CN1194808C - Pulse microwave reinforced high pressure low temperature plasma chemical reactor - Google Patents
Pulse microwave reinforced high pressure low temperature plasma chemical reactor Download PDFInfo
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- CN1194808C CN1194808C CNB001232541A CN00123254A CN1194808C CN 1194808 C CN1194808 C CN 1194808C CN B001232541 A CNB001232541 A CN B001232541A CN 00123254 A CN00123254 A CN 00123254A CN 1194808 C CN1194808 C CN 1194808C
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- high pressure
- coaxial
- low temperature
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Abstract
The present invention relates to a pulse microwave intensified high-pressure low-temperature plasma chemical reactor, which is characterized in that the reactor is formed by connecting a waveguide coaxial conversion device (1), a coaxial cavity (2), and a TM010 resonant cavity (3) with a reentry column, wherein an inner conductor (21) of the coaxial cavity (2) extends in the TM010 resonant cavity (3), and introduces plasma exciting voltage through a high-pressure introduce structure (22). The present invention can effectively control plasma, and consequently, can realize the industrialization of plasma chemical synthesis.
Description
The present invention relates to chemical reactor, a kind of pulse microwave reinforced high pressure low temperature plasma chemical reactor is provided especially.
Compare with conventional direct-current arc, high-frequency plasma, microwave plasma has characteristics such as reactivity height, capacity usage ratio height, pure electrodeless pollution and density height, at aspects such as carrying out chemical synthesis, material surface modifying special advantages is arranged, be applicable to preparation and the processing of making high purity substance, and process efficiency is higher.Microwave plasma can be divided into two kinds of low pressure (less than 760Torr) and hyperbars (greater than 760Torr) by its operating pressure.The low pressure microwave plasma has been used widely in fields such as thin film deposition, plasma etchings, but the negative pressure condition of work can't be applicable to such as commercial Application such as switching through of natural gas straight, poisonous and harmful industrial waste gas purifyings.In order to satisfy the needs that large-scale plasma chemistry is synthetic, reach the development new type light source, people have invented the exciting technique of multiple high-pressure microwave plasma in nearly 20 years, summary is got up to mainly contain following several: the exciting technique (CMP) of (1) Capacitance Coupled microwave plasma; (2) exciting technique (Surfatron) of coaxial base table ground roll microwave plasma; (3) exciting technique of waveguide-based surface wave microwave plasma (Surfaguide); (4) TM
010The exciting technique of resonator (MIP) microwave plasma.But angle from chemical reaction, the high-pressure microwave plasma exciting technique that these are traditional also is not suitable for being applied to most of chemical reactions, because the practice of plasma chemistry in decades shows to have only when plasma is in the low temperature nonequilibrium state, just be suitable for most chemical reaction.Our research group has made some significant work in this field; in the patent 00110422.5 of having been accepted, introduced a kind of high-pressure microwave plasma exciter; this device can accumulate microwave energy effectively, strengthen field intensity; do not needing the external world " can realize exciting and keeping of plasma under the condition of ignition in hydriding; can be under the condition of various hyperbar protective atmospheres, atmospheric flow, high power capacity, operation with security and stability.But, this microwave plasma generation technique, to encourage with keeping appearance is one, on structure, have high field intensity and energy accumulation, be easy to make the low temperature glow plasma moment that excites nonequilibrium state that the initial stage forms to carry out the transition to the high temperature arc plasma of near-equilibrium state, this just seems very unfavorable for those astable chemical species of preparation.Therefore,, make microwave plasma promote the chemical reaction technology really to possess the commercial Application condition, must find a kind of excitation of reliable hyperbar low-temperature microwave plasma and keep method for the advantage with the low pressure microwave plasma expands to hyperbar.
The object of the present invention is to provide a kind of pulse microwave reinforced high pressure low temperature plasma chemical reactor, it can make plasma be effectively controlled, thereby can realize the industrialization that plasma chemistry is synthetic.
The invention provides a kind of pulse microwave reinforced high pressure low temperature plasma chemical reactor, it is characterized in that: this device is by the TM of waveguide-coaxial conversion (1), coaxial cavity (2), band reentry post
010Resonator (3) connects and composes; The inner wire (21) of coaxial cavity (2) is deep into TM
010In the resonator (3), and introduce structure (22) by high pressure and introduce plasma exciatiaon voltage.
