CN102128819A - Method for measuring elastic modulus of hydrogenated silicon film - Google Patents
Method for measuring elastic modulus of hydrogenated silicon film Download PDFInfo
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- CN102128819A CN102128819A CN 201010569940 CN201010569940A CN102128819A CN 102128819 A CN102128819 A CN 102128819A CN 201010569940 CN201010569940 CN 201010569940 CN 201010569940 A CN201010569940 A CN 201010569940A CN 102128819 A CN102128819 A CN 102128819A
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- elastic modulus
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Abstract
The invention relates to a method for judging the elastic modulus of a hydrogenated silicon film, which is characterized by comprising the following steps of: performing micro-structure analysis on the prepared hydrogenated silicon film by using a Raman spectrum; expressing a film crystalline state component system and an amorphous interface component system by using a crystalline state ratio; and judging a value of the elastic modulus according to the one-to-one correspondence between the crystalline state ratio and the elastic modulus. In the method, the operation is simple and convenient, the film is not damaged, and the internal stress of the film is not influenced. Therefore, the method has the great application prospect in hydrogenated silicon film devices.
Description
Technical field
The present invention relates to a kind of measuring method of hydrogenated silicon film by utilizing elastic modulus, a kind of measuring method of harmless hydrogenated silicon film by utilizing elastic modulus is provided or rather, Raman spectrum with the general instrument test of laser raman hydrogenated silicon film by utilizing, calculate the elastic modulus of film by Raman spectrum, and to film without any damage, belong to the semiconductor film material field.
Background technology
The silicon thin film material is widely used in MEMS (micro electro mechanical system), and (microelectromechanical system, MEMS), classification has multiple, (is called for short crystalline state than (crystalline volume fraction uses according to the shared percent by volume of crystalline state composition in the film
X cExpression) can be divided into amorphous silicon (amorphous silicon successively, a-Si:H), microcrystal silicon (microcrystalline silicon, μ c-Si:H), nano-silicon (nanocrystalline silicon, nc-Si:H), polysilicon (polycrystalline, silicon, pc-Si:H) and monocrystalline silicon thin film (crystalline silicon, c-Si), according to the hydrogen atom content in the film, be accustomed to again amorphous silicon, microcrystalline silicon film and Nano thin film are referred to as hydrogenated silicon film by utilizing; In recent years, adopt the hydrogenated silicon film by utilizing for preparing with the compatible mutually enhancing chemical vapor deposition method (PECVD) of semiconductor technology, because unique advantages in researchs such as heterodiode, solar cell, thin film transistor (TFT), single-electronic transistor, has caused the great interest of people.Discover the piezoresistive effect (piezoresistance effect) of Nano thin film in early days, pressure sensitivity coefficient ratio monocrystalline silicon thin film to exceed 6～8 times, this provides condition for micro-nano electron devices such as research and development high-sensitivity miniature ultra micro pressure pressure sensor and displacement transducers, therefore studies its elastic modulus to the exploitation of thin-film device practicability highly significant.
In micro-nano system design and thin-film device industrialization, the semiconductive thin film elastic modulus is one of most important mechanical characteristics, the elastic modulus of film
EBe the physical quantity that characterizes adhesion power between atom, determining the structural response characteristic of device, simultaneously, accurately measure the elastic constant of material, all have engineering and theory significance for the interaction and the phase transformation of atom between research material.
The method of measuring semiconductor thin flexible film modulus commonly used is the nano impress method at present, elastic modulus is measured [Oliver WC, Pharr GM. An improved technique for determining hardness and elastic-modulus using load and displacement sensing indentation experiments. with the Oliver-Pharr method
J. Mater. Res., 1992,7 (6): 1564-1583], but the shortcoming of this method maximum is that film must have certain homogeneous thickness, otherwise can't determine the power that is made of pressing; Power is excessive, and needle point will crush film, and what test result reflected is the information of substrate, rather than the mechanical characteristic of film, causes erroneous judgement; Equally, the added power of pressing is too small, can not satisfy the requirement of elastic deformation, utilize the Elastic Contact theoretical error bigger, test result is inaccurate, therefore utilizes the elastic modulus of nano-hardness tester test hydrogenated silicon film by utilizing, and significant limitation is arranged, especially for the hydrogenated silicon film by utilizing of nanometer scale thickness, it is extremely inconvenient to operate.
Another big defective of the elastic modulus of nano impress method test hydrogenated silicon film by utilizing is to carry out destructive testing to small sample, need be to the film load mould; And for the hydrogenated silicon film by utilizing device, more be to carry out the original position non-destructive testing to film, after to film destruction, the influence of film internal stress can't be investigated, hydrogenated silicon film by utilizing by PECVD at low temperatures deposit form, stress between film and the film has directly influenced the physics of structure, performances such as Mechanics of Machinery.
Based on above shortcoming, the invention provides a kind of method of utilizing Raman scattering to compose to differentiate the hydrogenated silicon film by utilizing elastic modulus, the method is easy and simple to handle, the accuracy height, more crucial is to film itself without any destruction, can carry out the monitoring of in-situ test and membrane stress etc.
