CN101173953A - System and method for sampling tests - Google Patents
System and method for sampling tests Download PDFInfo
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- CN101173953A CN101173953A CNA2007101627903A CN200710162790A CN101173953A CN 101173953 A CN101173953 A CN 101173953A CN A2007101627903 A CNA2007101627903 A CN A2007101627903A CN 200710162790 A CN200710162790 A CN 200710162790A CN 101173953 A CN101173953 A CN 101173953A
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Abstract
The invention provides a test system for testing samples loaded on a carrier, comprising a closed empty cavity, a pre-treating unit, and a test unit, wherein, the closed empty cavity is provided with a first region and a second region; the pre-treating unit is used for pre-treating the sample when the carrier is positioned in the first region; the testing unit is used for testing the sample when the carrier is positioned in the second region after the sample is pretreated; the testing unit comprises a testing device for determining the characteristic of the sample.
Description
[technical field]
The present invention relates to a kind of system and method for specimen test, relate in particular to a kind of system and method for catalyst sample test.
[background technology]
In recent years, along with the development of technology and research method, many have premium properties and widely used new material constantly is developed.The exploitation of understanding in depth not only material to the new material performance has very big benefit, and production application of material etc. is had better guide significance.
Along with the application of combinational chemistry in investigation of materials, make the researcher can prepare the wide variety of materials sample simultaneously.Yet, in the short period of time the performance of a large amount of samples is tested and material is screened and make traditional research method face huge difficulty.In traditional research method, need to prepare wide variety of materials and be used for research, in such cases, R﹠D costs will improve, and research institute takes time manyly, are unfavorable for the research and development of material.
Yet the appearance of little reaction technology has solved this difficult problem.Little reaction technology is to place minisize reaction equipment to carry out traditional chemical reaction, significantly reduces the volume of reactant.Compare with traditional chemical reaction, the capable of reducing energy consumption and material consumption of little reaction reduces R﹠D costs, improves resource utilization.It has high heat transfer, high mass transfer and safe characteristics, and systematically response time quickening, has improved the work efficiency of system.In addition, its easier realization performance history is continuous and highly integrated.Data analysis and little reaction technology of current advanced person's process automation, sensing technology, detection technique and software view are combined, thereby produced the little reactive system of high flux.
In the little reactive system of high flux, the preparation of sample is a comparatively complicated process, may need to experience processes such as screening, grinding, dissolving or heating.In the whole process of preparation of sample, and in the process that the sample for preparing is shifted and preserves, sample may be subjected to environment pollution (such as, be subjected to the pollution of water in air steam or oxygen), make some composition in the sample may produce oxidation or other variations, this will produce very big influence to last test findings.
Therefore, need provide the system and method for a kind of sample pretreatment and test, make sample unaffected in the process of preparation, transfer or preservation.
[summary of the invention]
The invention reside in provides a kind of specimen test system and method, and it can make sample better participate in reaction.
One aspect of the present invention provides a kind of pilot system that is loaded into the sample on the substrate that is used to test.Described pilot system comprises enclosed cavity, pretreatment unit and test unit.Described enclosed cavity has first area and second area.Described pretreatment unit carries out pre-service to described sample when described substrate is positioned at the first area.Described test unit after described sample carries out pre-service and described substrate sample is tested when being positioned at second area, this test unit includes the characteristic that proving installation is used for determining described sample.
The present invention provides a kind of specimen test system on the other hand.This specimen test system comprises pretreatment unit and test unit.Described pretreatment unit includes the sample that can carry the substrate that is placed with sample and carries part and described sample is carried out pretreated pretreatment unit.Described test unit links to each other with described pretreatment unit, and after sample carried out pre-service, the described substrate that is placed with sample entered described test unit, and this test unit includes proving installation, is used for determining the characteristic of described sample.
The present invention provides a kind of test method that is positioned over the sample on the substrate that is used to test again, and it is included in the pretreatment unit described sample is carried out pre-service; By a passage that is communicated with described pretreatment unit the substrate that is placed with through pretreated sample is moved on to a test unit from described pretreatment unit, make described sample after described pretreatment unit pre-service and before test, not be exposed in the air; The described pretreated sample of test in described test unit is to determine the characteristic of sample.
The present invention also provides a kind of reactor that is used for specimen test, and it includes the top, can carry the bottom of the substrate that is placed with sample, the middle part between top and bottom, probe and and the plurality of conduits that links to each other of probe.Described top, middle part and bottom are formed with reaction chamber jointly, and described reactor also is provided with probe, and described probe is contained in the reaction chamber, and be installed at least middle part and bottom the two one of on.
The present invention also provides a kind of reactor that is used for specimen test, it comprises the reaction chamber and first light source, described reaction chamber has first opening, and described sample is tested in described reaction chamber, and described first light source is positioned at outside the described reaction chamber and can produces first light beam.Described reactor comprises also and is arranged at the secondary light source that described reaction chamber is used to produce second light beam outward that one of described at least first light source and secondary light source can be opened in the described reaction chamber by described first and operate.
Like this, utilize pilot system of the present invention and method just can better help the carrying out of testing.
[description of drawings]
Fig. 1 is the structural representation of one embodiment of the present invention, and wherein sample substrate is positioned at the first area.
Fig. 2 is the structural representation of the present invention's embodiment shown in Figure 1, and wherein sample substrate is positioned at second area.
Fig. 3 is structural representation and the substrate and the structures of samples synoptic diagram placed thereon of sample substrate of the present invention.
Fig. 4 is the structural representation of another embodiment of the present invention, and wherein probe is positioned at the first area.
Fig. 5 is the structural representation of the present invention's embodiment shown in Figure 4, and wherein probe is positioned at second area.
Fig. 6 is the structural representation of another embodiment of the present invention.
Fig. 7 is the structural representation of four embodiment of the invention, and wherein, the pre-service platform is positioned at primary importance.
Fig. 8 is the structural representation of four embodiment of the invention, and wherein, the pre-service platform is positioned at the second place.
Fig. 9 is the three-dimensional combination figure of preferred embodiment of the present invention, and this system comprises reactor and pretreater.
Figure 10 is the three-dimensional combination figure of pretreater in the system shown in Figure 9.
Figure 11 is the three-dimensional cutaway view of pretreater shown in Figure 10, and wherein, the combination of pre-service platform and shielding part 5 is positioned at the second place.
Figure 12 is the three-dimensional cutaway view of the combination of pre-service platform shown in Figure 11 and shielding part.
Figure 13 is the three-dimensional combination figure of the combination of pre-service platform shown in Figure 12 and shielding part.
Figure 14 is the section plan at top in the pre-service chamber of pretreater shown in Figure 10, and wherein, the pre-service platform is positioned at primary importance.
Figure 15 is the section plan of pretreater shown in Figure 10, and wherein, the pre-service platform is positioned at the second place.
Figure 16 is the section plan of pretreater shown in Figure 10, and wherein, the pre-service platform is positioned at primary importance.
Figure 17 is the three-dimensional combination figure of reactor of the present invention.
Figure 18 is the configuration diagram of the reactive system of reactor of the present invention.
Figure 19 is the part three-dimensional combination figure of reactor of the present invention shown in Figure 17.
Figure 20 is the enlarged drawing of regional A shown in Figure 19.
Figure 21 is the cut-open view of the probe of reactor of the present invention.
Figure 22 is the enlarged drawing of area B in the cut-open view of probe shown in Figure 21.
Figure 23 is the three-dimensional cutaway view of bottom cover plate of the probe of reactor of the present invention.
Figure 24 is the three-dimensional view of distributary division of the probe of reactor of the present invention.
Figure 25 is the pressure control configuration diagram in the reactor of the present invention.
Figure 26 is another pressure control configuration diagram in the reactor of the present invention.
Figure 27 is the system function module synoptic diagram of the reactive system of reactor of the present invention.
Figure 28 utilizes reactor of the present invention to carry out the schematic flow sheet of test operation.
Figure 29 is the structural representation of reactor bottom opening and light source and substrate in one embodiment of the present of invention.
Figure 30 is the another kind of structural representation of reactor bottom opening and light source and substrate in one embodiment of the present of invention shown in Figure 29.
Figure 31 is the third structural representation of reactor bottom opening and light source and substrate in one embodiment of the present of invention shown in Figure 29.
Figure 32 be shown in the structural representation of reactor bottom opening and light source and substrate in an alternative embodiment of the invention.
Figure 33 is the another kind of structural representation of reactor bottom opening and light source and substrate in an alternative embodiment of the invention shown in Figure 32.
Figure 34 is the vertical view of the opening offered on the reactor among another embodiment of the present invention.
