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Manufacturing Refractory Silica Bricks From Silica Sand

Article · January 2012

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 Manufacturing Refractory Silica Bricks From Silica Sand
                          Prof. Dr. Hussein H. Karim1 Prof. Dr. Hisham K. Ahmed 1 and Oday A. Al-Taie 2
 husn_irq@yahoo.com         hish1950@yahoo.com odayazez@yahoo.com

1. Building and Construction Engineering Department – University of Technology.

2. Ass. Lecturer, College of Engineering – Tikrit University.

Abstract
The investigation implies the use of silica sands, available in western desert of Iraq, as raw
materials for silica bricks manufacturing and compare their properties with specification requirements
in order to use these raw materials in manufacturing silica bricks to support industries and to replace
the imported silica brick. Results of chemical and mineralogical analysis reflect the high purity of
these raw materials for this industry. To study the effect of grain size distribution and mineralizers on
properties of silica bricks; crushing and grinding are carried out. Three mixes of silica sands, with
different grain sizes containing lime and iron oxide have been prepared. Besides, the investigation
studies the capability of using tunnel kiln for producing such bricks, and comparing the effect of firing
on the quality of silica bricks in both furnaces (tunnel and electrical). For this purpose, each group of
the prepared specimens is fired in electrical furnace for 80 hours according to firing program, whereas
firing in tunnel kiln requires 288 hours to complete. Results of X-ray diffraction tests on several fired
specimens reflect higher phase conversions for electrical furnace specimens compared to tunnel kiln
specimens, as well as results indicate that the mineralizers used and increasing fine sizes lead to
increase in the phase conversion. Moreover, chemical analysis results show the specifications of the
manufactured silica bricks agree with standard requirements specifications.
Laboratory test results obtained from silica brick specimens reflect the effect of firing, grain size,
quality and quantity of mineralizers on the properties of the manufactured bricks. In general, the firing
efficiency in electrical furnace is better than in tunnel kiln, but this is not an indicator of the
impracticability of the latter because most of tunnel kiln specimens indicate their agreement with
specification requirements. The results also show that the increases in fine grains enhance the cold
compressive strength, but cause decrease in spalling resistance to reach 12 cycles and increase in
apparent porosity to reach 24%. The use of iron oxide and lime improves most of manufactured silica
bricks properties except the increase in the values of apparent porosity and causes the slight decrease
in spalling resistance. Finally, results of manufactured specimens indicate that silica bricks can be
manufactured from the available local raw materials in tunnel kiln for firing not less than 12 days to
ensure the occurrence of phase conversions, taking in consideration the suitable grain size because the
increase in fine grains leads to increase in porosity besides cost.

‫ﺗﺼﻨﯿﻊ اﻟﻄﺎﺑﻮق اﻟﺤﺮاري اﻟﺴﻠﯿﻜﻲ ﻣﻦ اﻟﺮﻣﻞ اﻟﺴﻠﯿﻜﻲ‬

‫ ﻋﺪي ﻋﻠﻲ ﻋﺰﯾﺰ اﻟﻄﺎﺋﻲ‬.‫م‬.‫م‬ ‫ ھﺸﺎم ﺧﺎﻟﺪ أﺣﻤﺪ‬.‫ د‬.‫أ‬ ‫ ﺣﺴﯿﻦ ﺣﻤﯿﺪ ﻛﺮﯾﻢ‬.‫ د‬.‫أ‬
‫ ﺟﺎﻣﻌﺔ ﺗﻜﺮﯾﺖ‬-‫ﻛﻠﯿﺔ اﻟﮭﻨﺪﺳﺔ‬ ‫ اﻟﺠﺎﻣﻌﺔ اﻟﺘﻜﻨﻮﻟﻮﺟﯿﺔ‬-‫ﻗﺴﻢ ھﻨﺪﺳﺔ اﻟﺒﻨﺎء واﻷﻧﺸﺎءات‬

‫اﻟﻤﺴﺘﺨﻠﺺ‬
‫ ﻛﻤ ﻮاد أوﻟﯿ ﺔ ﻟﺘﺼ ﻨﯿﻊ اﻟﻄ ﺎﺑﻮق‬، ‫ اﻟﻤﺘ ﻮﻓﺮة ﻓ ﻲ ﻣﻨﻄﻘ ﺔ اﻟﺼ ﺤﺮاء اﻟﻐﺮﺑﯿ ﺔ ﻣ ﻦ اﻟﻌ ﺮاق‬، ‫ﯾﺘﻀﻤﻦ اﻟﺒﺤﺚ اﺳﺘﺨﺪام رﻣ ﺎل اﻟﺴ ﻠﯿﻜﺎ‬
‫اﻟﺴﻠﯿﻜﻲ وﻣﻘﺎرﻧﺔ ﺧﻮاص اﻟﻨﻤﺎذج اﻟﻤﺼﻨﻌﺔ ﻣﻊ ﻣﺘﻄﻠﺒﺎت اﻟﻤﻮاﺻ ﻔﺎت اﻟﻌﺎﻟﻤﯿ ﺔ وذﻟ ﻚ ﻟﻐ ﺮض اﺳ ﺘﺜﻤﺎر ھ ﺬه اﻟﻤ ﻮاد اﻷوﻟﯿ ﺔ ﻓ ﻲ ﺻ ﻨﺎﻋﺔ‬
‫ أظﮭ ﺮت ﻧﺘ ﺎﺋﺞ اﻟﺘﺤﻠﯿ ﻞ اﻟﻜﯿﻤﯿ ﺎﺋﻲ‬.‫ھ ﺬا اﻟﻨ ﻮع ﻣ ﻦ اﻟﻄ ﺎﺑﻮق اﻟﺴ ﯿﻜﻲ ودﻋ ﻢ اﻟﺼ ﻨﺎﻋﺔ واﺳ ﺘﺨﺪاﻣﮫ ﻛﺒ ﺪﯾﻞ ﻟﻠﻄ ﺎﺑﻮق اﻟﺤ ﺮاري اﻟﻤﺴ ﺘﻮرد‬
‫ ﻟﻐ ﺮض دراﺳ ﺔ ﺗ ﺄﺛﯿﺮ اﻟﺘ ﺪرج اﻟﺤﺒﯿﺒ ﻲ‬.‫واﻟﻤﻌ ﺪﻧﻲ اﻟﻨﻘ ﺎوة اﻟﻌﺎﻟﯿ ﺔ ﻟﮭ ﺬه اﻟﻤ ﻮاد وﺻ ﻼﺣﯿﺘﮭﺎ ﻟﺼ ﻨﺎﻋﺔ ھ ﺬا اﻟﻨ ﻮع ﻣ ﻦ اﻟﻄ ﺎﺑﻮق‬
‫( ﺧﻠﻄﺎت ﻣﻦ اﻟﺮﻣﻞ اﻟﺴﻠﯿﻜﻲ ﺑﺘﺪرﺟﺎت ﻣﺨﺘﻠﻔﺔ‬3) ‫واﻟﻤﺤﻔﺰات ﻋﻠﻰ ﺧﻮاص اﻟﻄﺎﺑﻮق اﻟﻤﺼﻨﻊ ﺗﻤﺖ ﻋﻤﻠﯿﺎت اﻟﺘﻜﺴﯿﺮ واﻟﻄﺤﻦ وﺣﻀﺮت‬
This paper is a part of M.Sc. Thesis entitled "Manufacturing Refractory Silica Bricks to Resist Concentrated Acids by Using
Quartzite Rocks" by Oday Ali Azez Al-Taie Under supervision of Prof. Dr. Hussein H. Karim and Prof. Dr. Hisham K.
Ahmed, 2005, Building & Construction Engineering Department, University of Technology.

