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Electrical Engineering & Electromechanics, 2022, no. 2 35

UDC 679.7:678:544 https://doi.org/10.20998/2074-272X.2022.2.06

V.M. Zolotaryov

, O.V. Chulieieva, V.L. Chulieiev, T.A. Kuleshova, M.S. Suslin

Influence of doping additive on thermophysical and rheological properties of halogen-free

polymer composition for cable insulation and sheaths

Introduction. The demand for halogen-free fire-resistant compositions for the manufacture of fire-retardant wires and cables

is constantly growing. Problem. Therefore, the creation and further processing of these materials is an urgent problem. Goal.

The aim of the article is to study the effect of the doping additive on the thermophysical and rheological properties of

halogen-free compositions for power cables with voltage 1 kV with the determination of both the temperatures of phase and

structural transformations of polymer compositions. Methodology. Experiments investigating the phase transformations were

carried out with the help device of thermogravimetric analysis and differential scanning calorimetry TGA/DSC 1/1100 SF of

METTLER TOLEDO company. Rheological studies of polymeric materials were conducted by using the method of capillary

viscosimetry in the device IIRT–AM. Results. The influence of the doping additive on the formation of the supramolecular

structure of the filled polymer compositions for cable products was determined, that resulted in the temperature increase of

the decomposition beginning by 11 °С and the end of decomposition by 7 °С. Originality. The effect of a doping additive on

reducing the effective melt viscosity of a polymer composition from 6·10

to 1·10

Pa·s with increasing shear rate has been

shown for the first time. The shear rate of the polymer composition containing the doping additive increases from 0.5 to 20 s

–1

with increasing shear stress. Practical value. The research results provide an opportunity to reasonably approach the

development of effective technological processes for the manufacture of the insulation and sheaths of power cables from

halogen-free polymer compositions. References 29, tables 3, figures 8.

Key words: cable production, doping additive, rheological properties,melting temperature, decomposition onset temperature.

Попит на вогнестійкі композиції, що не містять галогенів, для виготовлення пожежобезпечних проводів та кабелів

безперервно зростає. Тому розробка цих матеріалів є актуальною проблемою. Метою статті є дослідження впливу

легувальної добавки на теплофізичні та реологічні властивості композицій. Теплофізичні властивості визначено з

використанням приладу TGA/DSC 1/1100 SF компанії METTLER TOLEDO. Реологічні дослідження полімерних матеріалів

проведено методом капілярної віскозиметрії на приладі ИИРТ-АМ. Визначено вплив легувальної добавки на формування

надмолекулярної структури наповнених полімерних композицій. Встановлено зниження ефективної в’язкості розплаву

полімерної композиції в 6 разів зі зростанням швидкості зсуву в 40 разів при зміненні температури від 150 до 190 °С.

Швидкість зсуву полімерної композиції з легувальною добавкою зростає в 40 разів

з підвищенням напруження зсуву в 9

разів. Результати досліджень дають можливість обґрунтовано підходити до розроблення ефективних технологічних

процесів виготовлення ізоляції та оболонок силових кабелів. Бібл. 29, табл. 3, рис. 8.

Ключові слова: кабельна продукція, легувальна добавка, реологічні властивості, температура плавлення,

температура початку розкладу.

Introduction. In the last few decades, the demand

for halogen-free fire-resistant compositions for the

manufacture of fire-resistant wires and cables is

constantly growing. This is largely due to their

advantages in reducing smoke and reducing toxic and

corrosive gases during combustion compared to

traditionally used halogen-containing non-combustible

cable materials. Such compositions are preferably

materials containing a polymer based on polyolefins and a

significant proportion of inorganic flame retardants, in

particular aluminum hydroxide Al(OH)

[1, 2].

Polyolefins are one of the most flammable materials with

high heat of combustion, low oxygen index and high heat

dissipation, leaving little or no coke residue [3, 4].

