FLM

Final Progress Report

ASSESSMENT OF WATER REPELLENT PERFORMANCE ON CORRUGATED FIBER CEMENT ROOF SHEET USP Team:Prof. Dr. Vanderley Moacyr John, Prof. Dr. Kai Loh, MSc. Flvio Leal Maranho
So Paulo, 2007

ASSESSMENT OF WATER REPELLENT PERFORMANCE ON CORRUGATED FIBER CEMENT ROOF SHEET FINAL REPORT

Contents
Introduction ......................................................................................................................... 4 1.1 Objective: .................................................................................................................. 5 1.2 1.3 1.4 1.5 Project Design ....................................................................................................... 5 Laboratory Step ..................................................................................................... 5 Industrial Application ........................................................................................... 6 Structure ................................................................................................................ 7

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Preparation of Specimens .................................................................................................... 9 2.1 Objective.................................................................................................................... 9 2.2 Method ....................................................................................................................... 9 2.3 Materials .................................................................................................................. 12 2.3.1 Water Repellents............................................................................................... 12 First Round ........................................................................................................................ 14 3.1 3.2 3.3 3.4 3.5 Objective ............................................................................................................. 14 Materials and methods ........................................................................................ 14 Assessment Parameter ........................................................................................ 14 Specimens ........................................................................................................... 15 Results ................................................................................................................. 15

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3.4.1 Admixture Application ..................................................................................... 15 3.4.2 Post-treatment Application ............................................................................... 16 3.6 Conclusion .......................................................................................................... 18

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Second Round .................................................................................................................... 21 4.1 4.2 4.3 4.4 Objective ............................................................................................................. 21 Materials and Methods ........................................................................................ 21 Evaluation Parameter .......................................................................................... 22 Specimens ........................................................................................................... 23

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4.5

Results ................................................................................................................. 23

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4.5.1 Application Method .......................................................................................... 23 4.5.2 Superwetter ....................................................................................................... 24 4.5.3 Efflorescence .................................................................................................... 25 4.5.4 Water absorption............................................................................................... 26 4.6 Conclusions ......................................................................................................... 27

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Third Round....................................................................................................................... 30 5.1 5.2 5.3 5.4 Objective ............................................................................................................. 30 Materials ............................................................................................................. 30 Specimen Dimension .......................................................................................... 32 Results and Analysis ........................................................................................... 32

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5.4.1 Water Absorption ............................................................................................. 32 5.4.1.1 Conclusions ................................................................................................... 38 5.4.2 MOR ................................................................................................................. 40 5.4.3 Fracture Toughness .......................................................................................... 41 5.5 Conclusions ......................................................................................................... 43

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Industrial Application Report ............................................................................................ 46 Conclusions ....................................................................................................................... 51

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Introduction
Cellulose fiber has been used to substitute asbestos on Fiber Reinforced Cement (FRC) roof tiles, despite the fibers mineralization caused by the wet-and-dry cycles (Dias; John, 2005). Mould growth is another problem caused by the absorption of water and it influences the FRC aesthetical and thermal performance. To improve the FRC performance, hydrophobic products have been used in plants, despite the little amount of information published so far. Water repellents aim to prevent the materials degradation and to reduce soiling, which is mainly influenced by mould growth, thus improving the general appearance of the product and the energy efficiency of the building. The water repellent most widely used in building materials is silicone based materials (mainly silane and siloxane). These products have a good hydrophobic property (by the non-polar radical) and Si-O and Si-C bond stability. In FRC there are different ways to introduce water repellent products in plants. The first one is to treat the cellulose fibres directly (Abdelmowlett et al, 2004). The second is to add the repellent during the admixture of raw materials (Selley et al, 2006). The advantage of these methods is that they protect the thickness and edges of all sheets. However, they modify particle flocculation in plants and cement hydration kinetics, thus influencing the mechanical properties (mainly MOR) and the sheet layer adhesion. The third method used to protect FRC sheets is a post-treatment application (Selley et al, 2006), which is the most widely used in other building materials, such as mortar, concrete and stone. Many factors influence the hydrophobic performance in this method, such as: (i) method of application (spray, paint or dipping), (ii) product concentration and (iii) moment of application (before or after curing). It is not easy to compare the different methods because no complete published research has been identified in the literature.

For industrial plants, the post-treatment application is easier to put in action but its performance in service conditions is not well understood and is largely influenced by cracks (Lunk; Wittmann, 1998). As other application methods could influence the FRC mechanical properties and the flocculation process in the hatcheck machine, more researches are required before any industrial application.

1.1 Objective:
To select the most effective water repellent produced by Dow Corning to protect asbestos-free fibrocement corrugated sheets.

1.2
plant.

Project Design

The research was divided in two steps: one in USP laboratories and other in INFIBRA

The first step aimed to identify the water repellent and the concentration that showed the best performance in laboratory evaluations, while in the second step a semi-industrial application was tested. Figure 1 shows the methodology used.

