CN103234943A - Method for rapidly detecting metal thermal diffusion with laser-induced breakdown spectroscopy technology - Google Patents
Method for rapidly detecting metal thermal diffusion with laser-induced breakdown spectroscopy technology Download PDFInfo
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- CN103234943A CN103234943A CN201310122070XA CN201310122070A CN103234943A CN 103234943 A CN103234943 A CN 103234943A CN 201310122070X A CN201310122070X A CN 201310122070XA CN 201310122070 A CN201310122070 A CN 201310122070A CN 103234943 A CN103234943 A CN 103234943A
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Abstract
The invention relates to a method for rapidly detecting metal thermal diffusion with a laser-induced breakdown spectroscopy technology. According to the invention, laser is focused on the surface of a sample requiring detection; the surface of the sample is burned by the laser and plasma is produced, and photons carrying elemental composition information are radiated; characteristic photons are collected in real-time by using a spectrometer; metal and silicon characteristic spectral lines are selected, and intensities thereof are detected in real-time, such that metal content is calculated; with continuous burning of the laser, metal content information at different depths can be obtained; and metal depth distribution data can be recorded. According to the invention, with the laser-induced breakdown spectroscopy technology, thermal diffusion of aluminum in a silicon wafer is analyzed, depth distribution difference of aluminum in silicon under different temperatures can be identified, and a result with relatively high precision is obtained. Compared with other detection technologies, the technology provided by the invention assists in rapid and almost flawless detection of metal thermal diffusion.
Description
Technical field
The present invention relates to a kind of metal fever spread detection method, especially a kind of method of using the diffusion of Laser-induced Breakdown Spectroscopy technology fast detecting metal fever.
Background technology
In semiconductor silicon material industry, deposit some metal material to form electrode and transistor at silicon chip surface usually.Often be subjected to thermal process in subsequent processes, the metal level of deposition can be to the silicon wafer internal divergence, and this diffusion often has side effects, the transistorized Electronic Performance that weakens, even cause the inefficacy of transistor Electronic Performance.Therefore, the diffusion of detection metal in silicon chip in time is very important in semiconductor production.At present, often need several days time in the analytic process of silicon, and need a series of complicated sample preparation process.If last silicon does not meet standard, taste waste plenty of time and starting material.As seen, seek a kind of can fast detecting metal method of thermal diffusion in silicon wafer extremely being necessary.
Main element detection means has electron energy spectrum (EDS), x-ray photoelectron power spectrum (XPS), secondary ion mass spectrum etc. at present.XPS and secondary ion mass spectrum degree of detection height, but the elemental composition that is limited to surface micrometre-grade detects, and being difficult to the testing micro zone composition, the diffusion of metal in silicon often can reach tens of microns, so these two kinds of detection meanss are difficult in order to analyze the thermal diffusion of metal in silicon.EDS can carry out the microcell ultimate analysis, and can carry out line sweep with the detection elements depth profile to the transversal section of sample, but when this technology is done depth analysis to sample damage big (need strike disconnected sample) and need and the online use of scanning electron microscope (SEM), the big heavy discount of convenient and swift property; And the shortcoming of EDS maximum is that accuracy of detection is not high, and constituent content is differentiated with interior just being difficult to 1%.
Laser-induced Breakdown Spectroscopy (LIBS) technology is a kind of detection means of element fast, has higher element accuracy of detection (can reach 100 ppm ranks), and allow laser burn the depth profile that the sample surfaces same position can be easy to detection elements continuously, its detection is little damage, can carry out in atmosphere.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of in order to detect the new method of metal fever diffusion.
The present invention for the scheme that provides is provided is: detect the element depth distribution of metal level after the thermal diffusion under the different temperatures of silicon wafer surface by using the Laser-induced Breakdown Spectroscopy technology, obtain the tenor information of different depth in real time, finally can differentiate the difference of metal depth profile in silicon wafer under the different rate of diffusion.
The metal fever diffusion testing process of the inventive method specifically comprises the steps:
Step (1). open laser, the laser scioptics focus on the testing sample surface, and sample surfaces is produced plasma by laser burn, and the photon of elemental composition information is carried in radiation.
Step (2). utilize the real-time acquisition characteristics photon of spectrometer, show spectrum on computers in real time.The characteristic spectral line of selected metal and silicon detects its intensity in real time to calculate the content of metal simultaneously.
