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Temporary 3D printed fixed dental prosthesis materials: Impact of post printing

cleaning methods on degree of conversion as well as surface and mechanical

properties

Johannes Mayera, Marcel Reymus Dr. b, Felicitas Wiedenmann Dr. a, Daniel Edelhoff

Prof. Dr. a, Reinhard Hickel Prof. Dr. b, Bogna Stawarczyk Prof. Dr. Dipl. Ing (FH).

MSc a

a
Department of Prosthetic Dentistry, University Hospital, LMU Munich,

Goethestrasse 70, 80336 Munich, Germany

b
Department of Conservative Dentistry and Periodontology, University Hospital, LMU

Munich, Goethestrasse 70, 80336 Munich, Germany

Corresponding author:

Johannes Mayer

Department of Prosthetic Dentistry, University Hospital, LMU Munich

Goethestrasse 70

80336 Munich, Germany

+4917634496272

johannes_mayer@live.de

Submitted April 3, 2020; accepted February 3, 2021

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Abstract

Purpose: To investigate the influence of different cleaning methods for additively

manufactured fixed dental prostheses (FDPs) for long-term temporary use on the

degree of conversion (DC), surface roughness, Martens parameters, and biaxial

flexural strength. Materials and Methods: A total of 180 specimens per material

(3Delta Etemp, DeltaMed; Freeprint Temp, Detax; Temp PRINT, GC Europe; Temp

C&B and C&B MFH, NextDent; N = 180) were additively manufactured (D20 II,

Rapid Shape) and subsequently cleaned by different methods: by rinsing for 5

minutes in acetone (Höfer Chemie; 99.5%); butyl glycol (Algin Chemie; 100%);

ethanol (Otto Fischar; 96%); isopropanol (SAV LP; 100%); Yellow Magic 7 (Bradley

Systems; 100%); or by applying centrifugal force for 4 minutes (n = 30 per

subgroup). After postpolymerization (Otoflash G171, NK-Optik), the DC was

measured using Raman spectroscopy, and the surface roughness, as well as the

Martens parameters, were recorded. Biaxial flexural strength was investigated after

artificial aging (thermocycling for 10,000 cycles). Data were statistically analyzed

(Kolmogorov-Smirnov, Kruskal-Wallis, and Mann-Whitney U tests, and Pearson

correlation coefficient). Results: The highest DC was recorded after the use of butyl

glycol or isopropyl (P < .001 to P = .047). The highest surface roughness was

measured after the use of butyl glycol (P < .001 to P = .024). The use of centrifugal

force or Yellow Magic resulted in the highest Martens parameter values (P < .001 to

P = .036) and the highest biaxial flexural strength (P < .001 to P = .013), while

acetone and butyl glycol led to the lowest values. Conclusion: The use of

centrifugal force and Yellow Magic resulted in the highest Martens parameter values

and the highest biaxial flexural strength. Concerning Yellow Magic, no negative

effect on the mechanical properties was observed. The 3Delta Etemp material

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especially was prone to degradation after chemical cleaning. Int J Prosthodont 2021.

doi: 10.11607/ijp.7048

Introduction

Additive Manufacturing (AM) was originally introduced in the 1980s as Rapid

Prototyping and has developed dramatically over the past decades. It has found its

way into a variety of industrial branches including the medical sector [1].

In dentistry, Computer-Aided-Manufacturing (CAM) is a well-established technology.

Until today, it is often equated with subtractive manufacturing methods [2]. Yet, AM is

said to yield many advantages compared to subtractive methods: several objects

can be printed simultaneously, there is less waste of material and even the finest

details can be reproduced. In addition, production takes place passively without

application of force, unlike the subtractive method in which burs suffer from wear [3].

AM is being used for a wide range of different applications in dentistry, including

surgical [4] as well as endodontic [5] guides, occlusal devices [6, 7], dental models

[8], replicas for educational use [9, 10] and even maxillofacial prostheses [11]. There

are also restorative materials, certified for a temporary intraoral use, available on the

market [12].

All AM technologies are based on the principle of building objects layer upon layer

from 3D model data. The most common technique in the field of dentistry is vat

photopolymerization, which is a manufacturing process that uses a light source to

induce photopolymerization of the initially liquid resin [13]. The light source is

focused on a vat containing the photopolymer. For printing thin layers of curable

material on top of each other, either the vat or the light source is moved successively

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along the z-axis [2]. For this purpose, different approaches can be distinguished, for

example Stereolithography (SLA) and Digital light processing (DLP). In SLA, each

layer is exposed to a focused laser beam point-by-point, resulting in a continuous

solidification of each layer. DLP, on the other hand, uses a selectively masked light

source provided by a digital micromirror device (DMD), which is a semiconductor-

based array of thousands of individually controllable micromirrors. This leads to a

shortened production time due to the simultaneous polymerization of an entire layer

[14].

