CN102507875A - Method for quickly and nondestructively measuring thickness and band structure of graphene film - Google Patents
Method for quickly and nondestructively measuring thickness and band structure of graphene film Download PDFInfo
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- CN102507875A CN102507875A CN2011103511912A CN201110351191A CN102507875A CN 102507875 A CN102507875 A CN 102507875A CN 2011103511912 A CN2011103511912 A CN 2011103511912A CN 201110351191 A CN201110351191 A CN 201110351191A CN 102507875 A CN102507875 A CN 102507875A
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Abstract
The invention belongs to the technical field of integrated semiconductor circuit fabrication, and provides a method for quickly and nondestructively measuring thickness and energy gap of a graphene film. The method of the invention comprises the steps of: firstly obtaining elliptical polarization data of the film by elliptical polarization technology; and then, creating a proper theoretical model according to the structure of the measured film to analyze and fit the obtained elliptical polarization data so as to obtain the thickness and band structure of the measured graphene film. The method of the invention has the advantages of greatly simplifying the thickness test complexity of the ultrathin films and reducing the construction difficulty of other techniques, so that the method has an important application value in fabrication of large scale integrated circuits larger than 22 nanometers.
Description
Technical field
The present invention relates to a kind of method of measuring graphene film thickness and band structure; Be specifically related to a kind of quick nondestructive of after 22 nanometers, using in the large scale integrated circuit manufacturing and measure the method for graphene film band structure, belong to SIC (semiconductor integrated circuit) manufacturing technology field.
Background technology
Along with the continuous development of semiconductor technology, the continuous extension of Moore's Law and depth make the si-substrate integrated circuit device size more and more nearer apart from its physics limit.International semiconductor development course figure ITRS has planned the MOSFET material and technology in the 16 nanometer feature sizes technology, wherein the most important thing is the selection and the control of gate oxide level among the MOSFET, for example TiO
2, mix aluminium titanium dioxide, hafnia, zirconia etc., yet how to ultrathin membrane (physical thickness<10 nanometers) can't harm quick quality estimating particularly the measurement of band structure be a major issue.
Combining physical computing to set up a kind of quick nondestructive based on optical means, to measure the quality estimating way of ultrathin membrane Nano grade be one of key factor that improves lsi technology yield after 22 nanometers.
Summary of the invention
The objective of the invention is to propose to adapt to face width, quick nondestructive that measuring accuracy is high and measure the method for graphene film thickness and band structure, measure and the thickness match to solve the band structure of regulating in the energy gap process.
The quick nondestructive that the present invention proposes is measured the method for graphene film thickness and energy gap, is based on optical means and combines physical computing to set up, and concrete steps comprise:
The graphene film that needs measurement is provided;
Utilize the elliptic polarization technology to obtain the ellipsometric data of said graphene film;
Set up suitable theoretical model according to the structure of said graphene film;
On the theoretical model basis of being set up, resulting ellipsometric data is analyzed and match, obtained the band structure analysis of said graphene film.
Further, ultrathin films such as the thin graphene oxide film (FRGO) of described Graphene, GO for the several layers reduction.Described theoretical model is the Lorentz vibrator model.
The present invention is on the theoretical foundation of Density functional (DFT) analog computation; Select proper model (for example Lorentz vibrator model) for use; With the elliptically polarized light spectrometry defect level in the ultra-thin graphene film is surveyed, the method for a kind of non-destructive and the gradual change of contactless detection study graphene film band structure is provided.Non-destructive and non-contact optical are surveyed and can be broken through all process conditions restrictions at present, and can directly be integrated in the graphene film growth apparatus for example on ALD or the CVD, and then can in-situ monitoring and control energy gap size.
The present invention has simplified the complicacy that graphene film energy gap variation is in the past tested greatly, has reduced the degree of difficulty of utilizing other technical matters to implement; Relatively other technological means can significantly increase detection speed, after 22 nanometers, has significant application value in the large scale integrated circuit manufacturing.
Description of drawings
Fig. 1 is the structure of ellipse inclined to one side survey graphene film.
Fig. 2 (a) is the experiment (solid line) and the matched curve of the ellipsometric parameter of GO and FRGO film (c), and (b) (d) is the refractive index n and the extinction coefficient k of the match gained of GO and FRGO.
