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A preparation method and preparation device of xteo2·p2o5 (x=2,4) crystal

A te2p2o9, crystal technology, applied in the field of preparation of nonlinear optical crystal xTeO2·P2O5, can solve the problems of difficult control, phase transition, decomposition, etc., and achieve the effect of simple growth conditions, simple device structure and easy control

Active Publication Date: 2019-01-29
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the material obtained in this report is a small grain, not a complete single crystal, and there is still a big gap from the practical application of the crystal.
[0003] wxya 2 ·P 2 o 5 (x=2,4) crystal is a kind of inconsistent melting crystal, and for the inconsistent melting crystal, the preparation process mainly adopts the cosolvent method, because the inconsistent melting crystal has high requirements on the crystallization temperature, and it is very difficult to control it. It will decompose or change phase, resulting in no pure phase crystal
[0004] To date, no xTeO 2 ·P 2 o 5 (x=2,4) the growth method of bulk single crystal, propose the present invention for this

Method used

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  • A preparation method and preparation device of xteo2·p2o5 (x=2,4) crystal
  • A preparation method and preparation device of xteo2·p2o5 (x=2,4) crystal
  • A preparation method and preparation device of xteo2·p2o5 (x=2,4) crystal

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Experimental program
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Effect test

Embodiment 1

[0037] a xTeO 2 ·P 2 o 5 (x=2, 4) The crystal preparation device includes a growth furnace 4, the top of the growth furnace 4 is open, and the inner bottom of the growth furnace 4 is provided with an insulation layer 8, and the above insulation layer 8 is provided with The crucible 5, the top of the growth furnace 4 is obliquely provided with an observation hole 2, the center of the growth furnace 4 is provided with a seed rod 3, and the seed rod 3 is connected with a pulling device 1.

[0038] When the preparation device of this embodiment is used, the TeO 2 and P 2 o 5 Raw materials are put into crucible 5, start growth furnace 4, TeO 2 and P 2 o 5 The raw material is melted in the crucible 5 to obtain the melt 7, the pulling device 1 is started, and the seed crystal is obtained at the end of the seed rod 3; then the TeO 2 and P 2 o 5 The raw materials are put into the crucible 5, the crystallization temperature and the pulling rate are controlled to grow the cryst...

Embodiment 2

[0040] Growth of Te by pulling method 2 P 2 o 9 Crystals, including steps as follows:

[0041] (1) Platinum wire pulling to prepare seed crystal

[0042] TeO 2 and P 2 o 5 Raw materials are mixed evenly at a molar ratio of 2:1; put into a platinum crucible and heat up to 750°C, keep the temperature for 3 hours, the material is fully melted and the melt is mixed evenly; then pulled at a rate of 5mm / hour to obtain Te 2 P 2 o 9 Crystals, used to make seed crystals;

[0043] (2) Growth of Te by pulling method 2 P 2 o 9 the crystal

[0044] Preparation of Te by pulling method 2 P 2 o 9 The main growth conditions of the crystal are: a platinum crucible is used for growth in air, the growth temperature is 650-680° C., and the pulling rate is 0.2-1 mm / hour.

[0045] TeO 2 and P 2 o 5 The raw materials are mixed evenly at a molar ratio of 2:1; put into a platinum crucible and heat up to 750°C, overheat at a constant temperature for 3 hours to fully melt the material ...

Embodiment 3

[0050] Growth of Te by pulling method 4 P 2 o 13 Crystals, including steps as follows:

[0051] (1) Platinum wire pulling to prepare seed crystal

[0052] TeO 2 and P 2 o 5 The raw materials are mixed evenly at a molar ratio of 4:1; put into a platinum crucible and heat up to 650°C, keep the temperature for 4 hours, the material is fully melted and the melt is mixed evenly; then pulled at a rate of 5mm / hour to obtain Te 4 P 2 o 13 Crystals, used to make seed crystals;

[0053] (2) Growth of Te by pulling method 4 P 2 o 13 the crystal

[0054] Preparation of Te by pulling method 4 P 2 o 13 The main growth conditions of the crystal are: a platinum crucible is used for growth in air, the growth temperature is 590-600° C., and the pulling rate is 0.2-0.8 mm / hour.

[0055] TeO 2 and P 2 o 5 The raw materials are mixed evenly at a molar ratio of 4:1; put into a platinum crucible and heat up to 650°C, overheat at a constant temperature for 4 hours, so that the mate...

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Abstract

The invention relates to a preparation method and a preparation device of an xTeO2.P2O5 (x=2,4) crystal. The preparation method comprises the following steps: taking TeO2 and P2O5 as raw materials, preparing a seed crystal through platinum wire pulling and growing T2P2O9 and Te4P2O13 crystals through a pulling method. The preparation device comprises a growth furnace; an opening is formed in the top end of the growth furnace; a thermal insulation layer is arranged at the bottom inside the growth furnace; a crucible is arranged on the thermal insulation layer; observation holes are obliquely formed in the top end of the growth furnace; a seed crystal rod is arranged at the center of the growth furnace; a pulling device is connected to the seed crystal rod. The preparation method and the preparation device provided by the invention have the benefits that the technical defect that inconsistent melting crystals difficultly adopt the puling method to grow is overcome, the appropriate crystallization temperature and pulling rate are controlled, and the problems of easiness in decomposition or phase change in the crystal growth process are solved. The prepared T2P2O9 and Te4P2O13 crystals can be taken as laser frequency doubling materials and used in laser photocopying, medical treatment, storage, display and other fields.

Description

technical field [0001] The invention relates to xTeO crystals for nonlinear optics 2 ·P 2 o 5 The preparation method and preparation device of (x=2,4) belong to the technical field of photoelectric materials. Background technique [0002] Nonlinear optical crystals are the important material basis of laser technology, and the preparation and research of new nonlinear optical crystals is a frontier topic today. wxya 2 ·P 2 o 5 (x=2,4) belongs to the non-centrosymmetric structure, the band gap is 4eV, and its powder frequency doubling effect is α-SiO 2 It is 50 times higher than that of NLO and has good nonlinear optical properties. It is a new type of excellent nonlinear optical crystal. This type of crystal was first reported by V.S.Kozhukharov in TeO 2 -P 2 o 5 Two new inconsistent melting crystal phases Te are formed in the glass system 4 P 2 o 13 and Te 2 P 2 o 9 . However, this material has not been studied in depth for a long time. In 2010, Min Kyung K...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/16C30B15/20
CPCC01P2002/72C30B15/002C30B15/203C30B29/16
Inventor 李静董为民姚倩张俊英柳林涛
Owner SHANDONG UNIV
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