CN106990158A - One kind stains detecting system and detection method - Google Patents
One kind stains detecting system and detection method Download PDFInfo
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- CN106990158A CN106990158A CN201710223406.XA CN201710223406A CN106990158A CN 106990158 A CN106990158 A CN 106990158A CN 201710223406 A CN201710223406 A CN 201710223406A CN 106990158 A CN106990158 A CN 106990158A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Abstract
The present invention discloses a kind of contamination detecting system and detection method, including：Sample surfaces are degraded by laser ablation machine, and contamination is supplied into icp mses, or chemical liquids dissolving unit with aerosol form；Chemical liquids dissolve unit, the surface contamination that the laser ablation machine is degraded are dissolved and collected using corrosive liquids, and concentrated in a fluid sample；Icp mses, are switched by central control unit and select sample introduction, directly measure the aerosol of laser ablation machine offer, or measure concentrated liquid sample；And central control unit, blanket control is carried out to system and does to stain analysis in real time or do total stain with fluid sample with aerosol to analyze.The system can take into account the quantitative analysis (fluid sample) of low detection bottom line and the whole wafer of collection of illustrative plates formula stains distributional analysis (aerosol), powerful but with low cost.
Description
Technical field
The present invention relates to test analysis field, and in particular to one kind stains detecting system and detection method.
Background technology
Moore's Law it is surging promote under 14 nanometers based on fin formula field effect transistor (FinFET) for high-performance,
Low energy-consumption electronic device early has been enter into our life.But, to manufacture so powerful device needs to introduce a large amount of new chemistry members
Element, also so that reaching unprecedented difficulty to the contamination monitoring of chip processing factory.Due to shadow of each element to silicon-based devices
Sound is different, and some are required, are added to realize function, some are then brought inadvertently into, as reduction device performance
Even make the pollution sources of component failure.Therefore, all elements that may relate to are intended to strict monitoring.In the periodic table of elements, gold
Category element occupies the majority, and because of its active chemistry, physical property, will turn into stain in most cases.In contamination monitoring
It is referred to as metal contamination in work.
The online metal contamination detecting instrument of main flow before --- total reflection fluorescence spectrum analyzer (TXRF) to sodium, magnesium,
The detection bottom line of the elements such as aluminium is nearly 1E11Atom/cm2, bottom line, which is 1E, to be detected to iron, copper etc.9Atom/cm2.The above emphasis
The process that the first procatarxis of monitoring is added is different, can sometimes turn into reduction device performance, or even make the main pollution of component failure
Source.However, total reflection fluorescence spectrum analyzer can not meet element pollution monitoring demand (>=1E in itself9Atom/cm2).Though
So have the shortcomings that detection bottom line is high, total reflection fluorescence spectrum analyzer that Rigaku (Rigaku) company develops is mopped up
(sweeping) pattern can collect dirty data by multiple spot on a wafer, finally with collection of illustrative plates (mapping) form analysis
Whole wafer surface contamination situation.The pattern of mopping up of total reflection fluorescence spectrum analyzer considerably increases its application field, such as exists
If crystal round fringes 3~4 point detect the elements such as chromium, nickel and iron, it may determine that stainless steel machinery hand is likely to be exposed crystalline substance substantially
Circle.Meanwhile, take into account international semiconductor technical plan (International Technology Roadmap for
Semiconductor, abbreviation ITRS) crystal column surface stain concentration, make up total reflection fluorescence spectrum analyzer high detection bottom
The gas-phase decomposition metal contamination collection system (VPD) of line is introduced in on-line monitoring auxiliary type instrument.Gas-phase decomposition metal is stained with
The effect of dirty collection system is the natural oxidizing layer of the hydrogen fluoride steam corrosion crystal column surface with gas phase, becomes its water-wetted surface
It is hydrophobic.Then, the metal contamination for being scattered in whole wafer surface is received in the way of scanning wafer with special liquid collection liquid
Collect on a point, coordinate total reflection fluorescence spectrum analyzer to test.Because crystal column surface and a bleeding point are on area
There is the difference of the order of magnitude, so 2 orders of magnitude have dropped in the wafer scale detection bottom line of nearly all element, so greatly improve
It is totally reflected the measurement sensitivity (more than 100 times) of fluorescence spectrum analyzer board.But, VPD-TXRF is single-node analysis, can only
It is quantitative, this mode can not describe situations such as above-mentioned manipulator stains.