The mechanical properties of the printed objects are affected by various factors,

ranging from build parameters, such as layer thickness and print orientation, to post

processing [13]. Previous studies have already investigated the influence of printing

orientation [13, 15, 16] and layer thickness [17] as well as the effect of different post

polymerization units [16]. The impact of different solvents, like isopropanol, on the

mechanical properties of direct resin composites has been investigated in previous

studies suggesting a deteriorating effect [18,19]. However, there is only limited

information about a possible impact of the proposed cleaning techniques on

additively manufactured objects. The solvents selected for this study are either

recommended by the manufacturers (ethanol, isopropanol and centrifugal force),

known from other AM technologies (aceton for fused filament fabrication) or have

been discussed as a suitable alternative (butyl glycol, yellow magic). Subsequent to

the manufacturing process, correct post processing is mandatory to achieve

sufficient biological and physical properties of the objects [20]. The first step is to

remove unreacted resin from the objects’ surface. Variant cleaning processes are

recommended by the different manufacturers, namely cleaning the printed parts in a

bath of isopropanol or extracting excess resin by applying centrifugal force. Most

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manufacturers recommend the application of isopropanol [21]. In contrast to this

approach, centrifugal force would not chemically interact with the printed objects. To

meet the manufacturers’ specifications regarding mechanical properties, post curing

is of great importance [15]. Previous studies, that had investigated the influence of

different storage media on dental composites, could detect a deteriorating effect on

mechanical properties [22, 23], as well as on surface quality [18]. This effect was

particularly strong in relation to ethanol [22,18]. These results may be transferable to

additively manufactured objects. So, the question arises, whether adverse effects of

the cleaning process, which in most cases involves the use of isopropyl alcohol, can

be observed.

Accordingly, the aim of this study was to evaluate the influence of different cleaning

methods on materials’ properties of additively manufactured specimens. The

influence of five different rinsing solutions and one mechanical method, have been

investigated.

By artificially aging the test specimens, the present study furthermore investigated

whether ageing behavior was impacted by the cleaning method. The null hypothesis

stated that neither the cleaning method nor the different materials would have an

influence on the degree of conversion (DC), surface roughness, Martens parameters

or biaxial flexural strength.

Materials and methods

A disk of 12 mm in diameter and 1.5 mm in height was digitally designed using the

software Meshmixer (Autodesk Inc., San Rafael, CA, USA) and exported as an STL-

file. For preparing the printing process, the slicing software Netfabb Premium

(Autodesk Inc.) was used. The specimens were positioned vertically to the printer’s

platform. All print jobs were performed by using the DLP printer D20II (Rapid Shape,

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Heimsheim, Germany), which was calibrated beforehand according to the

manufacturer’s instructions. For this purpose, the designated parameters of each

material, as provided by the manufacturers, were applied. All materials were

processed in a layer thickness of 50µm, except 3Delta Etemp (Deltamed, Friedberg,

Germany), which was processed in 100µm layer thickness.

Five different 3D print resins labeled as provisional FDP material were examined

(Table 1; N=900, n=180 per material): (i.) 3Delta Etemp [3DE], (ii.) Freeprint temp

(Detax, Ettlingen, Germany) [FPT], (iii.) Temp PRINT (GC Europe, Leuven, Belgium)

[GCT], (iv.) C&B [NCB] and (v.) C&B MFH [NMF] (both NextDent, Soesterberg,

Netherlands). For achieving a homogeneous dispersion of each materials’

components, all materials were manually agitated by shaking the resins’ bottles for at

least 5 minutes prior to the printing process. Subsequent to the printing process,

remaining monomers on the specimens’ surfaces had to be removed. For this

purpose, six different cleaning methods have been investigated, including five

chemical and one mechanical method (Fig. 1).

For the investigated chemical methods, specimens (n=30 per subgroup) were

cleaned for five minutes in an ultrasonic activated bath (Sonorex Super RK 102H,

Bandelin, Berlin, Germany) of either (I.) 99.5% acetone (Höfer Chemie Gmbh,

Kleinblittersdorf, Germany) [ACE], (II.) 100% butyl glycol (Algin Chemie e.K.,

Neustadt-Glewe, Germany) [BUT], (III.) 96% ethanol (Otto Fischar GmbH,

Saarbrücken, Germany) [ETH], (IV.) 100% isopropanol (SAV LP GmbH, Flintsbach,

Germany) [ISO] or (V.) Yellow Magic 7 (Bradley Systems Inc., Des Plaines, IL, USA)

[YEL]. Compressed air was used to remove residue of the cleaning solution from the

specimens’ surface.

