CrystEngComm

View Article Online

PAPER View Journal | View Issue

The rapid growth of ADP single crystal

Cite this: CrystEngComm, 2016, 18,
Yafei Lian,†ab Lili Zhu,†d Tingting Sui,ab Guangwei Yu,ab Lisong Zhang,ab
Hailiang Zhou,c Mingxia Xu*ab and Xun Sun*ab
Published on 22 August 2016. Downloaded by Anna University on 16/11/2016 10:02:15.

7530

Ammonium dihydrogen phosphate (NH4HPO4, ADP) crystal can be used to generate second, third and
fourth harmonics. In this paper, the growth characteristics of ADP and the differences between the growth
solubility and structures of potassium dihydrogen phosphate (KDP) and ADP crystal are discussed in detail.
Received 4th July 2016, Ex situ atomic force microscopy (AFM) was applied to explore the growth morphology of ADP crystal at
Accepted 22nd August 2016
different supersaturation values. A series of ADP crystals were grown, and the transmission spectra of ADP
crystals across the whole transmission region were measured. Laser-induced damage threshold (LDT) was
DOI: 10.1039/c6ce01492e
measured, and was found to be higher than the average value of LDT of KDP and 70% deuterated DKDP
www.rsc.org/crystengcomm crystals.

1. Introduction cations, for example as a material for generating third and

fourth harmonics.
Ammonium dihydrogen phosphate (NH4HPO4, ADP) crystal is In recent years, much has been achieved regarding the
one of the most promising media for frequency conversion of rapid growth of KDP crystals, especially in the aspects of in-
Nd-laser radiation by third or fourth harmonic generation ow- creasing the growth rate and improving crystal quality.4–7,12
ing to its large nonlinear optical (NLO) coefficient, high trans- For ADP crystal, the work that has already been done has
mittance and high laser damage threshold (LDT).1–3 Like the mainly focused on the chemical structures, the microcosmic
isomorphs of potassium dihydrogen phosphate (KDP) crys- dynamics, and organic derivatives such as amino acid- and
tals, which could be grown in a relatively short period and EDTA-doped crystals.8–11,13–20 In 1983, Amandosov et al. grew
with a large size by the technique of point-seed rapid ADP crystals by point-seed rapid growth with a growth rate of
growth,4–7 ADP crystals are isomorphs of KDP in many re- ∼1 cm per day and found the required quality accessible in
spects, such as the crystal structures and their growth many situations.11 The influences of stirring velocity, pH value
regulation.8–10 Therefore, the rapid growth technique can be and temperature of the growth solution on the growth rate of
well employed in the growth of ADP crystals.1,11 Compared ADP crystals were studied by Wang Ximin et al. with regards to
with KDP and DKDP crystals, ADP has a larger NLO coeffi- the decrease in thickness of solute boundary layer and the in-
cient and LDT, and a shorter UV transmission cut-off. crease in “reaction rate” of crystal surface growth.15 Xu Dongli
According to Ji et al.,3 the conversion efficiency, the output and Xue Dongfeng et al. researched the chemical bonding of
energy and the angular bandwidth of the fourth harmonic ADP and predicted that the natural shape was a tetragonal bi-
generation of the ADP crystal are superior to those of deuter- pyramid,16 and they then studied the morphology and struc-
ated KDP (DKDP) crystals. Moreover, ADP crystals have better ture of KDP and ADP crystallites in water and ethanol solu-
homogeneity and lower production cost than DKDP crystals. tions.9 R. J. Davey and J. W. Mullin tested the effect of
Thus, ADP crystal shows promise for use in engineering appli- supersaturation on growth feathers on the {100} faces of ADP
crystals17 and Yu et al. of Chongqing University studied 2D
nucleation in the {100} faces of ADP.18 Shaohua Ji et al. grew
some ADP crystals and a series of deuterated ADP (DADP)
a
crystals and reported their noncritical phase-matching fourth
State Key Laboratory of Crystal Materials, Shandong University, Jinan 250100,
PR China. E-mail: [email protected]; Fax: +86 53188365200;
harmonic generation.19 Xi Feng et al. used the ADP pyramid
Tel: +86 53188365200 as the seed instead of the Z-cut plate and achieved the growth
b
Ministry of Education, Key Laboratory of Functional Crystal Materials and of relatively large-sized ADP crystals.20 In this work, the differ-
Device (Shandong University), Jinan 250100, PR China ences in growth solubility, structures and the microcosmic
c
School of Information Science and Engineering, Shandong Agricultural
growth between KDP and ADP crystals were compared. A se-
University, Taian 271018, PR China
d
School of Materials science and Engineering, Shandong Jiaotong University,
ries of ADP crystals were grown. Transmission spectra and
Jinan 250300, PR China laser-induced damage threshold (LDT) of the ADP crystals
† These authors contributed equally to this work. were measured.

