CN106018442A - Method for dynamically observing failure of group III-V field effect transistor gate dielectric at atomic scale - Google Patents
Method for dynamically observing failure of group III-V field effect transistor gate dielectric at atomic scale Download PDFInfo
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- CN106018442A CN106018442A CN201610376424.7A CN201610376424A CN106018442A CN 106018442 A CN106018442 A CN 106018442A CN 201610376424 A CN201610376424 A CN 201610376424A CN 106018442 A CN106018442 A CN 106018442A
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- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
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Abstract
The invention discloses a method for dynamically observing the failure of a group III-V field effect transistor gate dielectric at the atomic scale. The group III-V refers to a high-mobility material indium gallium arsenide. The method includes the following steps: preparing a sample and a nanometer tungsten probe which are suitable for a transmission electron microscope; arranging the prepared sample on a special copper mesh, and putting an in-situ sample rod in the transmission electron microscope; allowing the nanometer tungsten probe to be in contact with a sample grid; applying a constant electric field between the nanometer tungsten probe and the copper mesh; operating the transmission electron microscope to dynamically observe the morphology of the sample and the current change process in real time; and carrying out local chemical element analysis through an energy spectrum, comparing the energy spectrum with the energy information of the undamaged sample, and analyzing failure reasons. The failure process of a device can be analyzed in a fixed-point quantitative manner to find the location, the state and the change process of the failure, and the failure mechanism of the device is analyzed to obtain a solving measure. The in-situ transmission electron microscopy method has the advantages of losslessness, real-time property, and high resolution, and is more advanced than other spectral detection methods.
Description
Technical field
The invention belongs to material analysis field, relate to a kind of method that under atomic scale, dynamically observation iii-v field-effect transistor gate medium lost efficacy, specifically utilize focused ion bundle sample preparation, use in situ TEM added electric field and observation, utilize spectroscopy detection element information.
Background technology
Along with reducing of device size, need to accomplish grid oxic horizon the thinnest, but this can cause the reduction of electron mobility of the silicon inversion layer caused due to Partial charge and the long-range phon scattering of dielectric layer.One feasible method is material III-V material of the most heterogeneous integrated high mobility.One of thing followed challenge is the selection of gate dielectric layer, natural silicon dioxide oxide layer is had owing to III-V material is not as silicon, the biggest lattice mismatch is had to cause there is a lot of defect interface states between the grid of high-k and substrate, this not only can affect the mobility of device, make it reduce, also can affect the integrity problem of device.It is thus desirable to the failure mechanism of cognitive this III-V device, this is necessary to the development of the selection of gate medium with the improvement of technique and the most smaller high speed device, but technology is that the device after losing efficacy carries out the research of static state now, the device simulation technology of standard can only provide the average information of component failure electrical property, and the change of the whole process of component failure is not also observed, there is presently no work and can see this dynamic process of component failure from atomic scale in real time, this field still belongs to blank.
Summary of the invention
The method of a kind of realtime dynamic observation component failure based in situ TEM of method of a kind of detection III-V field effect transistor tube failure that the invention aims to overcome the defect of prior art and propose, the method using in situ TEM add in-place electric field, observes component failure process Real-time and Dynamic.The present invention can Real-time and Dynamic observe the failure procedure of device under nanoscale, by energy loss spectroscopy, the local analysis of device can be carried out constituent content change, elementary composition, chemical bond and electronic structure etc. quantitatively to component failure position and be analyzed.
The concrete technical scheme realizing the object of the invention is:
A kind of method that under atomic scale, dynamically observation iii-v field-effect transistor gate medium lost efficacy, feature is that the method includes step in detail below:
1) the sample sample preparation of transmission electron microscope
2) sample preparation of nanometer tungsten tipped probe
3) sample prepared by step 1) is mounted on the copper mesh of in situ TEM (TEM), the copper mesh having carried sample is put into specimen holder in situ, then transmission electron microscope intracavity will be loaded by specimen holder in situ；
4) by step 2) gate contact of sample that the tip of nano-probe prepared is prepared with step 1), between nano-probe and copper mesh, add a steady electric field；
5) operation in situ TEM, the change of monitoring sample topography in real time and the change increasing electric current in time, and record；
6) on inefficacy microcell, carry out topotaxial elementary analysis in inefficacy microcell power spectrum, compare with the sample spectral information before not damaging, it may be judged whether lost efficacy.
