Influence of the dentin surface properties on the laser radiation

absorption
Hana Chmelickova*a, Hana Sebestovaa, Helena Hiklovaa, Lenka Rihakovab
a
Institute of Physics of the Academy of Sciences of the Czech Republic, Joint Laboratory of Optics
of Palacky University and Institute of Physics of the Academy of Sciences of the Czech Republic,
17. listopadu 50a, Olomouc, 77207, Czech Republic;
b
Palacky University, RCPTM, Joint Laboratory of Optics of Palacky University and
Institute of Physics of the Academy of Sciences of the Czech Republic,
17. listopadu 50a, Olomouc, 77207, Czech Republic

ABSTRACT

Research of the optical radiation interaction with human tooth tissues has started early after the first laser construction.
Absorptivity of the particular tissue is dependent on the wavelength, thus CO2, Er:YAG and Nd:YAG lasers were used in
many experimental works all over the world. Near infrared radiation of the pulsed Nd:YAG laser was found to be
suitable for dentine hypersensitivity treatment by sealing of the open tubules with melted and re-solidified dentin. Series
of experiments were performed to find suitable process parameters in the laser laboratory equipped with the industrial
pulsed Nd:YAG laser system. Tooth samples were prepared and classified into five groups according to their different
degree of the surface grinding and polishing. Two types of antireflective agents, erythrosine and black ink, were applied
on the samples surfaces. Coated samples and reference ones without any agents were treated with a set of increasing
pulse energy values. Pulse frequency, pulse length, laser beam diameter on the sample surface and relative speed
remained constant. Lines of the melted spots were displayed by confocal microscope; surface profiles were scanned by
contact profilometer. Dimensions of the dentine melted spots were extracted from the measured data and their
dependence on the laser pulse energy, degree of the surface grinding and type of antireflective agent were evaluated.
Keywords: Dentin, Nd:YAG laser, Surface properties, antireflective agents

1. INTRODUCTION
Dental lasers are commercially manufactured and widely used in oral surgery to treat both soft and hard tissues. Soft
tissues (gingival, mucous membrane) absorb ultra-violet, visible and near infrared radiation (IR Diode lasers 808 nm –
980 nm, Nd:YAG laser 1064 nm) due to the content of pigments such as melanin and oxyhemoglobin. Mid infrared
radiation of Er:YAG (2940 nm) and Er,Cr:YSGG (2780 nm) lasers have the highest water absorption rate from any used
dental lasers and they are used for all tissues [1]. Wavelength of CO2 laser in far infrared region 10,600 nm is easily
absorbed in water and is widely used as a surgery scalpel. Dentine is hard tissue, creating bulk of the tooth. The main
structure is the dentinal tubule, which extends from the external surface to the pulp. Its walls are created by peri tubular
dentine, surrounded by inter tubular one. There are approximately 30,000 - 40,000 tubules per square millimeter, which
can transmit pain to the pulp if the dentine is exposed. Dentine consists of 70% inorganic material mainly composed by
calcium phosphate related to the hexagonal hydroxyl-apatite (Ca10(PO4)6·2(OH) and 30% organic as water, collagen and
mucopolysaccharine. Chemical composition of dentine and elements ratio were measured by Energy disperse
spectroscopy (EDS) [2] or by Differential thermal analysis (DTA) and Neutron activation analysis (NAA) [3] to
determine its composition both qualitatively and quantitatively. Optical properties and architecture of dentine are
discussed in many articles and thesis [4]. Dentine absorption coefficient depends on the radiation wavelength; in range of
near infrared region it reaches its minimal value. This property is successfully used in the selective treatment of the
caries that absorb near IR intensively.

*
hana.chmelickova@upol.cz; phone +420 585631516; fax +420 585631531

18th Czech-Polish-Slovak Optical Conference on Wave and Quantum Aspects of Contemporary Optics, edited by
Jan Perina Jr., Libor Nozka, Miroslav Hrabovský, Dagmar Senderáková, Waclaw Urbanczyk, Proc. of SPIE Vol. 8697,
86971C · © 2012 SPIE · CCC code: 0277-786/12/$18 · doi: 10.1117/12.2010260

