CN102157410B - Device and method for substrate analysis - Google Patents
Device and method for substrate analysis Download PDFInfo
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- CN102157410B CN102157410B CN201010602119.8A CN201010602119A CN102157410B CN 102157410 B CN102157410 B CN 102157410B CN 201010602119 A CN201010602119 A CN 201010602119A CN 102157410 B CN102157410 B CN 102157410B
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Abstract
The invention discloses a device and a method for substrate analysis. The substrate analysis device is a small and simple device capable of carrying out an etching process and a recovery process and enables analysis of films formed on a substrate regardless of the type of the films and local analysis of the substrate. The substrate analysis device comprises a nozzle body for sending or sucking out analysis liquid and a double-pipe nozzle formed by external pipes arranged on the periphery of the nozzle body. The recovery means is the nozzle body of the double-pipe nozzle, and the etching means is the etching gas supplied to a place between the nozzle body and the external pipes. The substrate analysis device also comprises a gas charging means which is a gas charging path arranged between the nozzle body and the external pipes which is arranged in an enclosing manner for sweeping analysis liquid and provided with extraneous gas inlet hole at the front end. According to the invention, the etching process and the recovery process can be carried out on a same device which also enables simple analysis or local analysis directed at a special part of a substrate.
Description
Technical field
The present invention relates to a kind of substrate analytical equipment being contained in the material for testing such as the trace meter of substrate in order to analysis package.Further, a kind of analytical method using this substrate analytical equipment is also related to.
Background technology
With regard to the analytical equipment being contained in the material for testing such as metal, organic substance of the substrates such as semiconductor wafer (wafer) with regard to analysis package, generally use: be formed in gas-phase decomposition device and the substrate analysis nozzles in order to reclaim material for testing remaining on the substrate after etching such as the silicon oxide layer of substrate or nitride film in order to etching.With regard to the analysis gimmick using these devices, first, substrate is positioned in VPD (VaporPhase Deposition; Vapour deposition) chamber (chamber) etc., and import the etching gass such as hydrogen fluoride, with the formation film of etch substrate.Then, by substrate analysis nozzle, the analytic liquid of trace is sent to through overetched substrate, carry out scraping on substrate drawing (sweeping) with sent analytic liquid.Because the material for testing on substrate is displaced in analytic liquid, scrape if therefore pass through with nozzle suction the analytic liquid drawn, material for testing can be reclaimed with the analytic liquid of trace, and the good analysis of accuracy can be carried out.
So, in substrate is analyzed, following two stage step is needed: by the step of gas-phase decomposition device etch substrate and the step by nozzle recovery material for testing.When this is owing to being formed with natural oxide film etc. on semiconductor wafer substrate surface, its surface becomes hydrophily, and when sending analytic liquid, analytic liquid is loose leaks, and cause reclaim difficulty therefore.Therefore, in recycling step, because substrate surface is necessary for hydrophobicity, therefore when hydrophilic oxide-film or nitride film etc. are formed on substrate, etching steps such as removing these oxide-films in advance must be had.
So, in the past when analyzing substrate, point other device of gas-phase decomposition device and substrate analysis nozzle was used to carry out the two stage step of etching step and recycling step.Particularly, gas-phase decomposition device is than relatively large device, during for measuring the analysis etc. of the substrate in semiconductor fabrication lines simply, also needing and the substrate for measuring is transferred to steps such as VPD chamber etc. and has inconvenience.Moreover, when substrate itself is also transferred between the device of gas-phase decomposition device and substrate analysis nozzle, there is the danger producing and pollute.
Therefore, the present inventor etc. provide a kind of and fully automatically carry out the etching step implemented by gas-phase decomposition device and the full-automatic gas phase decomposition device of recycling step implemented by substrate analysis nozzle by same device.According to this device, substrate contaminated risk when carrying out transferring between device can be reduced.
Moreover, such as, when being learnt on substrate containing positions such as metals by surface photovoltage electric power (Surface Photo Voltage:SPV) method, have and only this privileged site is analyzed partly, and for obtaining the isocyatic situation of metal.But, during as point other device analysis substrate in the past with gas-phase decomposition device and substrate analysis nozzle, have and cannot correctly analyze the tendencies such as the metal concentration of specific Part portions.This is due in the etching undertaken by gas-phase decomposition device or after etching, and the material for testing being included in the privileged site of substrate moves to the event in other positions.Under this background, propose there is a kind of lining processor (patent documentation 1) carrying out the etching of substrate partly.