At present, the rise of the related manufacturing of whole semiconductor, it is that various wafer fabs must that common metal, which stains detection,
The problem of must considering.It is totally reflected the board prices such as fluorescence spectrum analyzer itself costly.It is not special to meet budget
Abundant middle-size and small-size wafer fab takes into account the quantitative analysis of low detection bottom line and the whole crystalline substance of collection of illustrative plates formula to staiing detection demand
Circle stain analysis, the present invention disclose it is a kind of can be while realizing contamination detecting system and the detection side of above two test mode
Method.
The content of the invention
One kind, which stains detecting system, to be included：Including：Sample surfaces are degraded by laser ablation machine, and will be stain with gas
Solation is supplied to icp mses, or chemical liquids dissolving unit；Chemical liquids dissolve unit, utilize change
Learn corrosive liquid and dissolve the sample surfaces contamination, and concentrated as a fluid sample；Icp mses,
The aerosol of laser ablation machine offer, or the fluid sample that chemical liquids dissolving unit is provided are provided；And central control unit,
Carry out blanket control to system and do to stain analysis in real time or do total stain with fluid sample with aerosol to analyze.
Preferably, the optical maser wavelength of the laser ablation machine is one kind in 193nm, 213nm and 266nm or its combination.
Preferably, the chemical liquids dissolving unit includes：Very small chemical etching tank, chemical corrosion liquid source bottle and automatic sampling
Device, the very small chemical etching tank respectively with the laser ablation machine, the chemical corrosion liquid source bottle and the automatic sampling
Device is connected, wherein, the chemical attack source bottle supplies corrosive liquid to the very small chemical etching tank, and the laser ablation machine will
Sample surfaces stain formed aerosol and are passed through the very small chemical etching tank and are dissolved in its corrosive liquid formation fluid sample, institute
Automatic sampling device is stated to transmit to the inductively coupled plasma from the very small chemical etching tank extraction fluid sample
Mass spectrograph.
Preferably, the volume of the very small chemical etching tank is between 10mL~1000mL, the chemical corrosion liquid source bottle
Volume between 1L~10L.
Preferably, the very small chemical etching tank is multiple.
Preferably, the sample is silicon substrate.
Preferably, the composition of the chemical corrosion liquid is hydrofluoric acid, nitric acid, perchloric acid and water.
One kind stains detection method, comprises the following steps：Mode selecting step, collection of illustrative plates formula is selected by central control unit
Detection pattern or quantitative low detection bottom line detection pattern；
Under collection of illustrative plates formula detection pattern, including：Sample surfaces degrade sub-step, and sample surfaces are entered using laser ablation machine
Row is degraded, and sample surfaces are stain into feeding icp mses；Concentration mensuration sub-step is stain, inductance coupling is utilized
Close plasma mass spectrograph and measure contamination concentration in real time and data transfer to central control unit；And atlas analysis sub-step
Suddenly, it is real-time that the positional information and icp mses that central control unit is provided according to laser ablation machine are provided
Concentration is stain, atlas analysis is made；
Under quantitatively low detection bottom line detection pattern, including：Sample surfaces degrade sub-step, and laser ablation machine is to whole sample
Product surface is degraded, and sample surfaces are stain into feeding chemical liquids dissolution system；Stain and collect sub-step, chemical liquids dissolving unit
The sample surfaces that the etching laser machining degraded are dissolved and collected using corrosive liquids always to stain, and are concentrated in one
Fluid sample, is sent to icp mses；Concentration mensuration sub-step is stain, inductively coupled plasma matter is utilized
Spectrometer measures contamination concentration, and the interference that the various immunity modes elimination silicon substrates of startup are brought simultaneously transfers data to central control
Unit；And trace metal stains high-sensitivity analysis sub-step, central control unit makes trace metal and stains low detection bottom
Line analysis.