7530 | CrystEngComm, 2016, 18, 7530–7536 This journal is © The Royal Society of Chemistry 2016
 View Article Online

CrystEngComm Paper

2. Experimental Table 1 Content of the main metal ion impurities in different raw mate-
rials (ppm)
Two crystals of ADP and KDP were grown under the same
Raw material Fe Cu Na Cr Mg Pb Co
conditions by the temperature reduction method, as shown
in Fig. 1. It was found that the aspect ratio (Z/X) of KDP was A 43.3 1.5 2.2 3.1 0.9 0.002 0.002
B 0.017 — 0.01 0.01 0.001 0.08 0.11
obviously larger than that of ADP. Like the isomorphs of KDP
crystals, ADP has similar crystal structure and chemical bond
distribution, while there are some differences between them, cused by a lens with f = 5 m through a face into the bulk
including the solubility, the growth structures and the growth of the crystal. The image of the bulk damage region was
micro-morphology. Ex situ atomic force microscopy (AFM) captured orthogonally to the direction of laser propagation
measurements were implemented to explore the growth by three CCD cameras, through the input surface, the body
Published on 22 August 2016. Downloaded by Anna University on 16/11/2016 10:02:15.

micro-morphology using a Bruker Dimension Icon Scanning and the output surface of the samples. Laser-induced dam-
Probe Microscope (SPM) system in ScanAsyst mode with stan- age was investigated by the R-on-1 approach.
dard SiN cantilevers.21 ADP crystal samples were grown from
solutions at different supersaturation values and used for
AFM characterization. 3. Results and discussion
In order to explore the influence of growth conditions on 3.1. Growth differences between KDP and ADP
ADP crystals, raw materials A and B were selected to grow 3.1.1 Growth solubility. The solubility of solute is the most
ADP crystals from aqueous solution in a 5000 ml crystallizer fundamental parameter for the growth of crystals in aqueous
by the temperature reduction method;4,11,12 the main metal solutions. The following expressions for the solubility of ADP
ion impurities in different materials are shown in Table 1. (formula 1) and KDP (formula 2) are usually used:1
Then, raw material B was selected to grow large-scale ADP, as
discussed below. ln m = 36.422 − 3370.284/T − 4.901 ln T (1)
We measured the transmission spectra of ADP crystals
grown at different temperatures and by different growth c = 0.00602t 2 + 0.208t + 15.9 (2)
methods. The samples were cut in the pyramidal or prismatic
sectors as shown in Fig. 2, with Z-axis cutting (θ = 0, Φ = 0) where m is the mole fraction of ADP, T is the thermodynamic
and a size of 10 mm × 10 mm × 10 mm. All samples were ori- temperature (K), c is the solubility (grams of solute/100 grams
ented by X-ray orientation and polished on the faces to be il- of solvent) and t is the Celsius temperature (°C).
luminated. They were tested by Hitachi U-3500 spectrograph Thus, compared with KDP crystal, it is necessary to reduce
with a test band of 200–2000 nm. the cooling rate in the process appropriately to guarantee the
Then the LDT values of ADP crystals were measured. normal growth of ADP crystal.
Two type-II frequency tripling (θ = 59°, Φ = 90°) samples of 3.1.2 Growth structures. The crystal structures of KDP and
rapid-growth ADP crystal were chosen, as shown in Fig. 3. ADP are shown in Fig. 5.
The experimental scheme22,23 for the measurement of laser- Lattice parameters of ADP and KDP crystals are shown in
induced damage threshold is shown in Fig. 4. The laser- Table 2.1
induced damage threshold was measured using the third There are three kinds of chemical bonds formed among
harmonic of a Q-switch Nd:YAG laser (0.355 μm). The laser, all the crystallization processes for KDP and ADP
with area 0.22 mm2, was operated at a repetition rate of 1 crystal,8,24–27 i.e., α, β and γ. Thus, based on first principles,
Hz with a pulse width of 7.4 ns. The harmonics were fo- transmission spectra of the samples of raw material B)28 were
employed to examine their distributions. The general gradi-
ent approximation (GGA) of Perdew, Burke, and Ernzerhof
(PBE) was employed. The core and valence electrons were