1
 ‫ ﻛﻤﺎ ﺗﻀﻤﻦ اﻟﺒﺤﺚ دراﺳﺔ إﻣﻜﺎﻧﯿﺔ اﺳﺘﺨﺪام اﻟﻔﺮن اﻟﻨﻔﻘﻲ اﻟﻌﺎﺋﺪ ﻟﻤﻌﻤﻞ ﺣﺮارﯾﺎت اﻟﻔﻠﻮﺟﺔ ﻻﻧﺘﺎج ھﺬا‬.‫ﺣﺎوﯾﺔ ﻋﻠﻰ اﻟﻨﻮرة واوﻛﺴﯿﺪ اﻟﺤﺪﯾﺪ‬
‫ وﻟﮭ ﺬا اﻟﻐ ﺮض ﺗ ﻢ ﺣ ﺮق ﻛ ﻞ‬،‫اﻟﻨﻮع ﻣﻦ اﻟﺤﺮارﯾﺎت وﻣﻘﺎرﻧﺔ ﺗﺄﺛﯿﺮ اﻟﺤﺮق ﺑﯿﻦ اﻟﻔﺮﻧﯿﻦ اﻟﻨﻔﻘﻲ واﻟﻜﮭﺮﺑﺎﺋﻲ ﻋﻠ ﻰ ﻧﻮﻋﯿ ﺔ اﻟﻄ ﺎﺑﻮق اﻟﺴ ﻠﯿﻜﻲ‬
.‫ ﺳ ﺎﻋﺔ‬288 ‫ أﻣ ﺎ اﻟﺤ ﺮق ﺑ ﺎﻟﻔﺮن اﻟﻨﻔﻘ ﻲ ﻓﻘ ﺪ اﺳ ﺘﻐﺮق‬،‫ ﺳ ﺎﻋﺔ‬80 ‫وﺟﺒﺔ ﻣﻦ اﻟﻨﻤﺎذج اﻟﻤﻜﺒﻮﺳﺔ ﺑ ﺎﻟﻔﺮن اﻟﻜﮭﺮﺑ ﺎﺋﻲ ﺿ ﻤﻦ ﺑﺮﻧ ﺎﻣﺞ اﺳ ﺘﻐﺮق‬
‫أظﮭﺮت ﻧﺘﺎﺋﺞ ﻓﺤﻮﺻﺎت اﻷﺷﻌﺔ اﻟﺴﯿﻨﯿﺔ اﻟﺘ ﻲ أﺟﺮﯾ ﺖ ﻋﻠ ﻰ ﻋ ﺪد ﻣ ﻦ اﻟﻨﻤ ﺎذج اﻟﻤﺤﺮوﻗ ﺔ إﻟ ﻰ أن درﺟ ﺔ اﻟﺘﺤ ﻮل أﻟﻄ ﻮري ﻟﻨﻤ ﺎذج اﻟﻔ ﺮن‬
‫ إﺿﺎﻓﺔ ﻟﺬاﻟﻚ دﻟﺖ اﻟﻨﺘﺎﺋﺞ إﻟ ﻰ أن اﺳ ﺘﺨﺪام اﻟﻤﺤﻔ ﺰات وزﯾ ﺎدة اﻟﻤﻘﺎﺳ ﺎت اﻟﻨﺎﻋﻤ ﺔ أدى إﻟ ﻰ‬،‫اﻟﻜﮭﺮﺑﺎﺋﻲ ﻛﺎﻧﺖ أﻋﻠﻰ ﻣﻦ ﻧﻤﺎذج اﻟﻔﺮن اﻟﻨﻔﻘﻲ‬
‫ ﻟﻘﺪ ﺗﺒﯿﻦ ﻣﻦ ﻧﺘﺎﺋﺞ اﻟﺘﺤﻠﯿﻞ اﻟﻜﯿﻤﯿﺎﺋﻲ ﻣﻄﺎﺑﻘﺔ اﻟﻄﺎﺑﻮق اﻟﺴﻠﯿﻜﻲ اﻟﻤﺼﻨﻊ ﻣﻊ ﻣﺘﻄﻠﺒﺎت اﻟﻤﻮاﺻ ﻔﺎت‬.‫زﯾﺎدة ﻓﺎﻋﻠﺔ ﻓﻲ درﺟﺔ اﻟﺘﺤﻮل أﻟﻄﻮري‬
.‫اﻟﻌﺎﻟﻤﯿﺔ‬
‫ﺑﯿﻨ ﺖ ﻧﺘ ﺎﺋﺞ اﻟﻔﺤﻮﺻ ﺎت اﻟﻤﺨﺘﺒﺮﯾ ﺔ ﻟﻨﻤ ﺎذج اﻟﻄ ﺎﺑﻮق اﻟﺴ ﻠﯿﻜﻲ ﺗ ﺄﺛﯿﺮ اﻟﺤ ﺮق واﻟﺘ ﺪرﺟﺎت وﻧﻮﻋﯿ ﺔ وﻋ ﺪد اﻟﻤﺤﻔ ﺰات ﻋﻠ ﻰ ﺧ ﻮاص‬
‫ ﺑﺼﻮرة ﻋﺎﻣﺔ ﻛﺎﻧﺖ ﻛﻔﺎءة اﻟﺤﺮق ﺑﺎﻟﻔﺮن اﻟﻜﮭﺮﺑﺎﺋﻲ أﻓﻀﻞ ﻣ ﻦ اﻟﻔ ﺮن اﻟﻨﻔﻘ ﻲ إﻻ أن ھ ﺬا ﻻ ﯾﻌ ﺪ ﻣﺆﺷ ﺮا ﻋﻠ ﻰ‬.‫اﻟﻄﺎﺑﻮق اﻟﻤﻨﺘﺞ ﻗﯿﺪ اﻟﺒﺤﺚ‬
‫ إن زﯾ ﺎدة اﻟﻤﻘﺎﺳ ﺎت اﻟﻨﺎﻋﻤ ﺔ ﺳ ﺎﻋﺪ ﻋﻠ ﻰ‬.‫ ﻟﻜﻮن اﻏﻠﺐ ﻧﻤﺎذج اﻟﻔﺮن اﻟﻨﻔﻘﻲ أظﮭﺮت ﻣﻄﺎﺑﻘﺘﮭ ﺎ ﻟﻠﻤﻮاﺻ ﻔﺎت اﻟﻌﺎﻟﻤﯿ ﺔ‬،‫ﻋﺪم ﺻﻼﺣﯿﺔ اﻷﺧﯿﺮ‬
24 ‫ دورة وازدادت ﻗﯿﻢ اﻟﻤﺴﺎﻣﯿﺔ اﻟﻈﺎھﺮﯾ ﺔ ﻟﺘﺼ ﻞ إﻟ ﻰ‬12 ‫ ﻓﻲ ﺣﯿﻦ ﺗﻨﺎﻗﺼﺖ ﻣﻘﺎوﻣﺔ اﻟﺼﺪﻣﺔ اﻟﺤﺮارﯾﺔ ﻟﺘﺒﻠﻎ‬،‫ﺗﺤﺴﯿﻦ ﻣﻘﺎوﻣﺔ اﻻﻧﻀﻐﺎط‬
‫ إن اﺳﺘﻌﻤﺎل اوﻛﺴﯿﺪ اﻟﺤﺪﯾﺪ ﻣﻊ اﻟﻨﻮرة أدى إﻟﻰ ﺗﺤﺴﯿﻦ ﻣﻌﻈﻢ ﺧ ﻮاص اﻟﻄ ﺎﺑﻮق اﻟﻤﻨ ﺘﺞ وﯾﺴ ﺘﺜﻨﻰ ﻣ ﻦ ذاﻟ ﻚ اﻟﺰﯾ ﺎدة ﻓ ﻲ ﻗ ﯿﻢ اﻟﻤﺴ ﺎﻣﯿﺔ‬.%
‫ ﻛﻤﺎ أﺷﺎرت اﻟﻨﺘﺎﺋﺞ إﻟﻰ إﻣﻜﺎﻧﯿﺔ ﺗﺼ ﻨﯿﻊ اﻟﻄ ﺎﺑﻮق اﻟﺤ ﺮاري اﻟﺴ ﻠﯿﻜﻲ ﻣ ﻦ اﻟﻤ ﻮاد‬.‫اﻟﻈﺎھﺮﯾﺔ واﻟﻨﻘﺼﺎن اﻟﻄﻔﯿﻒ ﻟﻤﻘﺎوﻣﺔ اﻟﺼﺪﻣﺔ اﻟﺤﺮارﯾﺔ‬
‫ وﯾﺮاﻋﻰ ﻓﻲ ذﻟ ﻚ اﺳ ﺘﺨﺪام اﻟﺘ ﺪرﺟﺎت‬،‫ ﯾﻮﻣﺎ ﻟﻀﻤﺎن ﺣﺼﻮل اﻟﺘﺤﻮل أﻟﻄﻮري‬12 ‫اﻟﻤﺘﻮﻓﺮة ﻣﺤﻠﯿﺎ وﺑﺎﻟﻔﺮن اﻟﻨﻔﻘﻲ وﻟﻤﺪة ﺣﺮق ﻻ ﺗﻘﻞ ﻋﻦ‬
.‫اﻟﻤﻨﺎﺳﺒﺔ ﺣﯿﺚ أن زﯾﺎدة اﻟﻤﻘﺎﺳﺎت اﻟﻨﺎﻋﻤﺔ ﺗﺆدي إﻟﻰ زﯾﺎدة اﻟﻤﺴﺎﻣﯿﺔ ﻓﻀﻼً ﻋﻦ زﯾﺎدة اﻟﻜﻠﻔﺔ‬