Preferably, under the quantitative low detection bottom line detection pattern, laser ablation thickness is 0.1~10 micron.
Preferably, under the quantitative low detection bottom line detection pattern, the immunity mode is mode standard, collision mould
One or more kinds of combinations in formula and reaction pattern.
The contaminations detecting system of the present invention can take into account the low quantitative analysis (fluid sample) for detecting bottom line and collection of illustrative plates formula
Whole wafer stains analysis (aerosol), powerful and with low cost.
Brief description of the drawings
Fig. 1 is the functional block diagram for staiing detecting system.
Fig. 2 is the functional block diagram that chemical liquids dissolve unit.
Fig. 3 is the flow chart for staiing detection method.
Fig. 4 is the sub-process figure of collection of illustrative plates formula detecting step.
Fig. 5 is the sub-process figure of quantitatively low detection bottom line detecting step.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it will be appreciated that described herein
Specific embodiment only to explain the present invention, is not intended to limit the present invention.Described embodiment is only the present invention one
Divide embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making
The all other embodiment obtained under the premise of creative work, belongs to the scope of protection of the invention.
Fig. 1 is the functional block diagram for staiing detecting system.As shown in figure 1, staiing detecting system includes laser ablation machine 1, changes
Learn liquid dissolving unit 2, icp mses 3 and central control unit 4.Wherein, laser ablation machine 1 is to sample table
Face is degraded, and collecting sample surfaces and staiing makes its distillation form aerosol；Chemical liquids dissolving unit 2 is molten using corrosive liquids
The sample surfaces contamination that the etching laser machining 1 is degraded is solved, and is concentrated in a fluid sample；Inductively coupled plasma
The aerosol that the measurement laser ablation machine of constitution spectrometer 3 is provided, or the fluid sample that chemical liquids dissolving unit is provided；Center control
Unit 4 blanket control is carried out to system and done with aerosol stain in real time atlas analysis or with fluid sample do it is total stain collect it is low
Detection bottom line is precisely analyzed.
The contamination detecting system of the present invention takes into account the quantitative analysis of low detection bottom line and the whole wafer of collection of illustrative plates formula is stain and divided
Analyse two kinds of detection patterns.Under two kinds of detection patterns, function performed by system each unit and mutual annexation are
It is different.Specifically, as shown in figure 1, analyzing the distribution stain and concentration in collection of illustrative plates (mapping) formula (compared with high detection bottom line)
In the case of, the unit and annexation being related in the system are：Laser ablation machine 1 degrades to sample surfaces, by sample table
Stain feeding icp mses 3 in face；Icp mses 3 are measured stains concentration and handle in real time
Data transfer is to central control unit 4；Positional information and inductive that central control unit 4 is provided according to laser ablation machine 1
The real-time contamination concentration that plasma mass spectrograph 3 is provided, makes atlas analysis.If if quantitative low detection bottom line analysis,
The unit and annexation being related in the system be：The whole sample surfaces of 1 pair of laser ablation machine degrade, and sample surfaces are stained with
Dirt feeding chemical liquids dissolution system 2；Chemical liquids dissolving unit 2, which is dissolved using corrosive liquids and collects etching laser machining 1, to be shelled
The sample surfaces of erosion stain, and are concentrated in a fluid sample, are sent to icp mses 3；Inductance coupling
Close plasma mass spectrograph 3 and start various immunity modes and eliminate the interference that silicon substrates bring and measure contamination concentration and data are passed
It is defeated to arrive central control unit 4；Central control unit 4 carries out trace metal and stains high-sensitivity analysis.Further, center control
Unit 4 carries out staiing concentration unit conversion always according to sample size, by ppt and atom/cm2Between mutually phase transformation, be easy to contrast
Analysis.
