Rapid Growth of A Cuboid DKDP Crystal - Crystal Growth & Design

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Rapid Growth of A Cuboid DKDP Crystal Duanyang Chen, Bin Wang, Hu Wang, Lili Zheng, Hui Zhang, Hongji Qi, and Jianda Shao Cryst. Growth Des., Just Accepted Manuscript • DOI: 10.1021/acs.cgd.8b01876 • Publication Date (Web): 03 Apr 2019 Downloaded from http://pubs.acs.org on April 5, 2019

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Crystal Growth & Design

Rapid Growth of A Cuboid DKDP Crystal Duanyang Chen, ab Bin Wang, a Hu Wang, a Lili Zheng, c Hui Zhang, d Hongji Qi *a and Jianda Shao **a a

Key Laboratory of Materials for High Power Laser, Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800, China

b

Center of Materials Science and Optoelectronics Engineering ，University of Chinese Academy of Sciences, Beijing 100049, China c

d

School of Aerospace Engineering, Tsinghua University, Beijing 100084, China

Department of Engineering Physics, Tsinghua University, Beijing 100084, China

*Corresponding author: [email protected]; Fax: +86 21 6991 8028; Tel: +86 21 6991 8196 **Corresponding author: [email protected]; Fax: +86 21 6991 8028; Tel: +86 21 6991 8461

Abstract The pyramid-prism interface in “point-seed” rapidly grown DKDP crystals affects the quality of tripler-cut samples used in inertial confinement fusion devices. In this study, a cuboid DKDP crystal without a pyramidal sector was rapidly grown. The quality of the cuboid DKDP crystal was evaluated by measuring the deuterium homogeneity, crystalline quality, transmission spectrum, and laser-induced damage performance. The total number N of tripler-cut samples that can be obtained from the cuboid DKDP crystal is easily calculated. The size of the tripler-cut sample is approximately equal to the cross-section of this cuboid DKDP crystal. Moreover, as this cuboid DKDP crystal has a regular shape, calculating the mass of the crystal and accurately controlling the supersaturation of the solution during growth is easy. The successful crystal growth using this proposed approach establishes the possibility of growing large aperture cuboid DKDP crystal. Currently, research on the rapid growth of a cuboid DKDP crystal with an aperture of more than 40 cm is underway.

1 Introduction DKDP (KDxH2-x PO4) is the best nonlinear crystal used as tripler in inertial confinement fusion (ICF) facilities, because this crystal can minimize stimulated Raman scattering.1,2 It takes one-two years to get DKDP tripler for ICF facilities using traditional growth method therefore, the development of rapid growth method is important.3, 4 In “point-seed” rapid grown DKDP crystal, all prismatic and pyramidal crystallographic faces grow. Where these two crystallographic faces are next to each other, a pyramid-prism (PY-PR) boundary appears. 5 , 6 Using orthogonal polarization interferometry, the abrupt ∆(ne–no ) distribution near the PY-PR boundary was clearly identified. 7 And the abrupt ∆(ne–no ) of the PY-PR boundary has a detrimental effect on the harmonic generation and phase matching. 8 , 9 Threshold of the laser-induced damage (LID) near the PY-PR boundary of a “point-seed” rapid grown KDP crystal was also found to be less than half of other sectors.10 Negres et al.11 concluded that the LID density has a distinct aggravation near the PY– PR boundary compared to other sectors of a “point-seed” rapidly grown KDP crystal. To avoid the formation of PY-PR boundaries during the rapid grown KDP-type crystals, the Sankaranarayanan-Ramasamy (SR) method was proposed.12,13 Although there is no PY-PR boundary in the crystals grown by the SR method, 14, 15 the flow

conditions of the solution in this method is worse than that of KDP crystal grown on a rotating platform, 16-19 making it difficult to grow large-aperture KDP-type crystal. In this study, a cuboid DKDP crystal without the pyramidal sector was rapidly grown. The quality of the cuboid DKDP crystal was then evaluated by measuring the deuterium homogeneity, crystalline quality, transmission spectrum and laser-induced damage performance. The advantages of crystal shape is also discussed.