In described step (1), sample for use in transmitted electron microscope prepares by the following method: use focused ion beam system, electromagnetic lens is utilized iii-v field-effect transistor to be cut or after attrition process ion beam focusing, keep former field-effect transistor structure cross section, make thickness more than 20 nanometers, the sample being applicable in situ TEM less than 100 nanometers.
Nanometer tungsten tipped probe described in described step (2) is the nanometer tungsten tipped probe used in situ TEM (TEM), and described nanometer tungsten tipped probe uses electrochemical method to prepare, and the tip diameter of described nanometer tungsten tipped probe is more than 5 nanometers, less than 20 nanometers.
Power spectrum in described step (6) includes electron energy loss spectroscopy (EELS) or energy dispersion X-ray spectrum.
Described electrochemical method is particularly as follows: using the tungsten filament of a diameter of 0.15-0.35 millimeter as electricity anode, using stainless steel electrode as electricity negative electrode, electricity anode and electricity negative electrode are inserted electrolyte respectively, and the insertion depth of electricity anode is 5-10 millimeter, described electrolyte be the molar concentration of sodium hydrate aqueous solution and sodium hydrate aqueous solution be 3-5mol/L, then apply, on electricity anode and electricity negative electrode, the voltage that initial value is 5 volts, electricity anode is carried out electrochemical corrosion, when the electric current flowing through electricity anode is decreased to 20 MAHs, promote electricity anode, promoting speed is 1 ~ 8 micro-meter per second, when the electric current flowing through electricity anode continues to be decreased to zero, the current potential reducing electricity anode the current potential making electricity anode are less than electricity negative electrode, and make electricity anode leave electrolyte, obtain nanometer tungsten tipped probe.
The copper mesh of in situ TEM (TEM) described in step (6) refers to carry the copper mesh of sample, and it has three sample for use in transmitted electron microscope posts respectively, has the rectangle cavity of a 3-5 micron wherein for carrying sample in a sample column.
Described in described step (4), steady electric field refers to by sample is added scan voltage, draws out the electric current figure with change in voltage, finds out electric current and suddenly increases corresponding voltage, and added constant voltage is this corresponding voltage and deducts the value of 0.7 volt.
It is more than 1 order of magnitude of current break that described electric current increases corresponding voltage suddenly.
Specimen holder in situ put into by the sample utilizing focused ion bundle (FIB) technology to prepare by the present invention, is then placed in in situ TEM, makes the image of sample be in state clearly by operation Electronic Speculum.Then adding a constant voltage (steady electric field), added voltage is in advance sample to be added a scanning voltage, draws its electric current curve chart with change in voltage, then draws the numerical value of add in-place electric field required voltage according to breakdown voltage.The process that realtime dynamic observation device is punctured by constant voltage, this process include electric current change over situation and in the case of low power and high power the time dependent situation of device.Finally according to demand, it is possible to use the Elemental redistribution of the electron energy loss spectroscopy (EELS) sample to being in various process is analyzed.
Show that Lacking oxygen defect is the dominant mechanism causing gate dielectric layer to lose efficacy by analysis of the present invention, technique can be reduced by annealing the density of oxygen defect, thus improve the reliability of device.
The beneficial effects of the present invention is, use in situ TEM intuitively, in real time, dynamically can observe sample topography and see the change on yardstick in nanometer, a certain small region can be analyzed by the powerful function of transmission electron microscope, and device can be analyzed in chemically component analysis aspect by the combination with electron energy loss spectroscopy (EELS).By present invention determine that Lacking oxygen defect is the dominant mechanism causing gate dielectric layer to lose efficacy, technique can be reduced by annealing the density of oxygen defect, thus improve the reliability of device.