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For the mechanical method investigated, the specimens were transferred into

centrifugal tubes (Polypropylene Conical Tube 17x120mm, BD Falcon, Franklin

Lakes, NJ, USA) and centrifugated at 1,500 rpm for four minutes (Allegra X-15R,

Beckmann-Coulter Life Science, Indianapolis, IN, USA) (n=30 per subgroup). The

residual monomer was removed from the specimens’ surface by centrifugal force

[CEN].

Subsequent to the cleaning procedure, support structures were manually removed

using a scalpel. The specimens were then post cured in a post polymerization device

(Otoflash G171, NK Optik, Baierbrunn, Germany) under nitrogen atmosphere for

2,000 flashes from each side (flashlight; wavelength range 280-700nm, peaks at

approximately 400 and 500 nm). Before starting the measurements, the specimens

were stored in a dry and dark setting at room temperature (23°C) for 24 hours to

allow for a complete polymerization.

Following measurements were performed longitudinally examining the same

specimen. For this purpose, specimens were stored in a light-proof box and only

taken out during the time of measurement. Raman spectra were collected using a

Raman spectrophotometer (InVia, Renishaw, New Mill, UK). The samples were

illuminated at 758 nm by a diode-pumped solid state (DPSS) laser through a

microscope objective (50x). Raman spectra were recorded in the region from 1500-

2000 cm-1 at a resolution of 1 cm-1. The following settings were selected to perform

the scans: laser power: 100%; irradiation time: 10s; number of accumulations: 3.

The resulting spectra were processed with the software WiRe 4.2 (Renishaw), which

includes a curve fitting program for analyzing peak heights. The degree of

conversion was then calculated by comparing the change of band heights at

1610cm-1 and 1640cm-1 for the unpolymerized and polymerized resins. To obtain an

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average value for the uncured resins, thirty initial measurements of each material in

its liquid state were conducted. The following equation was applied:

1640𝑐𝑚!! /1610𝑐𝑚!! !"#$%

𝐷𝐶 % = 1 −
1640𝑐𝑚!! /1610𝑐𝑚!! !"#!$%&

In order to identify optical alterations of the specimens’ surfaces, the surface of five

randomly selected specimens of each subgroup (n=30) was imaged using a light

microscope (Leica DM2700 M, Leica Microsystems GmbH) with a magnification of

50x. The images were processed with the LAS X software and color adjustment was

performed automatically by the software.

For investigating the surface roughness, a profilometer (MarSurf 400 SD26, Mahr,

Göttingen, Germany) was used. Six measurements were conducted per specimen.

Track length set to 6 mm and track spacing at 0.25 mm. After the first three

measurements, the specimens were rotated by 90° and another three

measurements were recorded. Based on the acquired data, a mean surface

roughness value was calculated.

Martens parameters were determined using a universal hardness testing machine

(Zwick/Roell ZHU 0.2, Zwick, Ulm, Germany) in conformity with DIN EN ISO

4049:2019 [24]. The test set-up is based on the principle of pressing the apex of a

diamond indenter pyramid vertically into the surface of the specimen. The tests were

carried out at 9.8 N indenter load for 20 seconds. The maximum penetration depth

was 0,095mm. Three indentations at different locations on the surface were taken

per specimen. The Martens parameters were automatically calculated by the

software (TestXpert v.12.3 Master; Zwick) according to the following equations:

𝐹
𝐻𝑀 =
𝐴! ℎ

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where HM is Martens hardness (N/mm2); F is test force (N); AS(h) is the surface area

of the indenter penetrating beyond the zero-point of the contact (N/mm2).

!!
2𝐶 𝐴! (1 − 𝑣!! )
𝐸!" = 1 − 𝑣!! −
𝜋 𝐸!

where EIT is the elastic indentation modulus (kN/mm2); vs is the Poisson’s ratio of the

test piece; C is the compliance of the contact; Ap is the projected contact area; vi is

the Poisson’s ratio of the indenter; Ei is the modulus of the indenter.

Subsequently, thermocycling was performed to simulate fluctuations in temperature

as they occur in the oral environment. Specimens were exposed to 10,000 thermal

cycles in distilled water between 5° and 55°C with a dwell time of 20s (Thermocycler

THE 1100, SD Mechatronics, Feldkirchen-Westerham, Germany).

After a drying time of one hour, the biaxial flexural strength was tested in a universal

testing machine (Zwick Z010, Zwick) according to DIN EN ISO 6872:2015 [25] at

room temperature (Fig. 2). Loading was applied in the specimen’s center at

1mm/min until failure occurred. Prior to the test, the thickness of each specimen

(mm) was measured using IP65 digital micrometer screw (Mitutoyo Deutschland,

Neuss, Germany) to a precision of 0.01 mm. The biaxial flexural strength was

calculated using the following formula:

𝜎 = −0,25𝑁(𝑋 − 𝑌)/𝑏 !

