连续波光腔衰荡光谱装置的建立及其在非平衡等离子体HO_2和OH自由基定量测定中的应用
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摘要
高气压低温等离子体属于非平衡体系，其中中性粒子、离子的温度较低，而电子温度可高达数十万度，从而可由电子碰撞产生大量活性物种，引发一系列在常规手段下难以进行的物理-化学过程。自由基一般被认为是引发各种化学反应过程的重要活性物种，因此对等离子体中自由基的浓度进行原位定量诊断就成为研究和改进等离子体工艺，探索等离子体中基元物理-化学过程的重要手段。由于等离子体中自由基具有很高的反应活性，因而浓度较低，这就需要采用灵敏度较高的诊断技术。光腔衰荡光谱技术是上世纪八十年代末兴起的一种全新的激光吸收光谱技术。与传统的吸收光谱技术相比，光腔衰荡光谱技术具有极长吸收程和对光源光强波动不敏感两大优点，因此具有极高的探测灵敏度，特别适合痕量物质的检测。
本论文将光腔衰荡光谱技术与介质阻挡放电技术相结合，对介质阻挡放电等离子体产生的自由基进行光腔衰荡光谱原位定量测量，主要取得以下结果：
1．建立了国内首台连续波光腔衰荡光谱装置。在谐振腔长42 cm，放电电极长度10 cm，高反镜的反射率99．994％的条件下，所建光腔衰荡光谱装置的最小检测灵敏度为3×10~(-8)m~(-1)，相应的HO_2自由基的最小探测数密度为1×10~(11) molecules cm~(-3)，表明本设备的主要性能指标达到国际先进水平。
2．利用连续波光腔衰荡光谱技术，首次对HCHO／O_2／H_2O／N_2低温等离子体中的HO_2自由基的数密度进行了定量研究。以HO_2基电子态((?)~2A")的H-OO伸缩振动的第一泛频谱带为研究对象，一定实验条件下(U_P=6．5 kV,f_(a.c.)=5 kHz，1900 ppm HCHO，3．5％H_2O，P_(total)=30 Torr)，HCHO／O_2／H_2O／N_2 DBD放电过程中产生的HO_2自由基的数密度最初随体系中O_2含量的增加而增加，当氧气含量为20％时，HO_2的数密度到达最大值(1．3×10~(13)molecules cm~(-3))，此后随O_2含量的增加而缓慢下降。考察了HO_2数密度随放电气压和电压变化规律时，亦均出现极值现象。
采用“时间窗”方法，研究了半个放电周期内HO_2数密度的时间演变行为。一定实验条件下(U_P=4．5 kV,f_(a.c.)=5 kHz，1900 ppm HCHO，20％O_2，3．5％H_2O，P_(total)= 30 Tort)，放电电压．电流波形图显示放电为丝状放电模式，将时间窗的时间尺度设为2μs，研究结果显示，以放电电流的第一个脉冲对应的时间为基准点，HO_2的数密度在5μs内迅速增大至极值，而后逐渐减小。
3．首次利用连续波光腔衰荡光谱技术，对常压介质阻挡放电中的OH自由基的数密度进行了定量研究。利用OH基电子态(X~2Π_i)v'=2←v"=0泛频谱带，求得OH电子基态振动基态不同转动能级(P_1(7．5)e、P_2(6．5)f、P_1(6．5)f、P_1(6．5)e、P_2(5．5)f和P_1(5．5)e)上的粒子数分布，通过玻尔兹曼图解法对OH的转动温度进行了计算并考察了OH的转动温度随放电电压的变化情况。结果表明：在一定放电条件下(1 atm，6700 ppm H_2O／He，放电频率f_(a.c.)=70 kHz)，当外加电压从6 kV升高至10．4 kV时，转动温度从312±10 K近线性增长至363±10 K，相应的OH的总的数密度由(2．1±0．1)×10~(13)molecule cm~(-3)增加至(3．7±0．1)×10~(13) molecule cm~(-3)。当体系中加入少量的N_2或O_2时，OH的数密度分别在3％(N_2)和1％(O_2)出现极值。
In non-equilibrium plasmas, the electrons may be much hotter (with temperatures in the range of tens of thousands up to a hundred thousand Kelvin) than the ions and neutrals, whose translational temperatures are essentially equal and typically range from room temperature to a few times the room temperature. Non-equilibrium plasmas thus represent environments where very energetic chemical processes can occur (via the plasma electrons) at low ambient temperatures. The generation of chemically reactive free radicals by electron impact dissociation in molecular plasmas is an important precursor for plasma chemical reactions. Therefore, measurements of the radical number density are needed to characterize experiments and study physico-chemical processes. However, determining the radical concentration is a challenging problem in the atmosphere or in laboratory experiments because of its short lifetime and low concentration. In order to improve the detection sensitivity, various ultra-sensiive techniques have been developed. The technique of cavity ring-down spectroscopy (CRDS) has been developed in 1980s. The advantage of CRDS over normal absorption spectroscopy results from, firstly, the intrinsic insensitivity to light source intensity fluctuations and, secondly, the extremely long effective path lengths. In the past decades, the CRD technique has been especially powerful in gas-phase spectroscopy for absolute concentration measurements of trace gas.
