A Process of Lowering the Vitrification Temperature in the Manufacture of

Ceramic Wares Utilizing Sargassum ( brown algae) as Fluxing Agent

5 Field of the Utility Model

The present utility model relates to a process of lowering the vitrification

temperature in the manufacture of ceramic wares particularly red ceramic wares by
utilizing Sargassum ( brown algae) as a fluxing agent.
10
The present utility model further relates to a ceramic wares obtained by the
claimed process.

Background of the Utility Model

15
It is widely known that our country is rich in natural resources. A huge need
implanted in us is to utilize those resources wisely, especially now that we are in the
midst of a big global financial crisis, to make way for developments, sustain (or even
continuously improve) those advancements and eventually survive.
20
The biggest challenge facing industries now is how to increase productivity
at reduced operating costs. Technological advancements have helped improve
quality control techniques, material handling and storage, and other organizational
processes. However, basic manufacturing processes that require high energy
25 consumption remained unchanged.

The use of sargassum (commonly known as seaweeds or brown algae) as flux

in lowering the vitrification temperature of functional and decorative red clay
ceramic wares will be a major breakthrough that will change the basic ceramic firing
30 process commonly employed at temperatures above 1000°C. The incorporation of
this potassium-rich material into the locally-available red clay in producing ceramic
wares will allow early vitrification at a lower temperature without significant
changes in physical properties such as shrinkage, flexural strength, and porosity.

1
 Summary of the Utility Model

5 The present process primarily and specifically aims to produce a red clay-
ceramic ware at 850°C with the incorporation of sargassum as fluxing agent.
Moreover, it intents to evaluate the physical properties of these wares after firing
(in terms of percentage total shrinkage to determine the degree of contraction,
percentage water absorption to verify the extent of porosity and Modulus of Rupture
10 to confirm the flexural strength) and compare these properties with a known
structural ceramic ware standard (roofing tiles) to confirm the viability of sargassum
as a flux and validate the feasibility of producing functional ceramic wares with the
aid of this material at low temperature.

15 Detailed Description of the Utility Model

The present utility model will be advantageous to the ceramic industry,

especially in reducing both energy consumption and raw material importation costs
(costs of buying materials from outside sources or other places, including material
20 handling and storage cost and freight). Fuel consumption will be minimized because,
instead of processing above 1000°C which requires higher amount of energy and
longer time, processing could be attained at a lower temperature and shorter time.
Accordingly, since the material used (sargassum and red clay) are just available
locally, importation of raw materials can be avoided, thus minimizing (or eventually
25 eliminating) importation costs.

Manufacturing Process

In determining the effect of sargassum addition on the strength, shrinkage

30 and water absorption of Linamon clay-based ceramic ware, a one-factor Analysis of
Variance experimental design was conducted. Below are the process steps and
conditions:

2
 Treatment Means
Modulus
Firing Number of
Formulation % Total of % Water
Temperature specimens
shrinkage Rupture absorption
(kg/cm²)
3% 60 X1 Y1 Z1
60 X2 Y2 Z2
sargassum 850 ºC
5%
sargassum

5 Starting Raw Materials

The starting materials used are the following:

1. Linamon Clay from Robocon, Lanao del Norte.
2. Seaweeds from Samburon, Lanao del Norte.
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Preparation of Raw Materials

Linamon clay and sargassum were oven-dried at 110ºC for four hours to
remove their moisture content. The clay was then crushed in a blake-type jaw
15 crusher and fed in a pulveriser to further reduce the grain size. Sargassum, on the
other hand, was pulverized using mortar and pestle and screened using a 100-mesh
sieve to remove its impurities.

Production of Test bars: Soft Mud Method

20
1. Batching and Mixing
Two batches of plastic mass were prepared by mixing clay and sargassum
with water until the desired plasticity was attained:
a. 3000 grams of Linamon clay with 90 grams of sargassum
25 b. 3000 grams of Linamon clay with 150 grams sargassum

3
 These were then wrapped with cellophane and allowed to age for five days to
enhance plasticity.

5 2. Forming
The aged plastic masses were formed into test bars with 9cm x 2cm x 0.9 cm
dimensions. After that, the test bars were labelled and marked with 50-mm reference
mark.

