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Properties and processing of Wood Densification by THM Parviz Navi Thematic Session “Modelling of THM treated wood, Joined Action FP0802, FP0904 August 24, 2011, Helsinki

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Page 1: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Properties and processing of Wood

Densification by THM

Parviz Navi

Thematic Session “Modelling of THM treated

wood, Joined Action FP0802, FP0904

August 24, 2011, Helsinki

Page 2: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

contents

1- Compression methods

1.1 Open systems (atmospheric pressure)

1.2 Closed systems (pressurized gas environment)

1.3 Mixed systems

1.4 unidirectional (platen press)

1.4 Compression forming (Two-directional compression)

1.5 Isobar (membrane press, 3D)

Page 3: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

contents

2. Effects of THM processing on wood

2.1 Physical effects: Glass transition, Elasto-viscoplasticity,

and shape memory or compression set-recovery

2.2 Chemical : TH wood degradation, fixation set-recovery

2.3 Effects of THM parameters on wood properties

3. Conclusions

Page 4: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1- Compression methods

1.1 Open systems (atmospheric pressure)

Schema of the process

THM densification with open-system process using an hydraulic

press with heated plates, moisture content is 15% maximum

Page 5: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1.1 Open systems (atmospheric pressure)

Production of a rolled wooden tube in a mold (courtesy from P.

Haller)

a) charging b) Closing c) Forming

Page 6: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1.1 Open systems

Example of tube construction

Tube Spruce, fabricated by densified

bended wood panels, Photo P. Haller

(2008) Filament winding of moulded tubes

(Haller, 2009)

Page 7: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1- Compression methods

1.2 Closed systems (pressurized gas environment), THM treatment

Densifying Apparatus (pressure vessel) up to 150°C and saturated

steam: (a) closed condition, (b) open condition,1) chamber, 2) piston,

3) mould, 4) cover, 5) densified wood, (Navi & Girardet, 2000).

Page 8: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1.2 Closed systems (pressurized gas environment)

Photograph of a THM

(pressure vessel or reactor)

together with control panels

Schematic representation of a

THM reactor showing ingoing

and outgoing streams to

cylindrical chambers

Page 9: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1.2 Closed systems

Multi-layer THM reactor

Page 10: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Diagram of THM processing (Treatment chamber) – 4 stages

Page 11: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Forming a trunk by THM closed system

Photo of a two layered THM reactor, opened state.

Diameter of the cylinder is 20 cm.

Page 12: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Densified trunk of pine (one dimensional)

Two cross-sections of one directional radial densified trunk of pine

after drying. The trunk after densificatin sawn into two parts and

dried. This shows cracks formed on the wood during drying

(Girardet and Navi, 2007)

Page 13: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1.3 unidirectional densification

(a) (b)

(a) Spruce before densification

d= 430 kg/m3

(b) After densification

d= 1290 kg/m3

degree of densification 68 %

(c) Pine before densification

d= 490 kg/m3

(d) After densification

d= 1300 kg/m3

degree of densification 68 %

(Navi and Girardet)

(c) (d)

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Viscoelastic Thermal Compression device (VTC):

Diagram showing the press inside to the chamber, platens

and the specimen between the platens (F. Kamk)

1.3 unidirectional (platen press), VTC, (Mixed system)

Page 15: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1.3 unidirectional (platen press), VTC, (Mixed system)

Large Viscoelastic Thermal Compression device (VTC):

Photograph of the interior of the chamber (Courtesy of F. Kamk)

Page 16: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Viscoelastic thermal compression process

(VTC)

Phase 1 – steaming

Phase 2 – venting

Phase 3 – compression

Cooling – specimens are cooled under compression

Page 17: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1.4 Compression forming (Two-directional compression)

THM apparatus (pressure vessel or reactor) and the internal

moulding block (Ito et al. 1998 )

Page 18: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1.4 Compression forming (Two-directional compression)

• Transformation of a circular trunk to a square-section by two-

dimensional densification (Ito et al., 1998a)

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1.4 Compression forming (Two-directional compression)

Compressed Lumber Processing System

Temperature in the THM chamber during the post-processing

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1.4 Compression forming (multi-directional compression)

Photo of two pieces of densified wood fabricated by

“Compressed Lumber Processing system”

Page 21: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1.5 Isobar (membrane press - 3D)

• This is a 3D densification referring to the

membrane press method (pressure vessel + a

flexible membrane and steam) where

compression occurs under three-dimensional

uniform applied stress. Constant fluid pressure

(isobaric) on the membrane causes

compression of substrate in regions with least

resistence, (F. Kamke).

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2. Effects of THM processing parameters on wood

2.2 Chemical : TH wood degradation

Samples are compressed at different temperatures between110°C

and 200°C in a closed system.

Degree of set-recovery of compressed samples measured under

water soaking-drying cycles (Heger, 2004).

Page 23: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

2.2 Chemical : TH wood degradation

Set-Recovery (R) of samples compressed at different temperatures between

110°C and 200°C at a compression rate of 10 mm/min (Heger, 2004).

