Researches on various plasma

discharges and applications

Yang Si-Ze
Institue of Physics, Chinese Academy of Science, Beijing, China
Email: yangsz@aphy.iphy.ac.cn
Outline
 Application of plasma needle to sterilize bacteria
 Application of plasma needle to cancer
 Application of atmospheric DBD to exhaust gas
 Application of atmospheric DBD to seeds
 Surface treatment of biomedical material
 Treatment of cutting tools with pulsed high energy density
plasma(PHEDP)
Application of plasma needle to sterilize bacteria
Plasma needle
 Plasma parameter

Effect of O2 addition on the plume length with 0.1m3h-1(Pj=25W). (b) Image of the plasma jet
treated the human skin with 0.1m3h-1 He and 26 SCCM O2 addition (Pj=18W)
Temperature

Variation of temperature with distance Variation of temperature with treatment time

between the cell and the plasma nozzle
Plasma spectra

He plasma and the spectrum He+O2 plasma and the spectrum

Treatment of Streptococcus mutans bacteria
(Cooperative unit: Dental hospital, Peking university)

 S. mutans has been strongly implicated as the principal etiological

agent in human dental caries. It is also claimed to be the primary
agent of infective endocarditis.

S. mutans S. Mutans under microscope agar Inoculated agar

Published: J Appl. Phys. 105, 063302 (2009)

 Treatment effect

(a) Separation of needle-to-sample (b) Voltage (c) Exposure time

(d) Addition of O2

Treatment spots imaged after treated for different plasma treatment parameters at 0.1 m3 h−1
He. Each time, one parameter was adjusted: (a) separation of needle-to-sample, (b) voltage,
(c) exposure time, and (d) addition of O2.
 Treatment of Enterococcus faecalis
(Cooperative unit: Peking university)

 E. faecalis is gram-positive anaerobic bacteria，which can live

for 30 min at 60℃. It can endure the harsh condition in the teeth
root canal, not only induce single infection but also mixed
infection .

Plasma spectrum, 2mm under the agar

Power 15W，He 0.1m3· h−1，O2 26 ml· min−1，distance 12mm

Published : Acta. Phys. Sinica. 2009, 58(3) 1595-1602

Treatment Effect

(a) (b)

(c)

Treatment image at 0.1m3· h−1 He and treatment time 30s. Each time, one
parameter was adjusted:
（a）distance between plasma and sample（b）voltage（c）addition of O2.
Application of plasma needle to cancer
Ablation of liver cancer cells in vitro

 Treatment parameters：
time 30-60s
discharge gas ①He ，②He and O2，③Ar，④Ar and O2

Ar Ar and O2

Published: Appl. Phys. Lett. 93(2008)021502

Plasma spectra

120
N2
200

OH
N2

100

Ar I
150
OH
Rel.intensity (a.u.)

Rel.intensity (a.u.)
N2

Ar I
80

Ar I Ar I
100
N2

60

Ar I
Ar I

O II
Ar I

Ar I

Ar I
N+2

Ar I 40
50
Ar I

Ar I
Ar I
O II

O II

Ar I
H

OI
OI

O III
O II
20
0
0
100 200 300 400 500 600 700 800 900
100 200 300 400 500 600 700 800 900
wavelength (nm)
wavelength (nm)

Power 32W，Ar 200ml•min−1，O2 5ml• min−1

（left） 4mm to plasma plume （right） 2mm under the DMEM
 Treatment effect
(Cooperative unit: Cell Dept., 3rd Hospital, Peking university)

 It shows that O and OH radicals are the critical radicals to cell death

Pre-treatment After-treatment
Treatment effect

Survival curve of primary liver（BEL-7402）

Plasma power 32W，Frequency 22kHz
Application of atmospheric DBD to exhaust gas
Removal of NOx combining plasma with
SCR(Selective Catalysis Reduction)
（cooperative unit：Research Center for Eco-Environmental
Sciences, CAS ）

setup Exhaust discharge

Accepted: J Appl. Phys. 106 (2009)

Density of NOx, NO, NO2

Density of NOx, NO, NO2 as a function of treatment time

 Conversion of NOx and NO at different
temperature

100
NOx 100 100 100
90 NOx
NOx and NO conversion (%)

NO 90

NOx and NO conversion (%)

90 90

NOx and NO conversion (%)

NOx and NO conversion (%)

80 NO
80 80 80
70
70 70 70
60
60 60 60
50
40 50 50 50 NOx
30 40 40 40
NOx NO
20 30 30 30
NO
10 20 20 20
0 10
0 10 20 30 40 50 10 10
Applied power (W) 0 0 0
o
0 10 20 30 40 50 0 10 20 30 40 50 0 10 20 30 40 50
(a) temperature at 176 C Applied power (W) Applied power (W) Applied power (W)
o o o
(b) temperature at 200 C (c) temperature at 255 C (d) temperature at 300 C
176℃ conversion of 200℃ conversion of 255℃ conversion of 300℃conversion of
NOx improved from NOx improved from NOx improved from NOx improved from
6.4% to 40.7% 17% to 67% 66% to 90% 96% to 98%