1. Introduction
The aim of using fire bricks in lining the kilns is to confine the heat inside them and
prevent its infiltration to the outside atmosphere. During the design of the kiln, it has to be
kept in mind that temperature at the external surface of the kiln does not exceed 40oC
whatever the internal temperature may have been. Secondly, the brick should prevent the
external frame of the kiln from melting or folding because it is usually made out of steel. In
addition it helps in creating a suitable working atmosphere to the technician and engineers to
watch and follow the processes that go on inside the kiln (Shaw, 1972; Taber,2003).
Of the more than one hundred elements found in the earth’s crust, only a few have both
abundance and the ability to form stable refractories compounds. These are silicon (Si),
aluminum (Al), magnesium (Mg), calcium (Ca), chromium (Cr), zirconium (Zr), and carbon.
These form the useful oxides: SiO2, Al2O3, MgO, and ZrO2 (Norton, 1968; Raymond et.al.
2005).
Refractory materials can be subdivided on the basis of the following characteristics
(Budnikov,1964): size and shape: standard “straight” and “tapered” brick, and specially
shaped products (simple, complex, extra complex, and large block); method of manufacture:
products made by plastic molding (pressing), semidry pressing or tamping from non-plastic
powder mixtures, casting from slips or melts, and cutting from rock; type of heat treatment:
non-fired, fired, and melt-cast products; and degree of porosity: sintered refractories with a
porosity of less than 1%, dense refractories with a porosity of (10-30)%, and lightweight
refractories with a porosity of more than 50 %. Also, refractory materials can be classified the
chemical basis as: basic, neutral and acid products. The later, are those made of clay, of clay
silica mixtures, and of pure silica. The more silica is used in a mixture the more acidic are its
properties (Taber, 2003).
Silica bricks is very important due to withstand higher working temperatures and have
longer lives, they made from materials with high silica content. Silica bricks are used
specifically in kiln roofs and in exposed side walls, because of their high mechanical strength
and rigidity at temperatures approaching the melting point (Al-Tai et. al., 1977). They have a
large scope of applications in coke oven, blast furnace stoves, open-hearth furnaces, electrical
arc furnaces, soaking pits, and in other industries such as glass (Padgett, 1984; Abhijiti,
2010).
Silica bricks are acid refractory, capable of carrying a load 3.5 (Kg/cm2) to a few degree
of fusion points (1710-1730) oC, and which can safely be used in structures up to 1650 oC. It
is free from shrinkage at temperature up to its melting point and has a high thermal shock

