CN105214562A - Vacuum in situ reaction unit - Google Patents
Vacuum in situ reaction unit Download PDFInfo
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- CN105214562A CN105214562A CN201510761877.7A CN201510761877A CN105214562A CN 105214562 A CN105214562 A CN 105214562A CN 201510761877 A CN201510761877 A CN 201510761877A CN 105214562 A CN105214562 A CN 105214562A
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- stopper slot
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Abstract
The present invention proposes a kind of vacuum in situ reaction unit, comprise sampling device, reaction vessel, air extractor, heater, described reaction vessel is quartz pipe one, comprises in the middle part of opening portion connected successively, container and blind end; Described opening portion is tightly connected by sealing ring and abutted flange first end; Described sample stage comprises the first stopper slot for limiting described sample carrier position in vertical direction and the second stopper slot, and described sample carrier is the flat metal derby for holding the required sample of vacuum in situ reaction.The present invention can be the condition that high temperature and high pressure is created in vacuum in situ reaction, and the impurity simultaneously introduced is few, greatly reduces the interference that response sample is subject to.
Description
Technical field
The present invention relates to experiment equipment field, particularly a kind of vacuum in situ reaction unit.
Background technology
In catalytic chemistry and physical chemistry field, the reactions such as the absorption of gas on solid sample, absorption, catalysis and desorption, and before and after reaction, the change such as component, properity of sample is the research emphasis of new material exploration aspect always.Because a lot of reaction needed is carried out under high temperature, condition of high voltage, and in order to get rid of the impact of the inner gaseous component of reaction unit or extraneous air, reaction unit also needs to configure vacuum system, ensures that sample carries out in site measurement under vacuum conditions.This just proposes the requirements such as temperature, withstand voltage and vacuum to original position example reaction device.
Vacuum in situ reaction unit, for providing the reaction environment of HTHP, allows sample under the environment of high vacuum, to be delivered to other equipment for analyzing and testing in situ, to carry out follow-up test experiments simultaneously.
Under currently available technology, general and spectrum (infrared, the Raman) equipment of vacuum in situ reaction unit matches, and cavity generally all adopts stainless steel to design.Common stainless steel long operating temperature in active gas environment can only reach 500 degrees centigrade, limits the carrying out of a lot of higher temperature reaction experiment to a great extent; And at active gases as in hydrogen reaction experiment, stainless steel easily occurs to inhale hydrogen phenomenon, finally causes the hydrogen in stainless steel to be polymerized to hydrogen molecule, when internal stress exceedes the strength degree of steel, stainless steel inside can form tiny crackle (hydrogen embrittlement).
In addition, the general final vacuum of existing vacuum in situ reaction unit is not high (is 10
-1pa magnitude), sample surfaces sensibility analysis experimental facilities (as photoelectron spectrograph, surface sweeping tunnel microscope) can not be met for environment vacuum degree (10 residing for sample
-4pa magnitude) requirement, cause the change being difficult to record example reaction rear surface intrinsic properties (component, chemical valence state, the density of states etc.).
Summary of the invention
The present invention proposes a kind of vacuum in situ reaction unit, solves the problem that same device under currently available technology cannot meet high temperature and pressure experiment condition.
Technical scheme of the present invention is achieved in that
Vacuum in situ reaction unit, comprises sampling device, reaction vessel, air extractor, heater, and described reaction vessel is quartz pipe one, comprises in the middle part of opening portion connected successively, container and blind end; Described opening portion and abutted flange first end are tightly connected; Described sampling device and described abutted flange second end are tightly connected, and are communicated with described reaction vessel interior; The pump-line of described air extractor is communicated with described reaction vessel interior; Described vacuum in situ reaction unit also comprises the sample stage being arranged on described reaction vessel interior and the sample carrier that can be parked on described sample stage; Described sample stage is in the heated perimeter of described heater; Described sample stage first end is fixedly connected with described reaction vessel inwall, described sample stage comprises the first stopper slot for limiting described sample carrier position in vertical direction and the second stopper slot, described first stopper slot and described second stopper slot symmetrically shape, be horizontally set on the both sides of described sample stage second end respectively; Described sample carrier is used for holding the required sample of vacuum in situ reaction, by the transmission of described sampling device, slides in described first stopper slot and described second stopper slot.
Preferably, described sample stage is that external diameter is less than described reaction vessel internal diameter and the quartz pipe two coaxial with described reaction vessel, the first end of described sample stage is end, be connected with the blind end inwall melting of described reaction vessel, described sample stage second end is openend, described first stopper slot and described second stopper slot are the twice slit of described sample stage both sides tube wall, cave in from described sample stage openend to described sample stage end direction.