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 Pulsed Nd:YAG laser have been used to reduce dentin permeability by melting effect with crystallization of inorganic
component and the coagulation of fluids contained into the dentinal tubules, reported in many experimental studies all
over the world [5]. Common goal is to find optimal process parameters for the individual laser equipment to achieve
compact remelted dentine layer without cracks and carbonization. Irradiated samples were viewed usually by scanning
electron microscopy (SEM) to find out morphological changes of dentine surface. Some studies extended analysis by
energy-dispersive spectrometry (EDS) for evaluation of the increasing concentration of calcium and phosphorous in the
melted layer [6]. The aim of our experimental work was to find the dependence of the laser radiation absorption on the
dentine surface roughness and the kind of the anti-reflexive agents. Laser scanning confocal microscope (LSCM) was
used for affected surface evaluation, because of no need of their additional preparation. In comparison to SEM, LSCM
doesn’t require conductive samples. Coordinates from surface profile were collected by contact profilometer (CPM),
from which various plane or spatial graphical outputs has been obtain by attached software tool.

2. EXPERIMENT
2.1 Preparation of the tooth samples
Extracted human molars were washed in alcohol, dried, longitudinally and horizontally fixed and mounted on two-
component resin Specifix in the special little moulds. After the resin hardening the samples were grinding consequently
by SiC papers with increasing granularity 80, 180 up to 2400, marked according European standard FEPA, where
granularity (mesh) is defined as fiber number per inch in the selecting sieve. Five groups of samples with different
roughness were prepared by stopping grinding on the value 180, 320, 600, 1200 and 2400 respectively. The last group
was afterwards polished by the diamond paste with the grain size 3 μm. Before laser treatment all samples were
controlled by laser scanning confocal microscope LEXT OLS 3100 to view open dentine tubule in the plane of
preparation (Figure 1). Dentine surface roughness was evaluated Ra (average arithmetic profile deviation) for all samples
with various surface treatment by contact profilometer TALYSURF. The un-exposed samples roughness decreased
naturally with increasing grinding papers granularity from Ra = 0.6 μm to 0.06 μm, polished surface has one order lower
Ra = 0.016 μm. The extracted human tooth root surface measured without any treatment has roughness Ra = 1.94 μm.

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Figure 1: Grinded tooth with reveal dentine (left), detail of the open tubules, 1200x magnification, black scale 30 μm (right).

2.2 Laser system arrangement

Pulsed flash pumped Nd:YAG laser LASAG KLS 246 -102 with wavelength 1064 nm is primary determined for middle
power applications. Processing parameters can be set to low values of the pulse energy 30 mJ – 300 mJ, frequency about
30 Hz and pulse length 0.3 ms, that correspond to the dental lasers with maximal power up to 10 W. Fixed processing
head with focus lens 100 mm stands above positioning table, guided by servomotors in axis X and Y, value of the table Z
coordinate is set by independent linear axis. Output beam from plan-parallel resonator has quality BPP (beam parameter
product) 18 mm.mrad in range of low powers with main intensity maximum in the centre of transversal electromagnetic
mode TEM20. Theoretical beam diameter in the focal plane is 0.6 mm. Because collimated beam or direct fiber output is

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 not available from our safety interlocked compact system as is usual in case of dental lasers, the first experiments were
realized with the aim to find optimal distance (stand off) of the sample surface from the processing head focal plane,
where the laser beam diameter extends to theoretical value about 0.85 mm, the intensity maximum is less sharp and pulse
energy surface density is sufficient enough for dentine melting, but not for tissue vaporization. Setup 5 mm seems to be
optimal stand off position for next experiments. Diameter of the melted laser spots reaches values from 0.5 mm to
0.6 mm. The CNC program was edited to move samples in 8 mm long lines in X axis, shifted by 0.3 mm in Y axis to
ensure at least 50 % overlap of two successive lines. Mutual motion of the XYZ table and samples was 3.6 mm.s-1, laser
spot overlap about 80 % was created in each line (Figure 2).

Figure 2: Laser spot overlapping in the motion direction and lines overlap on polished sample colored by black ink, exposed
by energy 100 mJ, magnification 120x, black scale 320 μm (left), photo-simulation of the complete sample (right) .