The present work reports the determination of OH and HO_2 radicals in dielectric barrier discharge plasmas via continuous wave cavity ring-down spectroscopy. The main results presented in the dissertation have been summarized as followings:
1. An apparatus of continuous wave cavity ring-down spectroscopy (cw-CRDS) has beenconstructed for the fisrt time in China. The minimum measurable absorption coefficient for our setup is about 3×10~(-8) cm~(-1) in DBD plasmas, corresponding to an HO_2 radical number density of- 1×10~(11) molecules cm~(-3), which shows that the main technological characteristics of this instrument have reached the international level.
2. HO_2 radical number density in non-equilibrium plasmas has been experimentally determined for the first time via cw-CRDS. HO_2 radicals were observed in discharges of HCHO/O_2/H_2O/N_2 mixtures around 6625.7 cm~(-1) in the first H-OO stretching overtone, (2, 0, 0) - (0, 0, 0), of its ground electronic state (?)~2A". At certain discharge conditions (a.c. frequency of 5 kHz, peak-to-peak voltage of 6.5 kV, 1900 ppm HCHO, 3.5% H_2O in N_2, P_(total)= 30 Torr), HO_2 concentration rises as oxygen concentration increases initially but declined with its further increase. The effects of water concentration, the discharge voltage and the discharge gas pressure on the concentration of HO_2 radicals have been investigated.
The temporary evolution of HO_2 concentration within a half period of the sine wave applied voltage (U_P = 4.5 kV,f_(a.c.) = 5 kHz, 1900 ppm HCHO, 20% O_2, 3.5% H_2O in N_2, P_(total) = 30 Torr) has been studied using the method of "time window". The result shows that the concentration of HO_2 radical increases rapidly during the first 5μs following the first discharge current pulse. After its peak value, HO_2 concentration decreases slowly.
3. The hydroxyl radical, generated in atmospheric DBD plasmas, has been determined via cw-CRDS for the first time. The P-branches of OH X~2Π_i (v' = 2←v" = 0) bands were used for its number density measurements. P_1(7.5)e, P_1(6.5)e, P_1(6.5)f and P_1(5.5)e lines of X~2Π_(3/2) transition together with P_2(6.5)f and P_2(5.5)f lines of X~2Π_(1/2) transition were used to measure the OH rotational temperature (T_R). At certain experimental conditions (a.c. frequency of 70 kHz, 6700 ppm H_2O in He, 1 atm.), when the peak-to-peak discharge voltage varied from 6 kV to 10.4 kV, the determined OH radical concentration increased from (2.1±0.1)×10~(13) molecules cm~(-3) to (3.7±0.1)×10~(13) molecules cm~(-3). The plasma gas temperature, derived from the Boltzmann plots of OH rotational population distributions, ranged from 312±10 K to 363±10 K, when the discharge voltage was raised in the above range. The influences of O_2 and N_2 addition on the production of OH radicals have been also investigated.
本论文将光腔衰荡光谱技术与介质阻挡放电技术相结合，对介质阻挡放电等离子体产生的自由基进行光腔衰荡光谱原位定量测量，主要取得以下结果：
1．建立了国内首台连续波光腔衰荡光谱装置。在谐振腔长42 cm，放电电极长度10 cm，高反镜的反射率99．994％的条件下，所建光腔衰荡光谱装置的最小检测灵敏度为3×10~(-8)m~(-1)，相应的HO_2自由基的最小探测数密度为1×10~(11) molecules cm~(-3)，表明本设备的主要性能指标达到国际先进水平。
2．利用连续波光腔衰荡光谱技术，首次对HCHO／O_2／H_2O／N_2低温等离子体中的HO_2自由基的数密度进行了定量研究。以HO_2基电子态((?)~2A")的H-OO伸缩振动的第一泛频谱带为研究对象，一定实验条件下(U_P=6．5 kV,f_(a.c.)=5 kHz，1900 ppm HCHO，3．5％H_2O，P_(total)=30 Torr)，HCHO／O_2／H_2O／N_2 DBD放电过程中产生的HO_2自由基的数密度最初随体系中O_2含量的增加而增加，当氧气含量为20％时，HO_2的数密度到达最大值(1．3×10~(13)molecules cm~(-3))，此后随O_2含量的增加而缓慢下降。考察了HO_2数密度随放电气压和电压变化规律时，亦均出现极值现象。
采用“时间窗”方法，研究了半个放电周期内HO_2数密度的时间演变行为。一定实验条件下(U_P=4．5 kV,f_(a.c.)=5 kHz，1900 ppm HCHO，20％O_2，3．5％H_2O，P_(total)= 30 Tort)，放电电压．电流波形图显示放电为丝状放电模式，将时间窗的时间尺度设为2μs，研究结果显示，以放电电流的第一个脉冲对应的时间为基准点，HO_2的数密度在5μs内迅速增大至极值，而后逐渐减小。
3．首次利用连续波光腔衰荡光谱技术，对常压介质阻挡放电中的OH自由基的数密度进行了定量研究。利用OH基电子态(X~2Π_i)v'=2←v"=0泛频谱带，求得OH电子基态振动基态不同转动能级(P_1(7．5)e、P_2(6．5)f、P_1(6．5)f、P_1(6．5)e、P_2(5．5)f和P_1(5．5)e)上的粒子数分布，通过玻尔兹曼图解法对OH的转动温度进行了计算并考察了OH的转动温度随放电电压的变化情况。结果表明：在一定放电条件下(1 atm，6700 ppm H_2O／He，放电频率f_(a.c.)=70 kHz)，当外加电压从6 kV升高至10．4 kV时，转动温度从312±10 K近线性增长至363±10 K，相应的OH的总的数密度由(2．1±0．1)×10~(13)molecule cm~(-3)增加至(3．7±0．1)×10~(13) molecule cm~(-3)。当体系中加入少量的N_2或O_2时，OH的数密度分别在3％(N_2)和1％(O_2)出现极值。