2 Experimental section 2.1 Detail about the Crystal Growth A cuboid DKDP crystal was grown in a 65L tank rapidly. The crystal holder has two studdles to connect the upper baffle and the bottom baffle, as shown in Figure 1. Prior to crystal growth, a long DKDP seed was fixed between the upper and bottom baffles of the crystal holder. The deuterium content of the long DKDP seed was 50%. The dimensions of the long DKDP seed was 10 mm ×10 mm ×92 mm corresponding to the [100], [010] and [001] crystallography directions, respectively.

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to 1000 cm−1were obtained using a micro-Raman spectrometer (LabRAM HR Evolution). The spot size of a 633 nm excited laser was 4μm × 4μm. In addition, Raman spectra of a KDP sample was also measured as a standard.

2.2.2 High-resolution XRD FWHM of HRXRD is an important parameter for characterizing the crystalline quality. The HRXRD of the (200) face of the cuboid DKDP crystal was measured using an diffractometer (Bruker D8 DISCOVER), with an incident slit 10 mm long and 0.6 mm wide. And during the measurement, the operating power of the diffractometer is 40 kV × 40 mA.

2.2.3 Transmission spectra Fig. 1 Schematic diagram of the crystal holder. The parts of the crystal holder in contact with the solution are coated with Teflon with a thickness of 0.5 mm. At a supersaturation of approximately 5%, the four prismatic faces of the long seed began to grow rapidly. The average growth rate over the course of the growth is about 7 mm/day. And the upper and bottom pyramidal faces were inhibited due to the upper and bottom baffles. By driving the rotating shaft above the platform using the motor outside the growth vessel, the crystal was rotated 44 rpm alternatively. And during the change of the direction of rotation, there is a 3s rest of the platform. After 7 days, the temperature was decreased from 45 ℃ to 42 ℃ and a cuboid DKDP crystal with dimensions of 100×100×92 mm3 was grown, as shown in Figure 2. More details about the growth have been presented in our previous work. 20,21

The transmission spectra of the tripler-cut sample cutting from the cuboid DKDP crystal from 220 nm-1200 nm was tested using a spectrometer (Lambda 1050). Since the sensitivity of the spectrometer’s detector is very low and the energy of the light source varies greatly in near-infrared band, servo mode is used as the pattern of slit management. Except in the near infrared band, the slit width is 2 nm.

2.2.4 Laser-induced damage performance LID performance of the tripler-cut sample obtained from the cuboid DKDP crystal was performed with a Nd:YAG laser.26 The effective spot was 0.306 mm2 and the pulse duration of the laser was 7.8 ns. The LID was performed according to the R-on-1 test procedures. During the test, the polarization of the laser is perpendicular to the o axis of the sample. To identify different kinds of defect from the LID curve, the two-parameter degenerated model was used.27,28

3 Results and discussion 3.1 Advantages of the cuboid shape The schematic diagram depicting the cutting of tripler-cut samples from the cuboid DKDP crystal is shown in Figure 3. The length and height of the crystal are L and H. The length, width and thickness of the tripler-cut sample are L, W and T respectively. The angle α is equal to the phase matching angle of the tripler-cut DKDP sample. The total number N of tripler-cut samples that can be obtained from the cuboid DKDP crystal can be determined from the following simple formulas:

Fig. 2 The rapidly grown cuboid DKDP crystal. The white Teflon block above the crystal was used to fix the long seed in the center of the upper baffle.

2.2 Characterizations 2.2.1 Micro-Raman Spectroscopy For the DKDP crystal, the peak position of P(OD)2 stretching vibration is related to the deuterium content.22,23 The shift of each 1 cm−1 of the peak position of P(OD)2 vibration is equivalent to a change in deuterium content of 2.68%.24,25 With a spectral resolution of 0.15 cm−1, the Raman spectra from 800

(𝑇𝑠𝑖𝑛𝛼 + 𝑉) × 2 + 𝑠 = 𝐿;

(1)

𝑊𝑠𝑖𝑛𝛼 + 𝑇𝑐𝑜𝑠𝛼 + 𝐼𝑁/2 = 𝐻.