2.3 Influence of the antireflective agents

Graphs of the human various tissues absorption coefficient dependence on the radiation wavelength have been published
in the medical literature by many authors [7]. Dentine absorption coefficient is relatively high (104 cm-1) in ultraviolet
spectra region and for the wavelengths about 3 μm to 11 μm in the infrared region, contrary, minimum 0.1 cm-1 belongs
to the near infrared region 1 μm. Thus in praxis organic or inorganic agents are usually used to increase surface
absorptivity and laser energy coupling efficiency. We used two different dyes, mentioned in previous studies with
dentine sealing treatment, erythrosine and black ink [8]. Erythrosine is name for xanthenes dye 2-(6-Hydroxy-2,4,5,7-
tetraiodo-3-oxo-xanthen-9-yl) benzoic acid with formula C20H6I4Na2O5, also known as Acid Red 51 or food additive
E127, that is manufactured synthetically from cal tar. It is used in medicine as a dental plaque disclosing agent,
biological stain or a radiopaque medium. It is supplied and stored as maroon powder, soluble in water or ethanol [9].
After the application of 5% aqueous solution, pink red opaque layer covered tooth sample surface. The black ink is
commonly used medium for painting and drawing, it contains soot, binding agent and water.

2.4 Pulse energy optimization for samples of different surface roughness and color agents
The sequence of the prepared samples laser expositions was realized in laser system arrangement, described in section
2.2. Pulse energy was set by means of the flash lamp charging voltage on the lowest value 60 mJ and it was increased up
to 130 mJ with step 10 mJ. Related values of average power, peak power, energy density and peak power density are
4

outlined in Table 1. Presented energy values were read on the operator screen and they are measured by the built up
energy meter behind the output coupler in resonator. Sample surface was cooled by the week flow with compressed air.
A set of four laser traces 8 mm long and 50 % overlapped was applied across each sample surface with energy values
60 mJ, 70 mJ, 80 mJ, 90 mJ, 100 mJ and 110 mJ respectively for samples colored both by 5 % solution of erythrosine
and by black ink with goal to evaluate melted area dimension dependency on energy, kind of color agent and measure of
surface roughness. For un-coated samples exposition had to start at minimal value 100 mJ and set to 110 mJ, 120 mJ and
130 mJ respectively, because laser beam with lower energy was reflected or scattered from the sample surface.

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 Table 1. Process parameters overview of the laser treatment of the reveal dental tubules.

distance pulse pulse pulse beam energy average pulse peak peak power
of focus energy frequency length diameter density power power density
(mm) (mJ) (Hz) (ms) (mm) (J.mm-2) (W) (W) (W.mm-2)
5 60 30 0.3 0.85 0.106 1.80 200 352.7
5 70 30 0.3 0.85 0.124 2.10 233 425.9
5 80 30 0.3 0.85 0.141 2.40 267 470.8
5 90 30 0.3 0.85 0.159 2.70 300 529.0
5 100 30 0.3 0.85 0.177 3.00 333 587.2
5 110 30 0.3 0.85 0.195 3.33 367 647.1
5 120 30 0.3 0.85 0.212 3.60 400 705.3
5 130 30 0.3 0.85 0.230 3.90 433 763.5

3. RESULTS

3.1 Evaluation methods

All treated samples were inspected by the laser scanning confocal microscope LEXT OLS 3100 (LSCM) that enables,
beside other guaranteed possibilities [10], to record 2D images and 3D surface reconstruction both in real colors with
magnification (MGF) from 120x to 14,400x, , distances and areas measurement, profile extraction, etc. Laser spots and
lines were viewed in MGF 120x and MGF 480x to check up treated and un-treated regions and to measure dimensions of
melted spots. Morphology of the surface with re-solidified dentin granules was displayed in MGF 1200x. Representative
images for the black ink coated and 600 mesh SiC paper grinded sample are introduced on Figure 3. Longitudinal profile
in X axis was measured across lines of overlapped spots to evaluate roughness dependence on energy and initial surface
preparation (Table 2). Linear measurement in Y axis was made by CPM across whole exposed region to obtain
transversal profile of the re-solidified dentine tissue.

Figure 3: Real color image of the overlapped melted spots in two adjacent lines on 600 mesh grinded sample colored by
black ink, exposed by energy 80 mJ, MGF 480x, white scale 80 μm (left), black – white detail of the re-solidified dentine on
600 mesh grinded sample with 5 % erythrosine agent, exposed by energy 90 mJ, MGF 1200x, white scale 30 μm.

