OkinoLabGuide Eng PDF

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.
Nov. 2014
Development and Application of
Brand-new Atmospheric Plasma Sources
Okino Lab.
Department of Energy Sciences
Tokyo Institute of Technology

2008- Akitoshi Okino, All rights reserved.
What is plasma ?
Plasma is the fourth state of matter
A simple plasma consists of positive

ions, electrons, excited atoms and
radicals,,, in a sea of neutral atoms
(molecules).
The particles in the plasma are moving
in random directions.
Plasma has some different

characteristics from normal gas.
electron
ion
100
ice
water
Solid
Liquid
a few 1000
water vapor
Gas
ionized gas
Plasma
Generation method of plasmas

In industrial use, plasma generation method is chosen according
to demand of plasma pressure, temperature, purity, kind of gas,,
Discharge frequency
DC HF (kHz) RF (MHz) Microwave (GHz) or HV pulse
Electrode
Electrode discharge or Electrode-less discharge
Pressure
Vacuum Low Atmospheric High pressure
It's very special !
Why atmospheric plasma is so special ?
Merits
(1) Eliminate vacuum chamber, pumping system Low cost
(2) Eliminate pumping Continuous processing
(3) High density plasma High speed processing
(4) Applicable for large targets Car, Airplane
(5) Applicable for hear sensitive targets Human skin, Foods
Diculty
Low pressure
Atmospheric
Plasma generation is (was) not so easy
(compare with usual low pressure plasma)
Atmospheric low temperature plasmas

Atmospheric plasma research has been widely spread because
Low Temperature Plasma could be generated.
Barrier discharge
Applications
Improvement of
Adhesion
Paintability
Sterilization
Corona discharge
Plasma bullet
Merit:
Low temperature
(room temp 200)
Problems:
Limitation of target size/material
Limitation of plasma gas
Temperature is not controllable
Atmospheric damage-free MULTI-GAS plasma jet
Flow rate : 5 L/min

Voltage : 6 kV
Power : 617 W
Applicable for living body/metal/plastic/paper/textile
Applicable for surface treatments
such as cleaning, hydrophilization, oxidation, azotizing, coating
Irradiation of damage-free multi-gas plasma jet #1

You can touch the
plasma (left)
Acetone
Not ignite acetone (right)
Paper
Electronic substrate
Plastic
Glass
Inside of glass tube
Fireworks or candles
don't be ignited.
Fluits, Sashimi, Egg
No damage for
stocking.
Ice cream, ice, chocolate were little bit melted.
The plasma gas temperature is around 40.
Hydrophilization of Polyimide film
air
He
N2
Before
After
Ar
O2
Hydrophilized less than 1s plasma irradiation

Treatment speed was depend on kind of tha plasma gas
Can hydrophilize almost all materials

Rubber
Acrylic resin
Glass
Semiconductor
Copper
Polyimide lm
PTFE(Teflon

Gauze Cotton100
Knit Cotton100
Rayon
Weather Poly65, Cotton35
Shading curtain
Work clothes Poly65, Cotton35

Cardboard
Woods
Natural rubber
Bamboo
Drawing paper
Floor tile
Atmospheric damage-free MULTI-GAS plasma jet
PF-DFMJ01
1mm
4
We are selling the plasma from our venture company,

Plasma Factory, Inc.
High speed removal of copper oxide

50 mm
3 mm
Treated
No-treated
(Oxide)
Copper oxide ~ 10 nm
Carry speed
(mm/sec)
10
50
100
200
1 ~ 2 nmNatural oxide
Copper
Max carry speed: 700 mm/sec

Removal speed: 93 m/sec
PAT.P
Nikkan Kogyo Shimbun
2011.9.29
Atmospheric damage-free LINEAR plasma source

Applications
Improvement of
Adhesion
Paintability
Sterilization
Light weight 830g and handy
Outlet slit1mm x 335mm
Adhesion improvement of HDPE/epoxy resin

HIDEN to HIDEN adhesion test
Target samples are treated under
atmospheric pressure
Apply epoxy resin adhesive and cure
perform compress test
not glue at all
good gluing !
Atmospheric damage-free LINEAR plasma source
PF-DFL
We are selling the plasma from our venture company,

Plasma Factory, Inc.
Application for Medical Field
Two problems of common plasma sources
1. Limitation of plasma gas
2. Temperature is not controlable
Sterilization of E.coli
,O2
N2
CO2
CO2
O2
N2O
,O2
N2O
CO2
60s
10s
600s
N2O
,O2
EZ2C
Air
CO2
2010/03/12
600s
60s
Ar
EZ2C
10
10s
60
EZ2C
2010/03/19
2010/03/17
Irradiation time [sec]
600
2010/03/15
Sterilized
Not-sterilized
2010/03/15
2010/03/12
10s
60s
Ar+O2
ir
ir
Sterilization speed deeply depends on the plasma gas.