(2)

where V is equal to Wcosα, s denotes the width of the seed, I is equal to T/cosα. All of the samples cutting out of the cuboid DKDP crystal does not contain the PY-PR boundary. Given that the phase matching angle of the tripler-cut sample is approximately 60° (the phase matching angle fluctuates in a small range depending on the deuterium content), the length (L) of the tripler-cut sample is similar to the width (W). In the case of the growth of a large cuboid DKDP crystal, the width of the seed is negligible relative to the width of the grown crystal. Therefore, the tripler-cut samples obtained from large cuboid DKDP crystal are approximately square. Moreover, the size of the tripler-cut


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sample is approximately equal to the cross-section of the grown crystal. In addition, it is easy to calculate the mass of the crystal and to accurately control the supersaturation of the solution during growth given that the cuboid DKDP crystal has a regular shape.

Fig. 3 Schematic diagram showing the cutting of tripler-cut samples from the cuboid DKDP crystal. Only the right half of the crystal is shown with tripler-cut samples.

3.2 Deuterium homogeneity Deuterium content was determined in directions of the length, width and height (corresponding to the [100], [010] and [001] crystallographic directions, respectively) of the cuboid DKDP crystal. A total of 10 points were measured in each direction and the spacing between two adjacent test points was fixed. The distribution of these 10 points was as dispersed as possible, as shown in Figure 4. Since the long DKDP seed was 10 mm ×10 mm ×92 mm and the final cuboid DKDP crystal was 100×100×92 mm3, the value of the spacing between two adjacent points corresponding to the x-axis (the [100] crystallographic direction), y-axis (the [010] crystallographic direction), and z-axis (the [001] crystallographic direction) were 4mm, 10mm, and 10mm, respectively. 30 samples with the size of 3 × 3 × 1 mm3 were processed, and the center of each sample contained one test point. To avoid exposing the test points to the air for a long time, each sample is cut in the middle of the square surface before test. By fixing the newly cut sample on a two-dimensional mobile platform, the center of the newly cut section is where the test point located. The Raman spectrum acquired at these points were fitted using the Lorentz function to determine the exact position of the main peak.

Fig. 4 Locations of the test points used to measure the uniformity of the deuterium content. The directions of the length, width and height correspond to the [100], [010] and [001] crystallographic directions respectively. The uniformity of the deuterium content of the cuboid DKDP crystal is shown in Figure 5. In the x-direction, the deuterium content decreased sharply at first, then fluctuated for the three middle positions (Number 5, 6 and 7), followed by a slight decrease for the last few points. In the y-direction, the deuterium content initially increased followed by a decrease. This indicates that deuterium content has a slight tendency to decrease with the growth of the crystal. In the z-direction, except for the first point and the last point, the deuterium of the middle eight point have good uniformity and the fluctuation is less than 0.3%. As for the first point and the last point, since they are very close to the upper baffle and lower baffle, the flow field and the supply of fresh solute near the two points is different from where far away from the baffles, which is probably the reason for the large fluctuations of deuterium content of these two points. Overall, the deuterium content varied by less than 1% in each direction. The deuterium homogeneity shows here are on the same level as that reported by Chai et al.29

Fig. 5 The uniformity of the deuterium content in each direction. The locations of the 10 test points in each direction are shown in Figure 4.

3.3 Crystalline quality The result of the HRXRD of the (200) face of the cuboid DKDP



crystal is shown in Figure 6. Prior to testing, the sample was finely polished. During testing, the increment was 0.001°. And the FWHM of the (200) face is 0.010°. The FWHM of the DKDP crystal grown by a traditional growth method reported by Zhang et al is 74.808″,30 which is twice as big as the cuboid DKDP crystal presented here. As a new method, it is an improvement to achieve such a crystalline quality.

Fig. 6 The HRXRD of (200) face of the cuboid DKDP crystal.