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 Table 2. Roughness of the exposed dentine surface black ink coated for set of pulse energy and initial surface treatment.

last SiC granularity 180 mesh 320 mesh 600 mesh 1200 mesh polished
Ra (μm), initial 0.6023 0.3039 0.2507 0.0607 0.0157
Ra (μm), E = 60 mJ 2.9157 1.3675 1.8620 2.5169 1.5554
Ra (μm), E = 70 mJ 2.9378 1.5430 2.9521 3.2286 3.0854
Ra (μm), E = 80 mJ 3.3094 3.1010 2.1171 3.5035 1.9554
Ra (μm), E = 90 mJ 5.1755 1.8550 3.8920 3.6542 2.0788

3.2 Pulse energy influence

Interval of suitable pulse energies to effective absorption of laser radiation and dentine melting without tissue
carbonization or un-treated areas was found only about tens of millijoules. Corresponding energy surface density for
used experiment arrangement belongs to range 0.103 J.mm-1 – 0.23 J.mm-1. Amount of the melted mass grooved
proportionally with energy independent of initial surface treatment and antireflective coatings. Contrast between laser
melted spot periphery with elevated mass and its inner area was observed to be deeper for the highest energy E = 90 mJ
then contrast for E = 60 mJ. Computations of maximal vertical difference were realized by means of LSCM software as
average of thirty longitudinal profiles across line of spots, created with one energy value. Tendency to difference
growing from 3.7 μm (Figure 4) to 6.9 μm Figure 5) was found. Diameter of the melted spots increased proportionally
with energy too, for instance from value 530 μm for E = 60 mJ to value 570 μm for E = 90 mJ in case of black ink
colored sample 320 mesh grinding, that means increment 7.5 %.

67.000 -

53.600 -

40.200 -

26.800 -

13.400 -

0 -000 , 1 1

0.000 128.000 256000 38.1000 512.000 640000

Figure 4: Longitudinal profile of line of spots exposed by E = 60 mJ (black ink colored, 320 mesh).

62 -000 -

49.600 -

37.200 -

24.800 -

12.00 -

II

0 -000 , 1-
0 .000 128.000 256000 38,1000 512.000 640.000

Figure 5: Longitudinal profile of line of spots exposed by E = 90 mJ (black ink colored, 320 mesh).

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 Depth of laser beam penetration depends on the pulse energy more significantly than on spot diameter, as it is seen on
the Figure 6, where transversal profile across black ink colored and 600 mesh SiC paper grinded sample is displayed
after exposition by set of energies 60 mJ, 70 mJ, 80 mJ and 90 mJ respectively. The thickness of ablated tissue increases
with energy pulse from approximately from 30 μm to 45 μm.

Nm Length = 6.6147 mm Pt= 66.752 pm Scale =70 pm

70 I I I

60 mJ 70 mJ 80 ml 90 mJ
60 -
50 -
40 -
30 -
20

10 -
0
0 0.5 1.5 25 3.5 4.5 5.5 6 6.5 mm

Figure 6: Transversal profile across sample exposed by set of pulse energy (black ink colored, 600 mesh).

3.3 Antireflective agents coatings influence

Both 5% solution of erythrosine and black ink increased surface absorption, continuous dentine melting without local
untreated areas has started with energy 60 mJ in case of all samples up to grinding 1200 mesh. But in case of polished
surface, melting process had to start with higher energy 80 mJ to give comparable results with that of grinded surfaces.
Depths of ablated tissue were measured and transversal profiles were compared for two samples with the same level of
grinding but different kind of the antireflective agent (Figure 7). It was found out, that depth of ablated tissue on 5%
solution of erythrosine coated sample is approximately 22 μm – 28 μm that is less, than for the black ink that probably
absorbs laser radiation more efficiently. In case of un-coated samples, precise horizontal position, focus stand-off and
individual tooth physical properties seemed to be critical parameters for uniform dentine melting, that was achieved only
for sample 320 mesh with pulse energy 120 mJ. In other cases, absorption occurred randomly on impurities and edges or
craters with diameter about 70 μm and depth 30 μm were drilled in dentine, as is seen on the spatial reconstruction of the
segment of the un-coated polished sample, which was exposed by energy 130 mJ (Figure 8).
O
o
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Depth of the ablated tissue [um]
Depth of the ablated tissue [um]

O
o
A

A
W
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o
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N

N
O
O

O
CO
Ol
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Figure 7: Depth of the ablated tissue dependence on the pulse energy for 5% solution of erythrosine coated sample
600 mesh, (left) and black ink coated, 600 mesh (right).