10 Drying and Firing

The test bars were dried at room temperature (25° C) for seven days and were
further dried in an electric oven at 110 ºC for four hours to remove mechanical
water. Then, those two batches composed of 60 test bars each were fired in an
15 electric muffle furnace set at 850°C. After firing, the weight and dimensions of each
test bar was measured and recorded.

Determination of the Physical Properties

20 1. Determination of % total shrinkage

Reference marks were measured using vernier caliper after firing. The %
total shrinkage was determined using this formula:

% total shrinkage = (initial length - fired length/ initial length) x 100

25
2. Determination of percent water absorption
Test bars were boiled for four hours in a thermostatic water bath, soaked for
24 hours, and weighed. Water absorption percentage was then calculated using
the formula:
30
% water absorption = (wet weight - fired weight/fired weight) x 100

3. Determination of Modulus of Rupture

4
 Dimensions of test bars were measured. The test bars were placed in a three-
point loading set up on the Universal Testing Machine. The maximum load was
recorded at the breakage point of each test bars.

5 Modulus of rupture was computed using the formula:

MOR = 3PL/2bd²

Where:
10 P is the maximum load at breakage point
L is the distance between two supports
b is the width of test bar
d is the thickness of test bar

15 Results

Summary of the effect of sargassum addition on the physical properties at

850°C is presented in the table below. 5% sargassum addition reduced shrinkage and
water absorption, and at the same time increased the strength of ceramic article from
20 its initial value at 3% sargassum addition.

Table 3.1 Summary of Physical Property Test Results

% Total Modulus of % Water
Formulation
Shrinkage Rupture (kg/cm²) Absorption
3% sargassum 8.87 14.74 22.88
5% sargassum 8.40 18.09 22.16

25 The following graphs show the effect of sargassum addition on total

shrinkage, strength and water absorption of ceramic articles.

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 9
8.9

% Total Shrinkage
8.8
8.7
8.6
8.5
8.4
8.3
8.2
8.1
3% sargassum 5% sargassum
Formulation

Graph 3.1 Effect of Sargassum Addition on Total Shrinkage

The above graph shows that at 5% sargassum addition, shrinkage was reduced
5 by about 5% of its initial shrinkage at 3% sargassum addition. Although the
ANOVA results (see Appendix A) have shown that this is not significant at α = 0.05,
we can somehow conclude that sargassum could be a filler or non-plastic material, if
not an excellent one, because it reduces shrinkage which is possible only with non-
clay or non-plastic materials such as quartz, alumina and grog that restrain shrinkage
10 by not reacting or not allowing water to pass through its matrix.

The above statement is verified by Salmang (1961) who said that shrinkage is
associated with the clay content only. Any addition of non-plastic material will not
increase shrinkage as water vaporizes, instead it would lead to diminution of
15 contraction as what had happened when we incorporated sargassum on red clay. This
is, therefore, an evidence that sargassum does behave like other fluxes for it exhibits
non-plastic characteristic.

20

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 20

Modulus of Rupture (kg/cm2)

18
16
14
12
10
8
6
4
2
0
3% sargassum 5% sargassum
Formulation

Graph 3.2 Effect of Sargassum Addition on Strength

5 The 5% sargassum addition led to an increase of strength by about 4% of its

initial strength at 3% sargassum addition. According to Steinzor (1986), the more
alkali ion a flux has the more melt it produces and upon cooling, the denser and
stronger an article would become. In this case, since sargassum is rich in potassium
(one of the alkali elements), the incorporation of this material in red clay introduced
10 more potassium ion to it and upon firing this potassium ion reacted with other clay
impurity ions such as iron, calcium and sodium to form a melt. This melt in turn fills
the gaps between unreacted particles and reacts with its surface, if possible, and bind
them together into a denser mass, resulting to an increase in strength and decrease in
porosity.
15
Based on the results of Analysis of Variance (see Appendix B), sargassum
addition has no meaningful effect at α= 0.05. However, by observing the trend, we
could somehow hypothesize that if we further increase the addition of sargassum,
strength will also increase. In fact, according to Salmang (1961) strength could be
20 enhanced further if non-plastic addition will not exceed 63% of the body. Since we
have shown earlier that sargassum has non-plastic characteristic, increasing

