High homogenization technique

for micro-fibrillated bacteria cellulose

to fabricate electric testing prove disk

Doshisha Univ.,Kyoto,Japan
Kaho Matsuoka
Kazuya Okubo
Toru Fujii
1

Backgrounds

1/16

Prove disk Semiconductor testing devices

made of ceramics
not thermally expands
Recently,

Focus

Natural Fiber as an alternative materials

appropriate method
To solve such a problem,
propose an effective technique in fabrication of prove disk for semiconductor testing
device using cellulose

2/16

Purpose

To propose an effective technique in fabrication of prove disk

for semiconductor testing device
using cellulose as an alternative material of ceramics

3/16

Material
method
Bacterial Cellulose produced during vinegar fermentation
(BCV)

Sterilizing

48[h]

BCV

Wash the residue under

running water for 24 [h]

Web-like network

BCV
crashing

(Bacterial Cellulose
produced during
Vinegar fermentation)

4/16

Material method

Bacterial Cellulose Commercial Nata de coco (BCN)

48[h]

100[]
1[h]

BCN

running water

BCN

(Bacterial Cellulose
made of Nata de coco )
crashing

Material method

5/16

Traditional Bamboo Fiber (BF)

Bamboo

180[]
0.7-0.8[MPa]
9[times]

NaOH 1[wt%]
100[]
20[min]

Steam exported

NaOHtreatment

BF

BF
crashing

(Bamboo Fiber)

*T. Shito, et al., Bamboo J., 19, 15-23 (2002) **N. Takahashi, et al., Bamboo J., 22, 81-92 (2005)

6/16

Procedure of experiments
BCV
BCN
BF

Process homogenizer
Stone Milling
High Pressure
Homogenizer

MFC

40MPa, 30 cycles

Hot press

Vacuum Filter /
Oven
24h, 70C

In order to compare mechanical properties, we also prepared un-homogenized celluloses samples

7/16
Table 1. All types of materials used in this study
Pre-process
Finish-process
Stone milled

Processhomogenizatio
n

High-pressure
homogenized after preprocess

sBCV

sBCV-h

sBCN

sBCN-h

pBCN

pBCN-h

BF

BF-h

8/16

Experiments
Tearmal Expansion Tests
Shimadzu Thermomechanical Analyzer
Specimens dimensions : L 20mm, W 8mm, T 1.5 mm
Temperature Range 30-100
JIS C2141

3 Point Bending Tests

Specimens dimensions : L40mm, W 5mm, T 1mm
Test speed : 1mm/min JIS K7017

Thermal
expansion

heating

Thermal Expansion m

Thermal Properties of BCV

composites

9/16

linear

The thermal expansion

for all the specimens
showed to be linear
in this range.

Low thermal expansion was obtained

due to the high-pressure homogenizing technique.
Additional extension was restricted
by extended chains of cellulose at elevated temperature
when the sBCV-h was utilized for the materials.

Thermal Properties

10/16

by applying stone milling and process

homogenization
Thermal
expansion

heating
Stone milling

Process homogenizer

The process-homogenization was effective as the pre-process

before high-pressure homogenization to reduce the coefficient of thermal expansion.

The fiblils were well dispersed by the process homogenization.

11/16

Thermal Properties of BF composites

CTE of BF> CTE of BC

Remained lignin of BF promoted the thermal expansion.

BCs, which contained few or no lignin, were
useful for the materials of prove disks to reduce the coefficient of thermal
expansion.

Bending strength of sBCV

composites

12/16

The specimens fabricated with sBCVh had good property of bending strength
compared with that with original sBCV.
Effective bending strength was obtained
by high-pressure homogenization.

13

13/16

Bending strength of
sBCN composites
sBCN

sBCN-h
Fracture surface

The reason of high strength of sBCN-h specimens is

due to compress the web-like network structure

14/16

Bending strength of pBCN composites

The high pressure homogenization was also effective to the pBCN

that was pre-treated by conventional process homogenization.

15/16

Bending strength of BF composites

ase
e
r
nc
i
%
25

High strength of the specimens was obtained

The NaOH treatment was necessary if the bamboo fiber was
homogenized with high-pressure
to increase the bending strength
after stone milling process.
of the composites.
hydrogen bonds in the materials were
increased due to the homogenizing process.

16/16

CONCLUSIONS
The process-homogenization was effective as the pre-process
before high-press homogenization to reduce the coefficient of
thermal expansion.
The BCs (bacterial celluloses), which contained few or no lignin,
were useful for the materials of prove disks to reduce the
coefficient of thermal expansion.
The bending strength of the specimen fabricated with Bacterial
Cellulose was about 220MPa that was equivalent to that of an
aluminum alloy and was enough for the application of prove disk.
Excellent mechanical property was obtained when the highpressure homogenizing technique was applied to the fabrication
of prove disk for semiconductor testing device.

END

 Prove Card
IC IC
.
IC LSI

A PROBE CARD IS A TOOL FOR TESTING SEMICONDUCTORS USED AT WAFER TEST

TO CHECK QUALITY OF IC.

stiffener

10-12mm

0.4

>5000pins

Prove disk has 3layers,top,middle and bottom

Diameter of disk was 300mm.
There are hole of 0.4m interval
in order to use pin.

 mid
Value of middle layer of ceramic disk
Target Value
Bending strength 160MPa
Youngs Modulus 65Gpa
Hardness 2.2Hv
Coefficients of thermal expansion 9.8ppm/

TOP
MID
BTM

4.4-4.7ppm/
12-13GPa
300-320MPa
9.8 ppm/
65GPa
100-160MPa

Repeatability( )

I think there is repeatability, But we did not check .