2
resistance in the degree (600-1700)oC. It has a high resistance to attack by principal steel
furnace fluxes, namely iron oxide, lime, and acid slags generally, and high abrasion resistance
(Sinjer and Sinjer, 1963).
This article deals with the production of refractory silica bricks from the locally available
silica sands and to study their properties and suitability to meet standard requirements.

2. Experimental Work
This work is undertaken to produce refractories silica bricks from silica sands. Different
mixtures were prepared containing additives to produce silica bricks fired by electrical and
tunnel furnaces. The description of raw materials, additives, mix proportioning, preparation of
specimens, firing stages and experimental details will be stated in the sections below. The
main details of experimental program followed through this work are illustrated in Figure 1.
Materials Used
Raw Materials (Silica Sand): Silica sand is mainly located in Ardhumma quarry about 17
km-west of Rutba town in Al-Anbar Governorate (Gindy and Ibrahim, 1982). In present
study, silica sands have been examined as raw materials for silica bricks industry; these raw
materials has been supplied by the State Company of Geological Survey and Mining. The
chemical analysis of sand used in the present investigation compared with its typical
composition are given in Table 1. Besides, the mineralogical analyses for these raw materials
were done by X-ray diffraction are shown in Figure 2.
Additives
Dextrin: Dextrin was used as a bonding material in preparing silica brick specimens, which
was added to the mixes with a ratio of 0.7 % by weight. Although dextrin loses its resinous
properties at slightly low temperatures due to its decomposition, this is not weakness in its
behavior, because the main function is to give the moulded brick the required strength during
loading and transporting to the kiln (Skeist and Sinjer, 1963).
Slaked Lime: Slaked lime from Karbala factory have been used in this investigation as a
mineralizer in silica bricks specimens. Slaked lime was added as a ratio of 2% by weight.
Lime must be completely slaked, where the accumulation of lime in the form of lumps is
dangerous, since it is converted to CaO during firing, and if the silica bricks are stored for a
long time where moisture can affect it, the lime begins to slake intensively causing the
development of cracks (Budnikov, 1964). The chemical analysis of slaked lime done by the
State Company of Geological Survey and Mining shows the percentage of lime is 94.57 %.
Iron Oxide: Powder of iron oxide (Fe2O3) has been used as a mineralizer which was added
with slaked lime to produce mixes with two mineralizers. Iron oxide was added with a ratio
of 2 % by weight. The percentage of iron oxide which has been examined also in the (State
Company of Geological Survey and Mining) is 93.54 %.
Mixing Water: Tap water was used as mixing water for all mixes.
Manufacturing Silica Brick Specimens
Preparation of Raw Materials (Silica Sand): The preparation of silica sand for
manufacturing silica bricks requires two processes, crushing and grinding in order to attain
finer sizes. After the above processes the product has been divided into six groups, each group
was subdivided into three mains subgroups: “coarse, medium and fine” as illustrated in Table
2. For preparing mixes another three groups have been subdivided into three subgroups. The
first subgroup represents three different mixes with coarse group is predominant. While in the
second and third subgroups, the same number and subdivisions are made but the medium and
fine groups are predominant respectively. In comparison with this classification, Al-Hamdani
(1997) suggested 3 moderately different grain size groups for preparing silica bricks from
silcrete and silica sand.