!! !
where 𝜎 is flexural strength (MPa); N is fracture load (N); 𝑋 = 1 + 𝑣 ln +
!!

!! ! !! ! !! !
1 − 𝑣 /2 and 𝑌 = 1 + 𝑣 1 + ln + 1−𝑣 ; v is the Poisson’s ratio
!! !! !!

(=0,3); r1 is the radius of the support circle (mm); r2 is the radius of the loaded area

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(mm); r3 is the radius of the specimen (mm); b is the thickness of the specimen

(mm).

The obtained results were analyzed with SPSS (IBM SPSS statistics for Windows,

version 25; IBM Corp).

Subsequent to descriptive statistics, the assumption of normality was examined by

the Kolmogorov-Smirnov test. Kruskal-Wallis and Mann-Whitney U test were used to

evaluate significant differences between groups. The Pearson’s correlation

coefficient was calculated to test for possible correlations between the measured

parameters. All p-values below 0.05 were considered as statistically significant.

Results

The Kolmogorov-Smirnov test indicated a violation of the assumption of normality for

thirty-three groups. Consequently, the data were analyzed separately in a non-

parametric approach.

The Kruskal-Wallis test revealed significant differences between the different

cleaning methods within one material (p<0.001) and between the different materials

within one cleaning method (p<0.001 – p=0.005). Descriptive statistics are shown in

Table 2 – 4.

In order to check for significant differences between the cleaning methods or the

materials, Mann-Whitney-U-test was applied. Regarding degree of conversion and

the different cleaning methods, BUT and ISO resulted in the highest values (p<0.001

– p=0.047), while the lowest values were recorded for CEN followed by ACE

(p<0.001 – p=0.047). Regarding the materials, NMF showed the highest degree of

conversion (p<0.001 – p=0.026), whereas 3DE revealed the lowest values (p<0.001

– p=0.005). Regarding surface roughness, the cleaning method BUT resulted in the

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highest values for all materials except 3DE (p<0.001 – p=0.024). GCT presented the

highest surface roughness regardless of the cleaning method (p<0.001 – p=0.009),

followed by 3DE (p<0.001 – p=0.005), while NCB and PFT showed the lowest values

(p<0.001 – p=0.029). Regarding Martens parameters, the highest hardness values

were recorded after using CEN or YEL as cleaning methods (p<0.001 – p=0.036)

and the highest indentation modulus was recorded after the use of ISO, YEL and

CEN (p<0.001 – p=0.013). After ACE, though, the lowest values were recorded (HM:

p<0.001 – p=0.019; EIT: p<0.001 – p=0.024). Focusing on the materials, 3DE

revealed the highest Martens parameters (p<0.001) and NCB the lowest (HM:

p<0.001 – p=0.014; EIT: p<0.001 – p=0.002). Regarding biaxial flexural strength,

YEL and CEN resulted in the highest values (p<0.001 – p=0.013). Regardless of the

cleaning method, NMF revealed the highest flexural strength (p<0.001), while 3DE

revealed the lowest (p<0.001).

The calculation of correlations according to Pearson between the different

investigations revealed significant results (p<0.001) for all correlations except biaxial

flexural strength and Martens hardness (p=0.333). There was a positive correlation

for DC and flexural strength (0.279), surface roughness and the Martens parameters

(HM: 0.177; EIT: 0.318), Martens hardness and EIT (0.880). There was a negative

correlation for DC and surface roughness (-0.290), DC and Martens parameters

(HM: -0.256; EIT: -0.247), surface roughness and flexural strength (-0.416), and EIT

and flexural strength (-0.205).

Discussion

For all materials tested, the highest Martens Parameters and flexural strength values

were recorded after cleaning with either the chemical solvent YEL or by using a

mechanical approach (CEN). The use of ACE, on the other hand, resulted in the

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lowest mechanical properties. The material had a high impact on the recorded

values. In general, filled 3D print resins showed higher mechanical properties but

lower DC. Most interestingly, the cleaning strategy recommended by the single

manufacturers (CEN for 3Delta Etemp, ISO for all other materials) did not always

result in the highest mechanical properties of each material.

The tested null hypothesis that neither the cleaning method nor the use of different

resins had an influence on the DC, surface roughness, Martens hardness, elastic

indentation modulus, or biaxial flexural strength had to be rejected.