Preferably, described reaction vessel opening portion comprises extension neck, extending wall; Extending neck is a flat annulus, and described extending wall is column, and with coaxial in the middle part of described container, and external diameter is greater than in the middle part of described container; Described extension neck inner ring is connected with one end in the middle part of container is vertical, and described extension neck outer shroud is connected with described extending wall first end is vertical; Described extension neck both sides are laid respectively in the middle part of described extending wall, described container.
Preferably, described vacuum in situ reaction unit also comprises sealing device, and described extending wall second end applies pressure by sealing device and described abutted flange first end fits tightly; Described sealing device comprises sealing ring, sealing compressing tablet, positioner; Described positioner one end is fixed on after passing perpendicularly through described sealing compressing tablet in locating hole corresponding on described abutted flange, makes the first surface of the positioning cap press seal compressing tablet of the described positioner other end; Second of described sealing compressing tablet compresses described extension neck, and described extending wall second end is close to sealing ring first surface, and the first end of described abutted flange is close in described sealing ring second face.
Preferably, described sealing device also comprises the pad be arranged between sealing compressing tablet second and described extension neck.
Preferably, described sample carrier comprises body protruding in the middle; Described body comprises lug boss, and be positioned at first side and the second side on described lug boss both sides, described lug boss thickness is greater than the slit separation that the upper wall surface of described first stopper slot and lower wall surface are formed, and the thickness of described first side, second side is all less than the slit separation of the first stopper slot, described second stopper slot; The middle part of described lug boss upper surface is provided with the sample cell for placing sample.
Preferably, described sampling device comprises the sample fetching device that can capture and discharge sample carrier in reaction vessel; Described sample carrier also comprises the afterbody be fixedly connected with described body the 3rd limit, described afterbody comprises the first square and the second square, described first square two ends connect described body the 3rd limit and described second square respectively, and described first square width is less than described second square; Described sample fetching device comprises transmission lever, and described transmission lever inside is provided with elastic device, and described transmission lever end comprises and to extend internally and perpendicular to the baffle plate of described transmission lever shaft length direction, and the barrier slits that described in tolerable, sample carrier afterbody passes through; The clearance distance of described barrier slits is greater than width and the thickness of described first square, is greater than the thickness of described second square, and is less than the width of described second square; Described elastic device props up the medial surface of described baffle plate when off working state, prop up described second square end and provide outside elastic force time in working order.
Preferably, described vacuum in situ reaction unit also comprises inlet duct, the mass-flow gas meter that described inlet duct comprises air inlet pipe and is connected with described air inlet pipe; Described abutted flange is provided with air inlet, and described air inlet pipe one end is communicated with described reaction vessel interior by the air inlet on abutted flange.
Preferably, described vacuum in situ reaction unit also comprises and is arranged on described abutted flange first end side, for cooling the cooling device of described sealing ring.
Preferably, described cooling device is water cooling tube, and nested rings is around the first end side of described abutted flange.
The beneficial effect of vacuum in situ reaction unit of the present invention mainly contains:
1, reaction vessel adopts the material of quartz, and can be the condition that reaction experiment creates high temperature and high pressure, the impurity simultaneously introduced is few, greatly reduces the interference that response sample is subject to; The wall thickness of quartz material is directly related with high pressure resistant intensity, and the thickness of 10mm can bear the pressure of 10MPa, experimental pressure demand can regulate wall thickness;
2, sample stage adopts the design of quartz pipe and stopper slot, uses in conjunction with sample carrier and sample transferring device, response sample is transmitted more efficient, stable;
3, the outward extending design in reaction vessel opening portion, combination seal device and abutted flange use, and make the vacuum in reaction vessel reach 10
-5pa magnitude, the more condition of high vacuum degree demand that after can meeting high-temperature high-voltage reaction, sample in-situ is measured.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the structural representation of reaction vessel preferred embodiment in the present invention;
Fig. 2 is the partial structurtes schematic diagram of vacuum in situ reaction unit preferred embodiment of the present invention;
Fig. 3 is the structural representation of inventive samples platform and sample carrier preferred embodiment;
Fig. 4 is the Facad structure schematic diagram of sample carrier in Fig. 3;
Fig. 5 is the side structure schematic diagram of Fig. 3;
Fig. 6 is the structural representation of heater preferred embodiment of the present invention;
Fig. 7 is the structural representation of the preferred embodiment that sampling device of the present invention is connected with reaction vessel;
The structural representation of preferred embodiment when Fig. 8 is sampling device of the present invention crawl sample carrier;
Fig. 9 is the structural representation of transmission lever preferred embodiment of the present invention;
Figure 10 is the structural representation of the preferred embodiment of inventive samples holder afterbody when entering in transmission lever;
The structural representation of preferred embodiment when Figure 11 is transmission lever of the present invention crawl sample carrier.