Moreover, in the recycling step that above substrate is analyzed, there will be a known a kind of in order to also can short time and scrape the substrate drawing maximization efficiently, and increase nozzle diameter, and make the method that the contact area of analytic liquid and substrate surface becomes large.But, make nozzle diameter become large time, have scrape draw time analytic liquid easily from the tendency that nozzle comes off, and have analytic liquid remain in scrape the substrate after drawing problem produce.Viewpoint thus, the present inventor etc. in patent documentation 2, propose a kind of have outer rim forward the end face given prominence to of extreme direction and in described end face the nozzle of eccentric opening near outer rim.Moreover, in patent documentation 3, disclose to have and a kind ofly to have the nozzle of the mechanism of being aspirated in blast tube or reduce pressure.
Patent documentation 1: Japanese Unexamined Patent Publication 2005-311140 publication
Patent documentation 2: Japanese Unexamined Patent Publication 2008-132401 publication
Patent documentation 3: Japanese Unexamined Patent Publication 5-256749 publication
Described full-automatic gas phase decomposition device in the same manner as the gas-phase decomposition device of prior art, for than relatively large device.Moreover, though patent documentation 1 carries out the etching of substrate partly, recycling step must be carried out in addition afterwards, therefore have material for testing after the etching and move to other positions on substrate, and the situation of Correct Analysis cannot be carried out.
Moreover, even if in recycling step, in the nozzle that patent documentation 2 or patent documentation 3 are recorded, particularly when analysis has the substrate of the film such as polysilicon or tungsten silicide, or the so-called main body (bulk) analyzing the base materials such as silicon wafer itself is when analyzing, have scrape draw in produce the tendency come off of analytic liquid.
Summary of the invention
(invention institute for solution problem)
Therefore, the invention provides and a kind ofly carry out the small-sized of etching step and recycling step two step by same device and easy analytical equipment, no matter why the kind being formed in the film of substrate all can be analyzed, and is also useful in the analytical equipment of the partial analysis on substrate.
(means of dealing with problems)
Substrate analytical equipment of the present invention in order to solve described problem possesses: etching means, is comprised the substrate of material for testing by the etching of gas-phase decomposition method; And recovering means, from spray nozzle front end, analytic liquid is sent to substrate, after scraping draw substrate surface with sent analytic liquid, aspirate analytic liquid by spray nozzle front end and reclaim material for testing; It is characterized in that: possess the dual pipe nozzle be made up of the nozzle body sent by analytic liquid and aspirate and the outer tube that is configured in nozzle body periphery; Recovering means is the nozzle body of dual pipe nozzle; Etching means are the etching gas be supplied between nozzle body and outer tube.
Fig. 1 is that display uses substrate analytical equipment of the present invention to carry out the schematic diagram of substrate analysis.In FIG, with regard to its example, be illustrated for the situation that the substrate being formed with oxide-film Ox on substrate W is analyzed.Analytical equipment of the present invention as shown in Figure 1, possesses the nozzle of the dual pipe structure being configured with outer tube 20 in the periphery of nozzle body 10, as shown in the arrow of the upper figure of Fig. 1, etching means be supplied to towards spray nozzle front end direction between nozzle body 10 and outer tube 20 15 etching gas.Whereby, as shown in figure below of Fig. 1, the oxide-film Ox of the outer peripheral portion R sending the nozzle body of analytic liquid D is etched removal, and become the state that substrate W itself exposes.Therefore, even if when such as forming the hydrophilic film such as aerobic film or nitride film in substrate, the periphery sending the part of analytic liquid becomes the state that hydrophobic substrate exposes, and therefore analytic liquid can not wet loose, can suppress the reduction of the rate of recovery.
According to substrate analytical equipment of the present invention, as described in mode can carry out the etching of formation film and the recovery of material for testing of substrate with single device, therefore the pollution risk of substrate can significantly lower, and is also applicable to the analysis of locality.Moreover, drawing substrate surface by scraping with nozzle, the optional position on substrate, carrying out serially etching and reclaiming.So, as long as owing to making small-sized nozzle relative with substrate, can carry out etching and reclaiming, therefore compared with the situation such as large-scale gas-phase decomposition device using prior art, be more suitable for easy analysis.
As long as the etching means of substrate analytical equipment of the present invention can provide be formed at the etching gass such as the oxide-film of substrate in order to etching.Specifically, also can be bubble (bubbling) device possessing the steam generation making to belong to etching gas by mixed acid solutions such as fluoric acids, also can be the sprayer (nebulizer) possessing and mixed acid solution is atomized.Sprayer by etching gas stable supplying high for concentration, therefore can have effect at the point that can shorten etching period.