Each process site-directed quantitative of component failure can be analyzed by the present invention, find change procedure during position, state and the inefficacy starting to lose efficacy, the structure finding each stage during component failure corresponding by corresponding map of current changes, thus the failure mechanism of analysis device, and then obtain corresponding solution.The method utilizing in situ TEM is lossless, in real time, has high-resolution, more advanced than other spectral detection.
Accompanying drawing explanation
Fig. 1 is electric current time history plot of the present invention；
Fig. 2 is flow chart of the present invention；
Fig. 3 is the schematic diagram that step 4) sample of the present invention adds a steady electric field；
Fig. 4 is the transmission electron microscope picture that the present invention is corresponding with adding a steady electric field；
Fig. 5 is the step 5) sample of the present invention pattern when adding in the case of a steady electric field 40 seconds and map of current；In figure, size of current is about 2.5 × 10-6Ampere；
Fig. 6 is the step 5) sample of the present invention pattern when adding in the case of a steady electric field 200 seconds and map of current；In figure, electric current was undergone mutation about 147 seconds when, finally stable about 2 × 10-5Ampere；
Fig. 7 is the density of states figure of the first-principles calculations of interpretation of result of the present invention.
In the drawings: 1-is in the case of adding described constant voltage, and growth over time, incipient time, electric current is the least in increasing slowly, and electric current now is the leakage current that pressurization causes, and this electric current is relevant with the area of sample；
2-increases over time, and electric current starts the fluctuation as digital signal occur；
There is the fluctuation as analogue signal in 3-electric current；
There is steep increasing in the last electric current of 4-, and its size is bigger to more than 100 times than before, and now device is that unrepairable punctures, for hard breakdown；
The protective layer of 5-platinum; this protective layer is to prevent the surface of sample from being damaged deposited protective layer by the bombardment of focused ion bundle when making sample; subsequent process can be removed, do electrode and use, so sample described after process will comprise the protective layer of platinum；
6-titanium nitride layer；
The dielectric layer of 7-zirconium dioxide；
8-aluminium sesquioxide layer；
9-nanometer tungsten tipped probe；
10-indium gallium arsenide layer；
11-voltage source；
The adhesion layer of 12-platinum, this adhesion layer is to do binder with platinum to be sticked together with copper mesh by sample；
13-copper mesh.
A-is by 5,6,7,8,10 samples formed, and is the sample prepared by focused ion bundle.
Detailed description of the invention
In conjunction with specific examples below and accompanying drawing, the present invention is described in further detail.Implementing the process of the present invention, condition, experimental technique etc., outside the lower content mentioned specially, be universal knowledege and the common knowledge of this area, the present invention is not particularly limited content.
The present invention includes:
Step one: the sample sample preparation of transmission electron microscope
Using focused ion bundle that iii-v field-effect transistor is wanted the part of research carry out cutting processing, sample making becomes thickness be less than 100 nanometers and is applicable to the sample of transmission electron microscope, sample is as shown in Figure 3 and Figure 4.The sample of the present invention is chosen iii-v field-effect transistor and is made up of titanium nitride layer 6, the dielectric layer 7 of zirconium dioxide, aluminium sesquioxide layer 8 and indium gallium arsenide layer 10, wherein, indium gallium arsenide layer 10 is positioned at the bottom, aluminium sesquioxide layer 8 is positioned on indium gallium arsenide layer 10, titanium dioxide zirconium layer 7 is positioned on aluminium sesquioxide layer 8, and titanium nitride layer 6 is positioned on titanium dioxide zirconium layer 7.Protective layer 5 is done with platinum when utilizing focused ion bundle to make sample; it is positioned on titanium nitride layer; to prevent the surface of sample from being damaged by the bombardment of focused ion bundle; the protective layer deposited; subsequent process can be removed, do electrode and use, so sample described after process will comprise the protective layer of platinum i.e. shown in A; in Fig. 3 schematic diagram 12 are the adhesion layers of platinum, for being linked together with copper mesh 13 by rectangle sample A.