It is inductance and electric capacity composite construction that high pressure of the present invention is introduced structure (22), by external conductive casing (224), two capacitance sheets (221) (223) and inductance coil (222) constitute, one end of coaxial inner conductor (21) at first links to each other with a capacitance sheet (221), this capacitance sheet (221) constitutes capacitor I with the outer conductor of coaxial line, constitute capacitor I I between external conductive casing (224) and the capacitance sheet (223), capacitance sheet (221) links to each other by inductance coil (222) with capacitance sheet (223), because introducing the external conductive casing (224) of structure, the outer conductor of coaxial line and high pressure join, thereby on circuit, form capacitor I and connect relation in parallel with inductance again with capacitor I I.
In principle, capacitance and inductance value should be big as far as possible, and be big as far as possible for guaranteeing capacitance, can by increase capacity area and reduce between the capacitance sheet distance and between capacitance sheet filling medium realize; Increasing inductance can and place magnetic medium and realize by the number of turn of increase inductance coil in inductance coil.In the embodiment of this patent, reduce capacitance gap and be subjected to coupled high-tension restriction, along with reducing of gap, high voltage is easy to capacitor breakdown, thereby causes choking structure to lose efficacy.Generally capacitor needs working medium to isolate, and these media can be materials such as nylon, tetrafluoroethene, high purity aluminium oxide, magnesia, mica.The number of turn of inductance coil can suitably increase or reduce as required, the foundation of judgement be in debug process, measure the leakage of microwave can situation, guaranteeing to leak the quantity that as far as possible reduces inductance coil under can be less than the situation of 10 microwatt/square centimeters.Gap between the capacitor determines that according to the breakdown voltage of selected dielectric material when dielectric material was selected high purity aluminium oxide for use, capacitance gap was the 0.2-2 millimeter, and the number of turn of inductance coil is the 5-20 circle; When medium was tetrafluoroethene, the gap was the 0.2-1.0 millimeter, and the number of turn of inductance coil is the 10-30 circle; When medium was magnesia, the gap was the 1.0-3.0 millimeter, and the number of turn of inductance coil is the 5-30 circle; When medium was nylon, the gap was the 1.5-4.0 millimeter, and the number of turn of inductance coil is the 20-60 circle.
The present invention has following characteristics:
1, high pressure is introduced structure (double as choking structure), has both sealed electromagnetic field, has avoided the leakage of microwave energy, successfully high pressure is introduced in the microwave cavity again.
2, adopt waveguide-coaxial conversion, after connect the magnetic coupling structure, feed-in microwave energy in coaxial cavity simply efficiently.
3, a door flow structure is adopted in waveguide-coaxial conversion, and both Transmission Microwave energy in coaxial cavity effectively simultaneously made the degree of coupling adjustable again, and the utilization rate of microwave energy is improved.
4, " striking " high voltage mode of being adopted both can be direct current, interchange, also can be radio frequency high tension.
5, adopt pulse microwave that conventional high pressure mercerising plasma is modulated, increased the effective area (volume) of plasma on the one hand greatly, strengthen the activity of plasma simultaneously; On the other hand, can control plasma parameter effectively, stop plasma, successfully obtain the low temperature plasma of nonequilibrium state, also improve the utilization rate of microwave energy simultaneously greatly by the sudden change of nonequilibrium state to equilibrium state.
6, because whole device adopts coaxial cavity, coaxial line transmission, have the frequency band of broad, so this Design of device thought can be suitable for metric wave, decimetric wave and centimeter wave (as 2450MHz, 915MHz, 314MHz etc.).
When 7, this device busy pressure is in 1.0～1.8atm, can stably work.
8, this device can be applicable to gas-phase chemical reaction (as: switching through of natural gas straight system ethene, acetylene, the purification of poisonous and harmful industrial waste gas, etc.), chemical vapour deposition (CVD) (as the deposition of diamond film, etc.).