Fig. 1 The ADP (left) and KDP (right) crystals grown under the same
conditions. Fig. 2 Crystal sample position for transmittance test.

This journal is © The Royal Society of Chemistry 2016 CrystEngComm, 2016, 18, 7530–7536 | 7531
 View Article Online

Paper CrystEngComm

treated with ultrasoft pseudopotentials and shifted 4 × 4 × 4

Monkhorst–Pack29 meshes were used in this study. The
charge density and the chemical bonds of KDP and ADP are
shown in Fig. 6.
The first type of chemical bond in KDP is the K–O ionic
bond, which is made between O in the PO4 tetrahedron and
K+ in the face center of the ab faces, and its bond length is
about 2.897 Å, while that in ADP is the H(N)–O covalent bond,
which is between O in the PO4 tetrahedron and H of NH4+ in
Fig. 3 The positions of the ADP crystal samples for laser-induced the face center of ab faces, and its bond length is 2.650
damage threshold test.
Å.24–27 They constitute the α-bond chain, with their bond di-
Published on 22 August 2016. Downloaded by Anna University on 16/11/2016 10:02:15.

rections both practically parallel to the c-axis. Although the

H(N)–O bond is slightly shorter than the K–O bond, the bind-
ing energy of the ionic bond is always greater than that of
the covalent bond. Therefore, the bond strength along the
c-axis in KDP is higher than that of ADP. The second kind of
chemical bond, namely the β bond, still corresponds to the
K–O ionic bond, with bond length of 2.824 Å, and the H(N)–O
covalent bond, of about 1.956 Å,24–27 except for the difference
that the K–O bond is formed between O in the PO4 tetrahe-
dron and K+ in the ac or bc face, and the H(N)–O bond is
formed between O in the PO4 tetrahedron and H of NH4+ in
Fig. 4 Experimental setup for the measurement of laser-induced the ac or bc face. The direction of the β bond chain that they
damage threshold of crystals. form is perpendicular to the c-axis. Finally, the third kind of
bond, the γ bond, is H(O)⋯O between PO4 tetrahedrons, and
is remarkably similar in the two isomorphs, i.e. the bond
number, length and strength, as well as the bond direction,
are approximately same.
Although three kinds of chemical bonds exist in KDP and
ADP crystals, only the weaker chemical bonds formed in the
crystallization process have a dominant influence on the crys-
tal growth.25 There are ionic and hydrogen bonds in KDP
crystal, and the strength of the ionic bond is greater than
that of the hydrogen bond, leading to a high aspect ratio.

Fig. 5 Crystal structures of KDP and ADP (some hydrogen atoms of

ADP are omitted for clarity).

Table 2 Lattice parameters of ADP and KDP crystals

a, b (Å) c (Å) Radius (Å)

KDP 7.453 6.972 K+ = 1.330 Fig. 6 The charge density of KDP (top) and ADP (bottom) crystals and
ADP 7.502 7.546 NH4+ = 1.420 the chemical bonds are shown.

7532 | CrystEngComm, 2016, 18, 7530–7536 This journal is © The Royal Society of Chemistry 2016
 View Article Online

CrystEngComm Paper

However, the H(N)–O covalent bond shows a lower strength

than the hydrogen bond in ADP. That is, only weak hydrogen
bonds exist in ADP crystals, which will result in a weak
constraining force between growth units; the weak
constraining force will lead to a slow growth rate and a small
aspect ratio at the same supersaturation.
3.1.3 Growth micro-morphology. Ex situ AFM images of
the (100) face of ADP crystals grown at different supersatura-
tion values are shown in Fig. 7. As shown in Fig. 7, it is found
that there are two kinds of mechanisms for ADP growth,
namely spiral step growth and 2D nucleation. There is only
Published on 22 August 2016. Downloaded by Anna University on 16/11/2016 10:02:15.