Fig. 3 is that (a) is the experiment and the matched curve (point) of the ellipsometric parameter of GO and FRGO film (c), and (b) (d) is the refractive index n and the extinction coefficient k of the match gained of GO and FRGO.
Fig. 4 is the variation icon of the band structure in the graphene oxide reduction process.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.The method of measurement graphene film energy gap gradual change proposed by the invention goes for the measurement of graphene film electronics energy gaps such as FRGO, GO, and below what narrated is that the detection that changes with the energy gap of GO film before and after being reduced is the technological process of embodiment.
At first, growth one deck SiO on silicon substrate 101
2 Film 102 is transferred to SiO with GO or FRGO again
2On, film former 103, as shown in Figure 1.
Next, utilize the elliptic polarization technology to obtain the ellipsometric data of GO and FRGO film, the spectrum of GO and FRGO film is shown in the solid line part of Fig. 2 (a) in (c).
Next, the model that theorizes, we use classical Lorentz vibrator model to analyze here.Can be expressed as with the described complex permittivity of Lorentz oscillator:
This is the Lorentz model.In the formula
ε ∞ Be the high-frequency dielectric constant, the dielectric constant values when corresponding to extreme ultraviolet and being high-energy, ε
1Real part, ε for complex permittivity
2Imaginary part for complex permittivity.
A i Be the weight factor of vibration,
C i Be central energy,
ν i Be ratio of damping, E is a photon energy,
A i ,
C i ,
ν i Be unknown quantity, unit all is eV.Weight factor A wherein
iValue representation oscillator i shared proportion in whole oscillation system, central energy
C i In different systems, can represent different implications.Can draw the refractive index n and the extinction coefficient k of material by complex permittivity:
Next, on the Lorentz model basis of being set up, resulting ellipsometric data is analyzed and match.Use 2-5 rank oscillator so that match variance and measured value depart from minimum; Fitting result is as shown in Figure 3; Figure line (a), (c) be corresponding GO and FRGO respectively, and solid line is represented the ellipse inclined to one side value Δ and the Ψ of experiment measuring among the figure, and solid dot is according to Lorentz vibrator model match gained.It is fairly good to find out that match value and experiment value meet, and resulting electronic defects level parameters are as shown in table 1 after the match.
Because not isoplastic coverage, the energy gap that causes GO is at 1.8 eV, and 2.1 eV are among 2.8 eV, as shown in Figure 4.By in the Lorentz model to A
iDefinition, can think that it has represented the probability of the electronic state of the different coverages of different groups among the GO.From last table we can to find out that the A4 that represents the electronic state probability is accounting in sample leading, be illustrated in the sample GO film, the coverage that 1.8 eV are corresponding is most probable, the coverage that 2.8 eV are corresponding is also occupied certain weight.A3 remains on the level of an a small amount of, shows that the pairing coverage of 2.1 eV exists hardly.For FRGO, remove outside plasma concussion energy level 4.7 eV of exciton concussion characteristic energy level 4.6 eV and π key, 0.02 eV is as an oscillator that weight is very big, represented the energy of intraband transition of the FRGO of match acquisition.
As stated, under the situation that does not depart from spirit and scope of the invention, can also constitute many very embodiment of big difference that have.Should be appreciated that except like enclosed claim limited, the invention is not restricted at the instantiation described in the instructions.
Table 1
| GO | FRGO | |
| d (nm) | 9.08±0.049 | 4.10±0.027 |
| ε ∞ | 3.2217±0.0017 | 2.903±0.069 |
| A 1 | 2.0215 | 2.5334±0.094 |
| C 1(eV) | 2.8032±0.133 | 4.6002±0.032 |
| A 2 | 1.4385±0.0051 | 2.697±0.061 |
| C 2(eV) | 5.0031±0.0762 | 0.02±0.005 |
| A 3 | 0.4366±0.0037 | 0.0955±0.004 |
| C 3(eV) | 2.1493±0.064 | 4.7±0.047 |
| A 4 | 6.8171±0.2475 | |
| C 4(eV) | 1.8325±0.052 |
Claims (3)
1. method of measuring graphene film thickness and band structure is characterized in that concrete steps are:
(1) the ultra-thin graphene film that needs measurement is provided;
(2) utilize the elliptic polarization technology to obtain the ellipsometric data of said graphene film;
(3) set up suitable theoretical model according to the structure of said graphene film;
(4) on the theoretical model basis of being set up, resulting ellipsometric data is analyzed and match, obtained the thickness and the band structure of said graphene film.