In a word, the present invention combines conventional high pressure mercerising plasma structure with microwave structure, utilize mercerising plasma microwave reinforced, that expansion is conventional, the volume of conventional mercerising plasma is effectively amplified, impulse modulation by microwave simultaneously, the parameter of control plasma provides a practicable approach for plasma chemistry is synthetic.
Below by embodiment in detail the present invention is described in detail.
Accompanying drawing 1 pulse microwave reinforced hyperbar low temperature plasma chemical reactor structural representation,
Accompanying drawing 2 waveguides-coaxial conversion magnetic coupling structural representation,
Accompanying drawing 3 waveguides-coaxial change-over gate structural representation,
Accompanying drawing 4 high pressure are introduced structural representation,
Accompanying drawing 5 TM
010The cavity resonator structure schematic diagram.
Embodiment 1
The pulse microwave reinforced low temperature plasma exciting bank that is used for chemical reaction is as shown in the figure mainly introduced the introducing structure of structure, 50Hz ac high-voltage, the TM of band reentry post by waveguide → coaxial microwave
010Three parts such as resonator are formed.Fig. 1 is the structural representation of this device.
Microwave is introduced structure and is adopted waveguide-coaxial conversion, and microwave is carried out the transition to the coaxial line transmission from rectangular waveguide, and microwave is coupled to TM
010In the chamber.This device adopts magnetic coupling structure and door flow structure to realize waveguide-coaxial conversion, and the size of coaxial transmission inner and outer conductor can be amplified or dwindle as required, but this moment one section changeover portion must be arranged, to guarantee the impedance matching of transmission line.Fig. 2, Fig. 3 are respectively the structural representations of magnetic coupling structure and door flow structure.
The 50Hz ac high-voltage is introduced structure: introduce the 50Hz ac high-voltage, obtain thread glow plasma in the coaxial line internal excitation, this is the basic point of departure of this device.Must adopt effective choking structure to the inner high-voltage line of introducing of microwave cavity, promptly external high pressure can be introduced inside cavity, microwave can be ended again simultaneously, be unlikely to draw cavity.This device is to adopt inductance coil and electric capacity in conjunction with forming high impedance structures, and its structural representation is seen Fig. 4.
The TM of band reentry post
010Resonator is accumulation energy effectively, and coaxial inner conductor stretches into TM
010The length that resonator is certain, and stretch into length in the cavity by regulating rear end reentry post, decide the resonant frequency of resonator.Its structural representation is seen Fig. 5.
The operation principle of whole device is as follows: waveguide → coaxial transformational structure is transferred to microwave energy in the coaxial cavity, by coaxial line TM is arrived in microwave transmission again
010Resonator, when on coaxial inner conductor, applying ac high-voltage, and pulse microwave in addition, at this moment, by regulating TM
010The length that reentry post in resonator rear end stretches in the cavity makes its resonant frequency identical with microwave source frequency, can form plasma in the inner wire end.Because coaxial inner conductor is at TM
010Be in the position, axis in the resonator, field intensity around it is radiation and is symmetrically distributed, therefore the plasma that forms in its end also is a radiation regimes, if around inner wire reacting gas is used restraint, the energy that then can effectively utilize plasma promotes chemical reaction." the ignition in hydriding; pulse microwave reinforced; so plasma can be stable is in low temperature plasma away from equilibrium state; when the constraint plasma tagma; the reacting gas plasma activation district that can flow through fully again;, also can be used for chemical vapour deposition (CVD) (as utilizing natural gas depositing diamond film) because this device employing high pressure so be very suitable for gas-phase chemical reaction (as the direct conversion of natural gas, the purified treatment of poisonous and harmful industrial waste gas etc.).
For operating frequency is the microwave of 2450MHz, and the size of reaction unit is as follows: d
1=4～10mm, d
2=6～14mm, d
3=20～36mm, d
4=30～50mm, l
1=4～16mm, l
2～2～8mm, d
5=14～30mm, d
6～20～36mm, d
7=34～40mm, d
8=44～60, d
9=36～60mm, d
10=90～120mm wherein, bracing frame among Fig. 2 (hold concurrently hermetyic window) be a polytetrafluoroethylene (PTFE), waveguide-coaxial conversion employing magnetic coupling structure.