Figure 35 is the three-dimensional cutaway view of the opening offered among Figure 34.
Figure 36 is the side-looking structural plan synoptic diagram of the opening offered among Figure 34.
Figure 37 is the another kind of cross-sectional view of the opening offered among another embodiment of reactor of the present invention.
Figure 38 is the third cross-sectional view of the opening offered among another embodiment of reactor of the present invention.
Figure 39 is the heating system configuration diagram of reactor of the present invention.
[preferred embodiment]
As depicted in figs. 1 and 2, it is the synoptic diagram of an embodiment of pilot system of the present invention.System 1000 comprises an enclosed cavity 100 with first area 1020 and second area 1010.In the first area 1020 and 1010 of second areas be provided with path 10 30.Described system 1000 comprises that also the pretreatment unit 102 of a pretreatment sample in first area 1010 and one are in the test unit 101 of second area 1010 build-in test samples.A substrate 300 is used to carry described sample.
Described sample can be a catalyzer.Described pre-service can be that sample is reduced on the one hand, such as, for oxidized sample, described pretreatment unit includes a pretreatment unit, it can feed hydrogen by passage in pretreatment unit, and, make oxidized sample under the uniform temperature condition, reduce by the heating arrangement heated sample.Simultaneously, the unnecessary hydrogen and the water vapor that produces that reduces are exported from described pretreatment unit 102.On the other hand, described pre-service also can be that sample is carried out drying, such as, for pollute the sample that makes moist because of water vapor, need carry out drying to it, can pass through the heating arrangement heated sample, sample is controlled under the higher temperature environment, utilize inert gas will be under described higher temperature environment the formed water vapor of vaporizing of the moisture content in the sample take away.
As shown in Figure 3, n*n bearing area 301 can be set on the sample substrate 300, n is the integer greater than 1.Such as n equal 20 or n greater than 1 smaller or equal to 100.The material of sample substrate 300 can be quartz or silicon chip etc.Similar and different sample (sample) can be placed in each bearing area 301.It is relevant that sample 302 is positioned over the size and the required reaction of finishing of height h on the sample substrate 300 and each bearing area, and general h value is the 10-300 micron.In order to make being cemented on the substrate (carrying part) that sample can be comparatively firm, surface treatment can be carried out in each bearing area, make it increase roughness and come fixed tester sample, substrate also can be provided with lower concave part and place test sample book certainly, as the lower concave part that has disclosed in the prior art.
Continuation is provided with the test platform 15 that can place sample substrate 300 referring to shown in Fig. 1-2 in test unit 101.In the present embodiment, this test platform 15 can accurate move, and it is subject to Temperature Influence, especially be subjected to temperatures involved after, can reduce performance accuracy, influence result of use.Can also be provided with the probe 109 that can be used as test unit at test unit 101.Probe can be provided with sampling structure on 109, is used for the reaction product of collected specimens test as sampling channel 105, leads in the analytical equipment and analyzes.
In described specimen test unit 101, described probe 109 can move relative to each other with described test platform 15.Like this, by moving of described test platform (substrate carries part) 15, just can realize the location of aiming at of each bearing area 301 and described sampling channel 105 on the described sample substrate 300, make that sampling channel 105 can be relative with the testing site (being the bearing area that sample is reacting) on the sample substrate 300, thereby collect the reaction product on this testing site.In order to realize the relative positioning of each bearing area 301 and sampling channel 105 on the sample substrate 300 exactly, described test platform 15 should avoid being subjected to the influence of high temperature as far as possible, reduces the degree of accuracy of location to avoid its distortion back, influences result of use.
In addition, in the present embodiment, can be provided with input channel 106 and output channel 107 on the probe 109 in the described test unit 101, be used to provide required material (being generally gaseous material) the turnover test unit 101 of test.Certainly, described input channel 106 and output channel 107 also can be provided with in addition, and need not be arranged on the probe 109.
Described test unit 101 also is provided with heating arrangement 108, is used for controlling the temperature of specimen test, and it can be the device that LASER HEATING system, infrared heating system, heating collar or any other can heating objects.And described heating arrangement 108 is the multiple sample on a plurality of bearing areas of heated sample substrate 300 simultaneously, also can the multiple sample on a plurality of bearing areas of sample substrate 300 be heated successively.In the present embodiment, described heating arrangement 108 is arranged on the test unit 101, and it also can be provided with separately, and does not need to be arranged on the test unit 101.
In described pretreatment unit 102, be provided with the relative cap 204 of 25 and one on pre-service platform (substrate carries part) being used for placing described sample substrate 300 and described pre-service platform 25.But described pre-service platform 25 and 204 relative motions of described cap, the sample substrate 300 when moving to a certain position on it can and described cap 204 between form a gap, the distance between this moment cap 204 and the sample substrate 300 is between 0.5～1mm.Wherein, described pre-service platform 25 and described cap 204 are all movable; Also can fix by pre-service platform 25 cap 204 relative pre-service platforms 25 motions; Can also fix by cap 204 25 relative these caps 204 motions of pre-service platform.Described heating arrangement 208 can be installed on the described cap 204.
Described pretreatment unit 102 also is provided with input channel 206 and output channel 207, like this, when sample is carried out pre-service so that pretreatment gas enter described gap and from its discharge.Because the restriction in this gap, the gas of input channel 206 and output channel 207 supplies can form a relatively stable and concentrated air-flow, flows through sample.
Shown in Fig. 4-5, it is the synoptic diagram of another embodiment of specimen test of the present invention system, and same numeral is represented same element among itself and first embodiment.In the present embodiment, test unit 101 and pretreatment unit 102 with input channel 106 and output channel 107 as them shared input channel and output channel.Input channel 106 and output channel 107 are installed on the movable probe 109, this probe 109 can move between first area and second area, when the first area (as shown in Figure 4), input channel 106 and output channel 107 provide pre-service required gas, when second area (as shown in Figure 5), input channel 106 and the required gas of output channel 107 sampling test.Described cap 204 uses also can be worked as in the bottom surface 1040 of being somebody's turn to do probe 109 in addition.
Shown in Fig. 6-8, it is the synoptic diagram of other embodiments of the invention, its with Fig. 1-2 and Fig. 3-4 in identical label represent same element.In this embodiment, described specimen test system comprises sample product reactor 1 and the pretreater 2 that links to each other with reactor 1.Reactor 1 has reaction chamber 10, i.e. second area; Pretreater has reaction chamber 20, i.e. first area.Shown in Fig. 1-2 and Fig. 4-5, in the present embodiment, first area 20 and second area 10 are two cavitys independent mutually and that be communicated with, and this cavity 10 and 20 independent mutually and that be communicated with is communicated with by a passage 24.Like this, do not have the concrete device of pretreatment zone for existing pilot region, can change whole device, the cavity that the pretreatment zone of a correspondence of need making is used is coupled, just can realize purpose of the present invention, thereby can save cost.Moreover, pre-service cavity and test cavity (being reaction chamber) are set independently after, it is simpler, compact and reliable that wherein independent pre-service cavity and test cavity are all finished the device of pre-service and reaction test than one.In Fig. 6-8, a mobile device 28 is arranged on the sample pre-conditioner 2, is used for pretreated sample substrate from first area 20 and by moving to second area 10 behind the passage 24.Certainly, described sample mobile device 28 also can be used in the specimen test system shown in Figure 1.In the present embodiment, described mobile device 208 is a catch bar.
As shown in Figure 6, these passage 24 places can also be provided with an on-off element 210 that is used for the connection between described two cavitys 10 of opening/closing and 20.This on-off element 210 can be that gate valve or any other can be controlled the element of two regional connectivities.Certainly, also same on-off element 210 can be set among Fig. 7-8.
In Fig. 7-8, in the present embodiment, cap 204 is fixing, and 25 relative caps 204 motions of pre-service platform when pre-service platform 25 moves when primary importance (shown in Figure 7) with respect to cap 204, form described gap; When (shown in Figure 8), mobile device 28 can move on to described second area 10 to sample from described first area 20 on the second place.Certainly, as mentioned above, can select cap 204 and 25 relative motions of pre-service platform as required.Simultaneously, in this enforcement, sample pre-conditioner 2 belows are provided with drive unit 4 and are used for driving pre-service platform 25 and move up and down.
As shown in Figure 9, it is the three-dimensional combination figure of specimen test of the present invention system preferred embodiment, its with earlier figures in identical label can represent same element.Described sample comprises the catalyzer that contains noble metals such as platinum.In this embodiment, described specimen test system comprises a sample pre-conditioner 2, sample product reactor 1, drive unit 4 (shown in Figure 10), mobile device 28 and be used for connecting the pre-service chamber of pretreater 2 and the docking section 23 of the reaction chamber in the reactor 1.