3
Silica Sand: For preparing silica sand, sieving and grinding processes have been carried out.
Sieving sand and barring the passing through sieve size1.18 mm and impurities were retained
on the sieve, then silica sand was washed with water and dried in oven at temperature of 110
o
C for 48 hours. In order to attain finer sizes grinding process was also done by “Porcelain
Ball Mill”. Six groups were stated to silica sand as mentioned above (Table 2).
Mixes Preparation: Silica brick specimens were prepared from silica sand contained two
mineralizers (lime + iron oxide). Adding the additives to the mix, in each compound addition
the products were mixed roughly to obtain higher homogeneity for the mix (Table. 3).
Moulding
Fixing the Suitable Loading: To fix the suitable value of loading, several specimens have
been prepared by semi-dry compaction method under different selected loads (10, 20, 30, 40,
50 and 60) kN. Specimens under load of 60 kN were avoided due to deformation resulting
from powder cohesion with mould sides. Other specimens were fired in the same conditions
and according to a firing program. After firing: compressive strength, apparent porosity and
bulk density were examined to obtain the suitable loading.
The relationship of bulk density, apparent porosity and compressive strength with varied
loads indicate that apparent porosity decreases with increasing loads and it can be seen that
the minimum apparent porosity occurs between (40-50) kN. Also the results show the bulk
density increases with increasing load, and the maximum bulk density occurs between (40-50)
kN. Besides, compressive strength exhibits an increment with the increasing load and also the
maximum value occurs between (40-50) kN. According to these results the load of 44 kN was
chosen.
Shaping: The semi-dry compaction method was used with moisture content of 6% by weight
of mix. A locally manufactured cylindrical mould (40*100) mm was used. Shaping samples
were done by filling the mould with mix, compacted, loading under 44 kN using compression
machine type AVERY with a capacity of 2000 kN then releasing the specimens by pressing.
Drying and Firing
Drying: Electrical dryer was used to dry silica brick specimens at temperature of (50-60) oC
for 5 days.
Firing: In the present study two types of furnaces have been used, these are:
(A) Electrical program furnace belongs to Production and Minerals Engineering
Department of the University of Technology type “Gallenhamp” was used. The
firing temperature of this furnace was 1600oC. Firing program (Table 4) was
distributed on 8 firing stages including 4 soaking times to convolve the volumetric
expansion accompanied with quartz conversions. Four soaking times were done at
temperatures 573, 870, 1000 and 1400°C. The first three temperatures represent the
conversions of β-quartz to α-quartz, α-quartz to α-tidymite and α-quartz to α-
cristobalite respectively. And as silica conversion is rapid over 1250°C, so it is
necessary to increase firing time to 24 hrs to ensure the complete conversion.
(B) Tunnel kiln that belongs to Falluja Refractories Factory was used. This kiln, 150 m
in length, with temperature range of (1350 -1400) oC. Specimens were loaded in
trucks, which entered the kiln. After 12 days the specimens were taken from the kiln.
Testing Program
The details of specimens manufactured in this study are tabulated in Table 3.
Mineralogical and Chemical Analyses of Silica Bricks: These tests were done on several
specimens of manufactured silica bricks. Test results will be shown later .
Thermal Linear Change Cylindrical specimens (40*20) mm manufactured from silica sand
were used to examine linear change after firing. The average of three specimens was
calculated by using the following formula:
Linear change % = [L2 – L1] / L1 *100 (1)

4
 where:
L1: length of test specimens before firing, (mm).
L2: length of test specimens after firing, (mm).
Bulk Density and Apparent Porosity These properties were measured according to ASTM
C20-87(1989), by using (40*20) mm manufactured from silica sand. The average of three
specimens for each group was calculated by using the following equations:
V=w–S (2)
B = D/ V (3)
P % = [ (w – D) / V ]* 100 (4)
where:
V: Exterior volume, (cm3).
B: Bulk density, (gm/cm3).
P %: Apparent porosity.
D: Dry weight of specimen, (gm).
S: Suspended weight of specimen, (gm).
w: Saturated weight of specimen, (gm).
True Specific Gravity: A pycnometer method was adopted in this study to determine the true
specific gravity according to ASTM C135-86 (1989). True specific gravity is calculated from
the following formula:
True specific gravity= ( W-P ) / [ ( W1-P ) - ( W2-W ) ] (5)
where:
P = Weight of the pycnometer, (gm).
W = Weight of the pycnometer and sample, (gm).
W1=Weight of the pycnometer filled with water, (gm).
W2= Weight of the pycnometer, sample, and water, (gm).
Permanent Linear Change after Reheating: This test was conducted on cylindrical
specimens (40*20) mm manufactured from silica sand. According to B.S 1902-5.01 (1986),
the length of specimen was measured before and after reheating to 1400 °C for two hours as a
soaked period. The following equation is used to calculate the change:
ΔL % = [L2 – L1] / L1 *100 (6)
where:-
ΔL %: Percent of permanent linear change.
L1: length of test specimens before reheating, (mm).
L2 : length of test specimens after reheating, (mm).
Cold Compressive Strength: The compressive strength test was determined according to
ASTM C133 (2004), using (40*20) mm cylindrical specimens for silica bricks manufactured
from silica sand. In this test, 2000 kN capacity, ELE digital testing machine was used. The
recorded value represents an average of three reading measured on three specimens for each
group.
Thermal Conductivity: This test was carried out on (40*6) mm cylindrical specimens using
Lee’s disk with power supply type (PHYWE) available in the Applied Science Department of
the University of Technology. The following equations are used to calculate thermal
conductivity (Grimsehl, 1944):
IV=π r2e (TA+TB)+2πre [ dATA + dS 0.5( TA+TB )+ dBTB + dCTC ] (7)
K [(TB-TA)/dS]= e [TA+ 2/r ( dA+0.25 dS ) TA + 1/2 r dSTB ] (8)
where:
IV: Thermal energy passing through coil after reaching thermal equilibrium.
e: Amount of energy passing through material disk at unit area for each second
(W/m2.second)
d A, B, C, S : Disk thickness, (m).

5
 r: Disk radius, (m).
s: Specimen.
TA, B, C: Disk temperature.
K: Coefficient of thermal conductivity.
Spalling Resistance: The spalling resistance measurements were conducted on silica brick
specimens from silica sand by exposing the specimens to cycles of heating and cooling. The
specimen was heated to 450oC then it was cooled by forced air, this is considered as one
cycle. The cycles continue until failure of specimen (Mohanty et. al., 1982a). In this test
electrical furnace type “HERAENS – W 10/10, 1000 oC” was used in addition to tunnel kiln.