2. the method for measurement graphene film thickness according to claim 1 and energy gap is characterized in that, described ultrathin film is the graphene oxide film of several layers reduction.
3. the method for measurement graphene film thickness according to claim 1 and energy gap is characterized in that, described theoretical model is the Lorentz vibrator model; Be expressed as with the described complex permittivity of Lorentz vibrator model:
In the formula
ε ∞ Be the high-frequency dielectric constant, the dielectric constant values when corresponding to extreme ultraviolet and being high-energy, ε
1Real part, ε for complex permittivity
2Imaginary part for complex permittivity;
A i Be the weight factor of vibration,
C i Be central energy,
ν i Be ratio of damping, E is a photon energy,
A i ,
C i ,
ν i Be unknown quantity, unit all is Ev; Weight factor A wherein
iValue representation oscillator i shared proportion in whole oscillation system; Obtain the complex index of refraction of material by complex permittivity:
。
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Cited By (6)
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|---|---|---|---|---|
| CN103115927A (en) * | 2013-02-04 | 2013-05-22 | 中国人民解放军国防科学技术大学 | Nondestructive testing method for optical glass polishing sub-surface damages |
| CN103528961A (en) * | 2013-10-24 | 2014-01-22 | 南开大学 | Method for measuring number of graphene layers on transparent substrate |
| CN104502282B (en) * | 2015-01-21 | 2017-03-01 | 哈尔滨工业大学 | Consider the polarization characteristic numerical computation method of photon crystal surface oxide-film distribution |
| CN110687052A (en) * | 2019-10-24 | 2020-01-14 | 中国科学技术大学 | Method and system for measuring optical band gap |
| CN110824137A (en) * | 2019-10-10 | 2020-02-21 | 中国建筑材料科学研究总院有限公司 | Method and device for predicting crystallization order of silver film in low-emissivity glass on substrate |
| WO2020195670A1 (en) * | 2019-03-25 | 2020-10-01 | 東京エレクトロン株式会社 | Method for detecting abnormal growth of graphene, measurement method, and film formation system |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103115927A (en) * | 2013-02-04 | 2013-05-22 | 中国人民解放军国防科学技术大学 | Nondestructive testing method for optical glass polishing sub-surface damages |
| CN103528961A (en) * | 2013-10-24 | 2014-01-22 | 南开大学 | Method for measuring number of graphene layers on transparent substrate |
| CN103528961B (en) * | 2013-10-24 | 2015-11-25 | 南开大学 | Graphene number of plies measuring method in a kind of transparent substrates |
| CN104502282B (en) * | 2015-01-21 | 2017-03-01 | 哈尔滨工业大学 | Consider the polarization characteristic numerical computation method of photon crystal surface oxide-film distribution |
| WO2020195670A1 (en) * | 2019-03-25 | 2020-10-01 | 東京エレクトロン株式会社 | Method for detecting abnormal growth of graphene, measurement method, and film formation system |
| JPWO2020195670A1 (en) * | 2019-03-25 | 2020-10-01 | ||
| JP7134336B2 (en) | 2019-03-25 | 2022-09-09 | 東京エレクトロン株式会社 | METHOD AND MEASUREMENT DEVICE FOR DETECTING ANORMAL GROWTH OF GRAPHEN, AND FILM FORMING SYSTEM |
| CN110824137A (en) * | 2019-10-10 | 2020-02-21 | 中国建筑材料科学研究总院有限公司 | Method and device for predicting crystallization order of silver film in low-emissivity glass on substrate |
| CN110824137B (en) * | 2019-10-10 | 2022-03-11 | 中国建筑材料科学研究总院有限公司 | Method and device for predicting crystallization order of silver film in low-emissivity glass on substrate |
| CN110687052A (en) * | 2019-10-24 | 2020-01-14 | 中国科学技术大学 | Method and system for measuring optical band gap |
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Application publication date: 20120620 |