Shown in Figure 10-16, it is the system architecture diagram of the sample pre-conditioner 2 in the preferable pilot system of the sample of the present invention shown in Fig. 9.Shown in ginseng Figure 10 and 11, pretreater 2 has a cavity of being made up of upper cavity 21 and lower chamber 22, forms a columned pre-service chamber 20 in the cavity.Wherein, upper and lower cavity 21 and 22 links together by securing member 201, and the junction is by O-ring seal 202 sealings.This pretreater 2 also is provided with a docking section 23, is used for connecting with reactor 1, offers communication passage 24 in this docking section 23, is used for being communicated with the reaction chamber in pre-service chamber 20 and the reactor 1.
In this pre-service chamber 20 pre-service platform 25 is arranged, this pre-service platform 25 has a horizontal upper surface 250, is used for placing treating pretreated sample substrate.In the present embodiment, also be provided with the sample panel 30 that is used for loading described sample substrate, sample substrate can be installed in the groove of sample panel 30, in practical operation, by mobile example plate 30 mobile example substrates, handled easily.
Shown in Figure 15-16, connected one in the position of these pre-service platform 25 close cavity bottoms 221 and promoted cylinder 4, this promotion cylinder 4 can promote pre-service platform 25 and move between the primary importance (as shown in figure 16) and the second place (shown in Figure 11 or 15).The promotion cylinder 4 that adopts in the present embodiment has the function that prevents output shaft 41 rotations, thereby can avoid pre-service platform 25 rotation phenomenon to occur between the primary importance and the second place in the process of moving.The bottom of lower chamber 22 also is equipped with four supporters 29, is used for supporting fixing whole pretreater 2.
Shown in Figure 10,14 and 16, be provided with ring shaped heating mechanism (not shown) in the ring groove at the cavity top 211 of described pretreatment unit 2 212, and near cavity top 211, offer input channel 206 and output channel 207 (shown in Figure 10 and 14).When pre-service platform 25 is positioned at primary importance, near cavity top 211 input channel 206 and output channel 207, a narrow and small gap is formed on pre-service platform 25 and cavity top 211, sample is positioned at this gap, heating arrangement heats sample, input channel 206 is relative with sample with output channel 207, and by feeding the required gas of pre-service in the input channel 206 on sample, the gas that unreacted gas and reaction generate is discharged from output channel 207.
In the present embodiment, owing to fit in 211 both sides, top of pre-service platform 25 and pretreatment unit 2, so it is closed that described gap is tending towards, and can to a certain extent heat in the preprocessing process and gas be concentrated in this gap, reduce influence to other zones and structure.Because a narrow space has been formed on sample substrate and cavity top 211, the distance that has 0.5～1mm between the upper surface of sample substrate and the top 211, sample on the sample substrate does not contact with cavity top 211, ring shaped heating mechanism heats cavity top 211, and the cavity top 211 after the heating is transmitted heat by heat radiation and thermal convection to sample.
In the present embodiment, the outside at cavity top 211 adopts provision for thermal insulation to reduce scattering and disappearing of heat, this provision for thermal insulation is to coat spun-glass insulation cotton 213 in the outside at cavity top 211, and the skin of heat-preservation cotton 213 coats stainless steel casing 214, so that the outward appearance of installation and enhanced system.
In addition, because sample distribution is on the different bearer zone of a larger-size sample substrate, and that the size of input channel 206 compares is less, gas is comparatively concentrated during from 206 outputs of this input channel, if the gas that comes out from this port is without water conservancy diversion or just disperse and lead on the sample substrate, gas is difficult to flow through equably the sample on each bearing area on the substrate.
Therefore, shown in Figure 11～13, in the present embodiment, in order to make gas flow through the sample on each bearing area of sample substrate equably, on the position of the port of close input channel 206 on the pre-service platform 25, be provided with fair water fin 26, offer a plurality of diversion trenchs 260 that are divergent shape on the fair water fin 26, with the gas of input channel 206 ports equably water conservancy diversion to each bearing area of sample substrate.
Accordingly, on the pre-service platform 25 near also being provided with corresponding fair water fin 27 on the position of output channel 207 ports, will the flow through unreacted gas of the sample on each bearing area of sample substrate or gas that reaction produces of the diversion trench 270 on the fair water fin 27 is pooled to output channel 207 and discharges.
Wherein, the port of input channel 206 and output channel 207 is roughly on the relative position on the same straight line, and the port place straight line of this input channel 206 and output channel 207 is vertical with the direction of catch bar 28 mobile example plates 30. Fair water fin 26 and 27 is located at the position near the port of input channel 206 and output channel 207 respectively, and sample panel 30 can be positioned on the position between two fair water fins 26 and 27.For the ease of the position that sample panel 30 is imported between two fair water fins 26 and 27, that end of counter sample inlet 200 is provided with chamfering 261 and 271 respectively on fair water fin 26 and 27.For the ease of the position of sample panel 30 between two fair water fins 26 and 27 shifted onto the reaction chamber of reactor 1, that end of corresponding docking section 23 is provided with chamfering 262 and 272 respectively on fair water fin 26 and 27.
When the original state of pretreater, pre-service platform 25 is positioned at the second place, on promptly relative with sample inlet 200 and docking section passage 24 position.
The whole process of carrying out sample pretreatment comprises:
(1) sample location: will be mounted with the appropriate location of sample panel 30 from entering the mouth between 200 pre-service platform 25 baffle upper plates 26 and 27 that push in the pre-service chamber 20 of sample substrate 300 with catch bar 28, the location of sample panel 30 is determined by the advance distance of catch bar 28;
(2) sample preparation: drive and promote cylinder 4, locate after making pre-service platform 25 rise to primary importance, to stability of flow, heating and temperature control (setting of temperature timing curve) is set the pretreated time to the gas that the feeding pre-service is used (being hydrogen in the present embodiment);
(3) sample transfer: after sample preparation finishes, pre-service platform 25 is return the second place, will test reaction in the reaction chamber of sample panel 30 on the pre-service platform 25 by the 24 immigration reactors 1 of the passage in the docking section 23 with catch bar 28.
Because pre-service chamber 20 interconnects with reactor 1, may be penetrated in the reactor 1 and disturb ensuing test so in preprocessing process, feed hydrogen in the pre-service chamber 20.Therefore, can be after above-mentioned (3) step be finished, just sample transfer in the reaction chamber after, system is evacuated with whole test, gives then to feed reacting gas in the reactor 1 and test.In addition, also can in the docking section 23 that connects pretreater 2 and reactor 1 on-off element be set, for example gate valve is controlled the connection of described pretreater 2 and reactor 1.Be provided with under the situation of gate valve, sample transfer in the reaction chamber after, can closing gate valve, the connection of described pretreater 2 and reactor 1, and then reactor 1 is evacuated so that carry out follow-up test.
At the following of pre-service platform 25 shielding part 5 can be installed.In the present embodiment, described shielding part 5 is three layers of mirror board.The outer rim of described mirror board and cavity inner wall spacing are less, so just can prevent gas that pre-service uses a large amount of infiltrate into 20 belows, pre-service chamber, and the heat radiation that prevents 211 places, cavity top is to 20 belows, pre-service chamber, thereby avoided the member generation chemical change of 20 belows, pre-service chamber or produced losing efficacy.Such as, prevent the inefficacy of O-ring seal 202 at high temperature.
In addition, in the present embodiment, the upper surface 250 of described pre-service platform 25 also can be used as shielding part and uses.For example, polishing is carried out on this surface, or can prevent or reduce the material of radiation in the spraying, perhaps make described pre-service platform with the material that prevents or reduce radiation, shield as much as possible in described gap with the heat radiation that will produce in the preprocessing process, reduce heat radiation to other zone.
As shown in figure 11, for the heat that further reduces cavity top 211 transmits downwards, welded water cooling tube 209 at the middle part of upper cavity 21, force cooling to reduce heat conduction from top to bottom, preventing that the member of cavity lower part is overheated makes seal failure, improves system's usability and security.
Shown in Figure 11,12 and 14, in the present embodiment, join with a bit of metal hose 205 between pre-service platform 25 and the mirror board 5, mirror board 5 can move up and down with pre-service platform 25, because the deformability of metal hose 205, can be so that pre-service platform 25 upward movements during to primary importance, this pre-service platform 25 can be well and top 211 fit.
In addition, can connect gas flow and pressure control device (not shown) at input channel 206 front ends, the flow and the pressure of gas to input is controlled, can also from output channel 207, insert the thermopair (not shown) that the while thermometric is used, so that the temperature in the pretreatment unit is monitored.
