Anton Paar HTK 1200N Reference Manual
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Anton Paar HTK 1200N Reference Manual

Anton Paar HTK 1200N Reference Manual

High-temperature oven-chamber
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Measure
what is measurable
and make measurable
that which is not.
Galileo Galilei (1564-1642)
Reference Guide
HTK 1200N
High-Temperature Oven-Chamber with
CCU 1000 Control Unit

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Summary of Contents for Anton Paar HTK 1200N

  • Page 1 Measure what is measurable and make measurable that which is not. Galileo Galilei (1564-1642) Reference Guide HTK 1200N High-Temperature Oven-Chamber with CCU 1000 Control Unit...
  • Page 3 Changes, copyright, trademarks etc. This document and its contents may be changed or amended by Anton Paar at any time without prior notice. All rights reserved (including translation). This document, or any part of it, may not be reproduced, changed, copied, or distributed by means of electronic systems in any form (print, photocopy, microfilm or any other process) without prior written permission by Anton Paar GmbH.

  • Page 4: Table Of Contents

    4.1 Installation Requirements ....................... 17 4.1.1 Electrical Power and Computer Interface ................17 4.1.2 Cooling Water Requirements....................17 4.2 Mounting the Adapter on HTK 1200N..................... 17 4.3 Mounting HTK 1200N on the Goniometer..................18 4.4 Installing CCU 1000 ........................18 4.4.1 Power Supply for the Heater....................
  • Page 5 8.2.2 Operation as Heating Chamber ....................36 8.3 Operation under Vacuum........................ 37 8.4 Operation using Various Gases (except air) ................... 38 9 Putting HTK 1200N out of Operation....................39 10 Troubleshooting..........................40 10.1 Error Messages..........................40 10.2 General Messages on Display ...................... 40 10.3 Error Analysis..........................
  • Page 6 Contents B40IB006EN-D...

  • Page 7: Safety Instructions

    In case of damage or malfunction, do not con- life of the product and make sure it is easily tinue operating HTK 1200N. Do not operate the instrument under conditions which could result accessible to all people involved with the prod- uct.

  • Page 8: Radiation Safety

    • Make sure that the setup location is sufficiently Hot surface ventilated. The environment of HTK 1200N must This symbol calls attention to the fact that the be kept free of inflammable gases and vapors. respective surface can get very hot. Do not touch this surface without adequate protective •...

  • Page 9: Safety Signs On The Instrument

    1 CAUTION - Hot surface Wear protective gloves Fig. 1: Position of warning signs on the sample holder Wear protective gloves when handling flange the HTK 1200N. Wear safety goggles Wear safety goggles when handling CAUTION the HTK 1200N. Hot surface...

  • Page 10: Overview

    Both the base plate and the housing are water-cooled. The HTK 1200N is a heating stage for powder XRD The sample holder is inserted through the opening with a temperature range from 25 to 1200 °C.

  • Page 11: Lid

    CCU 1000. by heating the HTK 1200N up to 1000 °C in air. This will extend the life time of the heater consid- The lid has two tap holes into which guiding rods are erably.

  • Page 12: Sample Holder Flanges

    2 Overview 2.2.3 Sample Holder Flanges Sample spinner Two different types of sample holder flanges are available for the HTK 1200N: Stationary sample holder Fig. 6: Sample spinner 1 Sample carrier 2 Fixing ring for sample carrier 3 Sample holder body...

  • Page 13: Connector Box

    TIP: Please refer to chapter 7 for further informa- tion. The sample holder is inserted into the HTK 1200N chamber with two guide pins and fastened by four screws. 2.3 Connector Box...

  • Page 14: Ccu 1000 Front Panel

    2.4.1 CCU 1000 Front Panel 2.4.3 Overheat Protection The front panel of CCU 1000 contains all control HTK 1200N has two devices to prevent overheating buttons, status LEDs and the display. of the instrument. The flow control unit of HTK 1200N monitors the flow of cooling water through the housing of the sample chamber.