Step 2: the sample preparation of nano-probe.The method preparation using electrochemistry can be used for the nanoscopic tips that in situ TEM uses, and nano-probe is as shown in Fig. 3 and Fig. 49；The needle point of nanometer tungsten tipped probe contacts with platinum.Used here as tungsten do probe be contacting between tungsten with platinum be Ohmic contact, there is good electric conductivity, nanometer tungsten tipped probe tip can accurately contact with platinum layer less than 20 nanometers more than 5 nanometers, it is to avoid probe tip and other location contacts of sample.
Step 3: sample is mounted on special copper mesh, and load in situ TEM intracavity.
Step 4: by the gate contact at the tip of nano-probe Yu TEM sample, adds a steady electric field between nano-probe and copper mesh, the partial earthing that wherein nanometer tungsten tipped probe tail end is connected with wire, as shown in Figure 3 and Figure 4.
Step 5: first sample is added scanning voltage, when observe before current value sudden change and sudden change current value order of magnitude greater above time stop pressurizeing, record the magnitude of voltage corresponding to now current value sudden change, then this magnitude of voltage deducts 0.7V and is added on sample as constant voltage values, operation in situ TEM is monitored the change of sample topography in real time and increases over time the change of electric current, as shown in Figure 5 and Figure 6.The process adding scanning voltage described in before can't cause the change of sample contrast, does not punctures front sample media layer surface contrast homogeneous, does not change significantly.The size of electric current does not change significantly close to straight line, as shown in Figure 5.Dielectric layer in Fig. 6 has had obvious contrast to change compared with Fig. 5, and electric current has had obvious sudden change, (can be seen that Fig. 6 is the figure after puncturing from current time figure after this illustrates to puncture, because can be seen that device is in the case of adding constant voltage from Fig. 1 (Fig. 1 be to add constant voltage after the overall variation that increases in time of the electric current of device), growth over time, incipient time, electric current is the least in increasing slowly, electric current now is the leakage current that pressurization causes, this electric current label 1 relevant with the area of sample；Increasing over time, electric current starts the fluctuation as digital signal occur, and the now little label of current values 2 fluctuation as analogue signal occurs with after current, and now current values changes little label 3；There is steep increasing in last electric current, and its size is bigger to more than 100 times than before, and now device is that unrepairable punctures, and for hard breakdown, electric current has increased the above label of an order of magnitude 4 suddenly.This experimentation is 2 to 3 these processes) structure of gate medium there occurs change.
Step 6: carry out topotaxial elementary analysis in inefficacy microcell power spectrum (electron energy loss spectroscopy (EELS), energy dispersion X-ray spectrum).
nullInterpretation of result: the present invention is by the electron energy loss spectroscopy (EELS) in sample contrast change region greatly before and after detection energising pressure，Find that the distribution after oxygen element is before breakdown is different，The disappearance of obvious oxygen element is had after puncturing，Form the room of oxygen，Therefore，The inefficacy of the device that the increase of leakage current caused due to Lacking oxygen disappearance causes，By first-principles calculations (DOS)，Owing to the disappearance of Lacking oxygen can cause the band gap of gate dielectric layer (being zirconium dioxide here) to reduce and change towards metallicity，The insulating properties making gate medium is deteriorated，Electric current is caused to be easier to conducting，Cause component failure as shown in Figure 7，Can see from the upper, middle and lower three width figure of Fig. 7 that the straight line (fermi level) that energy is equal at zero progresses into conduction band from forbidden band，Illustrate that gate dielectric layer gradually changes toward metallicity from semiconductor property，Thus tutor's electric current is easier to conducting，And energy differences (band gap) minimizing at the bottom of valence band and between conduction band top also can illustrate that electric current is easier to conducting.
The protection content of the present invention is not limited to above example.Under the spirit and scope without departing substantially from inventive concept, those skilled in the art it is conceivable that change and advantage be all included in the present invention, and with appending claims as protection domain.