Shown in Figure 17-28, it is the system architecture diagram of the reactor 1 in the preferable pilot system of the sample of the present invention shown in Fig. 9.Certainly, employed reactor 1 also can be the structure that other has disclosed as prior art in specimen test of the present invention system.
In the system architecture diagram of the preferable reactor 1 of the specimen test of the present invention system shown in Figure 17-28, reactor 1 is frame structure, and it has top 150, the bottom 151 relative with the top and be positioned at top 150 and the middle part 152 of 151 of bottoms.A reaction chamber 153 (as Figure 18 and shown in Figure 19) has been formed jointly on this top 150, bottom 151 and middle part 152.Middle part 152 is a rectangular configuration, and its three different sides are separately installed with first, second and third drive unit 155,157 and 156.This first, second and third drive unit 155,157 and 156 tail ends are equipped with stepper motor, are used to drive the motion of reaction chamber 153 inner associated components.In the present invention, the side that middle part 152 is equipped with the 3rd drive unit 156 offers window 11, and can place a charge-coupled image sensor 158 (Charge Coupled Device is called for short CCD in these window 11 places.Shown in Figure 180).152 other relative two sides offer one group of perforate of different sizes and position respectively in the middle part, and this perforate is used to peg graft and reactor 1 is carried out the pipeline 159 of the supply of raw material reaction thing, discharge, product sampling, pressure control and various electrical equipment etc.As seen, in embodiments of the present invention, the various pipelines 159 that communicate with reaction chamber 153 all 152 pass through from the middle part.Certainly, as required, also can be partly or entirely from the top 150 or bottom 151 pass through.
The configuration diagram of reactor 1 residing reactive system of the present invention as shown in figure 18.Reactor 1 of the present invention is positioned at the reactive system middle part, and it is the core of whole reaction system system.Be provided with the platform (substrate carries part) 8 of probe 10 and placement substrate 300 in the reaction chamber 153 of reactor 1.Described probe 10 can be taken exercises with respect to platform 8, with platform as object of reference, the motion that described probe 10 can be done to require, as all around, move up and down, certainly, this moment, in fact described platform can be fixed, perhaps it can move; Otherwise, when described platform can be taken exercises with respect to described probe, to pop one's head in as object of reference, the motion that described probe can be done to require is as all around, move up and down, at this moment, in fact described probe can be fixed, and perhaps it can move.In this preferred embodiment, probe 10 can vertically move up and down, and platform 8 can all around move along X, Y-axis level.Shown in arrow among Figure 18, the raw material reaction thing passes through pneumatic stopping valve (not shown) successively, filtrator (not shown) arrives mass flow controller 160, then delivers to probe 10 through the input pipe 118 on reactor 1 middle part 152.In reaction chamber 153, the sample on raw material reaction thing and the substrate 300 participates in reaction, and resultant of reaction is delivered to the vacuum chamber 6 from the 10 process sampling pipes 123 of popping one's head in.The product that 161 pairs of detecting instruments are delivered in the vacuum chamber 6 carries out check and analysis.Follow-uply just can handle detect obtaining data.In addition, thereby taking place when preventing that resultant of reaction from carrying in sample lines, condensation blocks sample lines 123, so need heat temperature control to sampling pipe 123.Among the present invention, detecting instrument 161 is a quadrupole mass spectroscope, and mass spectrometric ionization filament and sampling pipe tail end distance can according to circumstances be optimized.
In addition, the unreacted raw material reaction thing of part is delivered to efferent duct 124 through probe 10 and then is exported by pressure and flow controller 162.Reaction chamber 153 and vacuum chamber 6 all are provided with independently pump group and valve control (not shown), to realize vacuum requirement separately.Vacuum chamber 6 plug-in elementary mechanical pumps and molecular pump are to realize higher vacuum requirement.And reaction chamber 153 against vacuum degree are less demanding, and it is just passable only to need that elementary mechanical pump is installed.In embodiments of the present invention, input pipe 118 is meant and is mainly used in the pipeline of carrying reactant gas (being the required gas of specimen test), do not get rid of in this reactant gas certainly and contain impurity.Simultaneously, described sampling pipe 123 is meant the pipeline of mainly product being sampled and carrying, and does not also get rid of certainly and is being mingled with other gas in the process of carrying product, as unreacted reactant gas etc.Described efferent duct 124 refers to be mainly used to discharge unnecessary reactant gas, certainly, is not precluded within to discharge and discharges other a small amount of gases in the unnecessary reactant gas process.
In conjunction with shown in Figure 17, Figure 19 removes the three-dimensional combination figure at top 150 for reactor 1 of the present invention.Bottom 151 convex being provided with along Y direction of reactor 1 are extended guidance part 114.Platform 8 movable being installed on the guidance part 114, this movable platform 8 are divided into the movable last lower platform that is installed together (not mark).Join shown in Figure 20ly, second drive unit 157 is output as a stainless steel (not shown), and this bar connects the lower platform of movable platform 8, and it is moving in guidance part 114 upper edge y-axis shifts to drive this lower platform.The 3rd drive unit 156 is output as stainless steel 119, and this bar 119 connects the upper mounting plate of movable platform 8, and upper mounting plate is moved in lower platform upper edge X-axis.Like this, drive unit 156 and 157 can make platform 8 do plane X, Y-axis motion jointly in reaction chamber 153.When the substrate 300 that contains tester (sample) is loaded on the movable platform 8, thereby second and third drive unit 157 and 156 can move substrate along X, Y-axis by driving platform 8.On the side of middle part 152 with respect to installation drive unit 156 1 sides of reactor 1, offer and load window 112, in pilot system of the present invention, docking section 23 in the pretreater 2 is contained in window 112 with this and links to each other, and substrate 300 can be loaded on the movable platform 8 in loading window 112 places.
Referring to Figure 19 and shown in Figure 20, reactor 1 is provided with an installation portion 113 in reaction chamber 153, in the present invention, this installation portion 113 is a beam structure, it is unsettled in reaction chamber 153 that its two end fixed relative two sides that are connected with the middle part 152 of first and second drive unit 155 and 157, this beam structure connect the pars intermedia (mark) of its two end.Certainly, even this installation portion 113 can be arranged at other positions of 152, middle part or be arranged on the bottom 151 of reaction chamber 153 is arranged on bottom 151 and the middle part 152.Installation portion 113 has protruded out rail portion 115 from top to bottom in the substantial middle position.Probe 10 can move up and down along the rail portion on the installation portion 113 115 by means of a support portion 116.Probe 10 is fixed together with support portion 116, in the present embodiment, support portion 116 roughly is platy structure and also can be used to play heat insulation effect, certainly, it can be other Any shape, moves up and down along rail portion 115 as long as it can make probe 10 be fixed thereon and can drive probe 10.In embodiments of the present invention, rail portion 115 is provided with two row's balls (not shown), and support portion 116 moves up and down along ball.Certainly, probe 10 also can directly be arranged on the rail portion 115, and moves along it.Support portion 116 is provided with grab (not mark) along the both sides of X-direction, and an end of pair of resilient members 117 (as spring) is hung on the grab, and the other end is hung on the installation portion 113.Certainly, as required, described grab also can be arranged on the probe 10.Drive unit 155 exports on the stainless steel 110 by the stepper motor of tail end, the free end by this bar 110 and then output on the contact site 111 of connecting link 110.The upper surface of contact site 111 contact sondes 10.In the present embodiment, described connecting link 110 and contact site 111 are independently parts of difference, and certainly, it also can be one-body molded.Drive unit 155 can press down probe 10 it is moved downward by driving contact site 111, and at this moment, a pair of spring 117 is elongated and deformation takes place.When drive unit 155 returned, contact site 111 no longer pressed down probe 10, and spring 117 moves upward owing to restoring force spurs probe 10.So the cooperation that moves up and down by drive unit 155 and spring 117 of probe 10 realizes.As required, described drive unit 155 also can be used to directly to drive probe 10 and moves up and down.In conjunction with shown in Figure 17, CCD 158 be arranged at window 11 places be used for to pop one's head in 10 and the distance that is positioned between the substrate 300 on the movable platform 8 adjust and proofread, with the relative position of better positioning probe 10 with substrate 300.