3. Results and Discussion

The chemical analyses of silica sand and silica brick specimen (for example specimen
TS2) reflect the high percentage of silica (98.63%) with a small amount of impurities in the
raw materials, these are in conformity with those stated by Shaw (1972), BS 4966:part1
(1982), GOST 4157-48 (1979) and DIN-1089 (1970) requirements as shown in Tables 1 and
5. While, high content of iron oxide in the specimen is attributed to the use of this oxide as a
mineralizer. The results of mineralogical analysis of silica sand using X-ray diffraction (Fig.
2) shows that silica sands are composed of quartz only.
The results of linear change after firing for specimens made up of silica is given in Figure
3. The effect of firing on linear change generally indicates that after firing its value for
electrical furnace specimens is lower than tunnel kiln specimens. Results of linear change for
electrical furnace specimens show a decrease of about (20.12-35.31)% of those fired in tunnel
kiln. This decrease may be attributed to the regularity of firing process in electrical furnace.
Thermal linear change also varies with particle size distribution tending to increase as the
amount of fine particle size of material increases. For specimens fired in electrical furnace,
generally, it increases with increasing fine grains as shown in Figure 3. Specimens with 60%
of fine group (S3 and TS3) exhibit an increase in linear change of about 28.8% and 14.3%
respectively of those specimens with 15% fines (S1 and TS1).
Results of apparent porosity before and after firing for all types of silica bricks (Table. 6
and Fig. 4) clearly show that the porosity of silica bricks before firing depends on grain size
(Fig. 4a). With fine increase, the porosity increases as contact areas between grains increase.
After firing, the porosity of all specimens fired in both electrical and tunnel furnaces have
higher values than those before firing. Besides, higher values of porosity have been noticed
for all specimens fired in electrical furnace than those fired in tunnel kiln with an increment of
about (8.1-10.4)% (Fig.4b). The increase in apparent porosity of silica bricks fired in
electrical furnace is related to the high degree quartz conversion to cristobalite and tridymite,
in which open structure is accompanied with the latter (Norton, 1974) which conforms results
obtained by Al-Hamdani (1997). The results also show the effect of grain size on porosity
after firing, where the porosity increases with the increasing fines. Results of silica brick of
mainly fines group fired in electrical furnace and tunnel kiln specimens (S3 and TS3) which
were made up of silica sand show an increase of about 7.1% and 4.9% of those coarse group
(S1 and TS1) respectively. This may be due to the fact that the nature of fine grains hastens
the conversion of quartz to cristobalite and tridymite as well as causes an increase in apparent
porosity. These results are in agreement with Sinjer and Sinjer (2001) whom report that the
difficulty of producing dense silica brick due to conversion of one crystal form to another
leads to complete rearrangement of grains. The obtained results of whole specimens are
coincident with the requirement of BS 4966: part1(1982), which constrains the value of
apparent porosity to 25% as a maximum. The apparent porosity of all specimens (except
specimens S3) are coincident with requirement of GOST 4157-48 (1979) which constrains the
maximum value of apparent porosity to 23%.

6
 The of bulk density results for silica bricks before and after firing (Table. 6 and Fig. 5)
obviously show that bulk density after firing is lower than before firing, and generally the
silica bricks manufactured from silica sand fired in electrical furnace show a decrease of
about (2.2-3.5)% of those fired in tunnel kiln. The possible logical explanation of this
phenomenon may be attributed to the relation of bulk density with the degree of conversion of
quartz to cristobalite and tridymite (Sinjer and Sinjer, 1963). The effect of grain size on bulk
density reflects that the increment of fines leads to decrease in bulk density, also its values are
lower for electrical furnace than tunnel kiln (Fig. 5). Also silica bricks manufactured from
silica sand were affected by grain size distribution. Bulk density for specimens (S3) and (TS3)
is lower by about 3.5 and 2.2% respectively with respect to (S1) and (TS1). This behavior
may be attributed to the effect of fine grains increment which speeds up the conversion of
quartz to other phases causing an increase in apparent porosity and in turn a decrease in bulk
density. Accordingly, a reverse relation is noticed between apparent porosity and bulk density
and this is in agreement with those results obtained by Jafar (1990) who examined such
properties for silica bricks made up of silica sand.
The results of true specific gravity for all types of silica bricks indicate the higher values
for specimens fired in tunnel kiln than that of those fired in electrical furnace (Fig. 6). For
silica bricks manufactured from silica sand fired in tunnel kiln show an increase of about (0.8-
1.3)% over those of fired in electrical furnace. The difference in values of specific gravity
may be attributed to the nature of firing in both furnaces, because a slight change in firing
temperatures will cause a significant effect on specific gravity for silica bricks (Chesters,
1973). Besides any deficiency in firing temperature may cause an increase in true specific
gravity of silica bricks (Budnikov, 1964), for this the specific gravity for tunnel specimens is
higher than that of electrical specimens. Also, the grain size has an effect on specific gravity
where the later decreases with the increase in fine grain size (Fig. 6). Regarding, silica brick
specimens (S3) and (TS3) show a decrease of about 1.7 and 2.1% of those specimens (S1) and
(TS1) respectively. This behavior may be attributed to a significant increment of fine grains
which in turn speeds up the conversion of quartz, and then decreases specific gravity for silica
bricks reaching 2.31-2.33 for a complete conversion (Budnikov, 1964) and this is due to
lower specific gravity of cristobalite and tridymite. These results are in agreement with those
of Jafar (1990) who investigated such property in silica bricks made up of silica sand.
Results of permanent linear change after reheating (Fig.7) show that electrical kiln
specimens have lower permanent linear change than that of tunnel kiln specimens. The silica
brick specimens (S3) and (TS3) showed a decrease about 49.3 % and 182 % respectively with
respect to specimens (S1) and (TS1). This behavior is attributed to the same explanation
regarding conversion process, because the fine grains increment leads to reduction in residual
quartz resulting in turn in low permanent linear change. This behavior is coincident with the
results obtained by Jafar (1990) who examined the permanent linear change of silica bricks
made up of silica sand.
Cold compressive strength values (Fig. 8) of specimens fired in electrical furnace are
higher than those of fired in tunnel kiln The specimens made up of silica sand with an
increase of about (18.7-48.1)%. The decrease for specimens fired in tunnel kiln may be
ascribed to the effect of firing process were low values indicate incomplete firing stage, since
silica bricks get its higher compressive strength by recrystallization during final stages of
firing Norton, 1968). These results are in agreement with those of Hasan et. al. (2001) whom
found that increasing the sintering time of the firing tends to improve the cold compressive
strength. It is clearly shown the compressive strength is improved with increasing fine sizes
(Fig. 8). The compressive strength for specimens of predominantly fine grain size fired in
electrical furnace and tunnel kiln (S3 and TS3) increases by about 37.6 and 10.2% of those
with coarse group specimens (S1 and TS1) respectively. This may be due to the increase in