Claims (8)
1. the method that under an atomic scale, dynamically observation iii-v field-effect transistor gate medium lost efficacy, it is characterised in that the method includes step in detail below:
1) the sample sample preparation of transmission electron microscope；
2) sample preparation of nanometer tungsten tipped probe；
3) sample prepared by step 1) is mounted on the copper mesh of in situ TEM (TEM), the copper mesh having carried sample is put into specimen holder in situ, then transmission electron microscope intracavity will be loaded by specimen holder in situ；
4) by step 2) gate contact of sample that the tip of nano-probe prepared is prepared with step 1), between nano-probe and copper mesh, add a steady electric field；
5) operation in situ TEM, the change of monitoring sample topography in real time and the change increasing electric current in time, and record；
6) on inefficacy microcell, carry out topotaxial elementary analysis in inefficacy microcell power spectrum, compare with the sample spectral information before not damaging, it may be judged whether lost efficacy.
Method the most according to claim 1, it is characterized in that, in step (1), sample for use in transmitted electron microscope prepares by the following method: use focused ion beam system, electromagnetic lens is utilized iii-v field-effect transistor to be cut or after attrition process ion beam focusing, keep former field-effect transistor structure cross section, make thickness more than 20 nanometers, the sample being applicable in situ TEM less than 100 nanometers.
Method the most according to claim 1, it is characterized in that, nanometer tungsten tipped probe described in step (2) is the nanometer tungsten tipped probe used in situ TEM (TEM), described nanometer tungsten tipped probe uses electrochemical method to prepare, and the tip diameter of described nanometer tungsten tipped probe is more than 5 nanometers, less than 20 nanometers.
Method the most according to claim 1, it is characterised in that the power spectrum in step (6) includes electron energy loss spectroscopy (EELS) or energy dispersion X-ray spectrum.
nullMethod the most according to claim 3，It is characterized in that，Described electrochemical method is particularly as follows: using the tungsten filament of a diameter of 0.15-0.35 millimeter as electricity anode，Using stainless steel electrode as electricity negative electrode，Electricity anode and electricity negative electrode are inserted electrolyte respectively，And the insertion depth of electricity anode is 5-10 millimeter，Described electrolyte be the molar concentration of sodium hydrate aqueous solution and sodium hydrate aqueous solution be 3-5mol/L，Then apply, on electricity anode and electricity negative electrode, the voltage that initial value is 5 volts，Electricity anode is carried out electrochemical corrosion，When the electric current flowing through electricity anode is decreased to 20 MAHs，Promote electricity anode，Promoting speed is 1 ~ 8 micro-meter per second，When the electric current flowing through electricity anode continues to be decreased to zero，The current potential reducing electricity anode the current potential making electricity anode are less than electricity negative electrode，And make electricity anode leave electrolyte，Obtain nanometer tungsten tipped probe.
Method the most according to claim 1, it is characterized in that, the copper mesh of in situ TEM (TEM) described in step (6) refers to carry the copper mesh of sample, there are three sample for use in transmitted electron microscope posts on it respectively, have the rectangle cavity of a 3-5 micron wherein in a sample column for carrying sample.
Method the most according to claim 1, it is characterized in that, described in step (4), steady electric field refers to by sample is added scan voltage, draws out the electric current figure with change in voltage, finding out electric current and suddenly increase corresponding voltage, added constant voltage is this corresponding voltage and deducts the value of 0.7 volt.
Method the most according to claim 7, it is characterised in that it is more than 1 order of magnitude of current break that described electric current increases corresponding voltage suddenly.
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| CN110954563A (en) * | 2019-12-10 | 2020-04-03 | 北京航空航天大学 | Device and method for in-situ observation of rheological behavior of semi-solid metal alloy |
| CN113506757A (en) * | 2021-06-29 | 2021-10-15 | 上海华力微电子有限公司 | Method for testing contact high-resistance position of interconnection line |
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Application publication date: 20161012 |