The size of nozzle body can be and the size of substrate analysis nozzle same degree that uses in recycling step in the past, according to the size etc. of the substrate for analyzing, can select arbitrary size.Relative to the size of the nozzle outer tube of this nozzle body, be preferably diameter 1.5 doubly to 2.5 times, be more preferably about 2 times.If within the scope of this, then the etching having to etch means execution will be carried out well, and positively can remove the tendency of the formation film of the outer peripheral portion of nozzle body.On the other hand, if be when not reaching 1.5 times relative to the diameter of the size of the nozzle outer tube of nozzle body, the etching then forming film when scraping on seeding sheet has insufficient situation, and at the diameter of the size of the nozzle outer tube relative to nozzle body for during more than 2.5 times, have etching and reach to unwanted part tendency inefficent local addresses analysis.
And, according to the nozzle that dual pipe of the present invention constructs, then scrape with the analytic liquid sent from nozzle body draw substrate surface time, also can at short notice efficiently to maximize substrate analyze.By to configure outer tube around the mode of carrying out scraping the analytic liquid drawn, the bore around the pipe of analytic liquid can be made to increase, and the amount of retainable analytic liquid can be increased, the contact area of analytic liquid and substrate surface can be made to increase, therefore also can shorten scraping of substrate surface entirety and draw the required time.Such as, relatively with the dual pipe of the present invention nozzle constructed and the nozzle constructed with the substance pipe of prior art the amount of retainable analytic liquid time, though different according to the bore of nozzle, but in the nozzle of dual pipe structure, be about 500 μ L to 1000 μ about L, in contrast, be about 100 μ L to 150 μ about L in the nozzle of substance pipe structure.
So, by adopting dual pipe nozzle, that can expect to shorten substrate surface scrapes the effect of drawing the time, if but when only making the bore of outer tube increase, sometimes have the situation of scraping and drawing middle analytic liquid and coming off from nozzle, and have and scraping the situation of the substrate retention analysis liquid after drawing.Therefore, in substrate analytical equipment of the present invention, except etching means, preferably possess the exhaust means as exhaust pathway between nozzle body and outer tube, and possess outer conductance hand-hole in outer tube front end.When possessing exhaust means and outer conductance hand-hole, scrape the analytic liquid drawing substrate surface and be not easy to come off from nozzle.In detail as aftermentioned, though analyze there is the substrate of the film such as polysilicon or tungsten silicide time or analyze in the so-called analysis of the main of the base materials such as silicon wafer itself, effective especially at the point come off that analytic liquid is less likely to occur.
The reason that analytic liquid comes off can be prevented by having the formation of exhaust means and outer conductance hand-hole, think owing to will be maintained the state easily keeping analytic liquid between nozzle body and outer tube as reduced pressure atmosphere by exhaust, and there is outer conductance hand-hole and prevent outer gas from flowing into event brokenly whereby.At this, with regard to " outer gas flows into the situation in exhaust pathway brokenly ", consider and be difficult to maintain the level of substrate, and when analyzing the situation of the state that substrate can tilt, or the situation of the coarse substrate of analytical table surface state.Such as, analyze the situations such as large-scale Semiconductor substrate, or become the coarse situation of substrate surface state by etching during pre-treatment.In said case, be difficult to the distance of carrying out scraping nozzle and the substrate drawn be maintained the event of certain tendency owing to having.
Specifically, usually as shown in (a) in Fig. 2, scrape and draw the middle distance by nozzle and substrate and remain roughly homogeneous, and keep analytic liquid under the state be filled between outer tube front end and substrate at analytic liquid.But, as previously mentioned, becoming the situation etc. of state of substrate tilting, in a part circumferentially for outer tube, easily produce the part elongated with the distance of substrate.Therefore, think the gap that can produce underfill analytic liquid between outer tube front end and substrate, because gas outer between this gap can the inner event of flow nozzle brokenly.To this, according to the present invention, even if when producing the gap of underfill analytic liquid because of the inclination etc. of these substrates between outer tube front end and substrate, the inflow of the outer gas along outer conductance hand-hole also can be promoted, is therefore less likely to occur coming off of analytic liquid.In addition, outer conductance hand-hole of the present invention is preferably multiple circumferentially arranging of outer tube front end, and shape can be made for nick shaped.