In order to pass various tests for compliance with

fire safety standards, compositions with content of the

appropriate filler at the level of 60-80 % can be used. Of

course, in this case there are quite complex problems

regarding the manufacturability and mechanical

properties of the compositions, which have to be solved

by both manufacturers of cable compounds and

manufacturers of cable products [5].

Rheological measurements of polymer melts are

widely used in processing technologies of polymer

compositions for quality control and process optimization.

Another interesting field of rheology is to obtain

information about the molecular parameters of polymers

and the structure of heterogeneous polymer systems. The

publication [6] provides an overview of the influence of

molecular weight, molecular weight distribution, the

degree of branching on various rheological

characteristics. For dispersed polymer systems, such as

materials with particles and polymer mixtures, rheological

measurements can be used as a simple method of

qualitative study of interactions between different phases

and changes in geometric structures created by

inhomogeneities [7].

Extrusion is the main method of polymer processing

in the cable industry. Almost all polymer processing

operations require an extruder for melting, mixing and

forming products [8, 9]. To understand and optimize the

extrusion process, it is first necessary to understand the

rheological properties [10]. In other words, it is difficult

to understand and optimize the polymer processing

operation without first having a complete understanding

of the thermoreological behavior of the polymer material

over a wide range of time. Moreover, using the

rheological properties in both shear and longitudinal

flows, it is necessary to determine the appropriate

equation that can capture the correct rheological response

of the material forced through the capillary and slit

extrusion heads [8-11].

36 Electrical Engineering & Electromechanics, 2022, no. 2

Some important rheological properties of polyolefins

and their mixtures related to extrusion are discussed in

[12-17], including: inlet pressure during extrusion,

important for determining the expansion of polymer

melts; influence of temperature and pressure on

rheological properties [18, 19]; wall penetration of

polymers [20-25].

However, for dispersed polymer systems, the

relationship between structure and rheological

characteristics is not clear, additional research methods

should be used to assess the contribution of different

structural elements [26]. In [27] the influence of the

modifier on the thermophysical properties of fire-resistant

composite materials was investigated.

Among the requirements for halogen-free cable

polymer compositions is the ability to provide high linear

extrusion rates. Thus, the study of the effect of alloying

additives on the rheological and thermophysical

properties of halogen-free polymer compositions is an

urgent problem.

The goal of the work is the study of the effect of

the alloying additive on the thermophysical and

rheological properties of halogen-free polymer

compositions for power cables for voltages up to 1 kV

with the determination of the temperatures of phase and

structural transformations of polymer compositions.

Polymer cable compositions. Halogen-free fire-

resistant polymer compositions were studied: sample 1

and sample 2. The polymer matrix (sample 3) for polymer

compositions is a mixture of polyolefins (linear low

density polyethylene; polyolefin elastomer and linear low

density polyethylene modified with maleic anhydride).

Flame retardant filler is alumina trihydrate. The content of

flame retardant in polymer compositions is 60 %. The

polymer composition in sample 2 contains an alloying

additive in an amount of 2 %.

Paraffinic hydrocarbons were used as an alloying

additive. The technical properties of the alloying additive

are listed in Table 1.

Table 1

Properties of the alloying additive

Indicator Value

Melt viscosity at temperature 140 °С, Pa·s, 10

180-300

Droplet temperature, °С, not less than 103

Penetration hardness, %, not more than 5

Volumetric resistivity at temperature 110 °С and

voltage not less than 100 V, ·cm, not less than

1·10

The polymer composition is made on the

compounding line of the X-Compound Company,

Switzerland. The line includes the following equipment:

compounder/mixer 120-16 L/D, feed extruder GS 140-6

L/D with granulating head, ingredient dosing system,

transport systems of ingredients and finished products,

granule cooling system.

