page 81: ...m the normal position upwards and turn it counterclockwise until it snaps into the upper end position In the normal sensor position the guide pins go through the holes in the sensor support If the sen...

Page 82: ...Loosen the phillips screws rear left corner furnace 21 Remove the furnace lift it upwards for reassembly of the 300 C furnace insert the furnace so that the furnace cable is placed in the rear left co...

Page 83: ...ps screws 23 Fix the frame with the phillips screws glass plate 24 Insert the glass plate B support plate 25 Insert the support plate B C sample holder plate support plate 26 Put the sample holder pla...

Page 84: ...t cover phillips screws plug connection 27 Connect the plug connection of the control elements push the front cover onto the instrument and fix it with the phillips screws hood 28 Push the hood onto t...

Page 85: ...gap of approx 2 3 mm between instrument cover and hood Danger of scratching when moving the slide unit cap 31 Push the cap onto the instrument on off switch 32 Switch on the instrument on the rear 33...

Page 86: ...the lower position so that the guide pins go through the holes in the sensor plate as shown in the figure Software settings software settings for the 300 C furnace The standard sample holder with Four...

Page 87: ...sample holder plate F adjusting plate sample Check that the height of the sample is not higher than the lower edge of the adjusting plate If not The height of the support frame can be adjusted by mean...

Page 88: ...re you can see the values for x and y position in mm which have to be entered into the measuring software 0 0 10 10 20 10 10 20 20 20 x y Position x y in mm top view coordinate plate After this remove...

Page 89: ...Cowan J Applied Physics 34 926 1963 3 Radiation Loss in the Flash Method for Thermal Diffusivity Clark and Taylor J Applied Physics 46 714 1975 4 Improved Data Reduction Methods for Laser Pulse Diffu...

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