3.4 Transmission performance The transmission spectra of the tripler-cut sample obtained from the cuboid DKDP crystal from 220 nm-1200 nm is shown in Figure 7. In the band of 387 nm-1021 nm, the transmittance of the sample was higher than 90%. The transmittance in the ultraviolet region decreased rapidly as the wavelength decreased. Given that the cuboid DKDP crystal is grown from four prismatic faces, the transmittance of the cuboid DKDP crystal shows here is as high as the rapidly grown DKDP crystal reported by Xu et al.31

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DKDP crystal was 13.4 J/cm2 (3 ns, 3ω). As reported by Cai et al, the 50% LID threshold of the DKDP crystal grown from conventional temperature cooling method is just nearly 10 J/cm2 (3 ns, 3ω). 33 This indicates that the cuboid DKDP crystal presents here exhibits superior laser-induced damage performance.

Fig. 8 LID performance of the cuboid DKDP crystal. The results fitted from the LID curve are listed in table 1. Although the LID threshold is only 8.1 J/cm2 (3 ns, 3ω), the fitted density of the first kind of defects is quite low, indicating that the cuboid DKDP crystal is of good quality. In addition to these two kinds of defects, part of a third kind of defect was seen in the right-most of Figure 8, at a fluence of 21.1 J/cm2 (3 ns, 3ω). This also indicates that the cuboid DKDP crystal exhibits excellent laser-induced damage performance. Table. 1 Identifying different defects from the LID curve. Defect types

Fitted LIDT

Fitted density

(J/cm2 @3ns,3ω)

(/mm3)

The first kind

8.1

0.45

The second kind

14.7

3.07

4 Conclusions

Fig. 7 The transmission spectra of the cuboid DKDP crystal.

3.5 Laser-induced damage performance The LID performance of a tripler-cut sample obtained from the cuboid DKDP crystal is shown in Figure 8. The pulse width is normalized to 3 ns according to the scaling law32.Different kinds of defects were extracted from the damage probability curve using the two-parameter degenerated model previously mentioned (in section 2.2.4). As shown in Figure 8, two kinds of defects were identified. The 50% LID threshold of the cuboid

By fixing a long DKDP seed between the upper and bottom baffles of the crystal holder, a high-quality cuboid DKDP crystal with dimensions of 100×100×92 mm3 was rapidly grown. The deuterium content varied by less than 1% in the [100], [010] and [001] crystallographic directions. The FWHM of the (200) face was 0.010 degree, indicating of the high crystalline quality. The transmission in the range 387 nm-1021 nm was higher than 90%. In addition, we are considering further enhancing the transmittance of the crystal in the ultraviolet region by thermal annealing. The 50% LID threshold of the cuboid DKDP crystal was 13.4 J/cm2 (3 ns, 3ω). The total number N of tripler-cut samples that can be obtained from the cuboid DKDP crystal is easily determined using simple formulas. The size of the tripler-cut sample was approximately equal to the cross-section of this cuboid DKDP crystal. Moreover, since the cuboid DKDP crystal has a regular shape, it is easy to calculate the mass of the crystal and to accurately control the supersaturation of the solution during crystal growth. The success of the proposed procedure establishes the possibility of growing large aperture cuboid DKDP crystals. Currently, research on the rapid growth of a cuboid DKDP crystal with an aperture of more than 40 cm is underway.


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For Tables of Contents Use Only

Rapid Growth of A Cuboid DKDP Crystal Duanyang Chen, Bin Wang, Hu Wang, Lili Zheng, Hui Zhang, Hongji Qi and Jianda Shao

Synopsis The pyramid-prism interface in rapidly grown DKDP crystals affects the quality of tripler-cut samples used in inertial confinement fusion devices. In this study, a cuboid DKDP crystal without a pyramidal sector was rapidly grown, and showed advantages of crystal shape, good deuterium homogeneity, crystalline quality, transmission and laser-induced damage performance




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Rapid Growth of A Cuboid DKDP Crystal - Crystal Growth & Design

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