When using substrate analytical equipment of the present invention described above to analyze substrate, simultaneously can scrape with the nozzle of dual pipe structure and draw substrate surface, one side carries out etching step and recycling step.
Draw can carry out with the method same with the recycling step of prior art with scraping of carrying out of dual pipe nozzle.Such as, can adopt and by one side, substrate be rotated, simultaneously make nozzle from medial movement to outside, and scrape and draw into gyrate method etc.Moreover as previously mentioned, nozzle of the present invention is also useful in the situation analyzing substrate partly, in this case, as long as only to make the substrate surface of the privileged site for analyzing carry out nozzle operation by the mode of dual pipe nozzle.
In addition, etching step and recycling step can carry out secondary and scrape and draw and each step is carried out respectively, also can once scrape to draw makes etching step and recycling step carry out simultaneously, and this carries out secondary and scrapes and to draw and the mode making each step carry out respectively is drawn after whole of substrate surface (or local) one side carries out etching step for first one side is scraped with dual pipe nozzle, once again recycling step is carried out to whole of substrate surface (or local).During for only analyzing a part of locality on substrate, preferably make etching step and recycling step carry out simultaneously.This is owing to can not produce because etching the diffusion causing material for testing, and can carry out well reclaiming event.
The formation film of substrate is oxide-film or nitride film geometric ratio when being easier to the film decomposed, shorter owing to etching the required time, therefore by with scraping to draw and make etching step and recycling step carry out once simultaneously, can shorten analysis time significantly.On the other hand, the formation film of substrate is that polysilicon, tungsten silicide, titanium, titanium nitride etc. are when comparing the film being not easy to decompose, recycling step can carry out in the shorter time, but time needed for etching is long, thus has the tendency being not easy overall analysis time to shorten.Therefore, when analysis is formed with the substrate of the films such as polysilicon, is preferably in the mode of carrying out recycling step after an etching step, carries out each step respectively.So, when carrying out recycling step dividually with etching step, when carrying out recycling step, during scraping with analytic liquid and drawing substrate surface, being exhausted between nozzle body and outer tube by exhaust means, coming off of analytic liquid can be prevented.
Therefore, particularly, the substrate analytical equipment possessing exhaust means and outer conductance hand-hole is applicable to possess polysilicon, tungsten silicide, titanium, the Semiconductor substrate of any one film of titanium nitride and the analysis of the wafer substrate of Semiconductor substrate.Moreover, be also applicable to the analysis of wafer at the irregular substrate of surperficial tool as formed circuit pattern.This is due to when substrate surface is the situation of non-hydrophobic, also can carry out scraping drawing when not producing the coming off of analytic liquid.That is, being not easy to be decomposed because the films such as polysilicon or wafer substrate compare, therefore when carrying out the etching of decomposing these films, nitration mixture or strong acid etc. that acid concentration is high must being used.Therefore, this is due to after film such as decomposition polysilicon etc., and because of etchings such as strong acid, substrate surface can be roughening and become non-hydrophobic, and have cause the tendency of the drop state being difficult to maintenance analytic liquid because of surface tension therefore.
As representative of the present invention, in the substrate analytical equipment possessing exhaust means and outer conductance hand-hole, when the situation that substrate surface is roughening, also coming off of analytic liquid can be prevented, therefore with analytic liquid, be not only the mixed solution of fluoric acid and hydrogen peroxide, also as the mixed solution etc. of fluoric acid and nitric acid, can use compared to the higher acid of art methods acid concentration or strong acid.Therefore, with regard to material for testing, even if when including copper etc. and being not easy to be dissolved in the situation of the metal of analytic liquid, also the rate of recovery can be promoted.
In the analysis comprising etching step described above and recycling step, drawing scraping of substrate surface draw with regard to speed with regard to scraping with nozzle, particularly when considering the kind of formation film of carrying out the substrate etched with etching step, suitably selecting the speed be applicable to.Specifically, as mentioned above, when the formation film of substrate is the situations such as polysilicon, long owing to etching the required time, therefore etch and scrape and draw speed and can be set as such as 5mm/sec.On the other hand, oxide-film etc. are shorter owing to etching the required time, therefore can be set as such as 30mm/sec.
With regard to the etching gas used in etching step, can use in the past used etching gas, be particularly preferred with hydrogen fluoride gas.Moreover, also the gases such as ozone and fluoric acid together can be imported and analysis personnel silicon (bulk silicon) (substrate itself).
In analytical method of the present invention described above, though the kind indefinite of analyzable substrate, be specially adapted to the analysis of the Semiconductor substrate such as wafer.