step growth at the supersaturation value of 0.004, as shown Fig. 8 Crystals made using different raw materials and growth
in Fig. 7(a). 2D nucleation appears at the supersaturation of temperatures. No macroscopic defects exist in crystals 1 and 5–7.
There are some macroscopic inclusions in crystals 2–4, as their raw
0.006, as is shown in Fig. 7(b). At the supersaturation of
material contains some ionic impurities.
0.008, 2D nucleation occurs with the typical topology shown
in Fig. 7(c).
The average height of the basic step as shown in Fig. 7(a)
is about 0.342 nm, equal to half of the height of the unit cell. the cylindrical surface. On the one hand, the ion impurity con-
And in Fig. 7(b) the macro-step height ranges from 1.30 nm tent of raw material A is much higher than that of B and the
to 3.27 nm, namely two to four layers of the unit cell. The ter- impurities can impede the expansion of the growth steps; on
race width is much larger than the step height. Thus, ADP the other hand, the inclusions easily occur with a large super-
crystal tends to have a lower aspect ratio than KDP under the saturation as a result of temperature reduction. That is, as the
same growth conditions. The typical topology of 2D nucle- growth steps can bypass the restraint of ion impurities and
ation with a platform area of about 0.09 μm2 is shown in continue to grow, they will encapsulate the ion impurities and
Fig. 7(c) and the height of the step is about 0.367 nm. solution, forming the defect of impurity inclusions in the
However, according to Bing Liu et al.,30 below the super- growth process of crystals 2–4. Crystals 1 and 5 have a slightly
saturation of 0.01, KDP is in the “dead zone” in which the lower aspect ratio than the others and, as the growth tempera-
crystal does not grow. Thus, compared with KDP crystal, ADP ture decreases, the aspect ratio of the crystals tends to increase
expands much more easily in the [001] direction at low gradually. Therefore, higher purity, an appropriate decreasing
supersaturation. of the temperature reduction rate, and a suitable choice of
growth temperature and supersaturation can lead to much
more stable growth and higher quality of a single crystal.
3.2. The rapid growth of ADP crystals A larger ADP crystal was then grown. This crystal is shown
ADP crystals formed by point-seed rapid growth from differ- in Fig. 9 and the growth parameters are in Table 4. The
ent ADP raw materials and at different growth temperatures growth experiments show that the extension of the crystal
are shown in Fig. 8 and described in Table 3. faces in all directions is easily realized at a lower supersatura-
As shown in Fig. 8, no macroscopic defects exist in crystals tion in the rapid growth process of ADP. In addition, the
1 and 5–7, whereas there are some macroscopic inclusions in experiments described below in this article show that the
crystals 2–4, because raw material B contains only low levels ADP crystals of rapid growth have good optical homogeneity;
of ion impurities, such as Fe, Cr and Co at less than 0.02 thus the rapid growth of larger-scale ADP is promising and
ppm, which can lead to inhibition of the normal growth of realizable.

Fig. 7 Ex situ AFM topology of (100) face of ADP crystal. (a) Only step growth occurs at the supersaturation value of 0.004. (b) Step growth and
2D nucleation at the supersaturation of 0.006. (c) 2D nucleation at the supersaturation of 0.008.

This journal is © The Royal Society of Chemistry 2016 CrystEngComm, 2016, 18, 7530–7536 | 7533
 View Article Online

Paper CrystEngComm

Table 3 Growth parameters of ADP crystals formed from different raw

materials by point-seed technique

Crystal Raw Seed Temperature reduction Crystal size

no. material type range (°C) (mm)
1 A Point 54.2–50.5 45 × 43 × 53
2 A Point 50.9–48.6 39 × 36 × 49
3 A Point 47.3–41.4 47 × 48 × 70
4 A Point 40.6–30.5 46 × 46 × 85
5 B Point 52.9–50.1 50 × 43 × 54
6 B Point 49.3–45.1 49 × 43 × 62
7 B Point 45.2–40.3 47 × 33 × 53
8 B Point 42.0–36.5 50 × 47 × 55
Published on 22 August 2016. Downloaded by Anna University on 16/11/2016 10:02:15.