Laboratory Step
First Round Second Round Third Round

Industrial test

Figure 1: Methodology used in the Research Program Figure 2

1.3

Laboratory Step

The experimental design was divided in three rounds. In the first round, nine water repellent products were tested (five applied as post-treatment and four as admixture) using only one concentration for each product. Water absorption after immersion for 24 hours was used as parameter for evaluation.

In the second round three products (520, 6683 and 16-606) at different concentrations were investigated using water absorption kinetics along 24 hours as parameter for evaluation. Superwetter performance, the application method (brush or immersion) and the prevention of efflorescence were also investigated. In the third round three products (520, 6683 and 16-606) at different concentrations were submitted to accelerated aging in laboratory conditions. The evaluation parameters were water absorption kinetics along ten days, MOR and Fracture Toughness. Table 1 shows the experimental design used.
Table 1: Methodology used in the laboratory program research

Round first

Products

Objective

9 (5 post-treatment and 4 as To screen three with the admixture) best performance (2 post- To determine the water repellent concentration; To about obtain the information Superwetter

second

products

treatment and 1 admixture)

performance; To develop application

procedure and to determine efflorescence prevention. third 3 products (2 post- To aging evaluate accelerated

treatment and 1 admixture)

1.4

Industrial Application

The industrial application was conducted in INFIBRA plant. A semi-industrial application was tested using only the best product and concentration identified in the laboratory steps. Emulsion absorption and consumption were identified.

1.5

Structure

This report is divided in seven chapters. In the first one an introduction about the research is presented. It also contains an overview about the theme and the methodology used in the project. In the second chapter the preparation method of the specimens and the raw materials used in the laboratory steps are presented. In Chapters 3, 4 and 5 the results and comments obtained in the first, second and third rounds, respectively, are presented. In Chapter 6, the industrial application is reported and in Chapter 7 the most important conclusions are pointed out.

Chapter 2: Preparation of Specimens

Preparation of Specimens 2.1 Objective

To present the raw material and procedures used to produce the specimens in the laboratory steps. The materials, except the cement, used in the different rounds were the same.

2.2 Method
The following steps were followed to produce the specimens: 1. Admixture of raw materials to produce the pulp, using a solid/water ratio of 0.20; 2. Apply vacuum (hatcheck); 3. Compression; 4. Curing in an oven at 65C and 90%RH for 18 hours; 5. Apply the post-treatment water repellents; 6. Curing in a plastic bag for 28 days; 7. Cut the specimens in suitable dimensions; 8. Seal the border; 9. Dry in an oven at 65oC and 50 RH for 2 days; 10. Test. Figure 3 and Figure 4 show the materials used in the research program.
Figure 3 Raw Materials used to produce the sheets

Cement (~30 bfSlag) Limestone Silica fume

Weight ( ) 70.2 20.0 5.0

PVA fiber

1.8

Dry cellulose

3.0
Figure 4: Materials used to produce the sheets

The admixture procedure was: Add water in the barrel; Add cellulose and mix for 2.0 minutes using a rotation rate of 400rpm (Figure 5);

Figure 5: Mixture barrel and the mixing with water and cellulose fiber.

Add the PVA fiber and mix for one more minute (Figure 6) Add cement, limestone and silica fume and mix for 3.0 minutes at the same rotation rate (Figure 7).

Figure 6: Mixture after adding the PVA fiber

Figure 7: Mixture of all raw materials

After this procedure the pulp was ready to produce the sheets.

For each sheet, two liters of pulp were poured into the mold with vacuum until no more water was eliminated (Figure 8). This process is similar to that used in fiber-cement plant technology and known as Hatcheck method.

Figure 8: Vacuum application

Finally each sheet was compressed on a Shimatzu Universal Machine with a 0.3MPa for 1.0 minute (Figure 9) and then stored in a plastic bag for 28 days. Only after this time the sheets were cut to produce the specimens used in each round.

Figure 9: Compression with a Shimatzu universal machine.

2.3 Materials
2.3.1 Water Repellents
Table 2 shows the water repellents used in this project. All concentration and dilution rates used in the test were based on the emulsion weight and not in the activity materials.
Table 2: Products used in the first step

Admix 16-606 6288 6777 772

Use level 0.5 0.5 0.5 0.5

General Description octyl functional silicone fluid octyl functional silicone fluid propyl siliconate methyl siliconate

Comments dispersed directly into water. dispersed directly into water. soluble in water soluble in water

Posttreatment

Dilution rate

General Description silane/siloxane emulsion, MeH containing silane/siloxane emulsion water repellent octylsilane water dispersible siloxane methyl siliconate

Comments

520 6683 6341 6184 772

10 10 10 20 5

dilute in plain water to recommended , based on 40 as-supplied. dilute in plain water to recommended , based on 40 as-supplied. dilute in white spirit, such as Shellsol D60 water dispersible -- dilute by adding 1-6184 to water, not by adding water to 1-6184. dilute in plain water to recommended , based on 40 as-supplied.