Your point is very nice.
We have to consider about repeatability in the future

Technique
Good point
Simple way
Material is stable
Problem
vacuum time is long.
I have to consider about this near future

PC and BC
PC BC

BF

BC has no lignin and

no hemi-cellulose
BC

Web-like network of nanofibers

We can see in this photo BF has lignin and hemicellulose

,BC has no lignin and no hemi-cellulose

Thermal Properties BCN

It was find that a part of the web-like network was broken due to high levels
homogenization.
The tests results suggested that local deformation was available into the
gap in the web-like structure of BCN.

Diameter of nano-fiber
sBCV
sBCV-h
sBCN
sBCN-h

43.2nm
14.9nm
33.7nm
8.7nm

Aspect ratio
Aspect ratio=L/d

The reason of the results ,I think CTE is depend on aspect ratio.

If aspect ratio is large, CTE is low.

1. Materials

7/19

Reinforcement 4

4. Bamboo Monofilament
Steam explosion
Steam
High temp.
High pressure

Suddenly
released

Put into NaOH solution

1N, 2-3hours, 90
Long bamboo fiber

Steam
exploded

175 oC, 0.12-0.18 MPa, 11 times

Monofilament like cotton

Monofilament

50m

Steam
High temp.
High pressure

Suddenly
released
Steam
exploded

Pressure MPa

Steam explosion

Steam explosion condition

Temperature: 175 oC
Pressure: 0.12-0.18 MPa
Bamboo fibers component
Decomposition temperature
Cellulose
Hemicellulose
Lignin

230oC
160oC
130oC

11 times
60

0.15

0.0
time[min]

Only hemi-cellulous and Lignin can be decomposed

175oC
Long fibers were separated easily

Why Biocomposites?
Problems
Persistence of plastics in the environment
Shortage of landfill space
Depletion of petroleum resources
Concern over emissions during incineration( )

Development of Green Composites

Excellent mechanical properties

Disadvantages

Good thermal properties

Moisture absorption

Low Density

Few usable matrices

Cost Advantages

Why Bamboo?
Abundant resource
High growth speed
High strength

Natural Glass fiber

Low density
Bamboo pollution

BAMBOO IS A NATURALLY OCCURRING COMPOSITE MATERIAL WHICH GROWS ABUNDANTLY

IN MOST OF THE TROPICAL COUNTRIES. IT IS CONSIDERED A COMPOSITE MATERIAL BECAUSE
IT CONSISTS OF CELLULOSE FIBERS EMBEDDED IN A LIGNIN MATRIX. AS A CHEAP AND
FAST-GROWN RESOURCE WITH SUPERIOR PHYSICAL AND MECHANICAL PROPERTIES COMPARED
TO MOST WOOD SPECIES, BAMBOO OFFERS GREAT POTENTIAL AS AN ALTERNATIVE TO WOOD.
IN FACT, WITH A MATURATION PERIOD OF 3-8 YEARS, IT GROWS MORE RAPIDLY THAN
ANY OTHER WOODS ON EARTH, AS FAR AS ITS KNOWN. THE HIGH STRENGTH WITH RESPECT TO
ITS WEIGTH IS DERIVED FROM FIBERS LONGITUDINALLY ALIGNED WITH IT BODY.
THEREFORE, BAMBOO FIBERS ARE OFTEN CALLED NATURAL GLASS FIBERS.
MOREOVER, THE USE OF BAMBOO COULD HELP IN REDUCING THE BAMBOO POLLUTION.

Micro Fibrillated Cellulose

(MFC)

THE PRIMARY COMPOSITION OF BAMBOO FIBER IS CELLULOSE, HEMI-CELLULOSE AND LIGNIN.

THEIR RATIO IS ABOUT 2:1:1.A SINGLE BAMBOO FIBER CONSISTS OF FOUR LAYERS,
WHERE CRYSTALLIZED CELLULOSE MICROFIBRILS (MFC) ARE LONGITUDINALLY ALIGNED
WITH SOME SMALL ANGLES WITH RESPECT TO THE FIBER AXIS, EXCEPT THE TOP (P) LAYER.
MOST OF THE CELL MATERIALS ARE LOCATED IN THE S2 LAYER. SINCE CELLULOSE CHAINS ARE
DEVOID OF CHAIN FOLDINGS AND CONTAIN ONLY A SMALL NUMBER OF DEFECTS,
EACH MICROFIBRIL COULD THEORETICALLY HAVE A MODULUS CLOSE TO THAT OF
THE PERFECT CRYSTAL OF NATIVE CELLULOSE.ALTHOUGH, IT MUST BE UNDERLINED THAT,
THE FIBER STRENGTH IS STRONGLY AFFECTED BY THE FIBRI ANGLE.

Backgrounds
Prove disk Semiconductor testing devices
made of ceramics not thermally expands
However
the ceramic disk often introduces
engineering problems

The part of the ceramic disk makes cracks due to the brittle behavior of the materials

To solve such problems...

An alternative is necessary

Cost
Ceramics

500,000yen

Celluloces (BCN) 130,000-170,000yen

The ceramic disk cost is 500,000yen,

If cellulose use, cost is 130,000-170,000yen.

Weight
Ceramics

14Kg

Cellulose

2Kg

The weight of ceramic disk is 15Kg.

If cellulose use, this weigh is under 2Kg.
It is very kind for worker to lighten workers load.

Another application
I think MFC can use another application
(dish ,small things and so on).
But this research limited prove disk.
So we did not think another application.