Page 24: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Sample of densified spruce

compressed to 35 %; detail of

a partially crushed earlywood

zone.

Sample of densified spruce

compressed at140°C under

saturated moisture conditions.

Page 25: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

2.2 Chemical : degradation of wood constituents

High temperature steam, chemically degrades

wood constituents (here only up to 200C° considered)

Chemical degradation of wood constituents

is function of Temperature, Moisture Content

and Processing Time.

In both Heat-treatment and THM wood

densification under the same T & H the

degradation is similar.

In THM densification the process needs water

or (steam).

Page 26: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

In wood at high temperatures, water plays three

important roles:

it makes hydrolysis possible

it ensures the mobility of the protons

it participates in the acidification of the reactive

medium

________________

Definition of hydrolysis : A chemical reaction in which

water is used to break down a compound; this is achieved

by breaking a covalent bond in the compound.

The most important of degradation is wood

hydrolysis (specially the hemicelluloses), function of

T, MC and t

Page 27: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

1- Hydrolysis of polysaccharides:

Treatments Man

Xyl Gal Ara Total

Reference (natural) 13.6 5.6 2.8 1.2 23.2

Densified 9.7 4.7 1.2 0.7 16.3

Densified and post-treated

(180°C, 30 min)

5.6 2.0 0.5 no-

traces

8.1

Densified and post-treated

(200°C, 5 min)

5.4 2.8 0.4 no-

traces

8.6

Quantitative analysis of hemicelluloses by GPC (gas

phase chromatography)

Percentages of the different neutral sugars in treated wood

after washing with water (the rest solved in water).

Page 28: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

2- Determination of the degree of polymerization of

cellulose by capillary viscometer (according to the AFNOR (NF G06-037)

Cellulose microfibrils are chemically more resistant

to the hydrolysis.

Degree of polymerization of three spruce samples

Treatments: densification densification densification

post-treatment at

180°C, 30 min

post-treatment at

200°C, 4 min

1533 947 837

Page 29: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

4- Index of crystallinity (CrI) of the cellulose and diameter (L) of cellulose crystallites

Treatment Temperatur

e (oC)

Time

(minutes)

CrI Diameter

, L

(Å)

No treatment - - 0.710 25.0

Densified 140 20 0.778 28.7

Densified and post-

treated under saturated

moisture conditions

140 60 0.809 31.3

-``- 140 120 0.804 31.3

-``- 140 180 0.830 32.5

Densified at 140°C and

post-treated under

saturated moisture

conditions

160

30

0.818 31.9

-``- 160 60 0.811 32.5

-``- 160 90 0.844 34.5

-``- 190 8 0.831 33.8

-``- 190 16 0.843 35.2

-``- 190 24 0.853 36.7

-``- 210 2 0.844 35.2

-``- 210 4 0.846 36.7

-``- 210 8 0.868 40.1

-``- 210 16 0.875 43.1

Page 30: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

5- Determination of the glass transition temperature (Tg) of lignin

by DSC (Differential Sweeping Calorimetry with a single scan)

Depending to temperature & time lignin condenses or

depolymerises

Page 31: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

What happens to wood after THM treatment

Page 32: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Unity or integrity of wood (cellulose-hemicelluloses-lignin)

Covalent and hydrogen bands

Page 33: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

2.3 Effects of THM parameters on wood properties

The swelling of beech as a function of time (logarithmic scale) during

humidification : (a) before densification, (b) after densification by open

system (Huguenin & Navi, 1995).

Page 34: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Shear strength of the initial wood (black) and wood

densified in a THM closed system (grey) for spruce and

maritime pine (average values) (Navi & Girardet, 2000).

Page 35: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Brinel hardness of initial wood and densified wood in a THM

closed system for spruce, beech and maritime pine (average

values) (Navi & Girardet, 2000).

Page 36: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Photograph of a specimen after fracture under tensile

testing (Navi & Heger, 2005).

Natural wood,

Wood densified at 140°C during 20 minutes

post-treated at 140°C for 3 hours, post-treated at 160°C for 1 hour,

post-treated at 180°C for 20 minutes, post-treated at 200°C for 4

minutes

From each type of sample, at least 10 specimens were tested in

tension.

MOR and MOE of THM wood

Page 37: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Longitudinal tensile strength and Young´s modulus of densified

samples

20 mi. 3h. 1h. 20m. 4mi.