Chapter 3: First Round

First Round 3.1 Objective

The objective was to evaluate the performance of nine different water repellents produced by DOW CORNING around the world and screen three with the lowest water absorption. Moreover, the aim was to investigate the influence of steam curing on the performance of the water repellents.

3.2

Materials and methods

The products used in this round are presented in Table 3. For the post-treatment application the concentration was based on the emulsion weight. The application was by dipping the specimens in the solution for 30 seconds. The admixture concentration was based on the total water weight used in the production.
Table 3: Materials and concentrations used in the first round.
Product Concentration(%)

16-606 6288 Admixture 772 6777 520 6341 Post-treatment 6683 772 6184

0.5 0.5 0.5 0.5 10 10 10 5 20

3.3

Assessment Parameter

The water absorption result after 24 hours of immersion was used as evaluation parameter. This parameter was decided by the project team (DCC and USP) in the meeting at 04/11/2006.

3.4
sealed with bee wax.

Specimens

In the first round, round specimens were used, as illustrated in Figure 10. The borders were

Figure 10: Illustration of the round specimens cut from the sheet.

3.5

Results

3.4.1 Admixture Application

Figure 11 shows the water absorption results for the water repellents used as admixture. In the figure the continuous lines represent the average value, while the dashed lines mean the standard deviation. Moreover, the green lines represent the untreated results, while the red lines, the treated results. The results clearly show that products 6288 and 16-606 had lower water absorption rates than the other ones.
25% Water Absorption (%) 20% 15% 10% 5% 0% 0 2 4 TIME (H^0.5) 6 8

6288
Water Absorption (%)

25% 20% 15% 10% 5% 0% 0 2

16-606

4 TIME (H^0.5)

25% 20% 15% 10% 5% 0% 0 2

772

25% 20% Water Absorption (%) 15% 10% 5% 0%

6777

Water Absorption (%)

4 TIME (H^0.5)

4 5 TIME (H^0.5)

Figure 11: Water absorption results for the admixture water repellents. All concentrations were 0.5% based on water (W/W).

3.4.2 Post-treatment Application

Figure 12 shows the water absorption results for the water repellents applied as posttreatment. The dilution rate used for each product is identified in the figures. The continuous lines represent the average value, while the dashed lines, the standard deviation. The blue lines represent the after-curing application1 and the red lines, the before-curing application. The green lines represent the untreated samples. The figures clearly show that the application after curing yields better results and lower water absorption than the before-curing application for all products tested. Moreover, all treated samples show a water absorption increase along three days of immersion, reducing their performance compared to the untreated samples. Comparing the results after only one hour and one day of immersion, it is clear that product 6683 applied after curing showed the best result. One important point is that products 520 and 6683, when applied before curing, showed some white staining on the surface of the specimens (Figure 13).

Curing = 18 hours in ventilated oven at 65C and 95%RH.

25% 20% 15% 10% 5% 0% 0 2

520 (10%)

25%

6683 (10%)
20% Water Absorption (%)

Water Absorption (%)

15% 10%

5% 0%

4 TIME (H^0.5)

4 5 TIME (H^0.5)

25%

6341 (10%)
Water Absorption (%) 20% Water Absorption (%) 15% 10% 5% 0% 0 2 4 TIME (H^0.5) 6 8 25% 20% 15% 10% 5% 0% 0 1

6184 (20%)

3 TIME (H^0.5)

25% Water Absorption (%) 20% 15% 10% 5% 0% 0 2

772 (5%)

Figure 12: Water absorption results for the post-treatment application. Green = untreated; blue = after curing; red = before curing; dashed lines = standard deviation.

4 TIME (H^0.5)

Figure 13: White staining on the specimen surface after curing

3.6

Conclusion

Table 4 presents all results obtained in the first round. The best products for each period of time are identified in green. The worst products are in red.
Table 4: Water absorption results in the first round

Water Absorption (%) 30sec. 60 sec.

2.54 1.56 0.93 1.87 0.94 2.76 4.40 13.88 13.33 3.35 2.75 0.46 0.69 1.50 3.81

240 sec.
5.68 2.46 1.41 3.41 1.50 4.54 5.77 18.00 16.22 9.35 5.77 0.61 0.65 2.54 6.74

1 hour
15.96 8.55 5.52 10.37 4.12 6.62 6.80 21.50 17.51 16.33 10.74 1.06 0.84 6.55 13.87

24 hours
19.08 13.45 10.14 16.34 8.68 11.79 9.61 21.75 18.28 19.33 15.20 2.88 2.85 15.67 15.79

96 hours
19.92 17.90 12.84 18.61 11.62 13.21 10.15 21.78 18.97 21.16 15.39 5.48 5.89 16.77 17.08

Untreated
BC 520 AC BC 6683 AC

2.03 0.57 0.43 1.14 0.75 1.63 3.05 9.13 8.40 1.83 1.90 0.25 0.49 1.15 2.17

Posttreatment

BC 6341 AC BC 6184 AC BC 772 AC 6288

Admixture

16-606 6777 772

The main conclusions are:

Products 6288 and 16-606 showed the best performance; For the post-treatment application, 520 and 6683 showed the best performances. The first one was better to reduce water absorption in the first minutes, while the other was better for longer exposure times; The application after curing in the post-treatment application was better than that before curing;

 Product performance seems to decrease along the time; Some products applied as post-treatment show a white staining after curing (520 and 6683); The solvent-base product (6341) showed a strong and undesired smell after curing and which remained for a long time; Product 6184 became a gel during the application.