Referring to pop one's head in 10 cut-open view of the present invention shown in Figure 21, probe 10 is the critical components in the reactor 1, and it has been born raw material sample introduction, sampling and pressure equilibrium and isolated impurity and has entered effects such as reaction chamber 133.In conjunction with the enlarged drawing of area B among Figure 21 shown in Figure 22, probe 10 comprises main part 125, is installed on the cover plate 126 and the shunting nuclear 137 of bottom, main part 125 below.The main part 125 medianly zygomorphic unstripped gas gas exhaust ducts 127 that are provided with two levels offer the vertical unstripped gas gas exhaust duct 128 that is communicated with and runs through main part 125 with horizontal gas exhaust duct 127 downwards in the end of unstripped gas gas exhaust duct 127.Main part 125 portion thereon offers product sampling conduit 129 and is provided with opening 1250 with sampling conduit 129 coaxial communication in its underpart.In conjunction with shown in Figure 23, cover plate 126 is recessed to form a depressed part 140 downwards in the position, intermediate portion, and the bottom surface of depressed part 140 roughly is concave structure.This substantial middle position, depressed part 140 bottom surface offers cylindrical hole 139 downwards and offers larger-diameter reaction chamber 133 in the end of this cylindrical hole 139.Reaction chamber 133 both sides offer air admission hole 131 and venthole 130 in the bottom surface of depressed part 140 lateral margin and depressed part 140 side symmetries.Bottom surface in described cover plate 126 upwards offers first groove 141 and second groove 142 that is connected respectively with all air admission holes 131 and all ventholes 130 ends again.Described air admission hole 131 and venthole 130 are on the peripheral circumferential that is arranged at reaction chamber 133 of annular.Certainly, but described air admission hole or venthole also polygonized structure such as other spread patterns such as square, triangle be arranged on the peripheral circumferential of reaction chamber.
In conjunction with Figure 22, shown in 24, shunting nuclear 137 central authorities are provided with the axis hole 138 that runs through on it, and its periphery offers semicircle orifice runner 134 from top to bottom along its axial direction, and certainly, this runner 134 also can be offered by curve form from top to bottom.When probe 10 main part 125, cover plate 126 and shunting nuclear 137 were assembled together, the exhaust passage 127,128 of main part 125 was connected with venthole 130 on the cover plate 126.The depressed part 140 of cover plate 126 has formed host cavity (not mark) jointly with the opening 1250 on the main part.The bottom of shunting nuclear 137 protrudes out downwards, the setting that matches with the concave bottom surfaces of the depressed part 140 of cover plate 126 just, otherwise can be also with.So just do not need other supplementary modes, shunting nuclear just can be positioned to shunt in the described host cavity easily.Shunting nuclear 137 is contained in this host cavity and with the sidewall spacers of host cavity and cooperates, and is certain, its also can with described host cavity interference fit.The sampling channel 129 coaxial settings of cylindrical hole 139, reaction chamber 133 and main part 125 on the axis hole 138 on the shunting nuclear 137 and the cover plate 126.In addition, the top of shunting nuclear 137 and the top of main part 125 openings, promptly hybrid chamber 136 has been formed jointly at the top of host cavity, and offers sample channel 135 on the sidewall of hybrid chamber 136.Referring to Figure 20 and shown in Figure 21, input pipe 118 is arranged in the sample channel 135, and sampling pipe 123 enters and runs through axis hole 138 and cylindrical hole 139 and then arrive reaction chamber 133 from sampling conduit 129, and efferent duct 124 is arranged in the exhaust passage 127.Sampling pipe 123 can be used kapillary, and the kapillary interior diameter can be the 10-100 micron, with different pressure differential between adaptive response chamber 153 and the vacuum chamber 6.Certainly, length capillaceous can be adjusted as required.
When probe 10 when carrying out work, at first the pressure in the reaction chamber 153 need reach the reaction pressure requirement, and need finish the stable supplying of unstrpped gas etc.; Then, drive unit 155,156 and 157 drive to be loaded with the platform 8 of substrate 300 and to pop one's head under the effect of motor and 10 reach preposition, in this process, CCD158 to pop one's head in 10 and the distance that is positioned between the substrate 300 on the movable platform 8 adjust and proofread; Subsequently, unstrpped gas enters hybrid chamber 136 from input pipe 118, unstrpped gas carries out arriving along the runner 134 of shunting nuclear 137 peripheries after to a certain degree the mixing upper surface of air admission holes 131 in hybrid chamber 136, and air admission hole 131 is shunted unstrpped gas again in air inlet; Then, unstripped gas enters first groove 141 and mixes again after air admission hole 131 comes out; And then after unstrpped gas went out first groove 141, the tested thing on fraction arrival reaction chamber 133 and the substrate 300 on the reflecting point reacted, and resultant of reaction is delivered in the vacuum chamber 6 via sampling pipe 123 and analyzed for quadrupole mass spectroscope 161; The unstrpped gas of another major part arrives at second groove 142 after venthole 130 is then discharged by exhaust passage 128 and efferent duct 124.
In reactor 1, the pressure equilibrium during reaction in the reactor 1 is an important requirement.Can charge into environmental gas in the reaction chamber 153 (ginseng Figure 18), be generally inert gas such as argon gas (Ar), make to reach predetermined pressure in the reaction chamber 153.As shown in figure 25, be arranged on the unstrpped gas sample channel flow controller 160 of improving quality and controlling the flow of unstrpped gas, mass flow controller 163 is being controlled the flow of the environmental gas in the reaction chamber 153, is arranged on pressure and flow controller 162 on the gas exhaust duct and is controlling pressure in the reaction chamber 153.Described environmental gas is to charge into the gas in the environment in the reactor.
During test, when unstrpped gas dividing potential drop when to reach environmental gas be pressure in the reaction chamber 153, influence reduces environmental gas to the reacting gas in the reaction chamber 133, and pressure and cavity pressures in the reaction chamber 133 reach balance.Like this, when the distance between probe 10 and the substrate 300 obtains appropriate value, the unstrpped gas of coming out from first groove 141 can form gas shield at substrate 300 between probe 10, just can stop the environmental gas in the reaction chamber 153 to enter the generation of reacting with influence in the reaction chamber 133.
Among Figure 25, the discharge of unreacted unstrpped gas is mainly controlled by pressure and flow controller 162 in the reaction chamber 153, but the entry position of vent port is arranged on the probe 10, and is very near apart from reaction chamber 133.Generally speaking, be subject to processing technology, detection, control device and system cost, the intermittent motion resolution between probe 10 and the substrate 300 is controlled at micron order, as the 10-20 micron.When the raw material reaction airshed is very little, as 1 to 2 milliliter of per minute, and the flow range of pressure and flow controller 162 is bigger, during as 500 milliliters of per minutes, the aperture of pressure and flow controller 162 may be difficult for realizing to the control of the pressure equilibrium in the reaction chamber 133, when the controlled variable of adjusting pressure and flow controller 162 still can not well solve pressure equilibrium, just needed another kind of control pressurer system.
Figure 26 is another pressure control configuration diagram in the reactor of the present invention.It is at the less relatively situation of raw material reaction airshed.Among Figure 26, pressure and flow controller 162 is being controlled the pressure of the environmental gas in the reaction chamber 153, mass flow controller 163 is being controlled the flow of the environmental gas in the reaction chamber 153, and pop one's head in pressure equilibrium on 10 and gas are discharged by mass flow controller 164 and realized.Here, the flow Q of mass flow controller 164 should with raw material reaction airshed Q resource, just the flow of the flow of the raw material reaction gas controlled of mass flow controller 160 is suitable, general, Q=10*Q resource.Perhaps, more simple mode is with the pipeline replacement mass flow controller 164 of a big flow resistance, such as kapillary.The flow value of mass flow controller 164 or internal diameter capillaceous and length value are with relating to parameters such as the environmental pressure in the reaction chamber 153, probe 10 height.
In this reactive system, what need the various control subsystem to work in coordination to guarantee to test well carries out.The system function module synoptic diagram of the reactive system of reactor of the present invention as shown in figure 27, this reactive system can comprise control module 40, motion and locating module 49, heating temperature control module 42, pump and valve module 45, raw material sample introduction module 46, reactor module 1, product analysis module 43, data processing module 44 etc.Control module 40 is being controlled locating module, heating temperature control module, pump and valve module and raw material sample introduction module, and then controlling the carrying out of reactor internal reaction, product flows to the product analysis module and carries out test analysis acquisition data from reactor, and then data are delivered to data processing module carry out data processing, for follow-up other steps are got ready.
As shown in figure 28, the flow process of carrying out process of the test in reactor of the present invention is followed successively by: opening initialization 50 comprises the Load System initialization files, checks that starting vacuum system, inspection source of the gas and inspection starts kapillary heating etc.; Dress sample 51 comprises and inserts the substrate that contains tester; Clean 52, comprise that utilizing reaction chamber to be inflated to preset pressure vacuumizes mode the other side then and answer the chamber repeatedly to clean; Location 53 comprises the setting of reaction chamber pressure, and probe, platform etc. are in initial position etc.; The test process is provided with 54, comprises the reacting gas parameter being set, the reaction chamber parameter is set, heating curves is set, response path is set and the flow controller parameter being set, and checks the source of the gas airshed, laser system (referring to Figure 39), cooling system etc.; Test is monitoring 55 in real time, comprises monitoring reaction conditions, ccd image, substrate state and checks reaction result etc.; Off-test 56; Unload sample 57 at last.