Numbering illustrates: reaction vessel 1, sample stage 2, sample carrier 3, opening portion 4, sealing ring 5, abutted flange 6, sealing compressing tablet 7, pad 8, positioner 9, air extractor 10, cooling device 11, air inlet pipe 12, mass-flow gas meter 13, heater 14, infrared lamp 15, heated center 16, sampling device 17, in the middle part of container 101, blind end 102, first stopper slot 201, second stopper slot 202, extend neck 401, extending wall 402, body 31, lug boss 311, first side 312, second side 313, afterbody 32, first square 321, second square 322, transmission lever 171, elastic device 172, baffle plate 173, barrier slits 174, transition chamber thereof 18, slide valve 19.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of vacuum in situ reaction unit, as shown in Figure 1, Figure 2, shown in Fig. 3, Fig. 6, Fig. 7, comprise sampling device 17, reaction vessel 1, air extractor 10, heater 14; Reaction vessel 1 is quartz pipe one, comprise be connected successively opening portion 4, in the middle part of container 101 with blind end 102; Opening portion 4 and abutted flange 6 first end are tightly connected; Sampling device 17 and abutted flange 6 second end are tightly connected, and are communicated with reaction vessel 1 inside; The pump-line of air extractor 10 is communicated with reaction vessel 1 inside; Vacuum in situ reaction unit also comprises the sample stage 2 being arranged on reaction vessel 1 inside and the sample carrier 3 that can be parked on sample stage 2; Sample stage 2 is in the heated perimeter of heater 14; Sample stage 2 first end is fixedly connected with reaction vessel 1 inwall, sample stage 2 comprises the first stopper slot 201 and the second stopper slot 202 for limiting sample carrier 3 position in vertical direction, first stopper slot 201 and the second stopper slot 202 symmetrically shape, be horizontally set on the both sides of sample stage 2 second end respectively; Sample carrier 3 is for holding the required sample of vacuum in situ reaction, and sample carrier 3 under the transmission of sampling device 17, can slide in the first stopper slot 201 and the second stopper slot 202.
Sampling device 17 of the present invention, air extractor 10, heater 14 can adopt existing technology and equipment.
Reaction vessel 1 is for the formation of reaction cavity, for response sample provides the environment of high temperature and high pressure in vacuum in situ reaction, what reaction vessel 1 of the present invention adopted is quartzy material, compared with the stainless steel adopted with reaction cavity of the prior art, the advantage of quartz material is can be high temperature resistant, can bear high temperature 1500 degrees centigrade, heating rate is fast, saves the heat time; Simultaneously the quartzy material foreign gas of releasing in a vacuum is little, to greatly reduce in experiment and test process reaction cavity itself to the interference of response sample; Quartz material voltage endurance capability is strong, and 10mm thickness can bear the pressure of 10MPa; In addition, quartzy material its structural strength below 1000 degrees Celsius is unaffected, maximizes while can realizing temperature and pressure.In a preferred embodiment, the opening portion 4 of reaction vessel 1 only has an opening, makes whole reaction cavity have higher sealing, and this opening is for being communicated with the parts such as sampling device 17, air extractor 10, heater 14.
Reaction vessel 1 and the connected mode of abutted flange 6 can be common nested, weld, bonding, press the modes such as connection, as long as reach the object of sealing joint.In a preferred embodiment, adopt the mode of directly welding to be welded together in the opening portion 4 of reaction vessel 1 and abutted flange 6, this fixed form can provide higher vacuum thus adapt to more harsh demand.
Heater 14 in the present invention both can be common focus type infra red heating device, also can be the infra red heating device of divergence form, the different and different of heater 14 type are looked in reaction vessel 1 and the position of heater 14, as long as sample stage 2 is positioned at the heat energy coverage of this heater 14.In a preferred embodiment, heater 14 adopts structure as shown in Figure 6, it is around arranging multiple infrared lamp 15, make ultrared Voice segment on heated center 16, axis between infrared lamp 15 is heat tunnel, as long as the sample stage 2 in reaction vessel 1 is parked on heat tunnel, the position that the sample carrier 3 being contained with response sample is placed in heated center 16 just can be heated.In a preferred embodiment, heater 14 also comprises high-frequency heating assembly (adopting high-frequency heating assembly of the prior art, as high frequency induction heater etc.), makes heating-up temperature more than 1500 degrees Celsius.
