Researches On Various Plasma Discharges And Applications
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Researches on various plasma discharges and applications Yang Si-Ze Institue of Physics, Chinese Academy of Science, Beijing, China Email: [email protected]
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 between the cell and the plasma nozzle
Variation of temperature with treatment time
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
0 100
Ar I
80
OI
Ar I
Ar I
20
O II
40
Ar I
60
O II O II O III
Rel.intensity (a.u.)
Ar I Ar I Ar I Ar I Ar I Ar I OI
H
O II
50
Ar I
N+2
N2
100
100 N2
OH
Rel.intensity (a.u.)
150
Ar I Ar I Ar I
N2
120
N2
200
OH
Plasma spectra
0 200
300
400
500
600
wavelength (nm)
700
800
900
100 200 300 400 500 600 700 800 900 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
70 60 50 40 30 20 10 0 0
10
20
30
40
50
Applied power (W) o
(a) temperature at 176 C
NO
80 70 60 50 40 30 20 10 0 0
10
20
30
40
Applied power (W) o
176℃ conversion of NOx improved from 6.4% to 40.7%
100
100
90
90
NOx and NO conversion (%)
80
NOx
90
(b) temperature at 200 C
200℃ conversion of NOx improved from 17% to 67%
50
NOx and NO conversion (%)
100
NOx NO
90
NOx and NO conversion (%)
NOx and NO conversion (%)
100
80 70 60 50 40
NOx
30
NO
20 10 0
80 70 60 50
NOx
40
NO
30 20 10 0
0
10
20
30
40
Applied power (W)
50
o
(c) temperature at 255 C
255℃ conversion of NOx improved from 66% to 90%
0
10
20
30
40
Applied power (W) o
(d) temperature at 300 C
300℃conversion of NOx improved from 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)
50
Fourier Transform Infrared (FTIR) spectra showing the effect of cand plasma-pluscatalysts 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 physiological index of pakchoi seedling
Effect of plasma voltage on dynamic changes of pakchoi’s total leaves number
Surface treatment of biomedical material coating
Experimental method
Two processes method (functional group) Plasma polymer
Second step: RF pulse plasma polymerization
Transition metal nitride film
substrate
First step: 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 (mV)
βa (mV/decade)
βc (mV/decade)
Icorr (µA cm-2)
Rp (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
Porosity
Result —Nanoindentation test of TaN film 18 16
Hardness (GP)
14 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
film
80
mixing Fe3
60
ACP(%)
atomic ratio Ta:N = 52: 45
region
70
Ta1 50
N1
40
mixing region
30 20
good adhesion
10 0 0
5
10
15
20
25
Sputter Time (min.) Vb= -200V
30
35
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
Density of NH2 in different medium on PPHA film prepared by three discharge modes
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.
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
AES test of TiN/YG8
Scratch 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 !
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 between the cell and the plasma nozzle
Variation of temperature with treatment time
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
0 100
Ar I
80
OI
Ar I
Ar I
20
O II
40
Ar I
60
O II O II O III
Rel.intensity (a.u.)
Ar I Ar I Ar I Ar I Ar I Ar I OI
H
O II
50
Ar I
N+2
N2
100
100 N2
OH
Rel.intensity (a.u.)
150
Ar I Ar I Ar I
N2
120
N2
200
OH
Plasma spectra
0 200
300
400
500
600
wavelength (nm)
700
800
900
100 200 300 400 500 600 700 800 900 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
70 60 50 40 30 20 10 0 0
10
20
30
40
50
Applied power (W) o
(a) temperature at 176 C
NO
80 70 60 50 40 30 20 10 0 0
10
20
30
40
Applied power (W) o
176℃ conversion of NOx improved from 6.4% to 40.7%
100
100
90
90
NOx and NO conversion (%)
80
NOx
90
(b) temperature at 200 C
200℃ conversion of NOx improved from 17% to 67%
50
NOx and NO conversion (%)
100
NOx NO
90
NOx and NO conversion (%)
NOx and NO conversion (%)
100
80 70 60 50 40
NOx
30
NO
20 10 0
80 70 60 50
NOx
40
NO
30 20 10 0
0
10
20
30
40
Applied power (W)
50
o
(c) temperature at 255 C
255℃ conversion of NOx improved from 66% to 90%
0
10
20
30
40
Applied power (W) o
(d) temperature at 300 C
300℃conversion of NOx improved from 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)
50
Fourier Transform Infrared (FTIR) spectra showing the effect of cand plasma-pluscatalysts 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 physiological index of pakchoi seedling
Effect of plasma voltage on dynamic changes of pakchoi’s total leaves number
Surface treatment of biomedical material coating
Experimental method
Two processes method (functional group) Plasma polymer
Second step: RF pulse plasma polymerization
Transition metal nitride film
substrate
First step: 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 (mV)
βa (mV/decade)
βc (mV/decade)
Icorr (µA cm-2)
Rp (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
Porosity
Result —Nanoindentation test of TaN film 18 16
Hardness (GP)
14 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
film
80
mixing Fe3
60
ACP(%)
atomic ratio Ta:N = 52: 45
region
70
Ta1 50
N1
40
mixing region
30 20
good adhesion
10 0 0
5
10
15
20
25
Sputter Time (min.) Vb= -200V
30
35
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
Density of NH2 in different medium on PPHA film prepared by three discharge modes
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.
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
AES test of TiN/YG8
Scratch 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 !
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