  • Page 15: Checking The Supplied Parts

    Table 3-1: Supplied Parts Pcs. Item Cat.No. HTK 1200N with stationary sample holder including: 16407 Heating chamber Stationary sample holder Sample carrier, 0.8 mm deep (2x) Fixing ring for sample carrier...
  • Page 16 3 Checking the Supplied Parts TIP: Check the supplied packages delivered with NOTICE the HTK 1200N for completion by comparing the Risk of damage parts to those listed in the appropriate packing lists. Always use the original packing material when shipping the instrument or parts of it.

  • Page 17: Installation

    Appendix E. foil underneath the Kapton foil will tear. 4.1 Installation Requirements TIP: When HTK 1200N is ordered together with the required adapter, the adapter is mounted on the chamber on delivery. When HTK 1200N is ordered together with a motor- ized alignment stage, the adapter is mounted on the alignment stage.

  • Page 18: Mounting Htk 1200N On The Goniometer

    5. Fasten the two upper parts of the alignment equipment (1) to the HTK 1200N base plate Make sure that the HTK 1200N chamber and (if using the two screws in the front of the upper applicable) the alignment stage are properly part.

  • Page 19: Power Supply For The Heater

    This instrument must be connected to protective ground. 4.4.1 Power Supply for the Heater Power for the heater of the HTK 1200N is supplied with two high current cables. Plug the cable for the heater to the heater connector on the rear side of the CCU 1000 (Fig.

  • Page 20: Connection Of Sample Spinner Motor

    4 Installation switch box on the back of the HTK 1200N to the connector "Flange Control" on the connector box (Fig. 8 (2)). 4.5 Connecting CCU 1000 with a Com- puter The RS 232 serial port at the rear panel of CCU 1000 allows you to connect the CCU 1000 to a computer for remote control (see Fig.

  • Page 21: Installing The Cooling Water Circuit

    The gas exhaust tubing can be connected to the water hoses with quick couplings. Water inlet (1) adapter. The type of gas connector depends on the and oulet (2) are located on the HTK 1200N lid. adapter type. Make sure that the water inlet is connected to nozzle...
  • Page 22 3 Venting valve 4 Reducer DN25 / DN40 5 Flexible stainless-steel hose (0,25 m length) 6 Turbomolecular pump 7 Plastic hose (3 m length) 8 Rotary-slide vacuum pump 9 Oil-mist filter 10 Display Fig. 12: Anton Paar GmbH high vacuum equipment B40IB006EN-D...

  • Page 23: Putting Htk 1200N Into Operation

    2 Slit for X-ray beam Risk of Damage 3 Thermocouple Perform the alignment of the HTK 1200N at Part of the HTK 1200N accessories is an alignment room temperature and with embedded sample slit to enable precise alignment. holder flange.

  • Page 24: Height Adjustment With Motorized Alignment Stage

    X-ray beam pass above the alignment slit, and The HTK 1200N chamber must be aligned on the turn the HTK 1200N housing until the X-ray beam is goniometer so that the sample holder surface is par- achieving maximum intensity.

  • Page 25: Checking The Instrument Condition

     = ½ • ( –  ), which means that the upper • Make sure that HTK 1200N is installed correctly edge of the alignment slit bisects the X-ray and that no collisions between the sample beam. chamber and components of the diffractometer can occur.

  • Page 26: Turning On The Instrument

    5 Putting HTK 1200N into Operation 5.7 Turning on the Instrument the HEATER is off the Error LED is flashing the display shows E03 to indicate that there If possible, switch on CCU 1000 with the cooling wa- is no water flow ter turned OFF in order to test the water flow monitor when starting operation.

  • Page 27: Operating Ccu 1000

    6 Operating CCU 1000 6 Operating CCU 1000 6.2 Keypad This chapter describes the operation of the CCU 1000 Combined Control Unit. CCU 1000 can be operated manually or by remote control. The keypad of CCU 1000 has 6 keys to select pa- rameters and enter values.

  • Page 28: Status Leds

    In the normal operation mode (process value LED is green), the display shows the actual tem- perature of the sample holder of HTK 1200N. By pressing the SCROLL button, the set point LED is green, which means that the target set point tem- perature can now be changed by using the UP or DOWN button.

  • Page 29: Navigation Diagram Of Ccu 1000

    PROCESS VALUE values between sample holder SET POINT ERROR Conf 0 (no rotation) of HTK 1200N read only and 10 (full PROCESS VALUE SET POINT rotation speed) ERROR rate rate can be adjusted code protected...