The effect of the sampling device 17 in the present invention is delivered in reaction vessel 1 by response sample by sample carrier 3, or taken out in reaction vessel 1 by sample carrier 3 after completion of the reaction; The form that sampling device 17 picks and places sample carrier 3 both can be simple mechanical gripping or prop up, and also can be to have come picked-up and release by the mode of common magnetic induction technology, sucker technology.
The effect of the air extractor 10 in the present invention is the gas in abstraction reaction container 1, make reaction vessel 1 have the vacuum of certain rank, what it adopted is existing vacuum-pumping equipment (as the vaccum-pumping equipment etc. that prime mechanical pump combines with molecular pump).
Abutted flange 6 can have multiple opening, and its effect is tightly connected respectively by different openings and reaction vessel 1, sampling device 17, air extractor 10.In a preferred embodiment, as shown in Figure 7, carry out picking and placeing of response sample for convenience, sampling device 17 and reaction vessel 1 are separately positioned on the both sides of abutted flange 6, are specially sampling device 17 and are tightly connected with abutted flange 6 second end by transition chamber thereof 18 and slide valve 19.
The mode that sample stage 2 first end and reaction vessel 1 inwall are fixedly connected with can be that melting is connected, also can be the common fixed form such as clamping, joggle, the point that sample stage 2 first end is connected with reaction vessel 1 both can on the inwall of the opening portion 4 of reaction vessel 1, also can be portion 101 in a reservoir inwall on, also can on the inwall of blind end 102, as long as the effect that sample stage 2 has fixed position in reaction vessel 1 can be realized.
Sample stage 2 is hollow structure, profile can be tubulose, square, spherical, forked etc., as long as meet the feature that both sides have the first stopper slot 201 and the second stopper slot 202, as shown in Figure 3 and Figure 5, first stopper slot 201 and the second stopper slot 202 comprise the upper lower wall of bottom land and symmetric shape respectively, and wherein lower wall is for supporting sample carrier 3.
Sample carrier 3 can under the transmission of sampling device 17, slides to the bottom of groove from the opening of the first stopper slot 201 and the second stopper slot 202 along the lower wall portion of groove.
First stopper slot 201 and the second stopper slot 202 1 aspect can the positions of fixed sample holder in vertical direction 3, make it significantly rock up and down, can support sample carrier 3 on the other hand by the lower wall portion of groove, realize parking function.In a preferred embodiment, sample stage 2 is only limitted to edge with the way of contact of sample carrier 3 and contacts, and makes the response sample on sample carrier 3 in heating process, be unlikely the stop being subject to too many contact point/face, improves the efficiency of heating surface; Simultaneously also convenient extraneous measuring instrument from above and below response sample is made measurements, is scanned and other information gatherings.
Sample carrier 3 can be block, also can be other common spherical, tubes, and a demand fulfillment normally can carry response sample and enters reaction vessel 1 inside and be parked in sample stage 2 under high-temperature and high-pressure conditions.Sample carrier 3 can adopt the materials such as high-purity copper, tantalum, molybdenum.In a preferred embodiment, as shown in Figure 3, sample carrier 3 is the flat tantalum metal derby of a both sides symmetrical shape, its upper surface is used for holding response sample, its dual-side can slide in the first stopper slot 201 and the second stopper slot 202 and park in sample stage 2, this design, for the object of saving material, makes sample carrier 3 become light and handy simultaneously.
In a preferred embodiment, sample stage 2 is less than reaction vessel 1 internal diameter and the quartz pipe two coaxial with reaction vessel 1 for external diameter; The first end of sample stage 2 is end, be connected with the blind end 102 inwall melting of reaction vessel 1, sample stage 2 second end is openend, and the first stopper slot 201 and the second stopper slot 202 are the twice slit of sample stage 2 both sides tube wall, cave in from sample stage 2 openend to sample stage 2 end direction.
Sample stage 2 is designed to the tube of quartzy material, and it at high temperature still can have higher-strength, reaches the object better supporting sample carrier 3, and the foreign gas of simultaneously self releasing is little.The fixed form of sample stage 2 adopts melting to connect, and improves the soundness of junction, also makes junction at high temperature discharge foreign gas as few as possible.