Below with a carbon monoxide (CO) oxidation test the application of the present invention in process of the test is described.
Test objective: the activity of CuO in the CO oxidizing process of different amounts on the test base reflecting point
Test condition: 1.CO:4.7%
2.O
2： 7.1％
3.Ar： 88.2％
4. overall flow: 17ml/min
5. heatable catalyst CuO spends from room temperature to 400
6. substrate is through 650 degree calcinings
Test findings: the CuO of different amounts has significant effects to the conversion ratio of CO, along with the increase of the amount of CuO in little reactive system, and its active increase.
In another embodiment of reactor of the present invention (not shown), described reactor includes top, the bottom relative with the top, the middle part of connection top and bottom, and the reaction chamber that is formed jointly by described top, middle part and bottom reaches the reactant draft tube that is arranged at described reactor middle part at least.
Like this, reacting gas feeds in the reaction chamber by reacting with the tested thing sample (sample) that is arranged in the reaction chamber, resultant of reaction stays in the reaction chamber, at this moment, its detection detects by the spectral detection instrument that is arranged at the reactor outside, can be referring to International Application PCT/CN2006/000945 number of applicant.
In specimen test of the present invention system, be provided with light supply apparatus, operation such as it can be used to heat, illumination or detection.Shown in Figure 29-33, in preferred embodiment of the present invention, it is arranged at reactor 1 outside, and certainly, meeting some requirements, it also can be applied to outside the pretreater 2.
Shown in Figure 29-31, it is for using an embodiment of light supply apparatus and reactor in the specimen test of the present invention system.With the preferable reactor embodiment of the present invention shown in Figure 180 is example, reactor 1 is provided with reaction chamber 153, offer first opening 60 on this reaction chamber 153, reaction chamber 153 is outside equipped with the secondary light source 72 that is used for producing first light source 71 of first light beam and is used for producing second light beam.At least can operate by the sample in 60 pairs of reaction chambers of first opening 153 for one in described first light source 71 and the secondary light source 72.At this moment, in described first light source 71 and the secondary light source 72 can operate by the sample in 60 pairs of reaction chambers of first opening 153 and just comprise three kinds of situations:
One, only first light beam is by described first opening;
Its two, only second light beam is by described first opening;
Its three, the first light beam and second light beam pass through described first opening simultaneously or not simultaneously.
In the present embodiment, shown in Fig. 3 and Figure 29-31, be provided with sample substrate 300 in the reaction chamber of reactor 1, appoint a bearing area 301 on the sample thief substrate 300, which is provided with sample (sample) 302.When situation about adopting shown in one and its two, light beam that light beam that first light source 71 produces or secondary light source 72 produce is only arranged by operations such as the sample on 60 pairs of bearing areas 301 of opening heat; When adopting its situation shown in three, the light beam that produces of first light source 71 and secondary light source 72 is respectively to different bearing area 303 as shown in figure 31, operations such as the sample on 304 heats, perhaps as Figure 29 or shown in Figure 30, the light beam that first light source 71 and secondary light source 72 produce is to operations such as the sample on the same bearing area 301 heat.
In addition, as Figure 29 and shown in Figure 30, the travel path of the light beam that first light source 71 and secondary light source 72 produces be independently or the path of two light beams can partially overlap.The light beam that first light source 71 and secondary light source 72 produce respectively can directly enter reaction chamber by opening the sample on the bearing area on the substrate is operated, perhaps in the travel path of light beam, be provided with and enter again in the reaction chamber after reflective mirror or convex lens come the path of light beam adjusted, need the eyeglass of unlike material at different light beams.
Another embodiment of light supply apparatus of the present invention shown in Figure 32-33 and reactor is an example with reactor shown in Figure 180 still, offers first opening 60 and second opening 61 on the bottom 153 of reactor 1.Reactor 1 is outside equipped with first light source 71 and secondary light source 72 can enter reaction chamber by first opening 60 and second opening 61 respectively.Like this, selectable sample on the bearing area is operated of first light beam and second light beam just has two kinds of situations:
One, shown in figure 32, second light beam that first light beam that first light source 71 produces and secondary light source 72 produce is respectively by operations such as the sample on different 60,61 pairs of different bearing areas 303,304 of opening heat.At this moment, first light beam and second light beam at every turn can be simultaneously or asynchronous sample on the bearing area of correspondence are operated, and perhaps operate for one, and another is not operated.
Its two, as shown in figure 33, second light beam that first light beam that first light source 71 produces and secondary light source 72 produce can be operated the sample on the same bearing area 301.Certainly, first light beam and second light beam can operate simultaneously or one operate, another is not operated.
Described first light beam or second light beam can be laser or infrared light etc., and it heats as heating source.Certainly, also can select diode light (Light Emitting Diode is called for short LED) to be used for throwing light on.
According to the difference of emitting material, laser can be divided into several types such as solid, gas, semiconductor, free electron.
Solid State Laser is to be produced by the material bar of meticulous screening, as ruby laser, sapphire laser etc.
Gas laser is that the gas atom with flash-over characteristic can be activated and launch and produce light, as carbon dioxide laser (CO
2Laser, wavelength 1036nm) etc.
Semiconductor laser is to be produced by the laser instrument that the two chip semiconductor materials that are connected constitute, this two chip semiconductor has passed through different processing in advance, contain different impurity, when a large amount of electric currents are flowed through this device, laser beam just occurs from the junction, as diode laser (Diode Laser also claims 808nm Laser).
In free electron laser, the free electron (promptly having broken away from atomic nucleus) from particular-accelerator or other energy generation equipment by a kind of undulator that is made of linear electromagnetic, is accelerated to light velocity speed, launches energy in the mode of synchronous acceleration ray.By changing the girth in magnetic field, just can adjust the density and the wavelength of this ray, so, be as short as microwave, grow to ultraviolet ray because it is that adjustable suitable wavelength coverage is wide.
According to different reaction requirements, can select dissimilar light beams, according to different light beams, in the present embodiment, it is different that the material of substrate requires.Certainly, when having adopted certain substrate material, also can select suitable light beam according to the difference of substrate material.Requirement along with development of technology and reaction, substrate can be selected other different materials, described light beam also can be selected light beams of different wavelengths, as long as selected light beam adapts with corresponding substrate, and can wounded substrate and can guarantee that the carrying out that reacts is just passable.
In one embodiment, described substrate material adopts silicon chip or quartz.When adopting silicon chip, can use the diode laser of wavelength 808 nanometers or the light beam that is used for throwing light on such as diode light; When adopting when quartzy, can use the carbon dioxide laser of wavelength 1036 nanometers or wavelength light beam, as diode laser or the light beam that is used for throwing light on such as the diode light etc. of wavelength 808 nanometers less than 1036 nanometers.
In addition, under reactor needs sealing state to a certain degree, can be provided with first translucent element and second translucent element in described first opening and second opening.Described translucent element is the material that the eyeglass of glass material or other can printing opacities.Being preferably described translucent element is glass material, and the glass material of first translucent element and second translucent element possibility is identical also may be inequality, in the present embodiment, be preferably and select first light beam and second light beam of different glass materials with corresponding different wave length.
Described glass material of a great variety, it includes but not limited to following several glass: (1) is with SiO
2Silicate glass for principal ingredient; (2) with B
2O
3, P
2O
5, Al
2O
3, GeO
2, TeO
2, V
2O
5Deng the oxide glass that is principal ingredient; (3) based on the nonoxide glass of chalcogenide compound, halogenide; (4) cool off metallic glass of forming etc. fast by some alloy.
In one embodiment, in first opening or second opening silicon dioxide (SiO is set
2) eyeglass or zinc selenide (ZnSe) eyeglass.When described light beam is carbon dioxide laser, corresponding employing zinc selenide (ZnSe) eyeglass; When described light beam is diode laser or diode light time, corresponding adopted silicon dioxide (SiO
2) eyeglass or zinc selenide (ZnSe) eyeglass.
Certainly, described reactor also can offer the 3rd opening, and it is used for by the 3rd light beam.Described first opening or second opening or the 3rd opening can be opened in top or the bottom or the middle part of reactor.Like this, may be identical or may be different in the position offered of described first opening, second opening and the 3rd opening.Same position herein is meant that three openings are arranged on top or one of middle part or bottom simultaneously.