The undertaken measurements were chosen because of the different aspects that

they illuminate. Indentation methods, like Martens parameters, are a good approach

to draw conclusions about the material’s elastic-plastic behavior [40]. Strength is an

important mechanical property that determines the clinical performance of a material

[41]. Cracks and defects that grow during artificial aging procedures can influence a

material’s strength, that is why thermocycling was used in this study to simulate a

long-term clinical situation. The DC has been discussed to provide important

knowledge about a material’s mechanical behavior and to correspond to its biological

behavior [42,43]. Surface roughness was measured to investigate the cleaning

capacity of the different methods. A high roughness might indicate pools of uncured

resin to be present on the surface after the cleaning process. Various factors, such

as the concentration of the photo initiators, inhibitors and diluting monomers have an

impact on the DC [26]. Compared to dental light-cured composite resins, 3D

printable photopolymers have a high concentration of photo initiators [20] and a low

viscosity [21]. Both factors contribute to an increase in DC [26, 27]. In addition, the

post polymerization in Otoflash G171 under nitrogen atmosphere prevents the

formation of an oxygen inhibition layer and thus improves monomer conversion [28,

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29].

3DE showed the lowest values for DC. This may be due to its high filler content (up

to 50wt% silicon dioxide) inhibiting free radical polymerization [30]. A previous study

about the effect of fillers on the conversion rate of resin-based composite equally

observed a negative correlation between DC and filler content [30]. Another

explanation might be that this material was the only one to be processed in a layer

thickness of 100µm and not 50µm, which might lead to a lower DC during the

printing process. Nonetheless, NMF reached the highest DC despite the presence of

fillers. This could be explained by the reduced filler content compared to 3DE.

Among the cleaning methods and their influence on DC, CEN and ACE exhibited the

lowest values. This may be related to an improper removal of residual monomer from

the surface of the centrifugated specimens or to a deteriorating effect of ACE. BUT

and ISO showed the highest DC values, which may be explained by the proper

cleaning of the specimens’ surface. Concerning the mechanical properties, the

Pearson’s correlation coefficient showed a weak negative correlation between DC

and the Martens parameters on the one hand and a weak positive correlation to

biaxial flexural strength on the other. As stated in previous studies, DC seems to be

a poor predictor for mechanical properties [31, 32]. They are much more dependent

on the stability of the polymeric network and the filler content [31, 32]. On the light

microscopic images (Fig. 3a-f), the individual print layers of test specimens that had

been cleaned with BUT, ETH and ISO are clearly visible. On the specimens cleaned

with ACE, the layers are still detectable, but the borders of the single layers are

interrupted and partly lost. This may be interpreted as a degradation of the material

and needs further investigation.

In contrast, no layers are visible in the groups CEN and YEL. In case of the

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centrifugated specimens, a thin layer of residual monomer seems to cover the

surface. The remaining layer on specimens treated with YEL creates a shimmering

surface, which might be caused by long-chain alcohols contained in the cleanser.

Regarding the surface roughness, the influence of the material seems to play a great

role, with the lowest surface roughness being achieved by the unfilled resins. Fillers

can generate scattering phenomena and compromise the transparency of the resin

[21], this might also compromise the surface quality.

3DE exhibited the highest value for HM and EIT, followed by GCT. Both materials

have the highest filler fraction of integrated fillers. A positive correlation between filler

content and surface hardness has been reported [33-35] in previous studies.

Specimens were positioned vertically to the printer’s platform during manufacturing,

which might increase the recorded hardness values in comparison to horizontal

positioning [13,16].

Unfortunately, the addition of fillers entails some problems as well. For additive

manufacturing, the particles must not undergo sedimentation or agglomeration and a

homogenous dispersion of the fillers should be guaranteed throughout the

production process [21].

Regarding the impact of the cleaning methods on Martens’ Parameters, statistically

significant differences could be detected between all materials. The groups CEN and

YEL presented the highest values. Apparently, the use of Yellow Magic had no

negative influence on the surface hardness, regardless of whether fillers were

present or not. As claimed by the manufacturer, YEL is a mixture of different

chemicals with long-chain alcohols as main component. They do not seem to interact

with the polymer structure probably due to their high molecular weight. The same

applies to the use of centrifugal force for which any chemical interactions are being

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avoided since it is a mechanical method. It is noteworthy that, in contrast to filled 3D

print resins, for unfilled resins, the use of isopropanol did not lead to a reduction in

surface hardness or indentation modulus.

In all other cases, a deteriorating effect of the cleaning solution on the material was

found, being most evident for ACE. Particularly in terms of ethanol, a softening effect

on composite-resins has been described [23, 34, 36, 37]. Softening is the

consequence of a diffusion of the solvent into the polymer structure causing swelling

and leaching out of various components and disintegration of filler particles [23]. The

filler content could make the material more susceptible to a degradative attack, as

there was no reduction in surface hardness in the unfilled resins when treated with

isopropanol. The extent of damage may depend mainly on the diffusion rate of the

penetrant [37] and the crosslink density of the polymeric material [34].