The groove depth of the first stopper slot 201 and the second stopper slot 202 has not a particular requirement, as long as the lower wall energy that can meet groove supports sample carrier 3.First stopper slot 201, second stopper slot 202 height in vertical direction also has not a particular requirement, preferably make the first stopper slot 201, second stopper slot 202 be in same level with the axis of sample stage 2, such benefit makes the bang path of response sample minimum.In a preferred embodiment, the end of sample stage 2 is connected with the positive middle part melting of reaction vessel 1 blind end, reaction vessel 1 and sample stage 2 with same axis for benchmark, axial symmetry respectively in small one and large one is cylindric, make not need when mounted to consider the inverted problem in top and bottom, the energy also making focus type heat can evenly arrive response sample place.
In a preferred embodiment, as shown in Figure 1, reaction vessel 1 opening portion 4 comprises extension neck 401, extending wall 402; Extending neck 401 is a flat annulus, and extending wall 402 is in column, and with 101 coaxial in the middle part of container, and external diameter to be greater than in the middle part of container 101; Extend neck 401 inner ring to be connected with 101 one end are vertical in the middle part of container, extend neck outer shroud and be connected with extending wall 402 first end is vertical; In the middle part of extending wall 402, container, 101 lay respectively at extension neck 401 both sides.
The extending wall 402 be connected, extend neck 401, in the middle part of container 1 cross section in "
" shape.In this preferred embodiment the design of reaction vessel 1 make the internal diameter container of opening portion 4 in the middle part of 101 internal diameters large, not only on being externally tightly connected, there is more branched support structure, expand the type of attachment with abutted flange 6, also the larger parts of a part of volume of sampling device 17 are made can to stretch into a segment distance in reaction vessel 1 as required, outside being unlikely to be blocked in.
In a preferred embodiment, composition graphs 1 and Fig. 2, vacuum in situ reaction unit also comprises sealing device, and extending wall 402 second end applies pressure by sealing device and abutted flange 6 first end fits tightly; Sealing device comprises sealing ring 5, sealing compressing tablet 7, positioner 9; Positioner 9 one end is fixed in locating hole corresponding on abutted flange 6 after passing perpendicularly through sealing compressing tablet 7, makes the first surface of the positioning cap press seal compressing tablet 7 of positioner 9 other end; Second of sealing compressing tablet 7 compresses extension neck 401, and extending wall 402 second end is close to sealing ring 5 first surface, and the first end of abutted flange 6 is close in sealing ring 5 second face.
In this preferred embodiment, sealing ring 5 is thin round with the contact surface of extending wall 402 second end, the pressure that the extension whole face of neck 401 is subject to is passed to the contact surface of thin round by extending wall 402 second end, this contact surface is made to be subject to enormous pressure, sealing ring 5 is higher with the laminating degree of extending wall 402 second end, thus has better sealing effectiveness.
The principle of this preferred embodiment is by applying pressure to extending neck 401, making the opening portion 4 of reaction vessel 1 seal and being adjacent to abutted flange 6 first end; Sealing ring 5 is elastic soft material, is generally the organic material that vacuum deflation rate is little, air-tightness is good, and sealing ring 5 is rubber ring in the preferred embodiment, and its material is the polyimides for high vacuum environment; Sealing compressing tablet 7 is rigid material, can adopt the materials such as stainless steel; Positioner 9 adopts common positioning element, can be the screw, screw etc. of band nut, its quantity has not a particular requirement, more than 4 and annular is arranged on around reaction vessel 1 opening portion 4 best, and locating hole corresponding on abutted flange 6 carries out adaptability setting according to the type of positioner 9; In the preferred the present embodiment of one, positioner 9 adopts screw, and screw hole corresponding on abutted flange 6 is crept into, other end nut compression seal compressing tablet 7 through sealing compressing tablet 7 in its one end.
In a preferred embodiment, as shown in Figure 2, sealing device also comprises the pad 8 being arranged on sealing compressing tablet 7 second and extending between neck 401.Pad 8 is that common cushion connects material, as rubber, silica gel etc., its Main Function is the seal degree improving sealing compressing tablet 7 and extend between neck 401 two kinds of rigid materials, avoid extending neck 401 due to uneven stressed and occur the situation of slight crack, also to a certain degree alleviate reaction vessel 1 simultaneously and excessive temperature is directly passed to sealing compressing tablet 7.In the present embodiment, pad 8 is rubber sheet gasket, and its material is polytetrafluoroethylene (PTFE).Adopt above-mentioned with the preferred embodiment of screw location and compression seal compressing tablet 7, rubber ring and rubber sheet gasket, the vacuum in reaction vessel 1 can be made to reach 10
-4more than Pa magnitude, be greatly better than can reach 10 of prior art
-1pa magnitude; On the basis of this preferred embodiment, can adopt and adopt multistage rubber ring difference form to be connected with the opening portion 4 of reaction vessel 1 at the first end of acting flange 6, make the vacuum in reaction vessel 1 reach 10
-5more than Pa magnitude.
