Physical Properties of a Promising Nonlinear Optical Crystal

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Physical Properties of a Promising Nonlinear Optical Crystal KBaLiAlBO F Bingqing Zhao, Bingxuan Li, Sangen Zhao, Xitao Liu, Zhenyue Wu, Yaoguo Shen, Xianfeng Li, Qingran Ding, Chengmin Ji, and Junhua Luo Cryst. Growth Des., Just Accepted Manuscript • DOI: 10.1021/acs.cgd.8b01054 • Publication Date (Web): 10 Oct 2018 Downloaded from http://pubs.acs.org on October 12, 2018

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Crystal Growth & Design

Physical Properties of a Promising Nonlinear Optical Crystal K3Ba3Li2Al4B6O20F Bingqing Zhao,†, ‡Bingxuan Li †, Sangen Zhao,*,† Xitao Liu †, Zhenyue Wu,† Yaoguo Shen,† Xianfeng Li,† Qingran Ding,† Chengmin Ji,† and Junhua Luo*,† †State

Key Laboratory of Structural Chemistry, Fujian Institute of Research on the

Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, China ‡College

of Chemistry, Fuzhou University, Fuzhou 350116, China

KEYWORDS: Physical properties, nonlinear optics, crystal growth

ABSTRACT: Beryllium-free nonlinear optical (NLO) crystal K3Ba3Li2Al4B6O20F (KBLABF) is a newly reported promising candidate in the generation of the significant UV coherent light. A 17× 12× 8 mm3 bulk single crystal is successfully grown with an optimized flux molar ration. The crystal specific heat increases from 0.65 J·g-1· ℃ -1 to 0.96 J·g-1· ℃ -1 with the increasing temperature. Meanwhile, the a-direction thermal conductivity of KBLABF is 1.11 W·m-1·K-1 at 25 ℃, which is also equivalent to that of the famous NLO crystal β-BaB2O4 (1.25 W·m-1·K-1). KBLABF crystal has moderate Vickers hardness along a-axis and c-axis (165.1 HV0.1 and 257.7 HV0.1, respectively), which indicates it is easy to be cut and polished. Remarkably, the laser damage threshold

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Crystal Growth & Design 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

of KBLABF is 3.32 GW·cm-2(1064 nm, 8 ns), which even exceeds those of some famous commercial NLO crystals. This result demonstrates that KBLABF is suitable for high-power NLO applications. This work will establish foundation for the future NLO applications of KBLABF crystal.



INTRODUCTION

Nonlinear optical (NLO) materials, which is able to effectively extend the fixed (or limited) wavelength of common laser sources, play an unique and indispensable role in laser technology including laser cutting, laser communication, and semiconductor lithography.1-3 In order to make full use of NLO materials, it is essential to satisfy some basic but strict optical requirements: relatively large second-harmonic generation (SHG) response, wide transparent window, moderate birefringence to ensure phase matching, and easiness to grow large single crystals.4-7 In 2016, a new promising beryllium-free borate K3Ba3Li2Al4B6O20F (KBLABF)8 was reported by our group. It maintains the structural advantage of the sole practically available deep-UV NLO crystal KBe2BO3F2 (KBBF)9 and overcomes the structural instability problem that limits the applications of famous NLO crystal Sr2Be2B2O7.10 Moreover, KBLABF crystal possesses relatively short UV cut-off wavelength (~190 nm), sufficiently large SHG response (1.5 × KH2PO4), moderate birefringence (0.06) to achieve phase-matching, as well as stable physical and chemical properties. Recently, our group successfully grew a KBLABF crystal with dimensions up to 18× 13× 8 mm3 through LiOH-BaF2-H3BO3 flux. Meanwhile, several


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important factors affecting crystal growth have been carefully analyzed and discussed, such as flux ratios, growth rates and so on.11 These results indicate that KBLABF is relatively easy to grow bulk single crystals, which is favorable for its potential industrial production. Therefore, KBALBF crystal is a promising candidate that is desirable for UV and deep-UV generation.12

In NLO applications, physical properties play an important role for the practical performance of a crystal.13,14 For example, the thermal properties, such as the thermal conductivity and the thermal diffusivity, have an important influence on the growth of high quality crystals, as the thermal mismatch along the different crystallo-physical directions can produce streaks or other defects.15-17 For another thing, the laser damage resistance of crystals may strongly influence the service time of optical devices.18,19 Therefore, it is meaningful to thoroughly investigate the physical properties of KBLABF for its NLO applications.