Fig. 10 Transmission spectra of ADP crystals grown under different

growth temperatures and of KDP crystal. (a) Prismatic sector, (b)
pyramidal sector.
Fig. 9 ADP crystal with 110 mm size grown by point-seed technique.

3.3. Optical quality two sectors in the other regions are similar, almost
3.3.1 Transmission spectra overlapping. That is, all the transmission spectra of the pyra-
Transmission spectra of ADP crystals with different growth midal sector are superior to those of the prismatic sector, es-
temperatures. As indicated above, macroscopic defects existed pecially in the UV region, as metallic impurities have much
in the samples of raw material A. Thus, transmission spectra more influence on the prismatic sector. This suggests that, as
of the samples of raw material B, namely crystals 5–8, were the growth temperature decreases, metallic impurities in the
investigated; the results are shown in Fig. 10. solution can more easily enter into the prismatic sector,
Compared with the transmission spectrum of KDP crystal, influencing the UV transmission. Furthermore, the defects in
as regards either the prismatic sector or the pyramidal sector, the crystals can also lead to a decrease of UV transmission.
ADP shows a similar behaviour except for the absorption peak As shown in Fig. 10(a), the transmission spectrum of sample
in the near-infrared region. This absorption peak, which is a III is abnormally decreased, as a result of the defects existing
multiple frequency peak, is caused by the vibration of the in the prismatic sector.
N–H group as shown in Fig. 11. The absorption peak in the Transmission spectra of ADP crystals grown by different
transmission spectrum appears at a wave number of about methods. Transmission spectra of ADP crystals grown from
9354.53 cm−1, while that in the near-infrared (NIR) spectrum the especially pure raw material B by traditional and rapid
appears at 9331.62 cm−1. Therefore, they are consistent. growth methods are shown in Fig. 12. As shown in the figure,
The growth temperature of samples from 5 to 8 decreases the transmission spectrum of ADP grown by the traditional
gradually. The comparison results of the prismatic sector are method in the whole transmission region is a little higher
shown in Fig. 10(a), and those of the pyramidal sector are than that for ADP grown by the rapid growth method,
shown in Fig. 10(b). With the decrease of the growth temper- especially in the UV and NIR regions.
ature, the transmission spectrum of the prismatic sector in The two samples were both cut from the prismatic sector
the UV region declines, while that of the pyramidal sector and adsorption due to metallic impurities can cause a de-
shows no obvious change. The transmission spectra of the crease of UV transmission. Under normal conditions, the
surface [PO4]3− groups are covered with [NH4]+, whereas with
metallic impurities such as Fe+ adsorbed, because of their
Table 4 Growth parameters of medium-sized ADP crystal made by different charge and radius, distortion and defects of crystal-
point-seed technique
line structure appear when they occupy the same positions.
Temperature As the cooling rate of the traditional method is very slow, the
reduction Growth Crystal crystal only expands in the [001] direction, which is beneficial
No. range (°C) period (day) weight (g) Crystal size (mm) for the units in the crystals to occupy exact positions. How-
12 53.7–47.8 26 1752.4 124 × 112 × 92 ever, in the rapid method the crystals have a high growth rate

7534 | CrystEngComm, 2016, 18, 7530–7536 This journal is © The Royal Society of Chemistry 2016
 View Article Online

CrystEngComm Paper

4. Conclusions
In this paper, differences between growth characteristics of
KDP and ADP have been discussed. It can be seen that the solu-
bility of ADP in aqueous solution is nearly twice that of KDP.
The bond energy of the chemical bond along the c-axis of ADP
is smaller than that of the bond perpendicular to the c-axis.
This will result in a weak constraining force between growth
units along the c-axis, a slow growth velocity and a lower aspect
ratio, as evidenced by the ex situ AFM topology of the (100) face
of ADP crystal at different supersaturation values and the
Fig. 11 Near-infrared spectrum of ADP crystal. The vibration peaks
Published on 22 August 2016. Downloaded by Anna University on 16/11/2016 10:02:15.

appear at 9331.62 cm−1 and 7706.29 cm−1. They are both multiple
growth of a series of small-scale ADP crystals. Transmission
frequency peaks caused by the vibration of the N–H group. spectra of ADP crystals grown by the rapid growth method are a
little lower over the whole transmission region than those of
ADP crystals grown by the traditional growth method, especially
in the UV and NIR regions. The LDT is higher than the average
value of LDT for 70%-deuterated DKDP crystal, which has been
widely used for third harmonic generation, and for KDP crystal.
The reason why the LDT of ADP is higher than that of KDP and
DKDP will be discussed in other articles.