In a preferred embodiment, composition graphs 3, Fig. 4, Fig. 5, sample carrier 3 comprises body 31 protruding in the middle; Body comprises lug boss 311, and be positioned at first side 312 and the second side 313 on lug boss 311 both sides, lug boss 311 thickness is greater than the slit separation that the upper wall surface of the first stopper slot 201 and lower wall surface are formed, and the thickness of first side 312, second side 313 is all less than the slit separation of the first stopper slot 201, second stopper slot 202; The middle part of lug boss 311 upper surface is provided with the sample cell 314 for placing sample.
Sample carrier 3 is the design of middle part convex shape, make depth to move on sample introduction direction in the middle part of it, and significantly can not move toward both sides, the further specification motion track of sample carrier 3, the transmission deviation of sample carrier 3 is reduced further, improve the stable degree that sample carrier 3 is laid on sample stage 2 simultaneously, avoid sample carrier 3 to skid off from sample stage 2 both sides.Sample carrier 3 peripheral shape is not particularly limited, and sample carrier 3 periphery is square in a preferred embodiment, and first side 311, second side 312, lug boss 311 are also square.The design of sample cell 314 makes response sample be not easy to topple over from sample carrier 3 or flow out, and sample cell 314 adopts common shape, can be square, circular, star etc., adopt rhombus as shown in Figure 4 in a preferred embodiment.
In a preferred embodiment, sampling device 17 comprises the sample fetching device that can capture and discharge sample carrier 3 in reaction vessel 1; Sample carrier 3 also comprises the afterbody 32 be fixedly connected with body 31 the 3rd limit, afterbody 32 comprises the first square 321 and the second square 322, first square 321 two ends connect body 31 the 3rd limit respectively and the second square 322, first square 321 width is less than the second square 322; Sample fetching device comprises transmission lever 171, transmission lever 171 inside is provided with elastic device 172, transmission lever 171 end comprises and to extend internally and perpendicular to the baffle plate 173 of transmission lever 171 shaft length direction, and the barrier slits 174 that tolerable sample carrier afterbody 32 passes through; The clearance distance of barrier slits 174 is greater than width and the thickness of the first square 321, is greater than the thickness of the second square 322, and is less than the width of the second square 322; Elastic device 172 props up the medial surface of baffle plate 173 when off working state, prop up the second square 322 end and provide outside elastic force time in working order.
Sample carrier 3 is as the shape of Fig. 4, strong with the surface analysis equipment compatibility such as existing a lot of electron spectrum (XPS), PSTM (STM), the slitless connection between vacuum in situ reaction unit and these commercialization surface analysis equipment can be realized.
The operation principle of this preferred embodiment is, the afterbody 32 of sample carrier 3 level can enter (shown in Figure 10) in barrier slits 174 by extraneous toward interior thrust, after second square 322 enters barrier slits 174 1 segment distance, start touching and elasticity of compression device 172, after the second square 322 have passed barrier slits 174 completely, transmission lever 171 can rotate to an angle α (being preferably 90 degree) by user in vertical direction, now cancel extraneous toward interior thrust, elastic device 172 will provide the horizontal force of outwards motion for the second square 322, because now barrier slits 174 and the relative position of the second square 322 have become vertical (shown in Figure 11), and the width of the second square 322 is greater than the clearance distance of barrier slits 174, therefore the second square 322 is stuck in transmission lever 171 end, now reach the object of transmission lever 171 clamped sample holder 3, when sample carrier 3 is passed on sample stage 2, when touching the bottom land of the first stopper slot 201, second stopper slot 202, owing to moving on, if transmission lever 171 continues the direction motion passing sample, then elastic device 172 will be compressed, now transmission lever 171 can be reversely rotated certain angle α by user in vertical direction, then the second square 322 becomes with the relative position of barrier slits 174 and is positioned at same plane, as shown in Figure 10, now transmission lever 171 retreats, and can reach release sample carrier 3, make sample carrier 3 stay object on sample stage 2.
Elastic device 172 adopts prior art to design, and the way of contact of elastic device 172 and the second square 322 is for slidingly contacting, and the present embodiment Elastic device 172 adopts spring.