In non-equilibrium plasmas, the electrons may be much hotter (with temperatures in the range of tens of thousands up to a hundred thousand Kelvin) than the ions and neutrals, whose translational temperatures are essentially equal and typically range from room temperature to a few times the room temperature. Non-equilibrium plasmas thus represent environments where very energetic chemical processes can occur (via the plasma electrons) at low ambient temperatures. The generation of chemically reactive free radicals by electron impact dissociation in molecular plasmas is an important precursor for plasma chemical reactions. Therefore, measurements of the radical number density are needed to characterize experiments and study physico-chemical processes. However, determining the radical concentration is a challenging problem in the atmosphere or in laboratory experiments because of its short lifetime and low concentration. In order to improve the detection sensitivity, various ultra-sensiive techniques have been developed. The technique of cavity ring-down spectroscopy (CRDS) has been developed in 1980s. The advantage of CRDS over normal absorption spectroscopy results from, firstly, the intrinsic insensitivity to light source intensity fluctuations and, secondly, the extremely long effective path lengths. In the past decades, the CRD technique has been especially powerful in gas-phase spectroscopy for absolute concentration measurements of trace gas.
The present work reports the determination of OH and HO_2 radicals in dielectric barrier discharge plasmas via continuous wave cavity ring-down spectroscopy. The main results presented in the dissertation have been summarized as followings:
1. An apparatus of continuous wave cavity ring-down spectroscopy (cw-CRDS) has beenconstructed for the fisrt time in China. The minimum measurable absorption coefficient for our setup is about 3×10~(-8) cm~(-1) in DBD plasmas, corresponding to an HO_2 radical number density of- 1×10~(11) molecules cm~(-3), which shows that the main technological characteristics of this instrument have reached the international level.
2. HO_2 radical number density in non-equilibrium plasmas has been experimentally determined for the first time via cw-CRDS. HO_2 radicals were observed in discharges of HCHO/O_2/H_2O/N_2 mixtures around 6625.7 cm~(-1) in the first H-OO stretching overtone, (2, 0, 0) - (0, 0, 0), of its ground electronic state (?)~2A". At certain discharge conditions (a.c. frequency of 5 kHz, peak-to-peak voltage of 6.5 kV, 1900 ppm HCHO, 3.5% H_2O in N_2, P_(total)= 30 Torr), HO_2 concentration rises as oxygen concentration increases initially but declined with its further increase. The effects of water concentration, the discharge voltage and the discharge gas pressure on the concentration of HO_2 radicals have been investigated.
The temporary evolution of HO_2 concentration within a half period of the sine wave applied voltage (U_P = 4.5 kV,f_(a.c.) = 5 kHz, 1900 ppm HCHO, 20% O_2, 3.5% H_2O in N_2, P_(total) = 30 Torr) has been studied using the method of "time window". The result shows that the concentration of HO_2 radical increases rapidly during the first 5μs following the first discharge current pulse. After its peak value, HO_2 concentration decreases slowly.
3. The hydroxyl radical, generated in atmospheric DBD plasmas, has been determined via cw-CRDS for the first time. The P-branches of OH X~2Π_i (v' = 2←v" = 0) bands were used for its number density measurements. P_1(7.5)e, P_1(6.5)e, P_1(6.5)f and P_1(5.5)e lines of X~2Π_(3/2) transition together with P_2(6.5)f and P_2(5.5)f lines of X~2Π_(1/2) transition were used to measure the OH rotational temperature (T_R). At certain experimental conditions (a.c. frequency of 70 kHz, 6700 ppm H_2O in He, 1 atm.), when the peak-to-peak discharge voltage varied from 6 kV to 10.4 kV, the determined OH radical concentration increased from (2.1±0.1)×10~(13) molecules cm~(-3) to (3.7±0.1)×10~(13) molecules cm~(-3). The plasma gas temperature, derived from the Boltzmann plots of OH rotational population distributions, ranged from 312±10 K to 363±10 K, when the discharge voltage was raised in the above range. The influences of O_2 and N_2 addition on the production of OH radicals have been also investigated.
引文
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