  • Page 30: Turning The Heater On And Off

    Manual operation of HTK 1200N is done with the keys on the front panel of CCU 1000. Proceed as follows to heat or cool the sample to the desired...

  • Page 31: Handling The Sample Holder And Sample

    HTK 1200N: the stationary sam- Holder Flange ple holder (Fig. 19) and the sample spinner (Fig. 20). The HTK 1200N is delivered with the sample holder The pedestal and the cup of the sample holder are mounted. made of alumina providing high corrosion resis- tance.

  • Page 32: Exchanging The Sample Holder Body

    7 Handling the Sample Holder and Sample 7.1.1 Exchanging the sample holder body To replace the sample holder body from the sample holder flange first demount the sample holder flange from the chamber (refer to chapter 7.1) and then fol- low the instruction below: 1.

  • Page 33: Matching Sample Holder Height To Sample Thickness

    ± 2.5 mm with the alignment equipment of the shieldings. HTK 1200N or automatically by ± 3.5 mm using the motor-driven alignment stage. For samples thicker than 2.5 mm (3.5 mm), the sample holder height can be varied by demounting the spacer ring (1).

  • Page 34: Applying A Sample

    6. Insert the sample holder flange into the cham- The sample holder of the HTK 1200N consists of the sample holder body, the sample carrier and a fixing NOTICE ring.

  • Page 35: Solid Samples

    TIP: A possible temperature deviation in the Make sure that the materials of the HTK 1200N HTK 1200N is not only influenced by its design, but are chemically resistant against the sample and also by the thickness, thermal conductivity, emissiv- reaction products! Please refer to Appendix A.

  • Page 36: Operation

    Take care that the cooling water hoses con- The CCU 1000 Combined Control Unit by Anton nected to the inlet/outlet nozzles are protected Paar GmbH is available for the HTK 1200N. For de- against unintentional disconnection. tailed ordering information, see Appendix E. The...

  • Page 37: Operation Under Vacuum

    HTK 1200N up to 1000 °C can reach up to 1200 °C. Make sure that the in air. This will extend the life time of the heater...

  • Page 38: Operation Using Various Gases (Except Air)

    After work in vacuum or inert gas, it is recom- mended to regularly regenerate this oxide layer NOTICE by simply heating the HTK 1200N up to 1000 °C Risk of damage in air. This will extend the life time of the heater Check and replace the gas hoses regularly! considerably.

  • Page 39: Putting Htk 1200N Out Of Operation

    9 Putting HTK 1200N out of Operation 9 Putting HTK 1200N out of Operation When you stop using HTK 1200N for a short period In order to remove HTK 1200N from the diffractom- without removing it from the diffractometer, proceed...

  • Page 40: Troubleshooting

    The protective ther- present Overtem- moswitch in the sam- perature ple stage housing is * not applicable for HTK 1200N (valid for other non ambient attachments) activated. 10.2 General Messages on Display Air Cool- Air cooling flow is off ing Failure or insufficient.*...
  • Page 41 --> contact Anton Paar water hoses dis- Connect the water hoses on switched off GmbH. connected HTK 1200N to the cooling (CCU 1000 was water circuit. overheated) no cooling water Turn on the cooling water. flow controller Connect the water flow con- 2.

  • Page 42: Technical Support

    If you need technical support, please contact the lo- cal service organization of your diffractometer man- bad RS 232 con- check RS 232 cable (null ufacturer or Anton Paar GmbH in Graz, Austria. nection modem required) and con- Contact details of Anton Paar GmbH:...

  • Page 43: Maintenance

    Check the window foil regularly and exchange it, NOTICE if it is leaky or foggy! Risk of damage. Do not operate the HTK 1200N chamber if the To mount or exchange the window foil, proceed as water flow controller does not work properly. follows: 1.
  • Page 44 11 Maintenance 2. Remove the clamps and the foil. 5. Mount the two clamps again. 6. Fasten the screws of the clamps, beginning from the side where the cooling tube (1) is fas- 3. If required, clean the area of window, O-ring and tened.

  • Page 45: Replacing The Thermocouple

    For this reason the thermocouple cannot be exchanged on its own, but only together with the sample holder. Contact your local Anton Paar GmbH representative for exchange. 11.3.4 Replacing the O-rings Generally, commercially available O-rings made of Viton are used.