(invention effect)
As described above, substrate analytical equipment of the present invention is the small-sized analytic device carrying out etching step and recycling step two step by same device.According to the present invention, etching step and recycling step can be carried out simultaneously, and when carrying out the situation of two steps respectively, also can carry out scraping in recycling step in the short time and drawing, and being less likely to occur to scrape coming off of the analytic liquid in drawing.Moreover device of the present invention is also applicable to the local addresses analysis of easy analysis or the privileged site for substrate.
Accompanying drawing explanation
Fig. 1 is the schematic diagram using the substrate of substrate analytical equipment of the present invention to analyze.
In Fig. 2, (a) is for possessing the drawing in side sectional elevation of the spray nozzle front end of the embodiment 3 that the sectional arrangement drawing of the substrate analytical equipment of exhaust means and outer conductance hand-hole and (b) are this device.
Fig. 3 is the sectional arrangement drawing of the substrate analytical equipment in embodiment 1.
Wherein, description of reference numerals is as follows:
10 nozzle bodies
20 outer tubes
21 outer conductance hand-holes
30 syringe pumps
T nozzle
W wafer
Ox oxide-film
D analytic liquid
Embodiment
Below, embodiments of the present invention are described.
[the first execution mode]
Embodiment 1:
With regard to embodiment 1, the nozzle of Fig. 3 is used to carry out the analysis of substrate.The nozzle of Fig. 3 is made up of the dual pipe formed with nozzle body 10 and outer tube 20.Nozzle body 10 is connected with syringe pump (syringepump) 30, and can send analytic liquid D.Moreover nozzle is connected with the generation device (not shown) of hydrogen fluoride (HF) steam between nozzle body 10 and outer tube 20, and can be used as etching means and supply etching gas towards the direction of arrow.In addition, with regard to the generation device of HF steam, can adopt and nitrogen be bubbled in HF solution and the device etc. such as device or sprayer producing HF steam.
In the present embodiment, use nozzle body is 10mm, and outer tube is 20mm, and the diameter of outer tube is the nozzle of the diameter 2 times of nozzle body.In addition, because the leading section of nozzle body attenuates, therefore with regard to the diameter of described nozzle body, with the size of the identical part of the diameter beyond leading section for benchmark.
Then, the specific analytical method using described nozzle is described.With regard to the substrate of analytic target, naked silicon wafer (the bare silicon wafer) base material of (inch) when using 8.For this base material, become 5 × 10 to make each metal concentration of the material for testing such as Na, Mg, Al
10atomicity/square centimeter (atoms/cm
2) mode of concentration of left and right, to drip making standard liquid on wafer and make it dry and the mandatory wafer polluted that becomes is used for analyzing.In addition, be directed to this wafer substrate, when directly sending analytic liquid when not carrying out etching, analytic liquid is wet to be dispersed on substrate.Therefore, think to be formed with natural oxide film at this wafer substrate.
For this Semiconductor substrate, use the dual pipe nozzle of Fig. 3, draw with scraping once and carry out etching step and recycling step simultaneously and analyze.First, dual pipe nozzle is immersed in comprises 3%HF, 4%H
2o
2analytic liquid, and to aspirate with syringe pump 30, the analytic liquid of 500 μ L be filled in the liquid bath of nozzle body 10.Then, nozzle is moved in wafer substrates, with 1L/min by nitrogen gas supply to sprayer, and use and supply the HF solution of HF concentration 49wt% and the steam supply that produces between nozzle body and outer tube with 200 μ L/min.While carrying out this steam supply, the analytic liquid of about 150 μ L is sent on substrate, utilize nozzle to draw substrate is scraped with the speed of 30mm/min, to carry out the recovery of material for testing.
Embodiment 2:
In the present embodiment, for substrate similarly to Example 1, after using the dual pipe nozzle of Fig. 3 to carry out etching step, carry out recycling step in addition.First, with 1L/min by nitrogen gas supply to sprayer, and use and supply the HF solution of HF concentration 49wt% and the steam supply that produces between nozzle body and outer tube with 200 μ L/min.Now, the speed that scraping on substrate regards it as 30mm/min is carried out.Then, dual pipe nozzle is immersed in comprises 3%HF, 4%H
2o
2analytic liquid, and to aspirate with syringe pump 30, the analytic liquid of 500 μ L be filled in the liquid bath of nozzle body 10.This analytic liquid of about 150 μ L is sent on substrate, utilizes nozzle to draw substrate is scraped with the speed of 30mm/min, to carry out the recovery of material for testing.