Equipment and methods. A series of experiments

to study phase and structural transformations, thermal

oxidative degradation processes were performed using

thermogravimetric analysis (TGA) and differential

scanning calorimetry (DSC) TGA/DSC 1/1100 SF

instrument of the METTLER TOLEDO Company at

heating rate of 10 and 50 deg/min.

Operating temperature range is from room

temperature to 1100 °С; heating rate is from 0.01 deg/min

to 100 deg/min.

Microbalance: the maximum weight during

mounting is 1 g. The resolution of the TGA device is 1 μg

in the entire weighing range.

DSC measurement range: 1 – ±350 mW; resolution

– 0.04 μW.

Determination of temperatures of phase and

structural transformations is carried out according to the

characteristic points of the description of physical

phenomena on DSC diagrams.

The beginning of the melting or vitrification effect is

defined as the point of intersection of the baseline with

the diagram before the phase transition. The end of the

effects is defined as the point of intersection of the

baseline with the diagram after the phase transition and

the tangent curve, which is drawn to the point of

inflection.

Determination of decomposition temperatures of

polymer compositions was performed using DSC

diagrams obtained using the instrument TGA/DSC 1/1100

SF (temperature rise rate is 10 deg/min). Decomposition

start and end temperatures were defined as the points of

intersection of the baseline with the diagram before and

after the decomposition of the polymer compositions and

the tangent to the diagram drawn to the inflection point.

Mass loss is defined as the distance on the ordinate axis

between the tangent to the TGA diagram and parallel to

the abscissa axis at the end of the process.

The study of the rheological properties of polymeric

materials was carried out by capillary viscosimetry on the

IIRT-AM instrument.

The properties of polymer compositions were

determined at temperature of 150-190 °C and loads from

37.24 to 211.82 N. Using the obtained data, the shear

stress, shear rate and effective viscosity were calculated.

Shear stress is determined by [28]

)(









, (1)

where τ is the shear stress, Pa; P is the force required

to ensure the flow through the capillary, N; Р

is the

input losses, N; R is the radius of the cylinder, cm; r is

the radius of the capillary, cm; L is the length of the

capillary, cm.

The shear rate is determined by [28]











, (2)

where





is the shear rate, s

–1

; Q is the material

consumption, cm

/s (Q = π·R

·h, where h is the stationary

immersion speed of the piston, cm/s; R is the radius of the

cylinder, cm); r is the radius of the capillary, cm.

The effective viscosity is determined by [28]











, (3)

where η is the effective viscosity, Pa·s.

Electrical Engineering & Electromechanics, 2022, no. 2

Graphs of shear stress versus shear rate and effective

viscosity versus shear rate and shear stress are plotted.

In order to estimate the energy required for the

transition of the system to the so-called transition state,

i.e. when the destruction and the establishment of

connections are balanced, the activation energy is

calculated.

The activation energy of a viscous flow is

determined by [28]

1221

)/ln(

ТТ

MFRMFRTTR

act







, (4)

where T is the measurement temperature, K; MFR

and

MFR

are the melt flow rates for Т

and Т

, g/10 min;

R is the universal gas constant (8.314 J/(mol·K)).

A series of experiments to determine the electrical

strength was performed using an instrument type AII-70,

electrical resistivity – an instrument type KISI-1.

Statistical analysis was performed by the method of

disperse analysis (ANOVA) using the model of

asymptotic regression according to the integrated

Levenberg-Marquardt algorithm with a significance level

of α 0.05.

Results of investigations. For the extrusion process

of halogen-free polymer compositions, it is important for

cable products to investigate their thermophysical

characteristics such as: temperatures of phase and

structural transformations, decomposition start

temperatures. The latter are also important for the

operation of cable products at elevated temperatures and

short-circuit temperatures. For power cables up to 1 kV

with halogen-free insulation, the short-circuit temperature

is 170 °С (duration not more than 5 s).

Figures 1, 2 show DSC diagrams of a polymer

matrix and a halogen-free polymer composition without

and with an alloying additive content.