7
fine grains which catalyze the conversion and in turn increase in compressive strength.
Besides the increase of fine grains leads to increase in the connection points and in turn leads
to uniformly distributed stresses within the brick and finally increases compressive strength.
These results are in agreement with those obtained by Al-Hamdani (1997) who investigated
such property for silica bricks.
Results of thermal conductivity of silica bricks showed that there is an inverse relationship
between thermal conductivity and apparent porosity (Fig. 9a). This is attributed to the
existence of pores filled with air leading to decrease in the thermal conductivity, and this is in
agreement with the study carried out by Hasan et. al. (2001) whom examined the thermal
conductivity for silica bricks. Besides, the nature of firing affects apparent porosity and in
turn the thermal conductivity. For silica bricks made up of silica sand, an increase about
(13.6-16.9)% with respect to electrical furnace specimens. This is attributed to the lower
apparent porosity for tunnel kiln specimens. The significant effect of grain size on apparent
porosity leads to an important effect on thermal conductivity (Figs. 9b). Generally, thermal
conductivity decreases with increasing fine grains. For silica brick specimens (S3) and (TS3)
show a decrease of about (37.6 and 38.2)% of those specimens (S1) and (TS1) respectively.
This behavior may be attributed to increase in fine grains leading to increase in apparent
porosity and consequently decrease in thermal conductivity.
Results of spalling resistance for all specimens presented in Figure 10, while the failure of a
specimen is shown in Figure 11. The effect of firing stage on spalling resistance indicate that
for tunnel kiln specimens is higher than that for electrical furnace specimens (Fig. 11). This
may be due to thermal conductivity for tunnel kiln specimens is higher than that of electrical
furnace specimens, and this leads to spalling resistance of tunnel kiln specimens being higher.
The effect of grain size distribution on spalling resistance has been examined indicating the
significant decrease in spalling resistance of silica bricks with increasing fines (Fig.10). It has
been attributed to the fact that thermal conductivity of fine grain specimens is lower than
those with coarse ones (Mohanty et. al., 1982b).

4. Conclusions
From the above results and discussions, the following conclusions can be drawn:
1. The chemical analysis results of silica sand show its high purity (98.63% SiO2). The
mineralogical analyses using XRD show that quartz is the main constituent suggesting its
suitability for silica brick manufacturing.
2. The chemical analysis results of manufactured silica bricks after firing are in conformity
with most standard requirements specification. Besides, XRD results indicate the
appearance and disappearance of different phases, which are due to the degree of
conversion which is affected by nature of firing, distribution of grain size and the type of
mineralizers used.
3. Firing in electrical furnaces is better than in tunnel kiln due to the complete quartz
conversions have been occurred whereas incomplete conversion is obtained in tunnel kiln.
4. Silica refractory bricks can be manufactured from silica sand by means of tunnel kiln but
with firing period not less than 12 days.
5. The effect of rate and type of firing temperature show the increase of some properties
when specimens are fired in tunnel kiln (with respect to electrical furnace) such as linear
expansion (20-35%), bulk density (2-3.5%), true specific gravity (0.8-1.3%), permanent
linear change (200-350%), thermal conductivity (14-17%) and spalling resistance (6-8%).
Whereas, other properties increase when specimens are fired in electrical furnace (with
respect to tunnel kiln) such as apparent porosity (8-10%) and cold compressive strength
(19-48%).

8
6. The effect of grain size distribution indicates that the increment in fine grain leads to
increase in the linear expansion for both electrical furnace and tunnel kiln firing
respectively (29-14%), apparent porosity (7-5%) and compressive strength (38-10%).
While a decrease is stated in bulk density (3.5-2%), true specific gravity (1.7-2%),
permanent linear change after reheating (49-280%), thermal conductivity (37.5- 38%) and
spalling resistance (26-25%).

References
1. Abhijit, J. Alkali Resistance (AR) of refractory lining materials (Bricks and Castable).
J. Eur. Ceam. Soc., Vol. 36, PP. 405-421, 2010.
2. Al- Hamdani, F. A.H. Geochemistry and mineralogy of Silcrete and silica sands from
the Western Desert and their suitabilkity for the manufacture of silica brick.
Unpublished Ph. D Thesis, College of Science, University of Baghdad, 1997,
167 P.
3. Al-Taie, M. H., Hajib, T., Al-Safar, N. S. and Abu-Safia, A. Refractory Bricks. Report,
University of Technology, 1977, PP.13-20.
4. ASTM C135-86. Standard Test Method for True Specific Gravity of Refractory
Materials by Water Immersion. Annual Book of ASTM Standards, Vol.15.01, 1989.
5. ASTM C397-83. Standard Practice for Use of Chemically Setting Chemical-Resistant
Silicate and Silica Mortars. Annual Book of ASTM Standards, Vol.4.05, 1989.
6. ASTM C267-82. Standard Test Method for Chemical Resistance of Mortars, Grouts,
and Monolithic Surfacings. Annual Book of ASTM Standards, Vol.4.05, 1989.
7. ASTM C 133. Standard Test Method of Cold Compressive Strength. Annual Book of
ASTM Standards, Vol.15.01, 2004.
8. ASTM C20-87. Standard Test Method for Apparent Porosity, Water Absorption,
Apparent Specific Gravity, and Bulk Density of Burned Refractory Brick and Shapes
by Boiling Water. Annual Book of ASTM Standards, Vol.15.01, 1989.
9. BS 1902, Section 5.10. Determination of Permanent Change in Dimension on Heating
of Dense Shaped Products. British Standards Institution, 1986, 6 P.
10. BS 4966, Part 1. Silica Refractories, Specification for Refractories for Use in Coke
Oven. British Standards Institution, 1982.
11. Budnikov, P. P. The Technology of Ceramics and Refractories. The M.I.T. Press,
Cambridge, Mass, 1964, 649 P.
12. Chesters, J. H. Refrctories Production and Properties. The Iron and Steel Institute,
Carlton House Terrace, London, 1973, 553 P.
13. DIN 1089. Refractory Building Materials, Coke Oven Bricks-Lime-bonded Silica
Bricks, Requirements and Testing. November, 1970, Sheet 1.
14. Gindy, L. and Ibrahim, N. Evaluation of Ga’ara Clays for Their Utilization in Ceramic
Industries. Report 72/82, Scientific Research Council, Baghdad, 1982, 52 P.
15. GOST 4175. Specifications of Silica Bricks for Open Hearth Furnace Roofs. 1979.7 P.
16. Hasan, S. A. and Al-Shama’a, Lamia. The Effect of Particle Size Distribution on The
Property of Silica Brick. Symposium on Refractories, March. 2001, PP. 2-8.
17. Jafar, M. Sh. A study of the effect of grain size on properties affecting thermal
conductivity of silica refractories. Unpublished M. Sc. Thesis, Chemical Eng. Dep.,
University of Technology, 1990, 135 P.
18. McColm, I. J. Ceramic Science for Materials Technologists. First Published, Furnival
House, Holborn, London, 1983, 357 P.
19. Mohanty, P. N., Singh, P. N. and Singh, G. D. Silica–A critical Study. Part 1 ,
Refractories Journal, No. 2, March/April, PP. 9-14, 1982a.