Summary of the invention
Based on the shortcoming based on nano-hardness tester test hydrogenated silicon film by utilizing elastic modulus recited above, the object of the present invention is to provide a kind of measuring method of hydrogenated silicon film by utilizing elastic modulus.
The present invention adopts the Raman spectrum of prepared hydrogenated silicon film by utilizing, simulates film crystalline state number percent by Raman spectrum, recently differentiates elastic modulus by the crystalline state percentage of film again.
Measurement and analysis for microstructure, Raman spectrum is strong instrument, especially in silicon nanophase (or amorphous phase), the quantitative change of structure preface has provided the multiplicity of atomic structure environment intuitively, and Raman spectrum provides deeper performance for disclosing this multiplicity.
As shown in Figure 1 be the Raman spectrum of the amorphous silicon membrane on monocrystalline substrate and the glass substrate, because phonon is not deferred to quasi momentum conservation rule in amorphous material, cause the shape at peak to broaden, phonon with corresponding wave vector can not be propagated in whole material, no longer be the phonon in original crystalline material, be called class optical mode and class acoustic mode, promptly class TO mould (TO-like mode) peak position is positioned at 475 ± 10cm
-1, class LO mould (LO-like mode) peak position is positioned at 380 ± 20 cm
-1, class LA mould (LA-like mode) peak position is positioned at 300 ± 10 cm
-1, class TA mould (TA-like mode) peak position is positioned at 150 ± 5 cm
-1General class LO mould is difficult to occur, and could show that class LO composes the peak, is illustrated in figure 2 as the Raman spectrum of microcrystalline silicon film after only reaching certain crystallization degree.
Nano thin film is made up of crystalline component and amorphous interface composition two parts, crystalline component is made up of atom in the crystal grain, the amorphous interface is made up of all atoms in the amorphous interface that is in each intergranule, and the class TO mould main peak of crystalline component is positioned at 520cm in the Raman spectrum
-1Near class TO mould main peak and the amorphous interface composition is positioned at 480cm
-1Near exist simultaneously, and mutual superposition and present asymmetric shape utilizes the intensity at these two peaks to estimate the volume ratio that crystalline component is occupied in the film in film, i.e. the crystalline state ratio
X c:
With
The center that is respectively is at 520 and 480 cm
-1The integrated intensity of phonon band,
Be monocrystalline silicon and the long-pending ratio of amorphous silicon integration raman scattering cross section,
Can be expressed as
In the formula
DBe average grain size, unit is nm
In the formula
BBe constant, for the intrinsic film,
BGet 2.0cm
-1Nm
2, the hydrogenated silicon film by utilizing of boron doping and phosphorus doping
BGet 2.24 cm respectively
-1Nm
2With 2.16 cm
-1Nm
2,
Directly from Raman spectrum, measure, for class TO peak position and body bill of materials crystal silicon single order characteristic peak are positioned at 520 cm
-1Deviation, utilize formula (1 ~ 3) can calculate the crystalline state ratio of prepared hydrogenated silicon film by utilizing.
The differentiation figure of the hydrogenated silicon film by utilizing elastic modulus on glass and the monocrystalline substrate and crystalline state ratio as shown in Figure 4, with Raman spectrum prepared hydrogenated silicon film by utilizing has been carried out Micro-Structure Analysis, recently characterize film crystalline component and amorphous interface composition system with crystalline state, concern one to one than with elastic modulus by crystalline state, can differentiate elastic mould value.
Description of drawings
What Fig. 1 provided is the Raman spectrum of amorphous silicon membrane;
What Fig. 2 provided is the Raman spectrum of microcrystalline silicon film;
What Fig. 3 provided is the Raman spectrum of Nano thin film;
Fig. 4 is the differentiation figure of hydrogenated silicon film by utilizing elastic modulus and crystalline state ratio on glass and the monocrystalline substrate.
Embodiment
Further specify substantive distinguishing features of the present invention and obvious improvement below by concrete enforcement, but the present invention only only limits to described embodiment by no means.
Concrete implementation step is as follows:
1. hydrogenated silicon film by utilizing prepares in capacitance coupling type PECVD system, and used rf frequency is 13.56MHz, and polar plate spacing is 30mm, and the base vacuum degree reaches 1 * 10
-4Pa, the reacting gas that uses be silane (95% the H of highly diluted
2With 5% SiH
4) and high-purity hydrogen (H
2) (99.9999%), impurity gas is phosphine (PH
3) or diborane (B
2H
6) concentration all is 0.5%, all the other 99.5% are H
2
Respectively with glass and monocrystalline silicon as substrate, all substrates all carry out the chemical cleaning of standard, are followed successively by triclene (under 80 ℃, 5min), acetone (under the room temperature, 5 min), the propyl alcohol that boils (5min), rinsing in deionized water then, and air-dry in nitrogen.Before cleaning, monocrystalline silicon is the scattering of avoiding rough surface to cause, and it is carried out twin polishing, for eliminating the damage that polishing causes, corrode 2min in the sulfuric acid under the monocrystalline substrate room temperature after the mechanical buffing after the hydrogen peroxide dilution, in 10% hydrofluorite, soak 10s again, remove oxide layer; Use the propyl alcohol rinsing at last, and in nitrogen, dry up.