Laser ablation machine and icp mses (ICP-MS) can use existing product.Laser ablation machine
It can be certain of the Analyte series of Teller Di Ni CETAC technology companys (Teledyne CETAC Technologies) company
A kind of wafer compatibility customization version, or a certain wafer compatibility customization version in the NWR series of ESI companies.Laser wave
Length can be 193nm, 213nm and 266nm a certain kind or combination.The operation principle of laser ablation machine is irradiated with laser beam
Crystal column surface makes its produce high temperature, allows sample rapid sublimation, while inert gas, usually helium or argon gas are passed through in cavity,
Range of flow is that between 0.1L/min~10L/min, inductively coupled plasma is brought into the solid sample formation aerosol of distillation
Constitution spectrometer is analyzed.Icp mses can be the 7xxx series or 8xxx series of Agilent company
Any one, or moor the NexIon (goods marks) of Er Jinaiermo companies any one, or Sai Mofei companies
Any one.
Chemical liquids dissolve unit 2, as shown in Fig. 2 comprising：Very small chemical etching tank 21, chemical corrosion liquid source bottle 22 and from
Dynamic sampler 23.Very small chemical etching tank 21 respectively with laser ablation machine 1, chemical corrosion liquid source bottle 22 and automatic sampling device
23 are connected, wherein, chemical attack source bottle 22 supplies corrosive liquid to very small chemical etching tank 21, and laser ablation machine 1 is by sample surfaces
Stain formed aerosol and be passed through chemical corrosion groove 21, the extracting liq from very small chemical etching tank 21 of automatic sampling device 23
Sample is that the sample surfaces dissolved by chemical corrosion liquid stain, and is transmitted to icp mses 3.Very small chemical is rotten
It can be one or more to lose groove 21, be shown in Figure 2 for two, its volume is between 10mL~1000mL, and shape can be
Cylinder or cuboid.Chemical corrosion liquid source bottle 22 in can pour into 1L~10L corrosive liquids, can by nitrogen press-in or
Very small chemical etching tank 21 is transported in modes such as miniature measuring pumps.For silicon substrate sample, the composition of chemical corrosivity liquid can be with
It is hydrofluoric acid, nitric acid, perchloric acid, water, wherein, hydrofluoric acid：Nitric acid：Perchloric acid：The scope of the volume ratio of water is 1~100:1~
100：1~100：1~1000.
Automatic sampling device 23 (autosampler) can be any of the SC systems class of Eleksen Ltd. (ESI)
One kind, or the serial any one of Agilent company ASX-500.Usual automatic sampling device carry ICP-MS calibration solutions,
Quality monitoring liquid (Quality Check, QC liquid), atomizer, spray chamber and various valves and control module are directly real with ICP-MS
When it is interactive.
Next, being illustrated with reference to Fig. 3~Fig. 5 for the contamination detection method of the present invention.Fig. 3 is to stain detection method
Flow chart.As shown in figure 3, the contamination detection method of the present invention comprises the following steps：First, in mode selecting step S1,
Collection of illustrative plates formula detection pattern or quantitative low detection bottom line detection pattern are selected by central control unit 4.Next, carrying out collection of illustrative plates formula
Detecting step S2 carries out quantitative low detection bottom line detecting step S3.
Specifically, as shown in figure 4, collection of illustrative plates formula detecting step S2 includes following sub-step：
In sample surfaces degrade sub-step S21, laser ablation machine 1 degrades to sample surfaces, and sample surfaces are stained with
Dirt feeding icp mses 3.
In concentration mensuration sub-step S22 is stain, inductivity coupled plasma mass spectrometry 3 is measured stains concentration and number in real time
According to being transferred to central control unit 4.
In atlas analysis sub-step S23, positional information and electricity that central control unit 4 is provided according to laser ablation machine 1
Feel the real-time contamination concentration that couple plasma mass spectrometer 3 is provided, make atlas analysis.
Quantitative low detection bottom line detecting step S3, as shown in figure 5, including following sub-step：
In calibration sub-step S31, automatic sampling device 23 is interactive with icp mses 3, completion pair
The calibration of icp mses 3.
In corrosive liquid supply sub-step S32, chemical attack source bottle 22 supplies chemical attack to very small chemical etching tank 21
Liquid.