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 sargassum addition further up to 63% of our clay material is still satisfactory to
increase strength.

23
% Water Absorption

22.8

22.6

22.4

22.2

22

21.8
3% sargassum 5% sargassum
Formulation
5
Graph 3.3 Effect of Sargassum Addition on Water absorption

ANOVA results (see Appendix C) showed that at α = 0.05, sargassum

addition has significant effect on water absorption. Addition of 5% sargassum
10 reduced water absorption by about 3% of its initial value at 3% sargassum addition.
This effect is due to the reduction of pores during vitrification.

Water absorption is related to the degree of porosity. According to Salmang

(1961), if we added 0 to 63% of non-plastic materials to clay, the porosity will
15 diminish. This is what happened as we increased sargassum from 3% to 5%. By just
a 2% increment, a significant effect was detected on its water absorption property.

To sum up everything we have presented earlier, the incorporation of

sargassum into red clay introduced potassium ion which reacted with other impurity
20 ions present in clay such as calcium, sodium and iron which led to melting. The
melts produced in turn fill the spaces between unreacted particles and react with its
surface, if possible, and bind them together into a denser mass upon cooling. This

8
 incorporation increased strength while reducing both linear shrinkage and water
absorption after firing. Due to these effects, the researchers are convinced that
sargassum is indeed a flux because it exhibited the characteristics of common fluxes
on firing.
5
Summary of Results

Sargassum’s capability as flux in lowering the vitrification temperature of red

clay down to 850 °C was presented. Its addition reduced shrinkage and water
10 absorption, and at the same time increased the strength of ceramic article. Moreover,
the values obtained for the physical properties sought, fell within the ideal range of
acceptability as a functional ware. These are summarised on the table that follows:

SUMMARY OF RESULTS
Physical
Ideal Range 3% sargassum 5% sargassum
Propertiexs
% Total Shrinkage 0 to 13 8.87 8.40
Modulus of
3.52 to 105.63 14.74 18.09
Rupture (kg/cm²)
% Water
0 to 23 22.88 22.16
Absorption

15 The above results show that sargassum is indeed a flux for it bears the
characteristics of fluxes. It was able to vitrify the ceramic material at a low
temperature which led to the reduction of pores, minimization of shrinkage and
enhancement of strength. Furthermore, the physical properties of the materials
obtained were suitable for use as a functional ceramic ware.
20

25

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 Appendix A: Analysis of Variance on the Effect of Sargassum Addition to
5 Shrinkage of Ceramic Article

1. Ho: Sargassum addition has no significant effect on shrinkage of ceramic article.

H1: Sargassum addition has significant effect on shrinkage of ceramic article.
2. α = 0.05
10 3. Test Statistics: F statistics
4. Critical Region: Fo > F0.05(1,4) = 7.71
5. Computations:
SSTotal = 0.3
SSTreatment = 0.113
15 SSError = 0.187

Analysis of Variance on the Effect of Sargassum Addition to the Shrinkage

of Ceramic Article
Source of Sum of Degrees of Mean Square Fo
Variation Squares Freedom
Treatment 0.113 1 0.113 2.42
Error 0.187 4 0.047
Total 0.3 5

Decision: Accept Ho, Sargassum addition has no significant effect on shrinkage of

ceramic ware at α = 0.05
20

25

1
0
 5 Appendix B: Analysis of Variance on the Effect of Sargassum Addition to the
Strength of Ceramic Ware