Step (3). along with burning that laser does not stop, can obtain the tenor information of different depth, the depth profile data of metal under the final entry.
Testing sample is the surperficial silicon wafer that has plated metallic film, and it is heat treated to realize thermal diffusion of different rates in different temperatures respectively.On the sample platform that test sample is fixed.
The invention has the beneficial effects as follows: by using the Laser-induced Breakdown Spectroscopy technology element depth analysis is carried out in the thermal diffusion of metallic element, this method does not need the complicated sample preparation, detection speed is fast, hardly can the loss test sample, and can obtain more high precision and a high-resolution result, can differentiate the difference of the element depth distribution of metal fever diffusion under the different temperatures.
Description of drawings
Fig. 1 is the employed system schematic of induced with laser deposition spectral technique among the embodiment 1.
Fig. 2 is the aluminium film X-ray diffraction after the thermal treatment (XRD) comparison diagram under different temperatures of magnetron sputtering on the silicon wafer of embodiment 1 preparation.
Fig. 3 is the heat treatments at different aluminium element degree of depth content distribution figure afterwards that Comparative Examples 1 usefulness electronics energy spectrum detects.
Fig. 4 is the spectrogram of aluminium film in induced with laser deposition spectral detection of magnetron sputtering on the silicon wafer of embodiment 1 preparation.
Fig. 5 schemes in the surface sweeping Electronic Speculum (SEM) of laser burn position the aluminium film of magnetron sputtering on the silicon wafer of embodiment 1 preparation.
Fig. 6 is the heat treatments at different aluminium element degree of depth content distribution figure afterwards that embodiment 1 usefulness induced with laser deposition spectral technique detects.
Embodiment
Below in conjunction with drawings and Examples the present invention is further set forth:
Embodiment 1:
Employed experimental technique is applicable to that the diffusion of all metallic elements detects in this example.Employed sample is in the example: use magnetron sputtering method that aluminium is plated to silicon wafer, make silicon wafer surface form the aluminium film of about 800nm, after the deposition, different samples are carried out in air with 300 and 610 ℃ of annealing in process of carrying out 24 h, to realize the thermal diffusion of aluminium different rates in silicon wafer.
Use induced with laser deposition spectral technique to detect: for the aluminium in the quantitative test silicon wafer, according to the NIST atomic spectra database, to select Al I emission line (396.152 nm) and Si II emission line (634.711 nm) to elect ionization meter as.For obtaining the aluminium diffusion concentration, laser beam is focused on the fixing silicon wafer carries out prolonged exposure.In this experiment measuring process, laser energy is 20 mJ, and the spectrum sample time is 4 milliseconds, and on average each sample detection is 20 times, takes the mean at last.
Comparative Examples 1:
In order to contrast the testing result of induced with laser deposition spectral technique, adopt the electron energy spectral technology to detect the depth profile of aluminium element for the sample among the embodiment 1.The sample of different temperatures diffusion is cut with glass cutter, in the surface sweeping Electronic Speculum transversal section is amplified, utilize online electron energy spectrum that the line surface sweeping is carried out in the transversal section, sweep limit is 5 microns.
Fig. 1 is the employed system schematic of induced with laser deposition spectral technique among the embodiment 1.System is made up of laser instrument, focusing system, spectrometer, computer four bulks as can be seen.
Fig. 2 is the aluminium film X-ray diffraction after the thermal treatment (XRD) comparison diagram under different temperatures of magnetron sputtering on the silicon wafer of embodiment 1 preparation.As can be seen, successfully plate layer of aluminum on the silicon wafer, and aluminium lamination changes after the thermal treatment little.
Fig. 3 is the heat treatments at different aluminium element degree of depth content distribution figure afterwards that Comparative Examples 1 usefulness electronics energy spectrum detects.The depth profile of the aluminium that spreads under the different temperatures can not be differentiated by the electron energy spectrum as can be seen.
Fig. 4 is the spectrogram of aluminium film in induced with laser deposition spectral detection of magnetron sputtering on the silicon wafer of embodiment 1 preparation.Aluminium and element silicon are wherein arranged as can be seen, and the nitrogen element is from the air.
Fig. 5 schemes in the surface sweeping Electronic Speculum (SEM) of laser burn position the aluminium film of magnetron sputtering on the silicon wafer of embodiment 1 preparation.Burn a little 400 microns of about diameters as can be seen.