When reacting, first light beam by first opening, second light beam by second opening and the 3rd light beam by the 3rd opening can be divided into following several situation to the operation of the sample on the bearing area:
One is operated the sample on the same bearing area simultaneously;
Two light beams in every batch of its two, three light beam are operated the sample on the same bearing area simultaneously, the another one light beam sample on another bearing area is carried out and previous bearing area simultaneously or asynchronous operation;
Its three, three light beams carry out while or all asynchronous operation to the sample on three different bearing areas respectively for every batch.
Described every batch of quantity that is meant according to light beam, finish once be operating as one batch of all light beams, during if any two light beams, for having finished one batch, this two light beams can simultaneously or not operated for every batch simultaneously when the operation finished two light beams.
In one embodiment, described first light beam or second light beam or the 3rd light beam can be diode laser or carbon dioxide laser or diode light, adopt diode laser such as first light beam, second light beam adopts carbon dioxide laser, and the 3rd light beam adopts diode light.
In addition, also can offer the 4th opening, the 5th opening or the like as required on reactor, it is used for by the 4th light beam, the 5th light beam etc.
Like this, requirement and light beam and open amount different according to reaction, can make up the operation of the sample on the bearing area on the substrate being carried out different situations to light beam by different openings, for example above-mentioned various combination situation when having two or three openings, by that analogy.
For the reflection that prevents light beam causes influence to slackening of incident beam etc., be preferably and scribble the antireflection tunic on the eyeglass, simultaneously, and also can painted black in the opening, perhaps processing comparatively coarse comes the absorption portion folded light beam in the opening.Certainly, when taking above-mentioned measure to reduce the influence of reflection to incident beam of light beam, also can avoid this kind influence by calculating adjustment to the angle of folded light beam and incident beam.In addition, can offer groove in the described opening, it is used for being provided with packoff, is preferably the O RunddichtringO.
Continuation is an example with reactor 1 shown in Figure 180, shown in Figure 34-36 for being arranged at a kind of hatch frame synoptic diagram on the reactor 1 of preferred embodiment of the present invention.For the opening shown in Figure 29-33, wherein the concrete structure in any opening can be according to the requirement of reaction, and the structure of any one opening in selection and Figure 34 or three openings shown in Figure 37 is identical or roughly the same.
Shown in Figure 34-36, outwards be recessed to form first opening 81 that runs through bottom 153 and second opening 82 and the 3rd opening 80 that is arranged at its both sides in its inside surface (not mark) on the bottom 153 of reactor 1.These first opening, 81, the second openings 82 and the 3rd opening 80 are included in first peristome 811,821,801 that the reactor inside surface outwards caves in and extends, the 3rd peristome 813,823,803 and connect first peristome, second peristome 812,822,802 of the 3rd peristome.Wherein, first peristome, 801, the second peristomes 802 of the 3rd opening 80 and the 3rd peristome 803 be perpendicular to reactor inside surface successively outwards depression extend.First peristome, 811,821, second peristome 812,822 of first opening 81 and second opening 82 and the 3rd peristome portion 813,823 all be tilt in the inside surface of reactor successively outwards depression extend.
First peristome of described opening can outwards be recessed to form from inside surface, or from the formation that caves inward of inside surface opposed outer surface, the inside surface or the outside surface that directly begin to form described first peristome herein can be defined as installed surface.Described translucent element can be fit in the corresponding opening in described installed surface place.
In the hatch frame shown in Figure 34 of the present invention-36, under the constant situation of bearing area and reactor relative position, when first opening 81, second opening 82 and the 3rd opening 80 be used to same bearing area operate the time, because the structure of reactor is less, so it is very compact that the structure between them need be provided with, especially first opening 81, first peristome 811 of second opening 82 and the 3rd opening 83,821,801 structure needs tightr, just might influence each other on making between each opening like this.
In addition, reactor needs sealing to a certain degree in course of reaction, especially when heating or observing response device are inner under the sealing that needs to a certain degree, first peristome 811,821,801 bottom is recessed to form groove (mark) respectively downwards and is used to accommodate packoff, as O type packing ring, and is equipped with on packoff and utilizes eyeglass that screw (not shown) fixes so that light beam passes through.First opening 81 shown in Figure 34-36 and first peristome 811,812nd of second opening 82 favour the inside surface of reactor, are obliquely installed in first peristome 811,812 so eyeglass and packoff also are inside surfaces with respect to reactor.The bed knife of fixing len and packoff is normally perpendicular to the inside surface of reactor, and like this, the pressure that puts on eyeglass and packoff just might be inhomogeneous, thereby might influence the carrying out of reaction.
Shown in Figure 37-38, it is the another kind of hatch frame synoptic diagram of the hatch frame of reactor 1 of the present invention.Outwards be recessed to form first opening, 91, the second openings 92 and the 3rd opening 90 that run through bottom 153 in its inside surface (not mark) on the bottom 153 of reactor 1.This first opening 91 and second opening 92 are arranged at the both sides of the 3rd opening 90 respectively.First peristome 911,921 that is provided with the outside depression of 153 inside surfaces that first opening, 91, the second openings 92 and the 3rd opening 90 are corresponding respectively in the bottom, 901, the three peristomes 913,923,903 and be communicated with second peristome 912,922,902 of first peristome and the 3rd peristome.Wherein, first peristome, 901, the second peristomes 902 of the 3rd opening 90 and the bearing of trend E of the 3rd peristome 903 overlap, and promptly the bearing of trend angle of first peristome, 901, the second peristomes 902 and the 3rd peristome 903 is a zero degree.
The bearing of trend A of first peristome 911 of first opening 91 is perpendicular to the inside surface of bottom 153, its bearing of trend E with the 3rd opening 90 is parallel, the bearing of trend B of its second peristome 912 and the 3rd peristome 913 favours the inside surface of bottom 153, the bearing of trend A of itself and first peristome 911 forms angle, as 30 degree.Equally, the bearing of trend C of first peristome 921 of second opening 92 is perpendicular to the inside surface of bottom 153, and its bearing of trend E with the 3rd opening 90 is parallel and form angle with the bearing of trend D of second peristome 922 and the 3rd peristome 923, as 45 degree.In addition, first peristome, 911,921,901 bottoms of first opening 91 or second opening 92 or the 3rd opening 90 all are d1 respectively apart from the distance of bottom 153 inside surfaces everywhere, d2, and d3, and d1, d2 also equates between the d3.According to the needs of reaction, be recessed to form flutedly downwards in first peristome, 911,921,901 bottom edge of first opening, 91, the second openings 92 and the 3rd opening 90, be respectively applied for and accommodate O RunddichtringO 33, and eyeglass (not shown) is set on O-ring seal 33.At this moment, because it is identical that the bottom of first peristome of opening is arrived the distance of reactor inside surface everywhere, so O-ring seal 33 and eyeglass can be parallel on the bottom that inside surface is arranged at first peristome, like this, the bed knife that puts on eyeglass and packoff is just more even, bad situation such as can well avoid leaking.
Referring to the structural representation of reactor shedding motion shown in Figure 38, its structure and shown in Figure 37 roughly the same, difference is that second opening 92 also is provided with the 4th peristome 924 that is communicated with second peristome 922 and the 3rd peristome 923 among Figure 38.
When testing, often need the sample on substrate 300 bearing areas be heated, referring to shown in Figure 39, it is for using the configuration diagram with LASER HEATING of the present invention system.The temperature control part branch loop of LASER HEATING comprises infrared thermometer 62, PID controller 63, laser controller 64 and laser instrument 65.Infrared thermometer 62 detects the temperature of bearing area and signal is changed; Signal is transferred to the input signal of PID controller 63 as the PID controller in the mode of 4-20 milliampere; Simultaneously, charge-coupled image sensor 66 (Charge CoupledDevice is called for short CCD) looks like to pass to computing machine 67 to the location drawing of detected bearing area so that determine hot spot, comes master control PID controller by computing machine 67 subsequently; At last, the PID controller is passed to the output laser power that laser controller 64 is controlled laser instrument 64 to output signal, generally is in 0% to 95%, comes the bearing area is heated.Power module 68 control laser instruments 65 switches, cooling system 69 comes cooling laser device 65.
In conjunction with Figure 35 and shown in Figure 37, first opening of offering on the bottom 153 of heating system by reactor 1 81,91 or second opening 82,92 or the 3rd opening 80,90 are selectable to be that sample on the bearing area heats to the test object point.In the preferred embodiment of the present invention, adopt laser to heat, the 3rd opening 80,90 places are carbon dioxide laser (CO
2Laser) heating, first opening, 81,91 places are diode laser (Diode Laser, also be 808nm Laser) heating, second opening, 82,92 places are provided with light emitting diode (Light Emitting Diode, be called for short LED) so that the response situation in the observing response device.The diode laser heating at first opening, 81,91 places is heated selectable unlatching with the carbon dioxide laser at the 3rd opening 80,90 places, and the light emitting diode at second opening, 82,92 places can in running order always or off working state.