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 z

06's um

wn000'0 056'ZZ

LS 00Z'
00P'Z0L wn000'Z6L
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Figure 8: Spatial reconstruction of the drilled craters in dentine of polished un-coated sample and energy 130 mJ.

3.4 Degree of surface treatment influence

Tooth samples are prepared to laser treatment usually by cutting both in horizontal or vertical direction to obtain planes
with open tubules. Surface roughness depends on used cutting tool. Our methods of grinding along lateral tooth side
enabled to prepare samples with different roughness. Laser radiation absorption could be then investigated in dependence
on the measure of initial surface roughness. Our hypothesis was that the laser radiation absorption would be highly
dependent on the sample surface roughness. But this hypothesis was not confirmed. Laser radiation with energy in the
range from 60 mJ to 90 mJ was reflected or scattered from all un-coated dentin surface with every level of grinding.
Even after the increase in energy up to 130 mJ any significant changes were not observed. Only on 320 mesh grinded
sample partial absorption of radiation with energy in the range from 100 mJ to 130 mJ was present. Experiments on
grinded samples with the anti-reflective agent of the same kind but different degree of grinding revealed that uniform
melting occurred for all samples exposed by minimal energy 60 mJ independently on the degree of surface treatment.
Polished coated samples showed different morphology. Exposition by energy 60 mJ was not sufficient to uniform
melting of hydroxyapatite. Some areas of melted and re-solidified dentin were observed on polished sample with 5 %
erythrosine. Neither energy 70 mJ was sufficient for uniform melting on polished samples which occurred after
exposition by energy up to 80 mJ (Figure 9). These observations showed that measure of surface roughness did not
influence the laser radiation absorption as hard as the surface application of dyes that is the critical parameter for laser
absorption.

Alpha = lgg° Beta = .13°

Figure 9: 3D continuous axonometric imaging of the section of polished black ink-coated sample, exposed with set of pulse
energies 70 mJ, 80 mJ, 90 mJ and 100 mJ respectively.

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 4. CONCLUSION
Laser near infrared radiation interaction with dentine tissue was realized by means of pulsed Nd:YAG laser with goal to
find a range of suitable parameters for dentine melting and its following re-solidification to continuous layer, that sealed
opening of dentine tubules on the tooth root surface. This method is used in dentistry for the treatment of dentine
hypersensitivity with special dental lasers [11]. Arrangement of our experiments was determined by the technical
condition of industrial laser system available in the laboratory that is equipped with computer control XYZ position table
and fixed processing laser head. Set of samples with different surface roughness at lateral tooth plane were prepared by
grinding machine with values of the average arithmetic profile deviation Ra from 0.6 μm to 0.016 μm. Occurrence of the
open dentine tubules were controlled by means of the laser scanning confocal microscope. Two types of the
antireflective agents were applied on the sample surfaces to increase absorption of the laser radiation, the first group with
5 % solution of Erythrosine, the second one with black ink, the third control group remained un-coated. Lines of
overlapped laser spots were created on the tooth surface with set of pulse energies from 60 mJ to 130 mJ. The minimal
value of pulse energy was found for each combination of the surface treatment and type of the coating to create
continuous dentine melting. In case of the samples coated by both antireflective agents, pulse energy 60 mJ was
sufficient for melting surfaces with Ra = 0.6 μm to 0.06 μm, higher minimal energy 80 mJ had to be used for polished
samples with Ra = 0.016 μm. Irradiation of the samples from third un-coated group had to started with energy 100 mJ,
due to higher surface reflection, but successfully melting was obtain only in case of the un-polished samples. It was
found, that application of the antireflective agents on the dentine surface is more critical parameter than measure of
surface grinding, because surface of human tooth in the normal physiological stage has always higher roughness that our
samples and a polishing is not used before dentin sensitivity treatment in medical praxes.

ACKNOWLEDGEMENTS

The authors gratefully acknowledge the support of the Technology Agency of the Czech Republic Project No.
TA01010517 “Moderní multivrstvé optické systémy”.

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