Fig. 6 is the heat treatments at different aluminium element degree of depth content distribution figure afterwards that embodiment 1 usefulness induced with laser deposition spectral technique detects.Induced with laser deposition spectral technique can be told the depth profile of the aluminium that spreads under the different temperatures well as can be seen.
Interpretation of result: electron energy spectrum institute testing result learns that according to the result all samples have similar diffusion profile as shown in Figure 3.In the degree of depth was about the scope of 700 nm, the content of aluminium descended gradually, and the degree of depth is almost constant above content after 700 nm, and the concentration gradient of aluminium almost is to distinguish in the distribution of all samples.The aluminium that uses induced with laser deposition spectral technique to detect to obtain and the intensity of silicon as shown in Figure 6, it can differentiate the depth profile of the aluminium that spreads under the different temperatures well.Induced with laser is deposited light technology gained experimental result and electron energy spectrum compare and can learn, induced with laser deposition spectral technique can further be distinguished at the silicon wafer nuance of the aluminum concentration put of deep-seated more.The testing result of induced with laser deposition spectral technique shows, under higher temperature, the aluminium atom will have faster rate of propagation and can be diffused into the darker degree of depth, and the description of this and diffusion theory meets fully.Because the fusing point of aluminium is 660 ℃, so sample is the highest only carries out annealing in process at 610 ℃.
The result meets induced with laser deposition spectral technique and the electron energy spectrum compares, and has higher degree of accuracy, and is more suitable in the metal diffusion that detects under the different temperatures.In addition, induced with laser deposition spectral technique detects and does not need complicated sampling, can obtain the testing result in very short time.Above advantage shows that induced with laser deposition spectral technique technology is the detection that is adapted at very much the metal diffusion of silicon wafer.
Claims (1)
1. use the method for Laser-induced Breakdown Spectroscopy technology fast detecting metal fever diffusion, it is characterized in that this method may further comprise the steps:
Step (1). open laser, the laser scioptics focus on the testing sample surface, and sample surfaces is produced plasma by laser burn, and the photon of elemental composition information is carried in radiation;
Step (2). utilize the real-time acquisition characteristics photon of spectrometer, show spectrum on computers in real time; The characteristic spectral line of selected metal and silicon detects its intensity in real time to calculate the content of metal simultaneously;
Step (3). along with burning that laser does not stop, can obtain the tenor information of different depth, the depth profile data of metal under the final entry;
Described testing sample is the surperficial silicon wafer that has plated metallic film, and it is heat treated to realize thermal diffusion of different rates in different temperatures respectively.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106033057A (en) * | 2015-03-10 | 2016-10-19 | 中国科学院微电子研究所 | Silicon chip surface granular pollutant component nondestructive rapid online detection method and system |
| WO2017120988A1 (en) * | 2016-01-15 | 2017-07-20 | 清华大学深圳研究生院 | Method of inspecting aging state of composite insulating material |
| CN112924437A (en) * | 2019-12-06 | 2021-06-08 | 核工业西南物理研究院 | Laser-induced breakdown spectroscopy absolute quantitative analysis method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102680435A (en) * | 2012-05-29 | 2012-09-19 | 杭州电子科技大学 | Standard-sample-free quantitative analysis method for element components through laser-induced breakdown spectroscopy |
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| CN102680435A (en) * | 2012-05-29 | 2012-09-19 | 杭州电子科技大学 | Standard-sample-free quantitative analysis method for element components through laser-induced breakdown spectroscopy |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106033057A (en) * | 2015-03-10 | 2016-10-19 | 中国科学院微电子研究所 | Silicon chip surface granular pollutant component nondestructive rapid online detection method and system |
| WO2017120988A1 (en) * | 2016-01-15 | 2017-07-20 | 清华大学深圳研究生院 | Method of inspecting aging state of composite insulating material |
| US10209197B2 (en) | 2016-01-15 | 2019-02-19 | Graduate School At Shenzhen, Tsinghua University | Method for inspecting aging state of silicone rubber composite insulating material |
| CN112924437A (en) * | 2019-12-06 | 2021-06-08 | 核工业西南物理研究院 | Laser-induced breakdown spectroscopy absolute quantitative analysis method |
| CN112924437B (en) * | 2019-12-06 | 2023-02-21 | 核工业西南物理研究院 | Laser-induced breakdown spectroscopy absolute quantitative analysis method |
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Application publication date: 20130807 |