Compound potassium lead borophosphate nonlinear optical crystal as well as preparation method and application thereof
A nonlinear optics, potassium lead phosphate technology, applied in nonlinear optics, chemical instruments and methods, optics, etc., can solve the problems of slow growth, difficult to obtain large-sized crystals, BBO phase transition, etc.
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Embodiment 1
[0033] Embodiment 1: (adopting melt method)
[0034] Potassium lead borophosphate (KPbBP) 2 o 8 ) compounds:
[0035] By chemical formula: K 2 CO 3 +2PbO+2H 3 BO 3 +4NH 4 h 2 PO 4 =2KPbBP 2 o 8 +CO 2 ↑+4NH 3 ↑+9H 2 O↑, prepared by solid phase reaction method:
[0036] Will K 2 CO 3 , PbO, H 3 BO 3 , NH 4 h 2 PO 4 Weigh it into a mortar with a molar ratio of 1:1:1:2, mix and grind it carefully, put it into a corundum crucible with an opening of Ф400mm×400mm, press it tightly, put it into a muffle furnace, and slowly raise the temperature to 500 ℃, constant temperature for 24 hours, take out the crucible after cooling, at this time the sample is relatively loose, then take out the sample and grind it evenly, then put it in the crucible, keep the temperature in the muffle furnace at 800℃ for 48 hours, take it out, put it in Pound and grind in a mortar to get KPbBP 2 o 8 compound, the product is subjected to X-ray analysis, and the resulting X-ray spectrum ...
Embodiment 2
[0041] Embodiment 2: (adopting melt method)
[0042] According to reaction formula K 2 O+2PbO+2H 3 BO 3 +4NH 4 h 2 PO 4 =2KPbBP 2 o 8 +4NH 3 ↑+9H 2 O ↑ Synthetic KPbBP 2 o 8 Compound, specific operation steps are carried out according to embodiment 1;
[0043] Preparation of KPbBP by pulling method 2 o 8 the crystal
[0044] Synthetic KPbBP 2 o 8 Put the compound into a Ф90mm×90mm open platinum crucible, put the crucible into a crystal growth furnace, raise the temperature to 980°C, keep the temperature for 10 hours, then cool it down to 867°C, cut the KPbBP along the c-axis 2 o 8 The seed crystal is fixed on the lower end of the seed rod with a platinum wire, and the seed crystal is introduced into the crucible from the small hole on the top of the furnace, so that the seed crystal is in contact with the liquid surface of the melt, and the temperature is lowered to 865°C, the rotation speed of the seed rod is 20rpm, and the pulling speed is 0.1 mm / h, increas...
Embodiment 3
[0046] Embodiment 3: (adopt melt method)
[0047] Reaction K 2 C 2 o 4 .H 2 O+2PbO+2H 3 BO 3 +4NH 4 h 2 PO 4 =2KPbBP 2 o 8 +CO 2 ↑+CO↑+4NH 3 ↑+10H 2 O ↑ Synthetic KPbBP 2 o 8 Compound, specific operation steps are carried out according to embodiment 1;
[0048] Preparation of KPbBP by Kyropoulos method 2 o 8 the crystal
[0049] Synthetic KPbBP 2 o8 Put the compound into an open platinum crucible of Ф80mm×80mm, put the crucible into a crystal growth furnace, raise the temperature to 1100°C, keep the temperature for 4 hours, then cool down to 865°C, cut the KPbBP along the c-axis 2 o 8 The seed crystal is fixed on the lower end of the seed rod with a platinum wire, and the seed crystal is introduced into the crucible from the small hole on the top of the furnace, so that the seed crystal is in contact with the liquid surface of the melt. After the crystal growth is over, the crystal is lifted from the melt surface, cooled to room temperature at a rate of 10...
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