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A Process of Lowering the Vitrification Temperature in the Manufacture of Ceramic Wares Utilizing Sargassum ( brown algae) as Fluxing Agent

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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.

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The present utility model further relates to a ceramic wares obtained by the claimed process.

Background of the Utility Model

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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.

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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

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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

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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.

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Summary of the Utility Model

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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

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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.

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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

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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

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eliminating) importation costs.

Manufacturing Process

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

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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:

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Treatment Means

 
 

Modulus

 

Formulation

Firing

Number of

% Total

of

% Water

Temperature

specimens

shrinkage

Rupture

absorption

(kg/cm²)

3%

 

60

X

1

Y

1

Z

1

sargassum

850 ºC

60

X

2

Y

2

Z

2

5%

     

sargassum

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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

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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

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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

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b. 3000 grams of Linamon clay with 150 grams sargassum

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

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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.

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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

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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

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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

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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:

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% water absorption = (wet weight - fired weight/fired weight) x 100

3. Determination of Modulus of Rupture

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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.

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Modulus of rupture was computed using the formula:

 

MOR = 3PL/2bd²

 

Where:

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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

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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

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its initial value at 3% sargassum addition.

 
 

Table 3.1

Summary of Physical Property Test Results

 
   

% Total

Modulus of Rupture (kg/cm²)

% Water

Formulation

Shrinkage

Absorption

3% sargassum

8.87

14.74

22.88

5% sargassum

8.40

18.09

22.16

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The following graphs show the effect of sargassum addition on total shrinkage, strength and water absorption of ceramic articles.

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% Total Shrinkage

9

8.9

8.8

8.7

8.6

8.5

8.4

8.3

8.2

8.1

% Total Shrinkage 9 8.9 8.8 8.7 8.6 8.5 8.4 8.3 8.2 8.1 3% sargassum 5%
% Total Shrinkage 9 8.9 8.8 8.7 8.6 8.5 8.4 8.3 8.2 8.1 3% sargassum 5%

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

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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

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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

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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.

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20 18 16 14 12 10 8 6 4 2 0 3% sargassum 5% sargassum
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18
16
14
12
10
8
6
4
2
0
3% sargassum
5% sargassum
Formulation
Modulus of Rupture (kg/cm2)

Graph 3.2 Effect of Sargassum Addition on Strength

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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

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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.

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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

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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.

     

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      23  
      23  
 

% Water Absorption

22.8

22.6

22.4

22.2

22

 

21.8

 

3% sargassum

5% sargassum

Formulation

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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

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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

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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

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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

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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.

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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

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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

     

Propertiexs

Ideal Range

3% sargassum

5% sargassum

% Total Shrinkage

0

to 13

8.87

8.40

Modulus of Rupture (kg/cm²)

3.52 to 105.63

14.74

18.09

% Water

     

0

to 23

22.88

22.16

Absorption

 

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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.

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Appendix A: Analysis of Variance on the Effect of Sargassum Addition to

Shrinkage of Ceramic Article

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

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2. α = 0.05

3. Test Statistics: F statistics

4. Critical Region: F o > F 0.05(1,4) = 7.71

5. Computations:

SS Total = 0.3

SS Treatment = 0.113

SS

Error

= 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

F

o

Variation

Squares

Freedom

 

Treatment

0.113

1

0.113

2.42

Error

0.187

4

0.047

 

Total

0.3

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Decision: Accept Ho, Sargassum addition has no significant effect on shrinkage of ceramic ware at α = 0.05

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1

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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. H 1 : Sargassum addition has significant effect on strength of ceramic article.

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2. α = 0.05

3. Test Statistics: F statistics

4. Critical Region: F o > F 0.05(1,4) = 7.71

5. Computations:

SS Total = 58.74

SS

SS Error = 41.71

Treatment

= 16.83

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

Source of

Sum of

Degrees of

Mean Square

F

o

Variation

Squares

Freedom

 

Treatment

16.83

1

16.83

1.61

Error

41.71

4

10.43

 

Total

58.74

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

ceramic article at α = 0.05

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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

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article. H 1 : Sargassum addition has significant effect on water absorption of ceramic

article.

2. α = 0.05

3. Test Statistics: F statistics

4. Critical Region: F

5. Computations:

SS Total = 1.184

o

> F

0.05(1,4)

= 7.71

SS Treatment = 0.785

SS Error = 0.399

Analysis of Variance on the Effect of Sargassum Addition to Water Absorption of Ceramic Article

Source of

Sum of

Degrees of

Mean Square

F

o

Variation

Squares

Freedom

 

Treatment

0.785

1

0.785

7.87

Error

0.399

4

0.0998

 

Total

1.184

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

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CLAIMS:

 

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1.

A process of lowering the vitrification temperature in the manufacture of ceramic wares comprising the steps of:

 

a.

Selection of Raw Materials

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Linamon clay materials;

and seaweeds (brown algae) were selected as raw

b.

Preparation of Raw Materials

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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;

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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:

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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;

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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

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50-mm reference mark;

d. Drying and Firing

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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

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dimensions of each test bar was measured and recorded;

e. Determination of the Physical Properties

Determination of the percentage total shrinkage, percent water absorption

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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.

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

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Engr. Ryan D. Corpuz, MAKER

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ABSTRACT

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.

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