  • Page 46: Appendix A: Technical Data

    Appendix A: Technical Data Appendix A: Technical Data Temperature range Operating temperature: Room temperature to 1200 °C Helium: Room temperature to 1000 °C Atmospheres Atmospheres applicable: Vacuum (10 mbar), air, inert gas Max. operating pressure: 1 bar above atmospheric pressure Temperature measurement &...
  • Page 47 CCU 1000 Dimensions: Width x Depth x Height: 450 x 410 x 180 mm Weight: approx. 26 kg CCU 1000 Electrical Data (For use with HTK 1200N): Voltage (mains): AC 230 V ± 10 % Frequency (mains): 50 ... 60 Hz Power consumption: max.
  • Page 48 Appendix A: Technical Data The HTK 1200N with CCU 1000 Combined Control Unit is CE-compliant according to: • Electromagnetic compatibility (2014/30/EU, OJ L 96/79 of 29.3.2014) Applied standards: EN 61326-1:2013 Electrical equipment for measurement, control and laboratory use - EMC requirements - Part 1: General requirements The product is classified as a class B equipment and is not intended for the use in industrial area.

  • Page 49: Appendix B: Cooling Water

    Water filter 16 µm filter- Part of the (supplied with the pressure • Use distilled water. Anton Paar flow reducer. • Add 1,68 grams (20 mmol) of NaHCO per liter controller) of distilled water. Saturation index: SI = pH - pH’s •...
  • Page 50 Appendix B: Cooling water Table 1: Conversion values for the calculation of Saturation index and Ryznar index Total dissolved Ca-hardness* Bi-carbonate Temperature material Ca++ content HCO mg/l Deg. C Deg. D chem. D eq/l 50-300 400-1000 11.5 14.5 18.0 22.2 1 D = 10 mg/l CaO 1 chem = 61 mg/l * This means Calcium hardness and not total hardness...

  • Page 51: Appendix C: Thermal Expansion Of The Sample Holder

    Appendix C: Thermal Expansion of the Sample Holder Appendix C: Thermal Expansion of the Sample Holder Due to the thermal expansion of the used materials Vertical sample holder expansion in vacuum: the height of the sample holder expands with in- creasing temperature which makes regular realign- ments during high- temperature XRD investigations Temperature [C°]...

  • Page 52: Appendix D: Warranty

    Appendix D: Warranty Appendix D: Warranty The warranty regulations for the HTK 1200N High- Temperature Oven-Chamber are in accordance with "General Terms of Delivery" of the Austrian Electrical and Electronic Industry. Anton Paar GmbH gives no warranty for: • ceramic parts.

  • Page 53: Appendix E: Accessories

    HTK 1200N SAMPLE CARRIER 0.8MM DEEP 16411 HTK 1200N SAMPLE CARRIER 0.4MM DEEP 16412 HTK 1200N SAMPLE CARRIER FLAT 15914 FIXING RING FOR SAMPLE CARRIER HTK 1200N 75850 SET OF WINDOW FOILS (AL-COATED KAPTON) 2600 SET OF GRAPHITE FOILS 2601...

  • Page 54: Appendix F: Swagelok Tube Fittings

    Appendix F: Swagelok tube fittings Appendix F: Swagelok tube fittings Appendix F.1: Installation instructions 2. Before tightening the Swagelok nut, scribe the nut at the 6 o’clock position. 3. Hold the fitting body steady with a backup wrench and tighten the nut 1 1/4 turns. Watch Swagelok tube fittings come to you completely as- the scribe mark, make one complete revolution sembled, finger-tight and are ready for immediate...

  • Page 55: Appendix F.2: Retightening Instructions

    Appendix F: Swagelok tube fittings Appendix F.2: Retightening instructions Connections can be disconnected and retightened 3. Tighten nut by hand. Rotate nut to the original many times. position with a wrench. An increase in resis- tance will be encountered at the original posi- The same reliable leak-proof seal can be obtained tion.

  • Page 56: Appendix G: Declaration Of Conformity

    Appendix G: Declaration of Conformity Appendix G: Declaration of Conformity B40IB006EN-D...

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