Air
Plasma gas
ir
600s
Sterilization of S.mutans
Confidential
Ar
N2
O2
Ar+O2
CO2
Air
Bactericidal eect against various bacteria
Confidential
Bactericidal eect against various bacteria
Confidential
Bactericidal eect against various fungi
Confidential
Effective for
highly resistant
bacteria
1O
O3
2.80 V
2 2.42 V
Effective for
viable bacteria
2.07 V
Ozone [M]
HO
Hydrogen peroxide [M]
Singlet Oxygen [M]
OH radical [M]
Reactive species in plasma irradiated water
H2O2
1.77 V
Temperature controllable plasma
PAT Japan, USA, China
We made a technic for control the plasma temperature from

high temp to below zero .
water freeze in a few second
Ice !
Gas temperature ()
Start cooling
zero
90
-90 plasma jet

Time (sec)
Its must use technic for medical/beauty use.
Comparison of low temperature plasmas

It's wide range and controllable !
"Real" Low temp. plasma Intermediate temp. plasma
Corona discharge
"Common" Low temp. plasmas
Barrier discharge
-100
Room
temp
100
Gas temperature ()
200
Control of the plasma gas temperature
10
Controllable from below 0 to high temperature
Nikkan Kogyo Shimbun2011.11.3
Fuji Sankei Business i.2012.2.22
Elemental analysis in single cell
Droplet nebulizer for single cell analysis
PAT Japan etc.
Single cell is included

in a single droplet
using microscope.
30 580 m
(14 pL 100 nL)
Individual analysis of single cell/particle

100 m
Nozzle tip
aqueous
solution
Droplet
Nebulizer head
14 pL~
Element anaysis of single umicelluar algae

Pseudococcomyxa simplex
Element
Absolute amountfg
Fe
360
Mg
92
63
Ca
26
Zn
0.91
Mn
0.73
Fe, Mg, Ca contained in a single cell were observed by AES.

2014.10.16
Measurement of adhesion material

on heat sensitive surfaces
Atmospheric Plasma Soft Ablation; APSA
PAT Japan etc.
to Mass Sprctrometer
to Mass
Sprctrometer
Touchable
Plasma
Sample
Flow
Sampling surface adhesion materials without damaging to the surface

Applicable to various mass spectrometers
Disease diagnostics by sweat

Security at airport
Quality inspection of foods/drugs
Measurement of cosmetics/sebum
Estaron Mocha
Boiling point: 178
Mass Signal [count]
MH+
195.10
Caffeine
2.0
1.0
Gas temp: 55
M = 194.19
[M+O]H+
211.10
2MH+
m/z
Saridon
isopropylantipyrine 150 mg
Ethenzamide 250 mg
B.P.319
B.P.302
Signal
[count]
Mass
Signal
[count]
MH+
231.18
Ethenzamide
Isopropylantipyrine
M = 165.19
M = 230.31
MH+
166.11
(M+O)H+
247.17
m/z
2MH+
461.35
Detection of chemical weapons

He gas
1,100 ml/min
National Research Institute of Police Science
Teflon
Deposited
chemical warfare agent
Ion trap
mass spectrometer
(Agilent technologies, 1100
Series LC/MSD trap)
NH3 (Blister agent)
1000 ppm in 5 L Hexane Boiling point143
C6H1235Cl3NH+
203.93
Signal [count]
Nitrogen mustard 3
C6H1235Cl237ClNH+
205.89
M = 204.53
C6H1235Cl37Cl2NH+
207.85
m/z
VX (Nerve gas)
1000 ppm in 5 L Hexane
Boiling point298
VX is the most danger in nerve gas.

Median lethal dose0.1 gmin/m3
C11H26NO2PSH+
268.05
VX
Signal [count]
M = 267.4
m/z
Isopropylantipyrine on a fingher
He gas
200 ml/min
Discharge capacitor12 F
Discharge voltage380 V
Dischrge frequency20 Hz
Ion trap
mass spectrometer
Isopropylantipyrine 50 ppm
= 0.540 g
in 10L methanol
(Agilent technologies, 1100

Series LC/MSD trap)
Measurement of isopropylantipyrine on a fingher
MH+
231.05
Isopropylantipyrine
Signal [count]
M = 230.31
m/z
2014.5.22
NIKKEI shimbun
2014.7.8
We have a plan to apply it for human skin/cosmetics
Irradiation of low temp. plasma
to Mass spectrometer
Atmospheric multi-gas thermal plasma

Can generate not only Ar but He, N2, O2, CO2, N2O, air
and their mixture gas plasma in atmospheric pressure.
High purity thermal plasma because it's electrode-less source.
High gas temp3,000 to 8,000 K
High electron temp 10,000 K
High electron number density1015cm-3
Only one device in the world!
Atmospheric multi-gas colona device
Atmospheric multi-gas large sized plane plasma
100 x 250 mm
High power pulsed multi-gas micro plasma
Multi-gas plasma generation is possible

High power drive up to 100 kW by pulsed operation
Battery drive is possible Mobile analysis/treatment
Scale up is easy by two/three dimensional set up
High gas temp1,000 to 5,000 K
High electron temp 30,000 K
High Electron number density1015cm-3
500 m
N2
Helium
Argon
Neon
O2
CO2
Air
PAT.P
Highly durable water repellency coating of nylon line
Iso Special
Fine Float
Matsuda Special
Black Stream Mark
On sale Oct. 2014 in Japan

spring 2015 in USA
Okino Lab., Tokyo Tech.