Chapter 4: Second round

Second Round 4.1 Objective

To evaluate the influence of water repellent concentration on hydrophobic performance and efflorescence prevention. Moreover, the influence of application method (brush or immersion) on the hydrophobic performance and the addition of Superwetter were investigated.

4.2

Materials and Methods

Table 5 shows the project design used in the second round

Table 5: Materials and concentrations used in the second round
Product Concentration 0.50% 0.25% Admixture 16-606 0.10% 0.05% 3% 520 Post-treatment 3% 6683 5% 10% 5% 10% Efflorescence, Application Method and Superwetter performance Efflorescence Test

For the post-treatment products, two coats of water repellent were applied using a foam roller. All applications were after curing. Superwetter (Q2-5211) is a surfactant that increases the absorption of the hydrophobic solution. This research used a concentration of 0.5% (W/W) based on the undiluted emulsion weight, according to DCC instructions. After the application of the water repellent the specimens were cured in a plastic bag for 28 days.

4.3

Evaluation Parameter

The evaluation parameters used in this round were: a) Superwetter: hydrophobic solution absorption and water repellency; The first parameter was obtained by measuring specimen weight before and after the application of the solution, while the second was obtained by measuring water absorption along 24 hours of immersion. b) Application method: compare the water absorption kinetics along 24 hours of immersion for samples treated by brushing or by immersion. c) Efflorescence: ice cube test (DCC instructions). According to this method an ice cube is left to melt and dry on the specimen surface (Figure 14).

Figure 14: Efflorescence test used in the second round

This method is qualitative and gives only comparative data. It is based on the increase of calcium hydroxide solubility as the temperature decreases (Figure 15). Products that show higher white staining in this test are more likely to produce efflorescence during service conditions.

1,4 1,2
Ca(OH) Solubility

1 0,8 0,6 0,4 0,2 0 0,0 20,0 40,0 60,0 80,0 Temperature (C) 100,0 120,0

Figure 15: Solubility of Calcium Hydroxide. Based on Taylor (1990)

4.4

Specimens

For the second round, 4cm square specimens were used and the borders were sealed with bee wax, similarly to the first round.

4.5

Results

4.5.1 Application Method

Figure 16 compares the water absorption kinetics along 24 hours of immersion for products 520 and 6683 at the concentration of 10%. The results show that brushing and immersion applications have similar results. In both products brushing was a little better (lower water absorption).
25%

6683
20%

Untreated

25%

520
20%

Water Absorption (%)

15%

15%

Immersion
10% 5%

10%

5%

Brushing
0% 0 1 2 3 TIME (H^0.5) 4 5 0% 0 1 2 3 TIME (H^0.5) 4 5

Figure 16: Results from different application methods for the post-treatment water repellent.

4.5.2 Superwetter
Figure 17 shows the absorption of the hydrophobic solution with (identified as with QI) and without (identified as without QI) Superwetter. It shows that: Q2-5211 did not increase the absorption of the hydrophobic solution; For 6683, Superwetter showed better results. The higher the WR dilution level, the higher the absorption of the solution;
3%

For 520, the lower the WR dilution level, the higher the absorption of the solution.

Solution Absorption

2%

1%

0%
Without With QI Without With QI Without With QI Without With QI Without With QI Without With QI QI QI QI QI QI QI

3%

5%

10%

3%

5%

10%

520

6683

Figure 17: Water repellent consumption with Superwetter (identified as QI) for 520 and 6683.

Figure 18 shows the water absorption after 24 hours of immersion.

18% Water Absorption after 24hours 16% 14% 12% 10% 8% 6% 4% 2% 0% 3% 5% TIME (H^0.5) 10% with Q2 5211 without Q2 5211

6683
Water Absorption after 24 houirs

18% 16% 14% 12% 10% 8% 6% 4% 2% 0% 3% with Q2 5211 without Q2 5211

520

5% TIME (H^0.5)

10%

Figure 18: The influence of Superwetter (Q25211) on water absorption at different concentrations.

It is clear that Superwetter did not increase water repellency performance for the products in the dilution rates tested.