Learnt by above result, in the analysis of embodiment 1,2, analytic liquid can not wet and be dispersed on substrate, can reclaim well.Moreover the time needed for analysis is also the shorter time.Specifically, in embodiment 1, can carry out etching with 5 minutes simultaneously and reclaim.Moreover the analysis time of embodiment 2 is etching 5 minutes, reclaims 5 minutes, adds up to 10 minutes.
On the other hand, relative to this, as shown in the analytical method of prior art, when the recovery carrying out possessing etching that the gas-phase decomposition devices such as VPD chamber implement and implement with nozzle, with regard to analysis time, etching need about 3 minutes, the recovery of material for testing needs about 5 minutes, and also must have and make substrate be transferred to step between device.Therefore, in the analytical method of prior art, if when also considering the transfer time of substrate, then need analysis time more more than embodiment 1,2.
Then, for the analytic liquid comprising the material for testing reclaimed by embodiment 1, inductive couple plasma (plasma) quality analysis apparatus (ICP-MS) is utilized to measure concentration in the wafer of the element shown in following table 1.Further, the analysis of recycling step described in total 3 times and concentration of element is repeatedly carried out for same substrate, to obtain the rate of recovery.The rate of recovery for calculated the 1st time by the ratio (rate of recovery) of the aggregate value relative to the concentration of element gone out with the analyzing and testing of 3 times analysis detected by concentration of element.Analytical method generally preferably can go out whole objects with the analyzing and testing of 1 time, and therefore the described rate of recovery is higher, more manifests the good result that can go out many elements with the analyzing and testing of the 1st time.
Table 1
Learnt by table 1, according to embodiment 1, for the material for testing of the trace contained by Semiconductor substrate, the high analysis of the rate of recovery can be carried out.
[the second execution mode]
In the present embodiment, for the Semiconductor substrate being formed with polysilicon film, except possessing etching means similarly to Example 1, the nozzle possessing exhaust means and outer conductance hand-hole is also utilized to analyze.
Embodiment 3:
The nozzle of Fig. 2 is utilized to carry out the analysis of substrate.The sectional arrangement drawing that in Fig. 2, (a) is nozzle, the drawing in side sectional elevation that in Fig. 2, (b) is spray nozzle front end.The nozzle of Fig. 2 is made up of the dual pipe formed with nozzle body 10 and outer tube 20.Nozzle body 10 is connected with syringe pump 30, and can send analytic liquid D.Moreover, similarly to Example 1, between nozzle body 10 and outer tube 20, be connected with the HF generation device (not shown) as the means of etching, and be connected with exhaust pump (not shown) using as being vented to exhaust means between nozzle body 10 and outer tube 20 towards the direction of arrow.In addition, HF generation device and exhaust pump switch by valve.Outer tube 20 possesses outer conductance hand-hole 21 at leading section, in the present embodiment, as shown in (b) in Fig. 2, is circumferentially provided with at outer tube the outer conductance hand-hole 21 be made up of the breach at 4 positions.In the present embodiment, use nozzle body is 10mm, and outer tube is 20mm, and the diameter of outer tube is the nozzle of the diameter 2 times of nozzle body.In addition, because the leading section of nozzle body shown in (a) in such as Fig. 2 can attenuate, therefore with regard to the diameter of described nozzle body, with the size of the identical part of the diameter beyond leading section for benchmark.
Then, for using the specific analytical method of described nozzle to be described.With regard to the substrate of analytic target, be used in by 8 time the wafer substrate that forms of silicon be formed
(100nm) silicon oxide layer and being formed on this oxide-film
(100nm) Semiconductor substrate of polysilicon film.
For this Semiconductor substrate, first after carrying out etching step, carry out recycling step.First, with 1L/min, nitrogen is supplied to sprayer, and the steam that will supply the HF solution of HF concentration 49wt% with 200 μ L/min and produce and the gas (carrying out gas discharge with the gas discharger exporting 200kW to the gas be made up of oxygen 20% and nitrogen 80% produced) containing ozone are supplied between nozzle body and outer tube.Now, the speed that scraping on substrate regards it as 5mm/min is carried out.