Regarding biaxial flexural strength, the data revealed that in the group CEN, all

materials exhibited similarly high values. This finding could indicate chemical

cleaning to impair flexural strength in contrast to mechanical cleaning. 3DE seems to

be the most prone to chemical cleaning methods. This could be due to its high filler

content. The chemical post treatment may make the material prone to a debonding

of the fillers or to an attack on the fillers. With the inclusion of all cleaning groups,

NMF showed the highest value for biaxial flexural strength. Regarding its high DC

this may be due to its great cross link density raising hygroscopic and chemical

stability. Unfortunately, the manufacturer does not provide any information regarding

the fraction or type of filler. Among the chemical cleaning methods, the best results

for biaxial flexural strength was observed for YEL.

For standardization, post-curing was performed with the same device (Otoflash) for

all investigated materials, although another device is recommended by the

15

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manufacturer for NCB and NMF. However, Otoflash resulted in the highest

mechanical properties and the greatest DC, regardless of the manufacturers’

recommendations in numerous previous studies [16,38,39]. Thus, it does not seem

likely that the selected post-polymerization strategy would have negatively affected

NCB or NMF.

Conclusions

Within the limitations of this in-vitro study, one can draw the following conclusions

restricted to the tested materials and employed test methods. The influence of the

degree of conversion of a material is no reliable indicator for its mechanical

properties. The filler content seems to have a more significant role. In general, the

use of YEL and CEN resulted in the highest surface hardness and flexural strength,

while the use of ACE resulted in the lowest values. Most interestingly, the

recommended cleaning methods of the manufacturers did not automatically result in

the highest mechanical properties of the materials.

References

1. Attaran M. The rise of 3-D printing: The advantages of additive manufacturing

over traditional manufacturing. Bus Horiz 2017;60:677-688.

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Figure 1: Study design

Figure 2: Biaxial flexural strength test

Figure 3: Optical imaging (50x magnification) of the specimens’ surface, exemplarily

shown with the material NextDent CB [a. Acetone b. Butyl glycol c. Centrifugation d.

Ethanol e. Isopropanol f. Yellow Magic]

Figure 4: Flexural strength of five different resins post processed with six different

cleaning methods.

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Fig 1

Fig 2

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Fig 3

Fig 4

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Table 1: Materials, abbreviations, printer, matrix, filler and LOT number.

Material Abbreviation Printer Matrix Filler LOT

3Delta 3DE Methacrylates silicon 0124

Etemp dioxide,
Dental glass
(50wt%)

Freeprint FPT Isopropylidenediphenol Peg-2 none 200703

temp Dimethacrylate 45-<60%, 1,6-
220101
Hexandioldimethacrylate 1-<5%, 2-
Hydroxyethylmethacrylate 1-<5%,
Diphenyl(2,4,6-
trimethylbenzoyl)phosphinoxide 1-
D20II, Rapidshape

<5%, Hydroxypropylmethacrylate 1-
<5%, Phenyl-bis(2,4,6-
trimethylbenzoyl)-phosphinoxide <1%

GC Temp GCT 7,7,9-Trimethyl -4,13-dioxo-3,14- Quartz 10- 1803021

PRINT dioxa-5,12- <25wt%

diazahexadekan-1,16-
diylbismethacrylat 50-<75%, 2,2'-
ethylenedioxydiethyl dimethacrylate
10-<25%

NextDent NCB Methacrylic oligomers >90%, none XK044N01

C&B Phosphine oxides <3%

NextDent NMF not stated Inorganic XG044N22

C&B MFH fillers

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Table 2: Degree of conversion of materials tested (3DE=3Delta Etemp, FPT=Freeprint Temp, GCT=TEMP Print, NCB=NextDent C&B, NMF=NextDent MFH) in
dependence of cleaning method (ACE=Aceton, BUT=Butyl gylkol, CEN=centrifugal force, ETH=ethanol, ISO=isopropanol, YEL=Yellow Magic)

Degree of conversion (%)

3DE FPT GCT NCB NMF

Mean±SD Min/Med/Max Mean±SD Min/Med/Max Mean±SD Min/Med/Max Mean±SD Min/Med/Max Mean±SD Min/Med/Max
A,a B,C,b A,a B,C,c,* A,b,c,*
ACE 74.7±4.2 63.9/75.4/81.4 86.3±4.1 80.0/87.0/92.9 79.5±10.7 57.9/79.9/95.8 92.3±2.0 88.7/92.6/95.7 89.2±5.9 71.7/90.2/97.5
C,a D,b B,C,b C,D,c,* B,d
BUT 88.1±1.9 84.9/87.9/91.5 91.4±2.9 81.5/91.7/94.8 90.4±2.6 83.0/90.5/93.8 94.0±2.3 87.7/94.8/97.4 96.0±1.4 92.3/96.3/98.3
B,a* A,a,* B,C,b,* A,b A,b,*
CEN 80.8±2.6 69.2/81.3/83.8 80.3±5.9 68.2/83.0/86.9 89.4±3.0 83.4/89.1/95.3 90.2±330 79.4/89.0/94.9 90.6±2.3 82.4/90.9/94.7
A,a C,D,c,* A,B,b,* C,D,c B,c
ETH 77.0±5.7 66.3/77.1/90.0 90.3±2.4 86.1/90.7/95.1 84.6±12.2 36.0/87.7/95.4 93.5±1.8 87.1/93.6/96.1 94.4±2.7 85.8/94.7/97.7
B,a D,b C,b D,c B,c,*
ISO 80.5±4.2 72.3/81.7/87.5 92.1±1.8 89.5/91.8/95.3 90.8±4.5 77.8/92.2/97.3 94.8±1.3 91.9/94.8/97.3 96.1±2.2 89.9/96.4/98.7
C,a B,a,* C,b,c A,B,b B,c
YEL 86.5±1.9 83.3/86.9/89.9 85.2±8.8 42.6/87.0/90.4 93.4±1.6 90.5/93.4/96.7 91.2±2.1 87.7/91.3/95.6 94.9±1.7 90.7/95.2/97.4