Vacuum in situ reaction unit can inject the specific gas needed for reaction after evacuation, because reaction vessel 1 adopts quartzy material, therefore can meet compatible a greater variety of gas, as hydrogen, oxygen, argon gas, nitrogen etc.In a preferred embodiment, as shown in Figure 2, vacuum in situ reaction unit also comprises inlet duct, the mass-flow gas meter 13 that inlet duct comprises air inlet pipe 12 and is connected with air inlet pipe 12.Abutted flange 6 is provided with air inlet, and air inlet pipe 12 one end is communicated with reaction vessel 1 inside by the air inlet on abutted flange 6.Adopt mass-flow gas meter 13 to reach and accurately control the quality of reacting gas and the object of flow velocity.Vacuum in situ reaction unit of the present invention also can meet the experiment of dynamic gas by adopting the design of prior art.
For avoiding sealing ring 5 be out of shape by temperatures involved or damage, in a preferred embodiment, vacuum in situ reaction unit also comprises and is arranged on abutted flange 6 first end side, cooling device 11 for coolant seal circle 5.Cooling device 11 can adopt existing design, and its type of cooling can be liquid or gas cooling.
In a preferred embodiment, cooling device 11 is water cooling tube, and nested rings is around the first end side of abutted flange 6.
The quartzy material that the present invention adopts all can pass through infrared ray, and reaction vessel 1, sample stage 2 and sample carrier 3 can experimentally require to be arranged to different thickness, weight, volume.In a preferred embodiment, reaction vessel pipe thickness is between 2 ~ 3mm, and internal diameter is between 20 ~ 22mm, and length is between 25 ~ 30mm; Sample stage 2 is tubulose, and its material thickness is between 1 ~ 2mm, and internal diameter is between 10 ~ 11mm, and length is between 15 ~ 25mm; Sample carrier 3 base area is at 300 ~ 400mm
2between; Above-mentioned feature makes vacuum in situ reaction unit reaction zone small volume and less weight, required narrow-minded, has very high-resolution and (generally can reach 10 in residual gas constituent analysis experiment
-6pa magnitude).
Various embodiment is in reconcilable situation above, can combinationally use mutually.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. vacuum in situ reaction unit, comprises sampling device (17), reaction vessel (1), air extractor (10), heater (14), it is characterized in that:
Described reaction vessel (1) is quartz pipe one, comprises (101) and blind end (102) in the middle part of opening portion (4) connected successively, container;
Described opening portion (4) and abutted flange (6) first end are tightly connected;
Described sampling device (17) and described abutted flange (6) second end are tightly connected, and are communicated with described reaction vessel (1) inside;
The pump-line of described air extractor (10) is communicated with described reaction vessel (1) inside;
Described vacuum in situ reaction unit also comprises the sample carrier (3) being arranged on the inner sample stage (2) of described reaction vessel (1) and can being parked on described sample stage (2);
Described sample stage (2) is in the heated perimeter of described heater (14);
Described sample stage (2) first end is fixedly connected with described reaction vessel (1) inwall, described sample stage (2) comprises the first stopper slot (201) for limiting described sample carrier (3) position in vertical direction and the second stopper slot (202), described first stopper slot (201) and described second stopper slot (202) symmetrically shape, be horizontally set on the both sides of described sample stage (2) second end respectively;
Described sample carrier (3), for holding the required sample of vacuum in situ reaction, by the transmission of described sampling device (17), slides in described first stopper slot (201) and described second stopper slot (202).
2. vacuum in situ reaction unit as claimed in claim 1, it is characterized in that: described sample stage (2) is described reaction vessel (1) internal diameter for external diameter is less than, and the quartz pipe two coaxial with described reaction vessel (1), the first end of described sample stage (2) is end, be connected with blind end (102) the inwall melting of described reaction vessel (1), described sample stage (2) second end is openend, the twice slit that described first stopper slot (201) and described second stopper slot (202) are described sample stage (2) both sides tube wall, cave in from described sample stage (2) openend to described sample stage (2) end direction.
3. vacuum in situ reaction unit as claimed in claim 2, is characterized in that: described reaction vessel (1) opening portion (4) comprises extension neck (401), extending wall (402); Extending neck (401) is a flat annulus, and described extending wall (402) is in column, coaxial with (101) in the middle part of described container, and external diameter is greater than (101) in the middle part of described container; Described extension neck (401) inner ring is connected with in the middle part of described container, (101) one end is vertical, and described extension neck (401) outer shroud is connected with described extending wall (402) first end is vertical; In the middle part of described extending wall (402), described container, (101) lay respectively at described extension neck (401) both sides.