Acknowledgements
Financial support came from the National Natural Science
Foundation of China (Grants No. 51323002 and 51402173),
Fig. 12 Transmission spectra of ADP crystals grown by different the Ministry of Education (Grant No. 625010360), the Natural
methods. Science Foundation for Distinguished Young Scholar of Shan-
dong Province (2012JQ18), and the Fundamental Research
Funds of Shandong University (2015GN027).
and can expand not only in the [001] direction, but also in
the [100] direction, in which condition lattice defects and in-
clusions can easily appear. Notes and references
3.3.2 Laser induced damage threshold. Table 5 shows LDT 1 L. N. Rashkovich, KDP-family single crystal, Published under
values and sample information. As is well known, the absorp- the Adam Hilger imprint by IOP Publishing Ltd, 1991.
tion of laser energy by damage precursors such as impurities 2 D. N. Nikogosyan, Nonlinear Optical Crystals: A Complete
and defects can cause the local melting of materials; thus de- Survey, Springer, Cork, Ireland, 2001.
formation appears in the surrounding regions, as a result of 3 S. Ji, F. Wang, L. Zhu, X. Xu, Z. Wang and X. Sun, Non-
fracture. As shown in Table 5, the LDT of R-1 was far higher critical phase-matching fourth harmonic generation of a
than that of R-2. There were no visible macroscopic defects 1053-nm laser in an ADP crystal, Sci. Rep., 2013, 3, 1605.
and inclusions in sample R-1, while there was an inclusion 4 J. J. De Yoreo, A. K. Burnham and P. K. Whitman,
which can affect the quality of crystals beside the cutting po- Developing KH2PO4 and KD2PO4 crystals for the world's
sition of sample R-2, where the LDT is far lower than the nor- most powerful laser, Int. Mater. Rev., 2002, 47, 113–152.
mal value. Although the LDT of R-2 is low, it is still higher 5 W. Han, et al., Evaluating the safe limit of large-aperture po-
than the average value of LDT of 70%-deuterated DKDP crys- tassium dihydrogen phosphate crystals associated with
tal, which has been widely used for third harmonic genera- transverse stimulated Raman scattering, Appl. Opt., 2015, 54,
tion. The reason why the LDT of ADP is higher than that of 4167–4171.
KDP and DKDP will be discussed in other articles. 6 L. A. Guzman, M. Suzuki, Y. Fujimoto and K. Fujioka, Habit
control of deuterated potassium dihydrogen phosphate
Table 5 The 3ω laser damage thresholds (LDT) of the ADP frequency crystal for laser applications, J. Phys.: Conf. Ser., 2016, 688,
triplers compared with KDP and DKDP 012024.
7 H. Yin, M. Li, C. Zhou and J. Song, KDP single crystal
Normalization LDT
growth via three-dimensional motion growth method, Cryst.
LDT (J cm−2, 7.4 ns) (J cm−2, 3 ns)
Res. Technol., 2016, 51, 491–497.
KDP 4.8 3.0
8 D. Xu and D. Xue, Chemical bond analysis of the crystal
R-1 35.4 19.4
R-2 6.7 4.3 growth of KDP and ADP, J. Cryst. Growth, 2006, 286,
70% DKDP 6.3 3.95 108–113.