Herein, we selected an optimized flux molar ration and successfully grew a bulk single crystal of KBLABF. With the bulk single crystal, thermal properties, including the thermal conductivity, thermal diffusivity and specific heat of KBALBF crystal were measured for the first time. The laser damage threshold of KBLABF crystal and the Vickers hardness were also determined. The characterization of these properties is helpful to the practical application of KBLABF crystal in the future.





EXPERIMENTAL SECTION

Crystal Growth. Firstly, the KBLABF polycrystalline, LiOH·H2O, BaF2 and H3BO3 in a molar ratio of 1: 5: 1: 7 were mixed and finely ground, then transferred this mixture in batches into a platinum crucible that was placed into a vertical, and set temperature program to 850 °C for 48 h. Secondly, a tentative seed crystal method was used to determine the saturation temperature (~787 °C).20,21 Finally, a regular seed crystal with good quality was selected to grow large KBLABF crystal. In order to dissolve impurities on crystal surface, seed crystal was slowly moved into the melt at 800 °C and remained 2 h. Then dropped this temperature to 787 °C within 2 h and began to grow crystal slowly by cooling at a rate of 0.16 °C/day. Seed crystal was rotated at 27 rpm rates with changing directions every 30 s. After about six weeks, the crystal achieved the desired sizes and quality. The as-grown bulk crystal with dimensions up to 17× 12× 8 mm3 was shown in Figure 1.

Figure 1. A KBLABF crystal with good quality. Scale bar, 5 mm.


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Thermal Properties. The specific heat measurement of KBLABF crystal was performed by laser flash mothed22 in the temperature range of 25-450 °C. The thermal diffusion coefficient was measured by using a laser flash apparatus (NETSZCH LAF45 Nanoflash). The used samples are pieces crystal with sizes up to 4 × 4 × 1 mm3 (Figure 2). The (100) and (001) crystallographic planes of KBLABF plate crystal were polished and then coated with graphite, which is propitious to enhance the emission of IR radiation and the absorption of flash energy.15

(a)

(b)

Figure 2. Photographs of the KBLABF plate crystal along the (a) (100) and (b) (001) crystallographic planes. Scale bar, 1 mm.

Laser damage threshold. A xenon laser was employed to measure the laser damage threshold of KBLABF crystal. The test condition was set to the laser wavelength of 1064 nm, the pulse width of 8 ns, and the laser frequency of 1 Hz. The laser beam was focused on the (001) and (100) planes by a lens. Crystal photographs after the laser illuminating have been taken by an optical micrograph and scanning electron microscope, which are shown in Figure 6.





RESULTS AND DISCUSSION

Specific Heat. Specific heat is a significant parameter which can greatly affect the laser damage threshold of NLO crystals in applications.21 It is usually anticipated that materials with higher specific heat will be of great help to improve the damage threshold of the devices.23,24 The specific heat of KBLABF crystals is shown in Figure 3. It is observed that the specific heat of KBLABF increases slowly from 0.65 to 0.96 J·g-1·°C-1 in 25-450 °C temperature range. These values of specific heat are common in borates.15

Figure 3. Specific heat curve of KBLABF crystal by the laser pulsed method.