4.5.3 Efflorescence
The main results are: The untreated samples showed a lot of white staini (Figure 19 staining 19); The post-treatment products (520 and 6683), at any concentration (3%, 5% or 10%), treatment reduced the stains ( (Figure 20 and 21). The higher the concentration, the smaller the ). white stains; The admixture water repellent (16 606) increased white staining (Figure 22). (16-606) (

Figure 19: Untreated samples showed typical white deposits after efflorescence test. :

3%

5%

10%

Figure 20: Specimens treated with WR 6683 showed typical white deposits after efflorescence test. :

3%

5%

10%

Figure 21: Specimens treated with WR 520 showed typical white deposits after efflorescence test.

0.10%

0.25%

0.50%

Figure 22: Specimens treated with WR 16-606 showed typical white deposits after efflorescence test.

Efflorescence reduction in the samples treated with post-treatment products is expected and well recorded in the bibliography, mainly because it reduces the cement alkalis dissolution. For both products (520 and 6683) the concentration of 5% showed very important reductions. On the other hand, increase of efflorescence in the admixture waters could not be justified by the test performed. It is a very important point in future researches focus on the admixture water repellent products.

4.5.4 Water absorption

Figure 23 shows the water absorption kinetics along 24 hours of immersion. All results presented do not have Superwetter.

25%

6683
20%
Water Absorption

25%

0%
20%

520

0% 3% 5% 10%

15% 10%

3% 5% 10%
15% 10% 5% 0% 0 1 2 3 Time (h^0.5) 4 5 0 1 2 3 Time (h^0.5) 4 5

5% 0%

25% 20%
Water Absorption

16-606

0%

Figure 23: Water absorption kinetics along 24 hours of immersion

15% 10% 5% 0% 0 1 2 3 Time (h^0.5) 4 5

0,05% 0,10% 0,25% 0,50%

The product used as admixture at any concentration showed a better performance than that of the post-treatment. For all products, the higher the concentration, the lower the water absorption. For post-treatment application, both products tested showed a very similar performance. However, WR 6683 was a little better.

4.6

Conclusions

Table 6 shows all water absorption results obtained in the water absorption test during the second round. The best options for each product are identified in green.
Table 6: Water Absorption results in the second round.

Water Absorption (%)

Time UNTREATED 10%withQ2 5211 10%withoutQ2 5211 5%withQ2 5211 5%withoutQ2 5211 3%withQ2 5211 3%withoutQ2 5211 10%withQ2 5211 10%withoutQ2 5211 5%withQ2 5211 30sec. 3.86 0.24 0.30 1.10 0.19 0.77 1.10 0.98 0.49 2.32 60sec. 5.53 0.27 0.26 1.09 0.76 0.84 1.09 1.54 1.11 3.40 240sec. 8.07 0.48 0.32 1.27 0.69 1.12 1.27 2.93 1.19 8.70 1hour 15.17 1.40 0.85 4.39 1.84 4.60 4.39 7.50 2.43 12.12 24 hours 20.46 11.52 7.09 14.32 12.75 16.67 14.32 12.91 7.68 15.89

Posttreatment 6683

520

Admixtur 16e 606

5%withoutQ2 5211 3%withQ2 5211 3%withoutQ2 5211 0.5% 0.25% 0.1% 0.05%

0.62 1.05 1.31 0.40 0.31 0.40 0.45

0.92 1.28 1.84 0.16 0.32 0.64 0.55

2.94 2.24 3.37 0.40 0.42 0.71 0.65

4.66 4.08 7.01 0.75 0.87 0.93 1.40

9.44 14.63 12.76 2.44 2.73 3.15 4.72

The main conclusions obtained in the second round are: The post-treatment application by brushing and immersion for 30 seconds showed similar performance for both products tested: 520 and 6683; Superwetter did not improve water repellent absorption and hydrophobic performance; The ice cube test is simple to perform and shows some important information about the prediction of efflorescence risk; The products applied as post-treatment reduced white staining in the efflorescence test, while the admixture increased it; The admixture water repellent at any concentration showed lower water absorption results than the post-treatment solutions.

Chapter 5: Third round

Third Round

5.1

Objective

To evaluate the influence of accelerated aging on water repellent performance.

5.2

Materials

The products used in the third round are presented in Table 7. For the post-treatment products, two coats were applied after curing using a foam roller. All applications were after curing. After the application of the water repellent the specimens were cured in a plastic bag for 28 days.
Table 7: Water repellents and concentrations used in the third round

Product

Concentration
0.50%

Test

Admixture

16-606

0.25% 0.10% 0.05% 3% Water Absorption MOR Toughness 150 cycles of accelerated aging

520 Post-treatment 6683

5% 10% 3% 5% 10%

Accelerated aging was performed at USP laboratories, using an automatic machine (Figure 24). It consists in 150 wet/dry cycles, each one lasting six hours: 6 hours 70C - drying 6 hours around 25C - wetting During the cycles only one side of the specimens was in contact with water (Figure 25), similarly to what may be observed in a roof.

