Abstract
In this study, we have investigated the development of the crystal growth stability and reproducibility for large and high-quality DAST. DAST crystal were grown from a saturated methanol solution by a slow cooling method and DAST was synthesized by the condensation of 4-methyl-n-methyl pyridinum tosylate, which was prepared from 4-pocoline and methyl toluenesulponate and 4-N-dimethyl amino-bezaldehyde in the presence of piperidine. We had synthesized DAST crystals in dry Argon atmosphere in order to avoid the formation of hydride organge co-crystals, DAST$.$$H_2O$. Since DAST molecules crystallize in a humid atmosphere, crystal structure become centrosymmetric, and then second order NLO (nonlinear optical) properties would be disappeared. We fixed the growth orientation of DAST crystal (001) surface. The crystal growth was proceeded at a cooling rate of $H_2O$/day and the cooling period is for 4 days. The dimensions of seed crystal was $2.5\times 3.6\times0.4\textrm{mm}^3$ and we have obtained a DAST crystal with the dimension of $10\times 10.5\times3.0\textrm{mm}^3$. The color of grown DAST crystal is red and it's surface appears to be metallic green.
본 실험은 대형의 고품질 DAST 결정을 위한 결정안정성과 재현성의 향상에 관하여 연구하였다. DAST 결정은 냉각법에 의한 메탄을 포화용액에서 성장시켰으며, 4-methyl-n-methyl pyridinum tosylate의 축합상태로 합성하였다. DAST 분말은 piperidine이 존재한 상태에서 r-picoline. methyl p-tolune sulfonate 그리고 P-dimethylaminobenzaldehyde로부터 제조하였다. 이때 DAST $H_2O$의 생성을 피하기 위하여 dry Argon분위기에서 합성하였다. 이것은 DAST분자가 습한 분위기에서 결정화될 경우 결정구조는 중심 대칭이 되고 그러한 경우에 DAST 미세결정이 습기를 함유하면 2차 비선형 광학특성은 사라지기 때문이다. 우리는 성장방향을 (001)면으로 고정시켰다. 성장조건은 $H_2O$/day로 서냉시켰으며 기간은 4일 동안이었다. seed 결정의 크기는 $2.5\times 3.6\times0.4\textrm{mm}^3$이며 $10\times 10.5\times3.0\textrm{mm}^3$의 DAST 결정을 제조했다. 육성된 DAST는 빨간색이며 메탈릭그린처림 보이는 표면특성을 나타내였다.