Claims (21)
1. one kind is used to test the pilot system that is loaded into the sample on the substrate, it is characterized in that: described pilot system comprises enclosed cavity, pretreatment unit and test unit, described enclosed cavity has first area and second area, and described pretreatment unit carries out pre-service to described sample when described substrate is positioned at the first area; Described test unit after described sample carries out pre-service and described substrate sample is tested when being positioned at second area, this test unit includes the characteristic that proving installation is used for determining described sample.
2. pilot system as claimed in claim 1 is characterized in that: described pretreatment unit includes heating arrangement and is used to heat described sample.
3. pilot system as claimed in claim 2 is characterized in that: described pretreatment unit also includes the substrate that is used to carry described substrate and carries part, and it is movable that this substrate carries part.
4. pilot system as claimed in claim 3 is characterized in that: described pretreatment unit also includes the shielding portion of heat in the first area that is used to keep described heating arrangement generation.
5. pilot system as claimed in claim 1 is characterized in that: described proving installation comprises probe, and it is used to test described sample.
6. pilot system as claimed in claim 1 is characterized in that: described sample is a catalyzer, and described probe can be used for testing this catalyst sample.
7. pilot system as claimed in claim 1 is characterized in that: described system also includes mobile device, is used for described sample is moved to second area from the first area.
8. pilot system as claimed in claim 1 is characterized in that: described pilot system includes switchgear, is used to control being communicated with of first area and second area.
9. specimen test system, it is characterized in that: this specimen test system comprises pretreatment unit and test unit, described pretreatment unit includes the sample that can carry the substrate that is placed with sample and carries part and described sample is carried out pretreated pretreatment unit; Described test unit links to each other with described pretreatment unit, and it can accommodate the substrate that is placed with sample that comes from described pretreatment unit, and this test unit includes proving installation, is used for determining the characteristic of described sample.
10. specimen test as claimed in claim 9 system is characterized in that: described pretreatment unit includes can be imported pretreatment gas and enter the passage of described pretreatment unit and the heating arrangement that sample is heated; Described proving installation comprises probe.
11. one kind is used to test the test method that is positioned over the sample on the substrate, it comprises:
In a pretreatment unit, described sample is carried out pre-service;
By a passage that is communicated with described pretreatment unit the substrate that is placed with through pretreated sample is moved on to a test unit from described pretreatment unit, make described sample after described pretreatment unit pre-service and before test, not be exposed in the air;
The described pretreated sample of test in described test unit is to determine the characteristic of sample.
12. reactor that is used for specimen test, it includes the top, can carry the bottom of the substrate that is placed with sample, the middle part between top and bottom, probe and and the plurality of conduits that links to each other of probe, described top, middle part and bottom are formed with reaction chamber jointly, it is characterized in that: described reactor also is provided with probe, described probe is contained in the reaction chamber, and be installed at least middle part and bottom the two one of on.
13. reactor as claimed in claim 12 is characterized in that: described reactor includes the installation portion that is arranged at described reactor middle part, and described probe is installed on this installation portion.
14. reactor as claimed in claim 13 is characterized in that: the two ends of described installation portion are installed on the described middle part, and the connecting portion that connects described installation portion two ends hangs in the described reaction chamber, and described probe is installed on the described connecting portion.
15. reactor as claimed in claim 13 is characterized in that: described bottom is provided with can carry the sample that is placed with sample and carry part, and described probe can carry the part motion with respect to described sample.
16. reactor as claimed in claim 12 is characterized in that: described sample is a catalyzer, and described probe can be used for testing this catalyst sample.
17. reactor as claimed in claim 12 is characterized in that: described pipeline comprises two in input channel, output channel and the sampling conduit at least, and it all runs through the middle part of described reactor.
18. a reactor that is used for specimen test, it comprises the reaction chamber and first light source, and described reaction chamber has first opening, and described sample is tested in described reaction chamber, and described first light source is positioned at outside the described reaction chamber and can produces first light beam; It is characterized in that: described reactor comprises also and is arranged at the secondary light source that described reaction chamber is used to produce second light beam outward that one of described at least first light source and secondary light source can be opened in the described reaction chamber by described first and operate.
19. reactor as claimed in claim 18 is characterized in that: described reaction chamber also has second opening, and described first light source and secondary light source are opened in the described reaction chamber by first opening and second respectively and operate.
20. reactor as claimed in claim 19 is characterized in that: described reaction chamber has the 3rd opening and is positioned at the 3rd light source that described reaction chamber is used to produce the 3rd light beam outward, and described the 3rd light source can enter in the reaction chamber by the 3rd opening; Described first, second and third light beam is respectively diode laser, carbon dioxide laser and LED light.
21. reactor as claimed in claim 18 is characterized in that: be separately installed with SiO in described first and second openings
2Glass mirror and ZnSe glass mirror.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101627903A CN101173953A (en) | 2006-09-30 | 2007-09-28 | System and method for sampling tests |
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610139043.3 | 2006-09-30 | ||
| CN200610139043 | 2006-09-30 | ||
| CN200610130890.3 | 2006-12-29 | ||
| CN200610173356.0 | 2006-12-29 | ||
| CNA2007101627903A CN101173953A (en) | 2006-09-30 | 2007-09-28 | System and method for sampling tests |
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| Publication Number | Publication Date |
|---|---|
| CN101173953A true CN101173953A (en) | 2008-05-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101627903A Pending CN101173953A (en) | 2006-09-30 | 2007-09-28 | System and method for sampling tests |
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| Country | Link |
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| CN (1) | CN101173953A (en) |
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| CN102418691A (en) * | 2011-07-12 | 2012-04-18 | 上海华力微电子有限公司 | Novel method for fully automatically detecting pump failure |
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| CN106596244A (en) * | 2016-12-14 | 2017-04-26 | 宁海德宝立新材料有限公司 | Temperature control sample stage |
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| CN109580717A (en) * | 2018-11-17 | 2019-04-05 | 金华职业技术学院 | The electric measurement method of sample after a kind of vacuum chemical reaction |
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| CN102418691A (en) * | 2011-07-12 | 2012-04-18 | 上海华力微电子有限公司 | Novel method for fully automatically detecting pump failure |
| CN102418691B (en) * | 2011-07-12 | 2014-12-10 | 上海华力微电子有限公司 | Novel method for fully automatically detecting pump failure |
| CN112362973A (en) * | 2014-06-06 | 2021-02-12 | 滤波器感知技术有限公司 | Radio frequency state variable measurement system and method |
| CN106483219A (en) * | 2016-10-11 | 2017-03-08 | 深圳市华星光电技术有限公司 | Photoresistance atomizing treatment equipment and photoresistance atomization process system |
| CN106483219B (en) * | 2016-10-11 | 2019-09-17 | 深圳市华星光电技术有限公司 | Photoresist atomizing treatment equipment and photoresist atomization process system |
| CN106596244A (en) * | 2016-12-14 | 2017-04-26 | 宁海德宝立新材料有限公司 | Temperature control sample stage |
| CN109569432A (en) * | 2018-11-17 | 2019-04-05 | 金华职业技术学院 | Chemical reaction method in a kind of vacuum |
| CN109580717A (en) * | 2018-11-17 | 2019-04-05 | 金华职业技术学院 | The electric measurement method of sample after a kind of vacuum chemical reaction |
| CN109580717B (en) * | 2018-11-17 | 2023-09-12 | 金华职业技术学院 | Electrical measurement method for sample after vacuum chemical reaction |
| CN109569432B (en) * | 2018-11-17 | 2023-10-27 | 金华职业技术学院 | Chemical reaction method in vacuum |
| CN109540610A (en) * | 2018-12-12 | 2019-03-29 | 深圳市福瑞康科技有限公司 | A kind of sample collecting apparatus |
| CN109540610B (en) * | 2018-12-12 | 2024-01-30 | 深圳市福瑞康科技有限公司 | Sample collection device |
| CN113488222A (en) * | 2021-06-28 | 2021-10-08 | 散裂中子源科学中心 | Neutron scattering electrostatic suspension device |
| CN113488222B (en) * | 2021-06-28 | 2024-05-24 | 散裂中子源科学中心 | Neutron scattering electrostatic suspension ware |
| CN113447341A (en) * | 2021-07-19 | 2021-09-28 | 安图实验仪器(郑州)有限公司 | Sample plate bearing device |
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Application publication date: 20080507 |