Conversion of NOx and NO as a function of discharge power（13KHz）

(755ppm NO, 51ppm NO2, 10% O2, 10% H20, balance gas :N2, total flow rate 2000ml/min,
Space Velocity=50000h-1, C2H5OH as reducer，Ag/Al2O3as catalyst)
Fourier Transform Infrared (FTIR) spectra showing the effect of cand plasma-plus-
catalysts combination on the NOx removal
Application of atmospheric DBD to seeds
Atmospheric DBD treatment to the seed of cockscomb

Pre-treatment After-treatment

After treatment, the plant and flower pattern of cockscomb turns larger,
and the blooming period is prolonged
Atmospheric DBD treatment to the seed of lettuce

Effect of plasma voltage treatments on seed of lettuce

Left: (a) 5950 V (b) 6290 V (c) CK
Right: physiological index
a：CK (untreated) b：5610V c：6630V
 Atmospheric DBD treatment to the seed of pakchoi

Effect of plasma voltage on Effect of plasma voltage on

physiological index of pakchoi seedling dynamic changes of pakchoi’s total leaves number
Surface treatment of biomedical material
coating
 Experimental method
Two processes method

(functional group)
Second step:
Plasma polymer
RF pulse plasma polymerization
Transition metal nitride film

First step:
substrate
Cathodic Vacuum Arc deposition
Setup

Cathodic Vacuum Arc deposition system Plasma polymerization system

Discharge Video
Results —Corrosion resistance of TaN film

Potentiodynamic polarization curves of the uncoated substrate and TaN coated samples
in Hank’s solution at 37℃

Specimen Ecorr βa βc Icorr Rp Porosity

(mV) (mV/decade) (mV/decade) (µA cm-2) (kΩ cm2)

SS317L -267.51 521.82 113.55 1.0929 32.66

Ta-N/SS317L (-50 V) -430.19 154.24 117.92 0.0054 3173.5 0.0050

Ta-N/SS317L (-200 V) -377.63 471.75 168.77 0.0650 790.68 0.0254

Result —Nanoindentation test of TaN film

18
16
14
Hardness (GP)

12
10
8
6
4
2
0 SS317L 0V -50V -100V -200V

Hardness of TaN film as function of substrate bias

Result— AES analysis of TaN film
90

80 film mixing
atomic ratio
70
region Ta:N = 52: 45
60 Fe3
Ta1
ACP(%)

50

40 N1
mixing region
30

20
good adhesion
10

0
0 5 10 15 20 25 30 35
Sputter Time (min.)

Vb= -200V
Experiment on fibroblasts culture in vitro

Resuscitation Inoculation Cultivation fixation

Cell adhesion
Cell expansion
Cell proliferation (a) fibroblasts on SS317L 20hours ×50 (b) fibroblasts on Ta-N 20hours ×50

Cell morphology

Cell cytotoxicity? (c) fibroblasts on Ti-N 20hours ×50 (d) fibroblasts on Si 20hours ×100

Morphologies of fibroblasts on different sample surface after

20h
Cell density

Cell density of fibroblasts on different sample surface after different period

 Morphologies of fibroblasts on TaN film

(a) fibroblasts on Ta-N 20hours ×300 (b) fibroblasts on Ta-N 70hours ×300 (e) fibroblasts on Ta-N 70hours ×3000 (f) fibroblasts on Ta-N 70hours ×2000

(c) fibroblasts on Ta-N 20hours ×2000 (d) fibroblasts on Ta-N 20hours ×2500 (g) fibroblasts on Ta-N 70hours ×1300 (h) fibroblasts on Ta-N 70hours ×1500
NH2 function film fabricated by plasma
polymerization（cooperative unit：CSRIO）
Traditional Continuous Wave （CW50)：
Density of NH2 is low，but stable in
aqueous solution

Traditional pulsed mode(P30)：

Density of NH2 is high，but not stable in
aqueous solution

New plasma mode – CW combined pulsed

mode（CW50+P30):
Density of NH2 is high，and stable in
aqueous solution. The most promising for
biomedical application.
Density of NH2 in different medium on PPHA
film prepared by three discharge modes
Treatment of cutting tools with pulsed high
energy density plasma(PHEDP)
Pulsed High Energy Density Plasma(PHEDP)

High electron energy: 10~100eV

High plasma density: 1014~1016cm-3
High axial speed: 10～100 km/s
High energy density:1~10J/cm2
Pulse width: 10-100μs
Quench speed: 108-1010 Ks-1

Schematic illustration of PHEDP

Nano-grain coating deposition
Ion implantation
Good adhesion strength with
substrate due to the large
transition area
 Entrance of the subway

Tunnel boring machine (TBM)

tunnel
 Properties of PHEDP coatings on cutter

Cutter material：YG8

Surface Cross-section

coatings

Interface

substrate

SEM results of TiN coatings on cemented tools XRD pattern of TiN/YG8

Properties of PHEDP coatings on cutter

Scratch test of TiN/YG8

AES test of TiN/YG8

Life time of TiN coatings deposited with different parameters

The fieldwork results in Beijing

Treated

Untreated
Evaluation of the service condition of tools
coated with Ta(C,N) by the users

Compared with the

untreated tools, the
cutting tip of the treated
tools presents smooth
surface and no obvious
wear trace. This indicates
that the coated tools
possess wearable
property.
Thank You !