9
20. Mohanty, P. N., Singh, P. N. and Singh, G. D. Silica–A critical Study. Part 2,
Refractories Journal, No. 3, May /June, PP.10-17, 1982b.
21. Norton, F. H. Refractories. McGraw-Hill, United State, 1968, 450 P.
22. Padgett, G. C. Refractory Materials-The Conflict with Nature. Refractories Journal,
No. 4, July/August, 1984, 6 P.
23. Raymond, P., Robert,W, and Andreas, B. Magnesium aluminate sipnel raw materials
for high performance refractories. J. Amerc. Ceram. Soc., Vol.34, PP. 87-99, 2005.
24. Shaw,K. Refractories and their uses. Applied Science Publishers, London,1972, 269 P.
25. Sinjer, F. and Sinjer, S. S. Industrial Ceramics. Chemical Publishing Co., New York,
1963, 1455 P.
26. Skeist, F. and Sinjer,S. S. Industrial Ceramics. Chemical Publishing Co., 1963, 1455 P.
27. Taber, W.A., Refractories for classification. Refractories Applications and News, V. 8,
No. 4, PP. 118-22, 2003.

Table. 1. Chemical composition of silica sand*.

Item Chemical Composition Silica Sand Content Typical Composition
% (McColm, 1983)
Silica SiO2 98.63 92.0 - 98.0
Lime CaO 0.1 0.2 - 1.6
Iron Oxide Fe2O3 0.08 0.15 - 3.0
Magnesia MgO 0.07 0.1 - 0.6
Titania TiO2 0.17 ……….
Alumina Al2O3 0.36 0.5 - 2.5
Alkalies K2O 0.09 0.2 – 0.5
Na2O 0.08
Loss On Ignition L.O.I 0.37 0.2 - 1.0
* Chemical analysis was made by State Company of Geological Survey and Mining Baghdad, Iraq.

Table. 2. Mixes for silica sand.

Subgroup Sieve Size (mm) Mixes Percentages Mixes Percentages Mixes Percentages
st nd
for 1 Group for 2 Group for 3rd Group

Mix (S1)% Mix (S2)% Mix (S3)%

Coarse 0.85 - 0.60 25 10 5

Group 0.60 - 0.425 25 10 5
Medium 0.425 - 0.30 20 35 15
Group 0.30 - 0.15 15 25 15
Fine 0.15 - 0.075 15 15 30
Group < 0.075 0 5 30

10
 Table. 3. Silica brick specimens prepared from quartzite.
Mix No. Specimens with lime and Specimens with lime and iron
oxide fired in tunnel kiln
iron oxide fired in
electrical furnace
1 S1 TS1
2 S2 TS2
3 S3 TS3

Table. 4. Firing Program in electrical furnace.

Temp. oC Heating rate (oC/ Soaking Time
hr.) (hr.)

Start…..573 70 ………….
573 …………. 12
573…..870 70 ………….
870 …………. 12
870…..1000 70 ………….
1000 …………. 12
1000…..1400 70 ………….
1400 …………. 24

Table . 5. Chemical analysis of silica bricks *.

Oxide Content (%) BS 4966: Part 1 GOST 4157-48 DIN-1089 (1970)
Specimen (TS2) (1982)
A B C

SiO2 94.97 94.0 (min.) 94.5(min.) 92.5 92.5 92.5

(min.) (min.) (min.)
CaO 2.19 ….. ….. 3.5 3.5 3.5
Fe2O3 1.96 ….. ….. ….. ….. …..
MgO 0.07 ….. ….. ….. ….. …..
TiO2 0.16 ….. …..
Al2O3 0.31 ….. ….. 1.5 2.5 2.5
K 2O 0.07 ….. ….. ….. ….. …..
Na2O 0.07 ….. ….. ….. ….. …..
L.O.I 0.0 ….. ….. ….. ….. …..
* Chemical analysis was made by State Company of Geological Survey and Mining Baghdad, Iraq.

Table. 6. Apparent porosity and bulk density of silica bricks before firing.
Specimen Porosity (%) Bulk Density (gm/cm3)
S1 19.58 2.093
S2 20.38 2.091
S3 21.26 2.089

11
 Raw materials (Silica sand)

Washing

Grinding, grading and sieving

Coarse mixes Medium mixes Fine mixes

Addition of additives (Dextrin, lime,

iron oxide and water)

Moulding

Drying

Firing in electrical Firing in tunnel kiln

furnace

Silica bricks from silica

sand

Chemical
analysis Mineralogical
Tests analysis

Linear Apparent Specific Permanent Cold Thermal Spalling

change porosity gravity linear compressive conductivity resistance
and change strength  
Bulk density  

Fig. 1. Schematic representation of the experimental program.

12
 Fig. 2. X-ray diffraction analysis of silica sand.  
                                             (The test was done by the State Company of Geological Survey and Mining).  
 
 

 
Fig.3. Linear change of silica sand bricks.

(a)
(b)               

Fig. 4. Relationship between apparent porosity and maximum grain size before (a) and after (b)
firing of silica sand specimens.

13
Fig. 5. Bulk density and maximum grain size after firing of silica sand specimen.

Fig. 6. True specific gravity and maximum grain size of silica sand specimens.

Fig. 7. Permanent linear change and maximum grain size of silica sand specimens.

14
 Fig. 8. Cold compressive strength of silica sand bricks.

(a) (b)
Fig. 9. Relation between thermal conductivity with apparent porosity (a) and grain size (b) of silica
sand brick specimens.

Fig. 10. Spalling resistance of silica sand bricks.

(a) (b)
Fig. 11. Cracks development in silica sand bricks before (a) and after (b) spalling.

15

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