Figure 24: Overview of the equipment used in accelerated aging

Figure 25: illustration of the water level during aging. Only one side of the specimens was wetted.

The modulus of rupture and the fracture toughness were evaluated using a four-point bending test. A support distance of 13.5cm, a load distance point of 5.0cm and a load rate of 1mm/min were used (Figure 26). This procedure has long been successfully adopted at USP laboratories. For the mechanical tests an Instron Universal Machine with a load cell unit of 1KN was used.

Figure 26: Equipment used in the mechanical evaluations

The modulus of rupture and the fracture toughness were calculated according to the equations:

Where: MOR= Modulus of Rupture (MPa) P = Maximum load (N) L = support distance (135mm)
b = specimen width (mm) e = specimen thickness (mm) = Fracture Toughness (KJ/m2)

Ap- = area below the curve up to the fracture (N.mm)

5.3

Specimen Dimension

In the third round, specimens measuring 16 cm x 3.7 cm x 0.5 cm were used. The borders were sealed with liquid rubber (3M product). The difference in dimension and border sealer was necessary to fit the temperature used in the accelerated aging equipment.

5.4

Results and Analysis

5.4.1 Water Absorption

a) WR 6683

Figure 27 shows the third round results for product 6683. It clearly shows that the higher the concentration, the lower the water absorption. After one day (24 hours) of immersion, for the concentration of 3%, and three days (72 hours), for the concentration of 5%, the results are similar to that of the untreated specimens.
25%

6683

Water Absorption

20% 0% 3% 5%

15%

10% 10% 5%

0% 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19

Time (h^0.5)

Figure 27: Specimens treated with WR 6683: water absorption kinetics after aging.

Figure 28 shows the results before and after aging for this product. Here, continuous lines represent the unaged results, while the dashed lines represent the aged results.

25%

6683

20%

0% 3% 5%

Water Absorption

15%

10%

10%
5%

0%

2 TIME (H^0.5)

Figure 28: Specimens treated with WR 6683: water absorption before (continuous line) and after accelerated aging (dashed line).

The comparative evaluation shows that: Accelerated aging has a small influence on 6683 performance; In first hour of immersion, the aged samples show higher water absorption, mainly at the highest concentration (Figure 29). 3% - ~0% 5% - +50% 10%- +150%

10% 9% 8% 7%

6683

Water Absorption \

6% 5% 4% 3% 2% 1% 0%

0% 3% 5% 10%

TIME (H^0.5)

Figure 29: Specimens treated with WR 6683: water absorption in the first hour before (continuous line) and after accelerated aging (dashed line).

b) WR 520 Figure 30 shows the third round results for product 520. The higher is the water repellent concentration, the lower was the water absorption (except at 5%, which probably showed some experimental error). One important point in this product is that after aging, all concentrations seem to show similar water absorption after four days of immersion. Figure 31 compares the unaged and aged results.

25%

520

20%
Water Absorption

0%
15%

10%

5% 4 days 3% 10%

5%

0% 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 TIME (H^0.5)

Figure 30: Specimens treated with WR 520: water absorption kinetics after aging.
25%

520

20%
Water Absorption

0% 3% 5% 10%

15%

10%

5%

0% 0 1 2 Time (h^0.5) 3 4 5

Figure 31: Specimens treated with WR 520: water absorption before (continuous line) and after accelerated aging (dashed line).

For this product the aging cycles reduce water absorption rates along the first day of immersion. This reduction was very important in the first hour (Figure 32). There is a 75% reduction for the highest concentration (10%), and a 55% reduction for the others (3% and 5%).

10% 9% 8%
Water Absorption

0%

7% 6% 5% 4% 3% 2% 1% 0% 0 Time (h^0.5) 1

3% 5%

10%

Figure 32: WR 520 water absorption in the first hour before and after accelerated aging. Continuous line= unaged, dashed line = aged

c) 16-606 Figure 33 shows the third round results for product 16-606. It clearly shows that all concentrations had a similar performance, and a continuous increase of water absorption along the ten days of immersion.
25%

20%

Water Absorption

15%

UNTREATED - after aging UNTREATED - Before aging 0,50% - after aging 0,50% - before aging 0,25% - after aging 0,25% - before aging 0,10% -After aging 0,10% - before aging 0,05% - after aging 0,05% - befor aging

16-606

10%

5%

0%

TIME (H^0.5)

Figure

34

25%

20%

Water Absorption

15%

UNTREATED - after aging UNTREATED - Before aging 0,50% - after aging 0,50% - before aging 0,25% - after aging 0,25% - before aging 0,10% -After aging 0,10% - before aging 0,05% - after aging 0,05% - befor aging

16-606

10%

5%

0%

TIME (H^0.5)

Figure 34 Figure 33: Specimens treated with WR 16-606: water absorption kinetics after aging