Then, the nozzle of Fig. 2 is immersed in comprises 1%HF, 4%H
2o
2analytic liquid, carry out aspirating with syringe pump 30 and the analytic liquid of 1000 μ L be filled in the liquid bath of nozzle body 10.Afterwards, make the analytic liquid D of 600 μ L send on Semiconductor substrate W, keep in the mode in the front end of outer tube 20 around analytic liquid D, and to make analytic liquid D by the mode manipulating nozzles of the surface integral of substrate W.Nozzle operation can make substrate W rotation one side that nozzle 10 is carried out the surface integral of substrate W from medial movement to methods such as outsides with such as one side.
In described nozzle operation, carried out the exhaust of the direction of arrow towards (a) in Fig. 2 with exhaust velocity 0.3L/min to 1.0L/min by exhaust pump.In the present embodiment, in above nozzle operation, can retention analysis liquid and nozzle operation is carried out to the surface integral of substrate W.
Just to above embodiment 3 comparatively speaking, the prior art nozzle be only made up of the nozzle body 10 (substance pipe structure) without outer tube 20 is used to carry out the analysis of substrate.Just carry out with regard to the substrate analyzed, use Semiconductor substrate similarly to Example 3, etching step is arrange Semiconductor substrate in VPD chamber after, and the gas containing ozone that sprayer makes the steam of the HF solution atomization of HF concentration 49wt% and carries out gas discharge with the gas discharger exporting 200kW to the gas be made up of oxygen 20% and nitrogen 80% and produce is given in confession.In addition, HF solution 4 and the quantity delivered containing the gas of aerobic are adjusted to and make the steam of hydrogen fluoride (HF) become 0.5L/min to 1.5L/min, make the gas containing ozone become 0.5L/min to 2.0L/min.Afterwards, use the nozzle that described substance pipe constructs, and use 1%HF, 4%H
2o
2material for testing is reclaimed as analytic liquid.Now, send to the analytic liquid D on Semiconductor substrate W and be set to 100 μ L to 150 μ L.
Moreover, with regard to another comparative example relative to embodiment 3, use the nozzle of the outer conductance hand-hole 21 do not had in Fig. 2 in (a) to analyze.In this comparative example, except use not there is outer conductance hand-hole nozzle beyond analysis condition be set as similarly to Example 3 method.
Described result, as described in Example 3, the situation analyzed is carried out with the double pipe nozzle possessing outer conductance hand-hole, relative to scrape draw period do not have analytic liquid to come off from nozzle completely situation, when using the nozzle of substance pipe or not there is the nozzle of outer conductance hand-hole, have analytic liquid can scrape draw in come off from nozzle, and easily remain in the tendency on substrate.Why can cause the reason of this tendency, may be when outer gas flows into nozzle interior, is difficult to keep the event of analytic liquid by nozzle.
Then, for the analytic liquid comprising material for testing reclaimed by embodiment 3, inductive couple plasma quality analysis apparatus (ICP-MS) is utilized to measure concentration in the wafer of the element shown in following table 2.Further, the analysis of total 3 described recycling steps and concentration of element is repeatedly carried out for same substrate, to obtain the rate of recovery.The rate of recovery is for by relative to the concentration of element detected by the analysis calculating the 1st time with the ratio (rate of recovery) of the aggregate value of the concentration of element detected by the analysis of 3 times.Analytical method preferably generally can go out whole objects with the analyzing and testing of 1 time, and therefore the described rate of recovery is higher, more manifests the good result that can go out many elements with the analyzing and testing of the 1st time.
Table 2
Learnt by table 2, in embodiment 3, also can carry out the high analysis of the rate of recovery for the material for testing of the trace being included in Semiconductor substrate.
(industrial applicability)
The present invention is included in technology that the metal of substrate etc. pollutes evaluating, and when carrying out detecting that the substrate of the pollutant of trace is analyzed with high sensitivity, can carry out abbreviated analysis or the privileged site of substrate being carried out to the analytical equipment of partial analysis.
Claims (4)
1. a substrate analytical equipment, possesses: etching means, is comprised the substrate of material for testing by the etching of gas-phase decomposition method; And recovering means, from spray nozzle front end, analytic liquid is sent to aforesaid substrate, after scraping draw aforesaid substrate surface with sent Such analysis liquid, aspirate Such analysis liquid by former nozzle front end and reclaim Such analysis object; It is characterized in that:
Possesses the dual pipe nozzle be made up of the nozzle body in order to Such analysis liquid is sent and to be aspirated and the outer tube that is configured in former nozzle body peripheral;
Aforementioned recovering means is the former nozzle body of aforementioned dual pipe nozzle;
Also possess the exhaust means as exhaust pathway between former nozzle body and aforementioned outer tube;
Aforementioned outer tube to configure around the mode of carrying out scraping the analytic liquid drawn, and has outer conductance hand-hole in front end;
Aforementioned etching means are be supplied to the etching gas between former nozzle body and aforementioned outer tube.
