The preparation method of lead niobate lead indate-lead titanate lead solid solution monocrystalline

The preparation method of lead niobate lead indate-lead titanate lead solid solution monocrystalline

  • CN 100,560,812 C
  • Filed: 04/07/2004
  • Issued: 11/18/2009
  • Est. Priority Date: 04/07/2004
  • Status: Active Grant
First Claim
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1. , a kind of preparation method of lead niobate lead indate-lead titanate lead solid solution monocrystalline is characterized in that comprising following method steps:

  • 1) determine x the value accurate afterwards following oxide raw material of weighing---analytically pure Indium sesquioxide, Niobium Pentxoxide, titanium dioxide and plumbous oxide according to (1-x) PIN-xPT chemical formula, the crystal chemistry according to design behind the raw material drying is formed (1-x) Pb ((In 1/2Nb 1/2) 0 3-xPbTi0 3Proportioning, x=0.05~

    0.70;

    2) again Indium sesquioxide, Niobium Pentxoxide, the titanium dioxide ball milling of being joined was mixed into uniform powder in 1~

    10 hour, expects as rising of crystal growth through hydrostaticpressure or compression molding;

    3) rising of seed crystal and crystal growth expected put into platinum crucible and carry out welded seal, place crystal growing furnace at 800~

    1400 ℃

    , react 1~

    4 hour pre-treatment products therefrom through fine grinding, sieve, the plumbous oxide that adds the metering ratio mixes, and places the platinum crucible of adding a cover 600~

    800 ℃

    of thermal treatments 1~

    2 hour then;

    4) control crystal growing furnace furnace temperature is 1200 ℃



    1400 ℃

    scopes, is 60 ℃

    /cm along the maximum temperature gradient of crucible descending direction, and crucible descends with 0.5~

    1.0mm/h speed, and the rotary acceleration of crucible is Treat that rising of crystal growth expect after the fusing, be incubated after 5~

    10 hours, lead niobate lead indate-lead lead titanate crystal begins to grow, the mechanical precision of crucible rotation fall off rate generally is controlled at ± and

    0.1%, along with the carrying out of growth, the furnace temperature of growth furnace heats up according to the speed of 10 ℃

    /h, with EUROTHERM 425A precision temperature controller the temperature of growth furnace is controlled, temperature-controlled precision is ±

    0.5 ℃

    , and the thermograde of steady-state growth stage solid-liquid growth interface is 40~

    80 ℃

    /cm;

    5) after crystal growth finished, to the crystal growing furnace cooling, all 700 ℃

    of insulations 4~

    6 hours, rate of temperature fall was 18 ℃

    /h to the crucible in the stove, and the temperature of crystal growing furnace is reduced to room temperature with the speed of 50~

    80 ℃

    /h then.

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