3. prepare respectively intrinsic hydrogenated silicon film by utilizing, boron-doping hydrogenated silicon film by utilizing and mix the hydrogenated silicon film by utilizing of phosphorus.Be illustrated in figure 1 as the Raman spectrum of the amorphous silicon membrane on monocrystalline substrate and the glass substrate, Fig. 2 is the Raman spectrum of microcrystalline silicon film, and Fig. 3 is the Raman spectrum of Nano thin film, and the class TO mould main peak of crystalline component is positioned at 520cm in the Raman spectrum
-1Near class TO mould main peak and the amorphous interface composition is positioned at 480cm
-1Near exist simultaneously, and mutual superposition and present asymmetric shape utilizes the intensity at these two peaks to estimate the volume ratio that crystalline component is occupied in the hydrogenated silicon film by utilizing in film, i.e. the crystalline state ratio
X c
4. the crystalline state ratio that simulates according to Raman spectrum
X cBe worth, just can differentiate the elastic modulus of hydrogenated silicon film by utilizing, as shown in Figure 4, be prepared in the hydrogenated silicon film by utilizing on the glass substrate owing to there is amorphous transition buffer layer, elastic modulus is less than the hydrogenated silicon film by utilizing that is prepared in accordingly on the monocrystalline substrate; Because the mixing of phosphorus, grain refinement in the film, the degree of order improves, and the crystalline state of film is than generally more than 40%, the mixing of boron, the crystalline state ratio reduces, and generally is lower than 40%; Find simultaneously mixing phosphorus, the hydrogenated silicon film by utilizing of the boron-doping of originally seeking peace, respectively about the crystalline state ratio is 45%, 30% and 15%, the elastic modulus minimum; Corresponding different crystalline state ratios
X c, elastic modulus is corresponding one by one between 50 to 130GPa, therefore the invention provides a kind of method of discrimination of hydrogenated silicon film by utilizing elastic modulus, the inventive method is easy and simple to handle, to film without any destruction.
Claims (3)
1. the measuring method of a hydrogenated silicon film by utilizing elastic modulus, it is characterized in that: simulate hydrogenated silicon film by utilizing crystalline state ratio by Raman spectrum, utilize the crystalline state of hydrogenated silicon film by utilizing to concern one to one than with elastic modulus, the crystalline state that calculates hydrogenated silicon film by utilizing is than the elastic modulus that just can obtain hydrogenated silicon film by utilizing.
2. the measuring method of a kind of hydrogenated silicon film by utilizing elastic modulus as claimed in claim 1, it is characterized in that: the crystalline state of described hydrogenated silicon film by utilizing than and elastic modulus concerns one to one is the elastic modulus of measuring the hydrogenated silicon film by utilizing of different crystalline state ratios by the nano impress method, obtain different crystalline state than with the relation curve of elastic modulus.
3. the measuring method of a kind of hydrogenated silicon film by utilizing elastic modulus as claimed in claim 1 or 2 is characterized in that: the crystalline state ratio of described hydrogenated silicon film by utilizing
,
With
The center that is respectively is at 520 and 480 cm
-1The integrated intensity of phonon band,
Be monocrystalline silicon and the long-pending ratio of amorphous silicon integration raman scattering cross section,
Be expressed as
,
DBe average grain size, unit is nm,
,
BBe constant, for the intrinsic film,
BGet 2.0cm
-1Nm
2, the hydrogenated silicon film by utilizing of boron doping and phosphorus doping
BGet 2.24 cm respectively
-1Nm
2With 2.16 cm
-1Nm
2,
Directly from Raman spectrum, measure, for class TO peak position and body bill of materials crystal silicon single order characteristic peak are positioned at 520 cm
-1Deviation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323444A (en) * | 2013-05-27 | 2013-09-25 | 江苏大学 | Method for discriminating disorder degree of polysilicon film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101246931A (en) * | 2007-02-14 | 2008-08-20 | 北京行者多媒体科技有限公司 | trace amount of boron doped intrinsic silicon hydride thin film |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101246931A (en) * | 2007-02-14 | 2008-08-20 | 北京行者多媒体科技有限公司 | trace amount of boron doped intrinsic silicon hydride thin film |
Non-Patent Citations (1)
| Title |
|---|
| 《物理学报》 20070831 王权等 氢化硅薄膜介观力学行为及其与微结构内禀关联特性 4835-4838页 1-3 第56卷, 第8期 2 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323444A (en) * | 2013-05-27 | 2013-09-25 | 江苏大学 | Method for discriminating disorder degree of polysilicon film |
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Application publication date: 20110720 |