1. Ho: Sargassum addition has no significant effect on strength of ceramic article.

H1: Sargassum addition has significant effect on strength of ceramic article.
10 2. α = 0.05
3. Test Statistics: F statistics
4. Critical Region: Fo > F0.05(1,4) = 7.71
5. Computations:
SSTotal = 58.74
15 SSTreatment = 16.83
SSError = 41.71

Analysis of Variance on the Effect of Sargassum Addition to Shrinkage of

Ceramic Article
Source of Sum of Degrees of Mean Square Fo
Variation Squares Freedom
Treatment 16.83 1 16.83 1.61
Error 41.71 4 10.43

Total 58.74 5

Decision: Accept Ho, Sargassum addition has no significant effect on strength of

20 ceramic article at α = 0.05

1
1
 5
Appendix C: Analysis of Variance on the Effect of Sargassum Addition to the
Water Absorption of Ceramic Ware

1. Ho: Sargassum addition has no significant effect on water absorption of ceramic

10 article.
H1: Sargassum addition has significant effect on water absorption of ceramic
article.
2. α = 0.05
3. Test Statistics: F statistics
15 4. Critical Region: Fo > F0.05(1,4) = 7.71
5. Computations:
SSTotal = 1.184
SSTreatment = 0.785
SSError = 0.399
20

Analysis of Variance on the Effect of Sargassum Addition to Water

Absorption of Ceramic Article
Source of Sum of Degrees of Mean Square Fo
Variation Squares Freedom
Treatment 0.785 1 0.785 7.87
Error 0.399 4 0.0998
Total 1.184 5

Decision: Reject Ho, Sargassum addition has significant effect on water absorption
of ceramic article at α = 0.05

25

1
2
 5

CLAIMS:

10 1. A process of lowering the vitrification temperature in the manufacture of

ceramic wares comprising the steps of:

a. Selection of Raw Materials

15 Linamon clay and seaweeds (brown algae) were selected as raw

materials;

b. Preparation of Raw Materials

20 Linamon clay and sargassum were oven-dried at 110ºC for four hours
to remove their moisture content; the clay was then crushed in a blake-type
jaw crusher and fed in a pulveriser to further reduce the grain size;
Sargassum, on the other hand, was pulverized using mortar and pestle and
screened using a 100-mesh sieve to remove impurities;
25
c. Production of Test bars: Soft Mud Method
Batching and Mixing
Two batches of plastic mass were prepared by mixing clay and
sargassum with water until the desired plasticity was attained:
30 a. 3000 grams of Linamon clay with 90 grams of sargassum
b. 3000 grams of Linamon clay with 150 grams sargassum;

These were then wrapped with cellophane and allowed to age for five
days to enhance plasticity;

1
3
 Forming
The aged plastic masses were formed into test bars with 9cm x 2cm x
0.9 cm dimensions after which the test bars were labelled and marked with
5 50-mm reference mark;

d. Drying and Firing

10
The test bars were dried at room temperature (25° C) for seven days and
were further dried in an electric oven at 110 ºC for four hours to remove
mechanical water; then, those two batches composed of 60 test bars each were
fired in an electric muffle furnace set at 850°C; after firing, the weight and
15 dimensions of each test bar was measured and recorded;

e. Determination of the Physical Properties

Determination of the percentage total shrinkage, percent water absorption

20 and Modulus of Rupture revealed that the product of the present utility model
utilizing seaweed as flux is superior that existing product and lower the fluxing
temperature as much as 30%.

2. A ceramic article obtained by the process according to claim 1.

25
3. A process according to claim 1, wherein the vitrification temperature is 850 °C or
less.

30

Engr. Ryan D. Corpuz,

MAKER

1
4
 5

ABSTRACT

10
The present utility model relates to a process of lowering the vitrification
temperature in the manufacture of ceramic wares specifically red clay ceramic wares
by utilizing Sargassum ( brown algae) as a fluxing agent . It further relates to a
ceramic article obtained by the claimed process.
15

1
5