Method for preparing large chlorine barium borate nonlinear optic crystal and application thereof
A technology of nonlinear optics and barium chloroborate, which is applied in the field of preparation of large-size barium chloroborate nonlinear optical crystals, can solve the problem of difficulty in obtaining large-size high-quality single crystals, the absence of barium chloroborate single crystals, and difficulties in crystal growth, etc. question
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Embodiment 1
[0031] Take reaction formula (1) as an example, but not limited to reaction formula (1).
[0032] Using high temperature solid phase method to react BaO+H 3 BO 3 +BaCl 2 ·2H 2 O→Ba 2 B 5 O 9 Cl+H 2 O↑ synthetic barium chloroborate (Ba 2 B 5 O 9 Cl) Compound;
[0033] Put BaO, H 3 BO 3 , BaCl 2 ·2H 2 O was put into a mortar at a stoichiometric ratio of 1.5:5:0.5, mixed and ground carefully, then put into an open corundum crucible of Φ200mm×200mm, compacted, put into a muffle furnace, and slowly heated to 500℃ After cooling for 10 hours, take out the crucible, take out the sample and grind it evenly, then put it in the crucible, keep it at 780℃ in the muffle furnace for 72 hours, take it out, put it in a mortar and grind to obtain the barium chloroborate compound. Perform X-ray analysis on the product, and the obtained X-ray spectrum is consistent with the X-ray spectrum of barium chloroborate single crystal ground into powder;
[0034] a. Combine the synthesized barium chloroborate c...
Embodiment 2
[0041] Take reaction formula (2) as an example, but not limited to reaction formula (2).
[0042] Using high temperature solid phase method to react BaCO 3 +H 3 BO 3 +BaCl 2 ·2H 2 O→Ba 2 B 5 O 9 Cl+H 2 O↑+CO 2 ↑Synthetic Ba 2 B 5 O 9 Cl compound, the specific operation steps were carried out according to Example 1;
[0043] Will be synthesized Ba 2 B 5 O 9 Cl compound and flux NaF and H 3 BO 3 Mix according to the ratio of the amount of the substance to 1:2:1, put it into an open platinum crucible of Φ80mm×80mm, raise the temperature to 950°C, keep the temperature for 40 hours, and then lower the temperature to 880°C to obtain a mixture of barium chloroborate and flux Solution
[0044] The seed crystal obtained in step b of Example 1 was tied to the lower end of the seed rod with platinum wire, and the seed crystal was introduced from the small hole on the top of the furnace to a distance of about 1-2 cm from the crucible, kept at a constant temperature for 15 minutes, and then immer...
Embodiment 3
[0048] Take reaction formula (3) as an example, but not limited to reaction formula (3).
[0049] High temperature solid phase method is used to react Ba(NO 3 ) 2 +H 3 BO 3 +BaCl 2 ·2H 2 O→Ba 2 B 5 O 9 Cl+NO 2 ↑+H 2 O↑ Synthetic Ba 2 B 5 O 9 Cl compound, the specific operation steps were carried out according to Example 1;
[0050] Will be synthesized Ba 2 B 5 O 9 Cl compound and flux NaF and H 3 BO 3 Mix according to the ratio of the amount of the substance to 1:6:3, put it into an open platinum crucible of Φ80mm×80mm, raise the temperature to 880°C, keep the temperature for 60 hours and then lower the temperature to 845°C to obtain a mixture of barium chloroborate and flux Solution
[0051] The seed crystal obtained in step b of Example 1 was tied to the lower end of the seed rod with platinum wire, and the seed crystal was introduced into the crucible from the small hole on the top of the furnace about 1 to 2 cm away from the crucible, kept at a constant temperature for 20 minutes...
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