Contrary to what was expected, and as shown in the unaged results, the highest WR concentration (0.5%) did not show the best performance. In this case, the lower water absorption was for the concentrations of 0.10% and 0.25%. For all concentrations water absorption was much lower than that of the untreated samples. It reaches a 70% reduction during the first 24 hours of immersion and 45% after ten days. Figure 34 compares the aged and unaged results. It shows that the higher the WR concentration, the higher the water absorption caused by accelerated aging: 0.50% concentration - 100% 0.25% concentration - 10% 0.10% concentration - 21% 0.05% concentration - 0%

25%

20%

Water Absorption

15%

UNTREATED - after aging UNTREATED - Before aging 0,50% - after aging 0,50% - before aging 0,25% - after aging 0,25% - before aging 0,10% -After aging 0,10% - before aging 0,05% - after aging 0,05% - befor aging

16-606

10%

5%

0%

TIME (H^0.5)

Figure 34: Specimens treated with WR 16-606: water absorption before (continuous line) and after accelerated aging (dashed line).

5.4.1.1 Conclusions
The main conclusions are: Accelerated aging caused an important reduction in the water absorption rates of the untreated specimens (23% after 24 hours of immersion). According to the literature this behavior is normal and is caused by the increase in cement hydration, which reduces the matrix porosity; All products tested were slightly affected by aging cycles. Water absorption normally increased; For the post-treatment application, 520 showed a better performance during the first 24 hours of immersion, while 6683 was better for longer periods of time (Figure 35); The admixture products showed a better performance than the post-treatment products (Figure 36) during 24 hours of immersion. During the first four hours, which is a more likely rain duration, the diference is neglible.

200%

150%
Water Absorption 6683/520

3%

100%

10% 5%

50%

0% 0 -50% 2 4 6 8 10 12 14

-100%

Time (H^0.5)

Figure 35: 6682/520 Water absorption rate x time

18%
Water Absorption

15% 12% 9% 6% 3% 0% 0 1 2 3 Time (h^0.5) 4 5

0%

6683 - 10% 520 - 10% 16-606 0,25%

Figure 36: Best product concentration after aging cycles.

5.4.2 MOR
Figure 37 shows the MOR results.

15 12 MOR (MPa)

Untreated
MOR (MPa)

15 12 9 6 3 0

6683

9 6 3 0 Unaged Aged

3% Unaged 15 12 MOR (MPa) 9 6 3 0

5% aged

10%

15 12 MOR (MPa) 9 6 3 0 3%

520

16-606

5% Unaged Aged

10%

0,05%

0,10% Unaged

0,25% aged

0,50%

Figure 37: MOR results

The main conclusions are: For the untreated samples, aging did not affect the MOR. This result is in accordance with the bibliography (Savastano, 2006 and Dias, 2005) Unaged:
15 MOR (Mpa) 12 9 6 3 0 0% 2% 4% 6% 8% 10% 6683 520

Post-treatment WR does not affect MOR (Figure 38) Admixture WR (16-606): important influence on the MOR (Figure 39)
15 MOR (Mpa) 12 9 6 3 0 0% 2% 4% 6% 8% 10% 6683 520

Unaged - post treatment

Aged - post treatment

Figure 38: MOR Results x Post-treatment water repellent concentration left = unaged and right =

aged
15 12 MOR (Mpa) 9 6 3 0 0% 0,05% 0,10% 0,25% 0,50% Unaged Aged

16-606

Figure 39: MOR Results x 16-606 concentration

Aged: 6683 the higher the concentration, the lower the reduction 520 no influence 16-606 increases the MOR

5.4.3 Fracture Toughness

Figure 40shows the results.
9

Untreated
(KJ/m2

6683

6 kJ/m2

0 Unaged Aged

0 3% Unaged 5% Aged 10%

9 6 3 0 3%

520

9 6 KJ/M2 3 0

16-606

KJ/M2

5% Unaged

10% Aged

0,50%

0,25% Unaged

0,10% Aged

0,05%

Figure 40:Fracture Toughness results

The main conclusions about fracture toughness are: The untreated specimens showed an important reduction after aging (>70%); Both products applied as post-treatment showed a slight influence before aging; 16-606 causes an important influence before aging. The higher the concentration, the lower the fracture toughness; The water repellents applied as post-treatment reduce the fracture toughness degradation by aging (Figure 41).
9

6683
KJ/M2

520

KJ/M2

0 0% 5% Unaged 10% Aged

0 0% 2% 4% Unaged 6% Aged 8% 10%

Figure 41: Fracture Toughness results x water repellent concentration left = 6683 and right = 520
9

16-606

KJ/M2

0 0% 0,05% 0,10% Unaged 0,25% Aged 0,50%

Figure 42: Fracture Toughness results x 16-606 concentration

5.5

Conclusions

The main conclusions for the third round are: Untreated samples: aging reduces toughness

aging does not affect MOR aging reduces water absorption

Water repellent treatment Prevents toughness degradation by aging MOR can be influenced by aging Water absorption is much smaller than in the untreated specimens