ABCD
Different letters present significant differences between cleaning methods within one material (Mann-Whitney-U-Test; p<0.05)
abcd
Different letters present significant differences between the materials within the same cleaning group (Mann-Whitney-U-Test; p<0.05)

* Violence of the assumption of normality (Kolmogorov-Smirnov-Test; p<0.05)

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Table 3: Martens parameters of materials tested (3DE=3Delta Etemp, FPT=Freeprint Temp, GCT=TEMP Print, NCB=NextDent C&B, NMF=NextDent MFH) in
dependence of cleaning method (ACE=Aceton, BUT=Butyl gylkol, CEN=centrifugal force, ETH=ethanol, ISO=isopropanol, YEL=Yellow Magic)
2
Martens hardness [N/mm ]

3DE FPT GCT NCB NMF

Mean±SD Min/Med/Max Mean±SD Min/Med/Max Mean±SD Min/Med/Max Mean±SD Min/Med/Max Mean±SD Min/Med/Max
A,c A,b A,b A,a,* A,a
ACE 127±16 80/128/151 83±16 52/77,5/125 83±14 55/83/107 63±7,7 30/64/73 70±10,1 43/71/93
B,c* B,a,b B,b B,C,a C,b
BUT 166±28 125/162/229 105±18 59/104/142 113±22 73/113/147 89±17 55/91/129 114±18 71/112/139
C,d C,b,* C,c C,a D,b
CEN 200±21 152/204/235 132±22 59/134/175 163±21 84/164/202 100±21 51/94/140 141±22 61/143/174
B,c,* B,C,b B,b B,a B,a
ETH 165±23 128/161/233 117±23 59/120/147 110±19 67/114/149 85±17 40/89/106 90±13 62/92/119
B,c C,b,* B,b B,C,a,* C,a,b
ISO 179±21 140/178/222 126±29 39/134/171 120±20 64/120/156 95±15 50/98/113 111±17 74/114/137
C,d C,b C,c B,C,a D,c
YEL 207±26 146/211/256 129±24 54/137/165 147±21 96/149/195 97±21 58/98/132 147±16 120/147/178

Elastic indentation modulus [kN/mm2]

3DE FPT GCT NCB NMF

A,c A,a,b,* A,b A,a A,b
ACE 3.78±0.87 1.90/4.62/7.00 2.34±0.77 1.17/2.12/3.73 2.69±0.80 1.30/2.92/3.73 1.75±0.38 0.87/1.77/2.57 2.46±0.78 0.83/2.60/3.80
B,d,* A,B,a,b B,c A,B,a B,C,b,c
BUT 4.71±1.27 3.10/4.62/6.97 2.59±0.53 1.67/2.63/3.40 3.56±1.04 1.90/3.80/4.90 2.16±0.58 1.23/2.12/3.43 3.19±0.84 1.53/3.08/4.67
B,d A,B,b B,c A,B,a B,C,b
CEN 4.69±0.54 3.37/4.72/5.53 2.87±0.55 1.40/2.93/4.00 3.82±0.57 2.17/3.80/4.87 2.08±0.52 1.13/2.00/3.23 3.29±0.63 1.37/3.30/4.33
B,c B,b A,B,b A,B,a A,B,b,*
ETH 4.61±1.00 3.23/4.47/6.50 3.03±0.81 1.37/3.02/4.10 3.32±0.81 1.87/3.60/4.77 2.12±0.51 1.13/2.08/3.10 3.02±0.67 1.80/3.13/4.07
B,d, B,b B,c B,a B,C,b,c
ISO 4.78±0.75 3.43/4.95/6.40 3.13±0.81 1.10/3.27/4.27 3.69±0.62 2.33/3.75/4.80 2.41±0.43 1.27/2.37/3.20 3.46±0.66 1.90/3.57/4.43
B,d A,B,b B,c A,B,a C,c
YEL 5.21±0.80 3.90/5.22/6.80 2.76±0.59 1.63/2.87/3.77 3.92±0.70 2.10/4.05/5.13 2.06±0.52 1.23/2.02/3.00 3.67±0.53 2.60/3.55/4.63