Fig. 1. DSC diagram to determine phase transitions

Temperatures of the beginning and end of

decomposition (Fig. 2) vary depending on the

composition: for the polymer matrix (curve 3) in the

range from 229 °С to 254 °С, for the polymer

composition (curve 1) – from 258 °С to 275 °С, and

for the polymer composition with an alloying additive

(curve 2) – from 269 °С to 282 °С.

Fig. 2. DSC diagram to determine the beginning and end

temperature of the decomposition

Figures 3, 4 show TGA diagrams of a halogen-free

polymer matrix and polymer composition without and

containing an alloying additive.

Fig. 3. TGA diagram.

Mass loss in the range from 200 to 450 °С

Table 2 shows the mass loss data determined from

the TGA diagram (Fig. 3) for the polymer matrix and

polymer composition that do not contain halogens without

and with the content of the alloying additive.

Based on the data in Table 2 it is shown that for

samples 1, 2 at mass loss from 5 % to 20 %, the

temperature is lower (from 298 °С to 376 °С) than for

sample 3 (from 334 °С to 383 °С). When the temperature

reaches 275 °С (Fig. 3), there is a sharp change in mass

loss (curves 1, 2). This is due to the process of

dehydration of alumina trihydrate with heat absorption

and water release. Sample 3 loses 50 % of the mass at

temperature of 426 °С.

Table 2

Mass loss

Temperature, °С

Mass loss, %

Sample 1 Sample 2 Sample 3

5 298,1 301,8 334,6

10 314,0 319,0 356,6

20 351,9 376,2 383,9

30 412,3 435,0 400,5

50 – – 426,1

38 Electrical Engineering & Electromechanics, 2022, no. 2

Analysis of the TGA diagram (Fig. 4) shows that the

polymer matrix loses 100 % of its mass at temperature of

525 °С. For samples 1, 2 already at temperature of 560 °С

mass loss does not change, the residue is 38 % of the total

mass of the polymer composition, which corresponds to

the loss of chemically bound water and coincides with the

theoretical calculations presented in [29].

Fig. 4. TGA diagram.

Mass loss in the range from 200 to 600 °С

Analysis of DSC and TGA diagrams (Fig. 1-4)

shows that polymer compositions should be used for the

manufacture of cable products in which the maximum

long-term temperature of the conductive core does not

exceed 90 °С, and the maximum temperature at short

circuit is 170 °С. At the same time, the optimal

temperature range of extrusion of polymer compositions

was established. Rheological studies were performed at

temperatures of 150, 170 and 190 °С.

Figures 5, 6 present the dependencies of the

effective viscosity on the shear rate and the effective

viscosity on the shear stress.

Fig. 5. Dependence of effective viscosity at different

temperatures on the shear rate of polymer compositions

In Fig. 5 for the polymer composition of sample 2

there is a more significant decrease in the effective

viscosity over the entire temperature range with

increasing shear rate compared to the polymer

composition of sample 1.

In Fig. 6 there is a decrease in effective viscosity

with increasing shear stress for sample 1 from 8·10

1.5·10

Pa·s, for sample 2 from 6.1·10

to 1·10

Pa·s. The

alloying additive provides efficient distribution of the

flame retardant filler in the polymer matrix, resulting in

the formation of an ordered supramolecular structure.

Fig. 6. Dependence of effective viscosity on shear stress of

polymer compositions at different temperatures

Figure 7 presents graphical dependencies of shear

rate on shear stress (flow curves) for polymer

compositions of samples 1 and 2, respectively. The nature

of the curves indicates that higher shear stress values are

required to achieve higher shear rate values during the

flow of polymer compositions. For the polymer

composition of sample 2, the flow curves (4, 5, 6) at fixed

values of the shear stress are shifted toward higher values

of the shear rate compared to the polymer composition of

sample 1 (curves 1, 2, 3).