Development of original atmospheric plasma sources
Multi-gas thermal plasma
Multi-gas low temperature plasma
Linear type plasma, Large sized plasma
Application for sensing/analysis

Droplet neblizer for single cell analysis
Measurement of surface adhesion materials; APSA
Ultra high sensitive plasma detector for GC
Application for medical/enviromnental field

Sterilization, Plasma medicine
Applicaion for Beauty, Foods, Agriculture
Portable sterilizer for disaster
Decomposition of medical waste gasesN2O, EOG
Front cover of international journals
Analytical Sciences
Journal of Analytical Atomic Spectrometry

www.rsc.org/jaas
Volume 28 | Number 5 | May 2013 | Pages 615770
11 3 5 1 10 29 12 25 12 10 259
ISSN 0 9 1 0 - 6 3 4 0
Analytical
Analytical
Sciences
Sciences
Vol.
Volume 29 Number 3 March 2014 Pages 377584
JAAS
Journal of Analytical Atomic Spectrometry
www.rsc.org/jaas
29
No. 12
2013
pages 11171230
Development of the atmospheric plasma soft-ablation method (APSA) for
elemental analysis of materials on heat-sensitive substrates.
T. IWAI, Y. TAKAHASHI, H. MIYAHARA, and A. OKINO (pp. 1141 1145)
ISSN 0267-9477
ISSN 0267-9477
COMMUNICATION
Kaori Shigeta et al.
Sample introduction of single selenized yeast cells (Saccharomyces cerevisiae) by
micro droplet generation into an ICP-sector field mass spectrometer for label-free
detection of trace elements
Journal Anal. At. Spectrom.

May 2013
The International Journal of

The Japan Society for Analytical Chemistry
PAPER
Akitoshi Okino et al.
Fundamental properties of a non-destructive atmospheric-pressure
plasma jet in argon or helium and its first application as an ambient
desorption/ionization source for high-resolution mass spectrometry
http://www.jsac.or.jp/analsci/ ANSCEN Vol.29(12) pp.1117 1230 (2013)
Analytical Sciences
Dec. 2013
Journal Anal. At. Spectrom.

Apr. 2014
We established two venture company

Plasma Concept Tokyo
Plasma Factory
Established in July, 2008
Established in July, 2011
Development of new plasma sources

Consulting about plasma
Selling original plasma sources

Plasma treatment service

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Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Development and Application of

Brand-new Atmospheric Plasma Sources

Department of Energy Sciences

Tokyo Institute of Technology

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Plasma is the fourth state of matter

A simple plasma consists of positive

Plasma has some different

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Generation method of plasmas

DC HF (kHz) RF (MHz) Microwave (GHz) or HV pulse

Electrode discharge or Electrode-less discharge

Vacuum Low Atmospheric High pressure

It's very special !

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Why atmospheric plasma is so special ?

(1) Eliminate vacuum chamber, pumping system Low cost

(2) Eliminate pumping Continuous processing

(3) High density plasma High speed processing

(4) Applicable for large targets Car, Airplane

(5) Applicable for hear sensitive targets Human skin, Foods

Plasma generation is (was) not so easy

(compare with usual low pressure plasma)

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Atmospheric low temperature plasmas

(room temp 200)

Limitation of target size/material

Limitation of plasma gas

Temperature is not controllable

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Atmospheric damage-free MULTI-GAS plasma jet

Flow rate : 5 L/min

Applicable for living body/metal/plastic/paper/textile

Applicable for surface treatments

such as cleaning, hydrophilization, oxidation, azotizing, coating

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Irradiation of damage-free multi-gas plasma jet #1

Not ignite acetone (right)

Inside of glass tube

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Irradiation of damage-free multi-gas plasma jet #2

Fluits, Sashimi, Egg

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Irradiation of damage-free multi-gas plasma jet #3

Ice cream, ice, chocolate were little bit melted.

The plasma gas temperature is around 40.

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Hydrophilization of Polyimide film

Hydrophilized less than 1s plasma irradiation

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Can hydrophilize almost all materials

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Can hydrophilize almost all materials

Weather Poly65, Cotton35

Work clothes Poly65, Cotton35

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Can hydrophilize almost all materials

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.

Atmospheric damage-free MULTI-GAS plasma jet

We are selling the plasma from our venture company,

Atmospheric Plasma and Spectroscopy, Okino Lab., Tokyo Tech.