Thermal diffusivity and thermal conductivity. When a NLO crystal is irradiated by a laser, the thermal load in the crystal for a long time will might result in the losses of output laser power and degradation of beam quality.25,26 It is noteworthy that the thermal conductivity is closely related to the latent heat of crystal during crystal growth and is a main index influencing the morphology and size of crystal.27 The thermal conductivity κ


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can be obtained by the crystal specific heat Cp, and thermal diffusivity T , according to equation below:

  T    C p

(1)

The thermal diffusion coefficients of KBLABF crystal were measured along the a-axis and c-axis in the 25 to 450 °C temperature range. As shown in Figure 4, the

Figure 4. The thermal diffusivity curve of KBLABF crystal.

a-axial thermal diffusivity coefficient exhibits slight amplitude fluctuations between 0.60-0.625 mm2·s-1 in the measurement temperature range. The c-axial thermal diffusivity coefficient increases to 0.53 mm2·s-1 and then decreases slowly to 0.50 mm2·s-1 while the temperature increases. According to equation (1) and the crystal specific heat, the thermal conductivity of KBLABF crystal was calculated. As shown in Figure 5, the a-axial thermal conduction coefficient is almost increase linearly over the



measured temperature range, and the value is 1.11 W·m-1·K-1 at 25 °C, which is equivalent to that of the famous NLO crystal β-BaB2O4 (1.25 W·m-1·K-1); the c-axial thermal conduction coefficient shows slowly increasing, and the value is 0.8 W·m-1·K-1 at 25 °C , which is lower than that of β-BaB2O4 crystal (1.64 W·m-1·K-1).15 Therefore, the a-axis thermal conductivity of KBLABF crystal is higher than that of c-axis, indicating it is favorable to avoid accumulation of thermal stress along the a-axis of KBLABF crystal and increase the service life of KBLABF crystal under high-power laser.

Figure 5. The thermal conductivity curve of KBLABF crystal.

Laser damage threshold. Owing to the high optical intensities involved in the NLO processes, one of the key indicators for judging an excellent NLO crystal device is its ability to resist laser damage.21,22 Based on the proportional relationship between power density and harmonic conversion efficiency, the output power can reach the maximum as long as the power density of the fundamental wave is continuously improved.28 However,


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a laser beam with high power intensity can cause irreparable damage to the crystals and may even be unusable. Hence, the study on laser damage threshold is a great deal for the practical application of NLO crystals.29,30 The laser damage threshold of crystals can be calculated by the following equation:

I

E …………………………………………………………………………… (2) A

Where A refers to the laser spot area, τ refers to the pulse width, and E is the laser energy required to cause damage. In present work, the surface laser damage threshold studies have been carried out for KBLABF single crystals with the thickness of about

Table 1. The surface laser damage threshold values of KBLABF and some commercial NLO materials.

Compound

Laser beam Pluse width Laser damage threshold (nm)

(ns)

(GW·cm-2)

1064

8

> 0.5

β-BaB2O432 1064

10

2.6

KTiOPO433 1064

11

1.5-2.2

KBLABF

8

3.32

LiB3O531

1064

1 mm. The test condition of a xenon laser was set to the laser wavelength of 1064 nm, the pulse width of 8 ns, the laser frequency of 1 Hz, and the power energy of 250 mJ. Thus, the calculated of (100) and (001) surface laser damage threshold is all as high as 3.32



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GW·cm-2. As compared with some famous commercial NLO crystals (Table 1), for example LiB3O5 (> 0.5 GW·cm-2 at 1064 nm and 8 ns),31 β-BaB2O4 (2.6 GW·cm-2 at 1064 nm and 10 ns),32 KTiOPO4 (1.5-2.2 GW·cm-2 at 1064 nm and 11 ns),33 the KBLABF crystal exhibits a comparable surface laser damage threshold, which indicating that KBLABF is suitable for high-power NLO applications.