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Influence of stress level on properties of THM wood

0

25

50

75

100

125

150

175

200

0

1

2

3

4

5

6

7

8

9

10

0 100 200 300 400 500

Tem

pera

ture

[oC

]

Pre

ssu

re o

r S

tress [

MP

a]

Time [s]

Stress Steam Temperature

Kutnar and Kamke, 2010

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Load

[MPa]

Temperature

[°C]

Saturated steam

pressure

[psi]

Compression

loading steam

environment

Venting time

prior to

compression

[s]

5.5 150 68 Saturated steam 0

Superheated steam 180

Transient conditions 10

160 98 Saturated steam 0

Superheated steam 180

Transient conditions 10

170 114 Saturated steam 0

Superheated steam 180

Transient conditions 10

Kutnar and Kamke, 2010

Test parameters of each THM treatment

Page 40: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Oven dry density after THM treatment

0

0.2

0.4

0.6

0.8

1

1.2

1.4

Transient Superheated steam Saturated steam

OD

density [g/c

m3]

150°C 160°C 170°C

Kutnar and Kamke, 2010

Page 41: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

0

1

2

3

4

5

6

7

8

9

10

Transient Superheated steam Saturated steam

Mois

ture

conte

nt

[%]

150°C 160°C 170°C

Moisture content of THM treated wood

after conditioning at 20°C and RH 65%

Kutnar and Kamke, 2010

Page 42: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Treatment Temperature [°C] MOE

[GPa]

MOE/ρemc

[GPa cm3/g]

Untreated - 7.67 (1.06) 19.5 (1.35)

Saturated steam 150 11.6 (2.08) 20.3 (3.68)

160 22.9 (4.90) 20.3 (4.26)

170 28.7 (6.63) 24.8 (5.21)

Transient conditions 150 16.5 (4.80) 19.2 (4.34)

160 22.6 (5.91) 20.8 (3.12)

170 31.8 (3.01) 26.9 (2.92)

Superheated steam 150 11.6 (2.08) 15.8 (1.68)

160 15.8 (4.83) 18.4 (4.04)

170 19.6 (5.02) 18.2 (2.93)

MOE and MOE/ρemc of THM specimens

Kutnar and Kamke, 2010

Page 43: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Treatment Temperature

[°C]

MOR

[MPa]

MOR/ρemc

[MPa cm3/g]

Untreated - 76.6 (10.9) 194 (9.60)

Saturated steam 150 222 (38.2) 193 (35.5)

160 219 (45.1) 194 (39.9)

170 249 (16.7) 215 (30.8)

Transient conditions 150 139 (42.0) 161 (36.7)

160 186 (55.4) 170 (19.6)

170 276 (16.7) 233 (16.3)

Superheated steam 150 101 (21.3) 137 (19.6)

160 140 (40.8) 164 (41.9)

170 171 (49.3) 158 (28.8)

MOR and MOR/ρemc of THM specimens

Kutnar and Kamke, 2010

Page 44: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

0

1

2

3

4

5

6

7

8

0 100 200 300 400 500 600

Time [s]

Ste

am

pre

ssu

re [

MP

a],

Co

mp

ressio

n s

tre

ss [

MP

a]

0

50

100

150

200

250

Te

mp

era

ture

[°C

]

Compression stress

Steam pressure

Temperature

Influence of post heat-treatment at 200°C

on properties of THM wood

Kutnar and Kamke, 2010

Page 45: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

MOR/ density post heat-treated THM wood at 200°C

Kutnar and Kamke, 2010

Page 46: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Viscoelastic thermal compression process

(VTC)

Phase 1 – steaming

Phase 2 – venting

Phase 3 – compression

Cooling – specimens are cooled under compression Kutnar and Kamke, 2008

Page 47: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

MOR and MOE of VTC wood

0,0

20,0

40,0

60,0

80,0

100,0

120,0

140,0

160,0

180,0

Control VTC 63% VTC 98% VTC 132%

MO

R [

MP

a]

0,0

5,0

10,0

15,0

20,0

25,0

MO

E [

GP

a]

MOR [MPa] MOE [GPa]

Kutnar and Kamke, 2008

Page 48: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Effect of densification temperature on

maximum bending strength (I) and tensile strength (II)

Fang C.H., Mariotti N., Cloutier A., Koubaa A., Blanchet P. 2011. Densification of

wood veneers by compression combined with heat and steam. Eur. J. Wood Prod.

DOI 10.1007/s00107-011-0524-4

aspen (black) and hybrid

poplar (grey).

Page 49: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Effect of densification temperature on

MOE of bending (I) and tension (II) (?)

Fang C.H., Mariotti N., Cloutier A., Koubaa A., Blanchet P. 2011. Densification of

wood veneers by compression combined with heat and steam. Eur. J. Wood Prod.

DOI 10.1007/s00107-011-0524-4

aspen (black) and hybrid

poplar (grey).

Page 50: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

3.Conclusions 1. Research on wood densification still

needs the laboratory works

2. Few attempts has been made to

commercialize the technology with open

system

3. Domain is with high innovation because

of T,H,M & t effects on mechanical and

chemical degradation

4. Challenges exist on the moulding of large

scale elements

5. Need for a Numerical simulation of Virtual

processing of THM

Page 51: Properties and processing of THM wood - TU Wiencost-fp0802.tuwien.ac.at/fileadmin/mediapool-cost/... · 1.4 Compression forming (Two-directional compression) • Transformation of

Acknowledgment

Dr. Frederic Heger,

Mr. Fred Girardet

Dr. Andreja Kutnar