4. vacuum in situ reaction unit as claimed in claim 3, it is characterized in that: described vacuum in situ reaction unit also comprises sealing device, described extending wall (402) second end applies pressure by sealing device and described abutted flange (6) first end fits tightly;
Described sealing device comprises sealing ring (5), sealing compressing tablet (7), positioner (9);
Described positioner (9) one end is fixed on after passing perpendicularly through described sealing compressing tablet (7) in the upper corresponding locating hole of described abutted flange (6), makes the positioning cap of described positioner (9) other end compress the first surface of described sealing compressing tablet (7); Second of described sealing compressing tablet (7) compresses described extension neck (401), described extending wall (402) second end is close to described sealing ring (5) first surface, and the first end of described abutted flange (6) is close in described sealing ring (5) second face.
5. vacuum in situ reaction unit as claimed in claim 4, is characterized in that: described sealing device also comprises the pad (8) be arranged between described sealing compressing tablet (7) second and described extension neck (401).
6. vacuum in situ reaction unit as claimed in claim 5, is characterized in that: described sample carrier (3) comprises body (31) protruding in the middle;
Described body (31) comprises lug boss (311), and be positioned at first side (312) and second side (313) on described lug boss (311) both sides, described lug boss (311) thickness is greater than the slit separation that the upper wall surface of described first stopper slot (201) and lower wall surface are formed, and the thickness of described first side (312), described second side (313) is all less than the slit separation of the first stopper slot (201), described second stopper slot (202); The middle part of described lug boss (311) upper surface is provided with the sample cell (314) for placing sample.
7. vacuum in situ reaction unit as claimed in claim 6, is characterized in that: described sampling device (17) comprises the sample fetching device that can capture and discharge described sample carrier (3) in described reaction vessel (1);
Described sample carrier (3) also comprises the afterbody (32) be fixedly connected with described body (31) the 3rd limit;
Described afterbody (32) comprises the first square (321) and the second square (322), described first square (321) two ends connect described body (31) the 3rd limit and described second square (322) respectively, and described first square (321) width is less than described second square (322);
Described sample fetching device comprises transmission lever (171), described transmission lever (171) inside is provided with elastic device (172), described transmission lever (171) end comprises and to extend internally and perpendicular to the baffle plate (173) of described transmission lever (171) shaft length direction, and the barrier slits (174) that sample carrier afterbody (32) described in tolerable passes through; The clearance distance of described barrier slits (174) is greater than width and the thickness of described first square (321), is greater than the thickness of described second square (322), and is less than the width of described second square (322); Described elastic device (172) props up the medial surface of described baffle plate (173) when off working state, prop up described second square (322) end and provide outside elastic force time in working order.
8. vacuum in situ reaction unit as claimed in claim 7, it is characterized in that: described vacuum in situ reaction unit also comprises inlet duct, the mass-flow gas meter (13) that described inlet duct comprises air inlet pipe (12) and is connected with described air inlet pipe (12);
Described abutted flange (6) is provided with air inlet, and described air inlet pipe (12) one end is communicated with described reaction vessel (1) inside by the air inlet on described abutted flange (6).
9. vacuum in situ reaction unit as claimed in claim 8, is characterized in that: described vacuum in situ reaction unit also comprises and is arranged on described abutted flange (6) first end side, for cooling the cooling device (11) of described sealing ring (5).
10. vacuum in situ reaction unit as claimed in claim 9, it is characterized in that: described cooling device (11) is water cooling tube, nested rings is around the first end side of described abutted flange (6).
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| CN201510761877.7A CN105214562B (en) | 2015-11-10 | 2015-11-10 | Vacuum in situ reaction unit |
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| CN201510761877.7A CN105214562B (en) | 2015-11-10 | 2015-11-10 | Vacuum in situ reaction unit |
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| CN105214562B CN105214562B (en) | 2017-11-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107029635A (en) * | 2017-05-25 | 2017-08-11 | 桂林理工大学 | A kind of method and device of prepare compound under vacuum conditions |
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| CN205199471U (en) * | 2015-11-10 | 2016-05-04 | 费勉仪器科技（上海）有限公司 | Vacuum in situ reaction device |
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| CN104368288A (en) * | 2014-11-25 | 2015-02-25 | 三明学院 | Low-vacuum low-temperature radio frequency inductively coupled plasma reactor and use method thereof |
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