Compound lead borate and nonlinear optical crystal of lead borate, preparation method thereof and purpose thereof
A nonlinear optics, compound technology, applied in nonlinear optics, chemical instruments and methods, optics, etc., can solve problems such as high price, long growth cycle, and easy deliquescence of crystals
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Embodiment 1
[0035] Embodiment 1: (adopting melt method)
[0036] Synthetic lead borate (Pb 4 O(BO 3 ) 2 ) compound:
[0037] The lead borate compound is synthesized by a solid-state reaction method, and its chemical equation is: 4Pb(NO 3 ) 2 +2H 3 BO 3 →Pb 4 O(BO 3 ) 2 +8NO 2 ↑+3H 2 O↑+2O 2 ↑;
[0038] Pb(NO 3 ) 2 、H 3 BO 3 Put it into a mortar with a stoichiometric ratio of 2:1, mix and grind it carefully, then put it into a corundum crucible with an opening of Φ400mm×400mm, press it tightly, put it in a muffle furnace, and slowly raise the temperature to 300°C, constant temperature 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 430°C for another 48 hours, take it out, put it in the mortar Pound and grind to obtain lead borate compound. Carry out X-ray analysis to this product, gained X-ray spectrogram and...
Embodiment 2
[0046] According to the reaction formula 4PbO+2H 3 BO 3 →Pb 4 O(BO 3 ) 2 +9H 2 O ↑ synthesis of Pb 4 O(BO 3 ) 2 Compound, specific operation steps are carried out according to embodiment 1;
[0047] Preparation of Pb by Pulling Method 4 O(BO 3 ) 2 Crystal:
[0048] a, the synthesized Pb 4 O(BO 3 ) 2 Put the compound into a Φ90mm×90mm open platinum crucible, heat it to a temperature of 370°C, and keep the temperature constant for 5 hours to obtain a mixed melt of lead borate;
[0049] b. Preparation of lead borate seed crystals: Slowly lower the mixed melt or mixed melt obtained in step a to room temperature at a rate of 0.5°C / h, and spontaneously crystallize to obtain lead borate seed crystals;
[0050] C, the crucible that fills the mixed melt that step a makes is placed in the crystal growth furnace, the Pb that the seed crystal that step b obtains is cut along the c-axis 4 O(BO 3 ) 2 The seed crystal is fixed on the lower end of the seed rod with a platinu...
Embodiment 3
[0053] Embodiment 3: (adopt melt method)
[0054] According to the reaction formula 4PbC 2 o 4 +2H 3 BO 3 →Pb 4 O(BO 3 ) 2 +4CO 2 ↑+3H 2 O↑+4CO↑Synthesis of Pb 4 O(BO 3 ) 2 Compound, specific operation steps are carried out according to embodiment 1;
[0055] Preparation of Pb by Kyropoulos method 4 O(BO 3 ) 2 Crystal:
[0056] a, the synthesized Pb 4 O(BO 3 ) 2 The compound is put into an open platinum crucible of Φ80mm×80mm and heated to melt, heated to a temperature of 450°C, and kept at a constant temperature for 25 hours to obtain a mixed melt of lead borate;
[0057] b. Preparation of lead borate seed crystals: Slowly lower the mixed melt obtained in step a to room temperature at a rate of 2 °C / h, and spontaneously crystallize to obtain lead borate seed crystals;
[0058] C, the crucible that fills the mixed melt that step a makes is placed in the crystal growth furnace, the Pb that the seed crystal that step b obtains is cut along the c-axis 4 O(BO ...
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