2. a substrate analytical method, is the method using the substrate analytical equipment described in claim 1 to analyze substrate, it is characterized in that having:
With the etching step that etching gas etches aforesaid substrate; And
The analytic liquid of former nozzle body interior is sent to aforesaid substrate, after aforesaid substrate surface is scraped drawing, Such analysis liquid is pumped to the recycling step of former nozzle body interior;
One side to be scraped aforesaid substrate surface with aforementioned dual pipe nozzle and is drawn, and one side carries out aforementioned etching step or aforementioned recycling step.
3. substrate analytical method according to claim 2, is characterized in that, with scraping to draw and carry out aforementioned etching step and aforementioned recycling step once simultaneously.
4. a substrate analytical method, is the method using the substrate analytical equipment described in claim 1 to analyze substrate, it is characterized in that:
Aforesaid substrate for comprising material for testing, and possesses polysilicon, tungsten silicide, titanium, the Semiconductor substrate of any one film of titanium nitride or the wafer substrate of Semiconductor substrate;
By former nozzle body, analytic liquid is sent to aforesaid substrate, to be exhausted by aforementioned exhaust means after one side to scrape with aforementioned analytic liquid and draw aforesaid substrate surface in one side, the Such analysis liquid comprising Such analysis object is pumped to former nozzle body.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009287205A JP4897870B2 (en) | 2009-12-18 | 2009-12-18 | Substrate analysis nozzle and substrate analysis method |
| JP2009-287205 | 2009-12-18 | ||
| JP2010-102950 | 2010-04-28 | ||
| JP2010102950A JP2011232182A (en) | 2010-04-28 | 2010-04-28 | Substrate analyzer and substrate analysis method |
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| JP5881166B2 (en) | 2012-06-14 | 2016-03-09 | 株式会社 イアス | Substrate analysis nozzle |
| JP5971289B2 (en) * | 2014-08-20 | 2016-08-17 | 株式会社 イアス | Substrate local automatic analyzer and analysis method |
| CN104332425A (en) * | 2014-11-18 | 2015-02-04 | 天津中环领先材料技术有限公司 | Silicon chip surface metal ion testing device |
| CN114464546A (en) * | 2015-03-12 | 2022-05-10 | 非视觉污染分析科学技术有限公司 | Substrate pollutant analysis device and substrate pollutant analysis method |
| JP6108367B1 (en) * | 2015-12-22 | 2017-04-05 | 株式会社 イアス | Silicon substrate analyzer |
| JP6156893B1 (en) * | 2016-03-01 | 2017-07-05 | 株式会社 イアス | Nozzle for substrate analysis |
| US10688485B2 (en) * | 2017-07-18 | 2020-06-23 | Ias, Inc | Substrate analysis nozzle and method for analyzing substrate |
| CN107627605B (en) * | 2017-08-08 | 2019-12-27 | 上海惠浦机电科技有限公司 | Double-face isomer micro-nozzle and manufacturing method thereof |
| JP6603934B2 (en) * | 2018-04-13 | 2019-11-13 | 東芝メモリ株式会社 | Analysis method of silicon substrate |
| CN108871900A (en) * | 2018-07-13 | 2018-11-23 | 上海华力微电子有限公司 | The collection device of hydrophily silicon chip surface drop in VPD board |
| CN113130366B (en) * | 2021-03-17 | 2024-02-13 | 江苏鲁汶仪器股份有限公司 | Nozzle for wafer scanning and system and application thereof |
| CN117393452B (en) * | 2023-12-11 | 2024-03-22 | 合肥晶合集成电路股份有限公司 | Method for collecting metal on surface of wafer |
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| JP3179175B2 (en) * | 1992-03-12 | 2001-06-25 | 株式会社ピュアレックス | Analysis pretreatment method |
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| JPH0830701B2 (en) * | 1992-12-30 | 1996-03-27 | 株式会社島津製作所 | Solid-phase extraction pretreatment device |
| JP4662531B2 (en) * | 2004-04-23 | 2011-03-30 | 有限会社Ｎａｓ技研 | Substrate processing apparatus and substrate processing method |
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| JP特开2005-311140A 2005.11.04 * |
| JP特开平5-256749A 1993.10.05 * |
| JP特开平6-201667A 1994.07.22 * |
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| TWI529833B (en) | 2016-04-11 |
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