In quality testing sub-step S33, automatic sampling device 23 extracts sample and the QC carried from miniature etching tank 21
Liquid, does quality testing.If miniature etching tank 21 has unexpected contamination, undesirable, then another miniature corrosion is automatically switched to
Groove 21, repeats quality testing, if neither met the requirements, and is alternately rinsed with high purity deionized water and chemical corrosion liquid
Miniature etching tank 21 is up to standard until quality testing.
In sample surfaces degrade sub-step S34, laser ablation machine 1 degrades all contaminations of collection sample surfaces, i.e., from whole
The uniform substrate for degrading 0.1 micron~10 microns, such as silicon on individual sample surfaces, and the aeresols of generation are passed through contained
The miniature etching tank 21 of full chemical corrosion liquid.
In collection sub-step S35 is stain, by sample surfaces pollutant (mainly metal and substrate such as silicon grain) micro-
Homogeneous corrosion extracts sample by automatic sampling device 23 and is transported to inductively coupled plasma into ion in type chemical corrosion groove 21
Constitution spectrometer 3.
In concentration mensuration step S36 is stain, icp mses 3 carry out mass-spectrometer measurement, so as to measure
Stain concentration.It is possible to further eliminate silicon using one or more kinds of combinations such as mode standard, crash mode and reaction pattern
The interference that matrix is brought.
Finally, in trace metal stains high-sensitivity analysis sub-step S37, central control unit 4 makes trace metal
Stain low detection bottom line analysis.
The present invention can take into account the quantitative analysis of low detection bottom line and the whole wafer of collection of illustrative plates formula stains analysis, and cost
It is relatively low, it disclosure satisfy that budget is not special standby abundant middle-size and small-size wafer fab to staiing detection demand.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, the change or replacement that can be readily occurred in, all should
It is included within the scope of the present invention.
Claims (10)
1. one kind stains detecting system, it is characterised in that
Including：
Sample surfaces are degraded by laser ablation machine, and are supplied to inductively coupled plasma by staiing with aerosol form
Mass spectrograph, or chemical liquids dissolving unit；
Chemical liquids dissolve unit, and dissolving the sample surfaces using chemical corrosion liquid stains, and is concentrated as a liquid-like
Product；
Icp mses, measure the aerosol of laser ablation machine offer, or chemical liquids dissolving unit is provided
Fluid sample；And
Central control unit, blanket control is carried out to system and does to stain to analyze or do with fluid sample in real time with aerosol to be always stained with
Dirt analysis.
2. contamination detecting system according to claim 1, it is characterised in that
The optical maser wavelength of the laser ablation machine is one kind or its combination in 193nm, 213nm and 266nm.
3. contamination detecting system according to claim 1, it is characterised in that
The chemical liquids dissolving unit includes：Very small chemical etching tank, chemical corrosion liquid source bottle and automatic sampling device, it is described micro-
Type chemical corrosion groove is connected with the laser ablation machine, chemical corrosion liquid source bottle and the automatic sampling device respectively, its
In,
The chemical attack source bottle supplies corrosive liquid to the very small chemical etching tank, and sample surfaces are stained with by the laser ablation machine
The aerosol that dirt is formed is passed through the very small chemical etching tank and is dissolved in its corrosive liquid formation fluid sample, the automatic sampling
Device extracts the fluid sample from the very small chemical etching tank and transmitted to the icp mses.
4. contamination detecting system according to claim 3, it is characterised in that
The volume of the very small chemical etching tank between 10mL~1000mL, the volume of chemical corrosion liquid source bottle 1L~
Between 10L.
5. according to claim contamination detecting system according to claim 3, it is characterised in that
The very small chemical etching tank is multiple.
6. contamination detecting system according to claim 1, it is characterised in that
The sample is silicon substrate.
7. contamination detecting system according to claim 6, it is characterised in that
The composition of the chemical corrosion liquid is hydrofluoric acid, nitric acid, perchloric acid and water.