This journal is © The Royal Society of Chemistry 2016 CrystEngComm, 2016, 18, 7530–7536 | 7535
 View Article Online

Paper CrystEngComm

9 D. Xu, D. Xue and H. Ratajczak, Morphology and structure 19 S. Ji, et al., Room temperature, high-efficiency, noncritical
studies of KDP and ADP crystallites in the water and ethanol phase-matching fourth harmonic generation in partially deu-
solutions, J. Mol. Struct., 2005, 740, 37–45. terated ADP crystal, Opt. Lett., 2013, 38, 1679–1681.
10 P. Rajesh, P. Ramasamy and G. Bhagavannarayana, Growth 20 X. Feng and L. Zhu, et al., Growth and highly efficient third
of ADP–KDP mixed crystal and its optical, mechanical, harmonic generation of ammonium dihydrogen phosphate
dielectric, Piezoelectric and laser damage threshold studies, crystals, RSC Adv., 2016, 6, 33983–33989.
J. Cryst. Growth, 2013, 362, 338–342. 21 F. Liu, et al., Effect of supersaturation on hillock of
11 A. T. Amandosov, Z. S. Pashina and L. N. Rashkovich, directional Growth of KDP crystals, Sci. Rep., 2014, 4, 6886.
Quality of ADP crystals formed by rapid growth from a point- 22 M. Xu, X. Sun and Z. Wang, et al., Laser-induced damage of
like seed, Quantum Electron., 1983, 13, 271–272. DKDP crystal under different wavelengths, Cryst. Res.
12 Z. Xinxin, Y. Wang, Z. Guozong, S. Genbo, H. Youpin, L. Technol., 2010, 45, 763–766.
Published on 22 August 2016. Downloaded by Anna University on 16/11/2016 10:02:15.

Xiuqin and X. Zhihuang, The rapid growth of large-scale 23 B. Liu, G. Hu, Y. Zhao, M. Xu, S. Ji, L. Zhu, L. Zhang, X. Sun,
KDP single crystal in brief procedure, J. Cryst. Growth, Z. Wang and X. Xu, Laser induced damage of DKDP crystals
2011, 318, 700–702. with different deuterated degrees, Opt. Laser Technol.,
13 Z. Li, X. Huang, D. Wu and K. Xiong, Large crystal growth 2013, 45, 469–472.
and measurement of electro-optical coefficients of ADP, 24 D. Xue and H. Ratajczak, Effect of hydrogen bonds on
J. Cryst. Growth, 2001, 222, 524–527. physical properties of ammonium dihydrogen phosphate
14 M. Meena and C. K. Mahadevan, Growth and electrical crystals, J. Mol. Struct.: THEOCHEM, 2005, 716, 207–210.
characterization of L-arginine added KDP and ADP single 25 D. Xu and D. Xue, Chemical bond analysis of the crystal
crystals, Cryst. Res. Technol., 2008, 43, 166–172. growth of KDP and ADP, J. Cryst. Growth, 2006, 286,
15 X. Wang, S. Xu and K. Zhang, Study on rapid growth and 108–113.
related properties of ADP crystals, Rengong Jingti Xuebao, 26 L. Tenzer and B. C. Frazer, A Neutron Structure Analysis of
1994, 23, 33–38. Tetragonal NH4H2P04, Acta Crystallogr., 1958, 11, 505–509.
16 D. Xu and D. Xue, Chemical bond and microscopic growth 27 C. Sun and D. Xue, Hydrogen bonding nature during ADP
habit of ADP crystals, Rengong Jingti Xuebao, 2005, 34, crystallization, J. Mol. Struct., 2014, 1059, 338–342.
823–827. 28 G. Kresse and J. Furthmüller, Efficient iterative schemes for
17 R. J. Davey and J. W. Mullin, The effect of supersaturation ab initio total-energy calculations using a plane-wave basis
on growth feathers on the {100} faces of ammonium set, Phys. Rev. B: Condens. Matter Mater. Phys., 1996, 54,
dihydrogen phosphate crystals, J. Cryst. Growth, 1975, 29, 11169.
45–48. 29 H. J. Monkhorst and J. D. Pack, Special points for Brillouin-
18 J. Yu, M. Li and X. Wang, {100} surface topography under 2D zone integrations, Phys. Rev. B: Solid State, 1976, 13, 5188.
nucleation growth of ADP crystals: ex situ investigation by 30 B. Liu, et al., Measurement of growth kinetics of KDP
atomic force microscopy, Gongneng Cailiao, 2008, 39, prismatic faces with laser-polarization-interference tech-
1034–1036. nique, Qiangjiguang Yu Lizishu, 2008, 20, 1283–1287.

7536 | CrystEngComm, 2016, 18, 7530–7536 This journal is © The Royal Society of Chemistry 2016