Among the embodiment 1, if the inner wire bracing frame of waveguide-coaxial transformational structure (double as hermetyic window) is when being boron nitride, d
1=4～10mm, d
4=45～80mm.
Among the embodiment 1, if the inner wire bracing frame of waveguide-coaxial transformational structure (double as hermetyic window) is when being aluminium oxide, d
1=4～10mm, d
4=100～176mm.
Embodiment 4
Among the embodiment 1,, high pressure only adopt capacitance sheet to come promptly to remove inductance coil, d by microwave as choking structure if introducing part
8=60～90mm.
Embodiment 5
Among the embodiment 1, if the door flow structure is adopted in waveguide-coaxial conversion, device size is as follows: d
1'=20～40mm, d
2'=10～20mm, d
3'=20～46mm, d
4'=70～100mm.
Claims (5)
1, a kind of pulse microwave reinforced high pressure low temperature plasma chemical reactor is characterized in that: this device is by the TM of waveguide one coaxial conversion (1), coaxial cavity (2), band reentry post
010Resonator (3) connects and composes; The inner wire (21) of coaxial cavity (2) is deep into TM
010In the resonator (3), and introduce structure (22) by high pressure and introduce plasma exciatiaon voltage; It is inductance and electric capacity composite construction that described high pressure is introduced structure (22), by external conductive casing (224), two capacitance sheets (221) (223) and inductance coil (222) constitute, one end of coaxial inner conductor (21) at first links to each other with a capacitance sheet (221), this capacitance sheet (221) constitutes capacitor I with the outer conductor of coaxial line, constitute capacitor I I between external conductive casing (224) and the capacitance sheet (223), capacitance sheet (221) links to each other by inductance coil (222) with capacitance sheet (223), because introducing the external conductive casing (224) of structure, the outer conductor of coaxial line and high pressure join, thereby on circuit, form capacitor I and connect structure in parallel with inductance again with capacitor I I.
2, by the described pulse microwave reinforced high pressure low temperature plasma chemical reactor of claim 2, it is characterized in that: during described capacitor dielectric material selection high purity aluminium oxide, capacitance gap is the 0.2-2 millimeter, and the number of turn of inductance coil is the 5-20 circle.
3, by the described pulse microwave reinforced high pressure low temperature plasma chemical reactor of claim 2, it is characterized in that: when described capacitor dielectric was tetrafluoroethene, the gap was the 0.2-1.0 millimeter, and the number of turn of inductance coil is the 10-30 circle.
4, by the described pulse microwave reinforced high pressure low temperature plasma chemical reactor of claim 2, it is characterized in that: when described capacitor dielectric was magnesia, the gap was the 1.0-3.0 millimeter, and the number of turn of inductance coil is the 5-30 circle.
5, by the described pulse microwave reinforced high pressure low temperature plasma chemical reactor of claim 2, it is characterized in that: when described capacitor dielectric was nylon, the gap was the 1.5-4.0 millimeter, and the number of turn of inductance coil is the 20-60 circle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001232541A CN1194808C (en) | 2000-11-15 | 2000-11-15 | Pulse microwave reinforced high pressure low temperature plasma chemical reactor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001232541A CN1194808C (en) | 2000-11-15 | 2000-11-15 | Pulse microwave reinforced high pressure low temperature plasma chemical reactor |
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| CN1351901A CN1351901A (en) | 2002-06-05 |
| CN1194808C true CN1194808C (en) | 2005-03-30 |
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| CN101998747B (en) * | 2009-08-19 | 2012-05-23 | 中国科学院金属研究所 | Low-temperature plasma device |
| CN103691948B (en) * | 2013-12-25 | 2015-06-17 | 山东晶鑫晶体科技有限公司 | Device and method for machining high-density aluminum oxide by plasma |
| CN104357522B (en) * | 2014-11-11 | 2017-11-07 | 四川龙王洞生态农业开发有限公司 | A kind of method for extracting collagen of casting off a skin of utilization giant salamander |
| CN108963239B (en) * | 2018-08-14 | 2020-06-30 | 上海力信能源科技有限责任公司 | Preparation method of titanium dioxide coated nickel cobalt lithium manganate positive electrode material |
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