8. one kind stains detection method, it is characterised in that
Comprise the following steps：
Mode selecting step, collection of illustrative plates formula detection pattern or quantitative low detection bottom line detection pattern are selected by central control unit；
Under collection of illustrative plates formula detection pattern, including：Sample surfaces degrade sub-step, and sample surfaces are shelled using laser ablation machine
Sample surfaces are stain feeding icp mses by erosion；Concentration mensuration sub-step is stain, inductive etc. is utilized
Gas ions mass spectrograph measures contamination concentration and data transfer to central control unit in real time；And atlas analysis sub-step, in
The real-time contamination that the positional information and icp mses that centre control unit is provided according to laser ablation machine are provided
Concentration, makes atlas analysis；
Under quantitatively low detection bottom line detection pattern, including：Sample surfaces degrade sub-step, and laser ablation machine is to whole sample table
Face is degraded, and sample surfaces are stain into feeding chemical liquids dissolution system；Stain and collect sub-step, chemical liquids dissolving unit is utilized
Corrosive liquids dissolves and collected the sample surfaces that the etching laser machining degraded and always stains, and is concentrated in a liquid
Sample, is sent to icp mses；Concentration mensuration sub-step is stain, icp mses are utilized
Contamination concentration is measured, the interference that the various immunity modes elimination silicon substrates of startup are brought simultaneously transfers data to center control list
Member；And trace metal stains high-sensitivity analysis sub-step, central control unit makes trace metal and stains low detection bottom line
Analysis.
9. contamination detection method according to claim 8, it is characterised in that
Under the quantitative low detection bottom line detection pattern, laser ablation thickness is 0.1~10 micron.
10. contamination detection method according to claim 8, it is characterised in that
Under the quantitative low detection bottom line detection pattern, the immunity mode is mode standard, crash mode and reaction mould
One or more kinds of combinations in formula.
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| CN109444248A (en) * | 2018-11-20 | 2019-03-08 | 中国地质大学（武汉） | A kind of method that the solution based on laser degrades that sample introduction is analyzed |
| CN110196275A (en) * | 2019-05-15 | 2019-09-03 | 中国科学院上海硅酸盐研究所 | It is a kind of for the high temperature real-time sample pond of laser ablation system and its detection method |
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| WO2023284205A1 (en) * | 2021-07-16 | 2023-01-19 | 江苏鲁汶仪器有限公司 | Online sampler and contamination analysis system |
| CN116773507A (en) * | 2023-06-09 | 2023-09-19 | 上海凯来仪器有限公司 | Three-dimensional laser ablation mass spectrometer, combined detection system and detection method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108020542A (en) * | 2017-12-21 | 2018-05-11 | 重庆超硅半导体有限公司 | The detection method of pollutant load in a kind of film magazine |
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| CN109444248A (en) * | 2018-11-20 | 2019-03-08 | 中国地质大学（武汉） | A kind of method that the solution based on laser degrades that sample introduction is analyzed |
| CN109444248B (en) * | 2018-11-20 | 2020-10-30 | 中国地质大学（武汉） | Solution ablation sample injection analysis method based on laser |
| CN110196275A (en) * | 2019-05-15 | 2019-09-03 | 中国科学院上海硅酸盐研究所 | It is a kind of for the high temperature real-time sample pond of laser ablation system and its detection method |
| WO2022163143A1 (en) * | 2021-01-26 | 2022-08-04 | 富士フイルム株式会社 | Analysis device and analysis method |
| WO2023284205A1 (en) * | 2021-07-16 | 2023-01-19 | 江苏鲁汶仪器有限公司 | Online sampler and contamination analysis system |
| CN116773507A (en) * | 2023-06-09 | 2023-09-19 | 上海凯来仪器有限公司 | Three-dimensional laser ablation mass spectrometer, combined detection system and detection method |
| CN116773507B (en) * | 2023-06-09 | 2024-01-26 | 上海凯来仪器有限公司 | Three-dimensional laser ablation mass spectrometer, combined detection system and detection method |
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|---|---|
| CN106990158B (en) | 2020-02-07 |
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