Accelerated aging: minor effect on hydrophobicity Post-treatment: higher contents are better Higher hidrophobicity Increase resistance to mechanical degradation

16-606 Unaged: MOR reduction After aging: great improvement in the MOR and fracture toughness

Chapter 6: Industrial Test

Industrial Application Report

Objective: To test the post-treatment water repellent application procedure on asbestos-free asbestos corrugated sheets at INFIBRA Industrial Plant Date: 07/13/2007 Team: David Selley and Marcos Antonio (DCC); Vanderley John, Kai Loh and Flvio Maranho (USP), Luiz Fernando and Paulo Doniseti (INFIBRA) Materials: o Water repellent 520 at a concentration of 10% o Asbestos-free free corrugated sheets after steam curing Size

2.44X0.48X0.006m Report: Only product 520 was tested because there was no available time for the other one. All one corrugated sheets used in this test were asbestos-free and had been steam cured for 18 hours asbestos e a few minutes earlier. There is no specific information available about the composition of raw materials used. Two hundred kilos of water repellent were deposited in a plastic container (Figure 43), ( which was then filled with water, reaching a dilution of 10%, as previously agreed upon. Figure 44 shows the container dimension.

Figure 43: Water Repellent deposition in the : container Figure 44: Dimensions of the plastic container used in lastic

the industrial test

In the first stage ten corrugated sheets were immersed manually and individually for four minutes in the container with the water repellent solution. Then seven stacks, each one with eleven piled sheets, were dipped in the container for four minutes (Figure 45).

Figure 45: Immersion of the stack of corrugated sheets in the container.

The water repellent consumption was determined by measuring the volume of the solution before and after the immersion of the sheets. The result was 0.96 dm3/m2. Therefore, for a single sheet measuring 2.44m x 0.48m, the solution consumption was 112ml. The dipping time was determined by INFIBRA and corresponds to the time available in the normal demolding process. After four minutes of immersion, all sheets piled in the stack show uniformly and totally wet surfaces (Figure 46), which confirms the good absorption of the solution.

Figure 46: Surface of corrugated sheets after immersion for four minutes.

Along the first hour after immersion it was observed that the upper corrugation usually dried first (Figure 47). One hour after the immersion no stain was observed (Figure 48).

Figure 47: Illustration of dry behavior

Figure 48: Surface with no stain one hour after immersion

After the treatment, four stacks were separated for natural aging evaluation. Two of them were treated with 520 water repellent (manual and stack application) and two were not treated.

Treated by Stack

Untreated

Treated manually

Figure 49: Treated and untreated corrugated sheets

Chapter 7: Conclusion

Conclusions
Water repellent products have a large application potential in asbestos-free products, mainly because they reduce water absorption, mould growth, cellulose degradation and color alteration during service conditions. The Project design performed was effective to evaluate the performance of silicone-base water repellents and point out the best products. The water repellents used as admixture were clearly shown to be more efficient to reduce water absorption than the post-treatment. However, they influence the mechanical properties, and modify the flocculation kinetics in the hatcheck machine, thus requiring more researches before any industrial application. The post-treatment products are easier to introduce in industrial plants and, at a concentration of 10%, they show a very good performance (especially 520). The main conclusions obtained in all rounds of this first project are: Concerning the water repellent application: Post-treatment applications after steam curing are better than before curing Brushing and immersion are similar Superwetter did not work properly

16-606 increases the efflorescence risk, while the products applied as post-treatment strongly reduce it; The post-treatment application is easier and faster to introduce in plants; The products applied as admixture showed the lowest water absorption rates; 150 wet/dry cycles did not cause any important influence on the hydrophobic performance; Water repellent products (post-treatment and admixture) improve long-term toughness performance; Some WR reduce long-term MOR: 6683 (after aging)

16-606 (before aging)

The industrial application confirms a good water repellent emulsion absorption; The water repellent emulsion consumption observed in the industrial plant was around 10mL/m2.

Nome do arquivo: final.docx Diretrio: D:\Docs Flavio\empresas\dow corning\fibrocimento\files\final report\versao final Modelo: C:\Documents and Settings\Flavio\Dados de aplicativos\Microsoft\Modelos\Normal.dotm Ttulo: Final Progress Report Assunto: ASSESSMENT OF WATER REPELLENT PERFORMANCE ON CORRUGATED FIBER CEMENT ROOF SHEET Autor: USP Team:Prof. Dr. Vanderley Moacyr John, Prof. Dra. Kai Loh, Msc. Flvio Leal Maranho Palavras-chave: Comentrios: Data de criao: 18/9/2007 11:22:00 Nmero de alteraes:10 ltima gravao: 18/9/2007 12:39:00 Salvo por: Flavio Tempo total de edio: 85 Minutos ltima impresso: 18/9/2007 12:40:00 Como a ltima impresso Nmero de pginas: 52 Nmero de palavras: 6.235 (aprox.) Nmero de caracteres: 33.673 (aprox.)