Meanwhile, the laser damage on crystal surface was observed by optical microscope and scanning electron microscope.27 Figure 6 shows the morphology of KBLABF crystal surface damage, from which the nature of the damage can be judged and the possible origin of the damage can be analyzed. Under the optical microscope (Figure 6a), the light halation and dark spot caused by high-power laser appear on the

(a)

(b)

Figure 6. (a) Photograph of the KBLABF crystal surface damaged by laser under the optical microscope. Scale bar, 1 mm. (b) Scanning electron microscopy of laser spot. Scale bar, 200 μm.

crystal surface. The dark spot was also observed by scanning electron microscope


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(Figure 6b). It is clear that a crack and some blobs in the damage pattern of KBLABF around the core of the damage. Some investigations revealed that the temperature of laser damage point can achieve 10000 ℃ above,24 so the damage of KBLABF crystal surface may be caused by the transient thermal effects of high intensity laser beam irradiation resulting in decomposition or melting of the crystal surface.

The Vickers hardness. Using processed KBLABF crystals, we tested the micro Vickers hardness on (001) and (100) plane. As shown in Figure S1, the average scratch width of (100) is 33.51 μm, and the corresponding Vickers hardness value is 165.1 HV0.1. The average scratch width of (001) is 26.825 μm, and the corresponding Vickers hardness value is 257.7 HV0.1. According to Table S1,34,35 the Morse hardness of (100) and (001) crystallographic planes are about 3.6 and 4.1, respectively, which indicates KBLABF crystal is easy to be cut and polished.



CONCLUSION In conclusion, a bulk KBLABF crystal with dimensions up to 17× 12× 8 mm3 is

successfully achieved using an optimized flux molar ration. The crystal specific heat increases from 0.65 J·g-1· ℃ -1 to 0.96 J·g-1· ℃ -1 with the increasing temperature. The thermal conductivity coefficients are calculated to be κa = 1.11 W·m-1·℃ -1 and κc = 0.8 W·m-1·℃ -1 at room temperature, respectively. KBLABF crystal shows moderate Vickers hardness of 165.1 HV0.1 along the a-axis and 257.7 HV0.1 along the c-axis, indicating it



is easy to be cut and polished. Remarkably, its laser damage threshold is as high as 3.32 GW·cm-2 at 1064 nm, which is comparable to those of some commercial NLO crystals and is favorable for high-power NLO applications. We believe that this work will establish foundation for the future applications of such a promising NLO material.



ASSOCIATED CONTENT

Supporting Information Figures S1, the Vickers’s hardness values of K3Ba3Li2Al4B6O20F crystal along the (100) and (001) directions. Table S1, comparison of Mohs’s scale with Vickers’s hardness numbers. 

AUTHOR INFORMATION

Corresponding Author *E-mail: [email protected]. *E-mail: [email protected]. Notes The authors declare no competing ﬁnancial interest. 

ACKNOWLEDGMENT


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This work was supported by the NSFC (21833010，21571178, 21525104, 21622101, 51502288), the Strategic Priority Research Program of Chinese Academy of Sciences (XDB20000000). S.Z. gratefully acknowledges funding support from Youth Innovation Promotion of CAS (2016274), NSF for Distinguished Young Scholars of Fujian Province (2016J06012),

and

Young

Elite

Scientists

Sponsorship

Program

by

CAST

(2017QNRC001). 

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For Table of Contents Use Only Physical Properties of a Promising Nonlinear Optical Crystal K3Ba3Li2Al4B6O20F Bingqing Zhao,†,

‡

Bingxuan Li †, Sangen Zhao,*,† Xitao Liu †, Zhenyue Wu,† Yaoguo

Shen,† Xianfeng Li,† Qingran Ding,† Chengmin Ji,† and Junhua Luo*,† A new nonlinear optical crystal K3Ba3Li2Al4B6O20F exhibits a high laser damage threshold up to 3.32 GW·cm-2 at the wavelength of 1064 nm, which even exceeds that of the commercial benchmark crystal β-BaB2O4 (2.6 GW·cm-2).


Physical Properties of a Promising Nonlinear Optical Crystal

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