Fig. 7. Dependence of shear stress on the shear rate of polymer

compositions at different temperatures

Figure 8 shows the graphical dependencies of the

activation energy of the viscous flow on the load for the

polymer compositions of sample 1 and sample 2.

The activation energy of a viscous flow determines

the energy barriers that are overcome in the elementary

act of flow and determines the effect of temperature on

the effective viscosity: the higher the activation energy,

the greater the effect of temperature on the effective

viscosity.

For the polymer compositions of sample 1 and

sample 2, the activation energy decreases with increasing

load, and the activation energy of the polymer

Electrical Engineering & Electromechanics, 2022, no. 2

composition of sample 1 becomes smaller compared to

the polymer composition of sample 2.

Fig. 8. Dependence of viscous flow activation energy on load

for polymer compositions

The electrophysical properties of polymer

compositions of sample 1, sample 2, and sample 3 have

been studied. The electrical resistivity is determined by

the presence of free charges (electrons and ions) and their

mobility. Electrical strength is the electric field strength at

which a breakdown occurs.

The results of the study are presented in Table 3.

Table 3

Electrophysical indicators of polymer compositions

Indicator Sample 1 Sample 2 Sample 3

Volumetric resistivity,

·cm

1,15·10

1,32·10

1·10

Electrical strength,

kV/mm

45,0 48,5 23,5

It is advisable to compare fire-hazardous polymer

compositions that do not contain halogens: sample 1 and

sample 2.

From data of Table 3 it can be seen that with the

introduction of the alloying additive, the volumetric

resistivity increases from 1.15·10

to 1.32·10

·cm, the

electrical strength increases from 45 to 48.5 kV/mm.

Conclusions.

1. The influence of alloying additive on the formation

of supramolecular structure of filled polymer

compositions for cable products is determined, due to

which the temperature of the beginning of decomposition

by 11 °С and of the end of decomposition by 7 °С

increases.

2. The expediency of using fire-retardant compositions

for the manufacture of cable products, in which the

maximum long-term temperature of the conductive core

does not exceed 90 °С and the maximum temperature in

the event of a short circuit is 170 °С, is shown.

3. For the first timethe effect of an alloying additive on

reducing the effective melt viscosity of a polymer

composition from 6·10

to 1·10

Pa·s with increasing

shear rate is shown. The shear rate of the polymer

composition containing the alloying additive increases

from 0.5 to 20 s

–1

with increasing shear stress.

4. For the first time the influence of an alloying

additive on the electrophysical properties of fire-

hazardous halogen-free polymer compositions has been

studied. With the introduction of the alloying additive, the

electrical resistance increases from 1.15·10

to 1.32·10

·cm, and the electrical strength increases from 45 to

48.5 kV/mm.

5. The results of research provide an opportunity to

reasonably approach the development of effective

technological processes for the manufacture of insulation,

sheaths of power cables from halogen-free polymer

compositions.

Conflict of interest. The authors of the article state

that there is no conflict of interest.

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Received 08.12.2021

Accepted 15.01.2022

Published 20.04.2022

V.M. Zolotaryov

, Doctor of Technical Science, Professor,

O.V. Chulieieva

, Doctor of Technical Science,

V.L. Chulieiev

, PhD,

T.A. Kuleshova

, Senior Engineer,

M.S. Suslin

, Engineer,

PJSC «YUZHCABLE WORKS»,

7, Avtogennaya Str., Khakiv, 61099, Ukraine,

e-mail: [email protected];

[email protected] (Corresponding author);

[email protected]; kules[email protected];

[email protected]

How to cite this article:

Zolotaryov V.M., Chulieieva O.V., Chulieiev V.L., Kuleshova T.A., Suslin M.S. Influence of doping additive on thermophysical and

rheological properties of halogen-free polymer composition for cable insulation and sheaths. Electrical Engineering &

Electromechanics, 2022, no. 2, pp. 35-40. doi: https://doi.org/10.20998/2074-272X.2022.2.06