INSTRUMENTATION

 

Belt-tYPE PRESS

CONAC PRESS

PistOn-CylindEr tYPE PRESS

EQUIPMENT FOR HYDROTHERMAL SYNTHESIS

cONTROLLED ATMOSPHERE FURNACE

 

 

            BELT-TYPE PRESS (CNRS, Grenoble)

 

Belt Press 

Components of Pressure cell

Detail of the pressure chamber and the WC pistons

 

The laboratory has got a belt-type press that can works at high pressure and temperature in the   0-80 Kbar  and  0-1700 ºC ranges. In the left part (Left photo), the equipment formed by a hydraulic pressure, a power supply  and temperature controller (from Eurotherm) is shown; the process is fully authomatic . 

There are two exchange pressure chambers (Right photo) with an internal cooling circuit. The large chamber can work up to 40 kbar of pressure and a maximum of 300 mg of sample can be obtained, while in the small chamber 80 kbar can be reached and the yield is of the order of 100 mg of sample. 

In the central part, different components of a pressure cell are shown (Central photo): two teflon rings, two conic pyrophyllite pieces, a graphite furnace, an alumina cylinder sleeve,  two alumina tapes and a gold cup (for temperatures < 1100 ºC). The type of furnace (graphyte or Mo) and cup (Cu, Au, Pt or Ta) to be used depend on the temperature ranges of work.

 

CONAC PRESS (from Cyberstar, France)

 

Conac Press 

Components of Pressure cell

Details of the pressure chamber

The Conac press from Cyberstar (France) can works at high pressure and temperature in the   0-100 Kbar  and  0-1800 ºC ranges. In the left part (Left photo), the equipment formed by a hydraulic pressure, a power supply  and temperature controller (from Eurotherm) is shown; the process is fully authomatic . 

There are several exchange pressure chambers (Right photo) with an internal cooling circuit. The small chamber (CONAC 15) can work up to 100 kbar of pressure and a maximum of 200 mg of sample can be obtained, with the intermadiate one (CONAC 28) 75 kbar can be reached and 750 mg the sample obtained, and finally, the big chamber (CONAC 40) can work up to 55 kbar and obtain 2.0 g of sample. 

In the central part, different components of a pressure cell are shown (Central photo): three cartoon rings, two steel pistons, two calcite pieces, two molibdenum and two tantalum disks, two calcite tapes, a steel capsule, two concenctric calcite cylinder sleeves, a graphite cylinder furnace, and calcite container. The type of furnace (graphyte or Mo) and cup (Cu, Au, Pt or Ta) to be used depend on the temperature ranges of work.

 

    PISTON-CYLINDER TYPE PRESS (Rockland)

 

Piston-Cylinder Type Press

Components of pressure cell

 

The piston-cylinder type press (Left photo) allow to work in the 0-35 Kbar and 0-1700 ºC ranges of pressure and temperature. In the left part, the equipment ready to work is shown. In this equipment the control of temperature is carried out by a thermocouple placed just on the top of the cup, as shown in the right part. In this case, the larger pressure chamber allow to reach 20 kbar with 1 g. of sample, while the smaller one can be used at 35 Kbar of maximum pressure and 0.5 g. of sample . In the right part, the different components of a pressure cell are shown (Right photo): two pyrex sleeves,  two MgO tapes, a graphyte furnace, a steel base plug, a thermocouple and a cup.

  EQUIPMENT FOR HYDROTHERMAL SYNTHESIS

The equipment for hydrothermal synthesis allows the synthesis under a maximum hydrostatic pressure of 2.5 bar and temperatures of 900 ºC in an aqueous medium. Inconel autoclaves are used for synthesis performed above the critical point of water, (from Autoclave Engineers Inc.) while stainless steel autoclaves lined  with teflon and fitted with an external manometer are preferred for work below that critical point. In this case, working limits are 230 ºC and 150 bar, but a better control of the synthesis conditions is achieved. The product yield can reach 100 g.

 

Different types of used autoclaves

Autoclave made of Inconel alloy to be used  with sealed  gold or quartz blisters containing the reactants. Pressures up to 3 Kbar and temperatures up to 900 ºC can be reached. Pressure is generated by heating pre-compressed water filling the autoclave but external to the sample.

Stainless steel  autoclave with a teflon liner to be used in a furnace at temperatures < 230 ºC. The manometer shows the internal pressure which has to be maintained below 150 bar.

Stainless steel  autoclave with a teflon liner to be used in a furnace at temperatures < 230 ºC.

 

 

 CONTROLLED ATMOSPHERE FURNACE

This equipment is made up a tubular furnace and a vacuum system (< 0.001 mbar) with a quartz tube which allows to obtain all type of precursors in optimal conditions for the high pressure synthesis. Treatments in oxygen or argon atmospheres at pressures below 1.5 atm can be carried out .  The type of connection between the quartz tube and vacuum system  favors the replacing of samples from and to a "controlled atmosphere" chamber.

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