ABCD
Different letters present significant differences between cleaning methods within one material (Mann-Whitney-U-Test; p<0.05)

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abcd
Different letters present significant differences between the materials within the same cleaning group (Mann-Whitney-U-Test; p<0.05)

* Violence of the assumption of normality (Kolmogorov-Smirnov-Test; p<0.05)

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Table 4: Surface roughness, biaxial flexural strength of materials tested (3DE=3Delta Etemp, FPT=Freeprint Temp, GCT=TEMP Print, NCB=NextDent C&B,
NMF=NextDent MFH) in dependence of cleaning method (ACE=Aceton, BUT=Butyl gylkol, CEN=centrifugal force, ETH=ethanol, ISO=isopropanol, YEL=Yellow
Magic)


Surface roughness (µm)

3DE FPT GCT NCB NMF

Mean±SD Min/Med/Max Mean±SD Min/Med/Max Mean±SD Min/Med/Max Mean±SD Min/Med/Max Mean±SD Min/Med/Max

ACE 2.81±0.82
C,D,b
1.40/2.71/4.30

1.00±0.28
A,a
0.68/0.93/1.79

3.49±1.20
B,c,*
1.29/3.67/5.22

0.82±0.27
A,a
0.47/0373/1.49

1.08±0.35
A,B,a
0.64/0.95/1.73

B,C,b B,a B,c B,a B,a

BUT 2.26±0.63 1.56/2.03/3.81 1.42±0.49 0.65/1.27/2.26 3.50±1.48 1.03/3.46/6.21 1,25±0.38 0.62/1.19/2.19 1.45±0.62 0.65/1.36/3.03
A,a,b A,B,a,b A,c A,B,a A,B,b
CEN 1.38±0.44 0.77/1.30/2.49 1.26±0.33 0.83/1.20/1.97 1.86±0.64 0.70/1.96/2.91 1,01±0.33 0.50/1.06/1.67 1.41±0.51 0.69/1.35/2.63
D,b A,a B,b,* A,B,a A,B,a
ETH 2.94±0.90 1.65/2.82/5.21 1.05±0.40 0.55/0.93/1.97 3.08±1.07 1.62/2.91/5.70 0.98±0.27 0.59/0.96/1.58 1.27±0.41 0.62/1.29/2.01

B,C,D,b A,a B,c* A,a A,B,a
ISO 2.54±0.68 1.25/2.46/3.81 1.05±0.46 0.51/0.90/2.21 3.38±1.21 1.37/3.46/5.62 0.86±0.32 0.43/0.80/1.61 1.28±0.42 0.71/1.18/2.41

B,b A,B,a A,B,c A,B,a A,a,*
YEL 2.02±0.55 1.03/2.03/3.38 1.20±0.35 0.63/1.18/1.85 2.73±1.06 0.85/2.83/4.75 1.05±0.38 0.43/1.00/2.04 1.02±0.31 0.60/0.95/1.88

Biaxial flexural strength [MPa]

3DE FPT GCT NCB NMF

A,a A,B,c B,b B,d A,B,d
ACE 81.6±26 42/76/150 274±113 30,5/259/437 215±76 78/231/305 331±64 174/346/453 359±33 240/367/397

A,B,a,* B,C,b A,a,* B,b A,b
BUT 107±36 75/97/257 357±80,0 193/357/506 139±49 87/128/273 340±64 145/341/449 345±66 115/346/441

D,a D,a D,a,* C,a,* C,a
CEN 466±55 303/481/549 473±54,5 366/474/568 445±55 277/461/516 434±49 305/431/510 437±33 365/436/489

B,a A,b,* B,b,* A,b B,c,*
ETH 137±50 68/131/278 237±110 78/197/450 238±98 87/274/386 245±91 122/227/455 385±33 294/388/437
B,a,*
A,B,b,c B,b B,c,d B,d,*
ISO 153±52 94/134/291 289±125 106/266/571 250±58 150/249/351 343±90 152/360/479 394±52 203/407/448
C,a C,D,b,c C,a,b,* C,b,c,* C,d
YEL 347±106 159/356/574 435±77 178/440/544 378±60 278/386/518 418±63 238/432/521 444±32 343/438/491

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ABCD
Different letters present significant differences between cleaning methods within one material (Mann-Whitney-U-Test; p<0.05)
abcd
Different letters present significant differences between the materials within the same cleaning group (Mann-Whitney-U-Test; p<0.05)

* Violence of the assumption of normality (Kolmogorov-Smirnov-Test; p<0.05)

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