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CN113823555B - Method for preparing germanium film on insulator - Google Patents

Method for preparing germanium film on insulator Download PDF

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CN113823555B
CN113823555B CN202111029511.2A CN202111029511A CN113823555B CN 113823555 B CN113823555 B CN 113823555B CN 202111029511 A CN202111029511 A CN 202111029511A CN 113823555 B CN113823555 B CN 113823555B
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film
germanium
insulator
depositing
deposition method
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CN113823555A (en
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扈静
芮祥新
汪穹宇
李建恒
赵杰
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Zhejiang Lide Instrument Co ltd
Hefei Ande Keming Semiconductor Technology Co ltd
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Zhejiang Lide Instrument Co ltd
Hefei Ande Keming Semiconductor Technology Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02367—Substrates
    • H01L21/0237—Materials
    • H01L21/02422—Non-crystalline insulating materials, e.g. glass, polymers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02436—Intermediate layers between substrates and deposited layers
    • H01L21/02439—Materials
    • H01L21/02488—Insulating materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02524—Group 14 semiconducting materials
    • H01L21/02532—Silicon, silicon germanium, germanium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/76—Making of isolation regions between components
    • H01L21/762—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers
    • H01L21/7624—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers using semiconductor on insulator [SOI] technology

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Formation Of Insulating Films (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

The invention provides a method for preparing germanium film on insulator and application thereof, which comprises the steps of depositing on insulator substrate by atomic layer deposition methodThe simple substance germanium film is deposited to the required thickness by an atomic layer deposition method on the transition layer film, so that the simple substance germanium film can be simply and efficiently deposited on an insulator and can be applied to the field of semiconductors.

Description

Method for preparing germanium film on insulator
[ Field of technology ]
The invention belongs to the field of semiconductor preparation, and particularly relates to a method for preparing a germanium film on an insulator.
[ Background Art ]
With the advancement of semiconductor device technology nodes, the original channel material silicon is slowly replaced by silicon germanium or elemental germanium. Germanium has the advantage of having 3 times the electron mobility and 4 times the hole mobility of silicon, can increase the device operating speed, reduce power consumption, and can produce nFET and pFET devices by doping different elements. In contrast to other candidate materials, such as group III-V InAs, gaAs, while electron mobility is nearly 30 times that of silicon (InAs for example), hole mobility is nearly as high as that of silicon, and can only be used to fabricate nFETs, and cannot be used to fabricate high performance pFETs.
Currently, the fabrication of chips using Silicon On Insulator (SOI) as a substrate is a mainstream technology approach, namely Silicon-on-Insulator (SOI), and its structure is shown in FIG. 1. If Germanium is used instead of silicon, the substrate of the chip may be called a Germanium-on-Insulator, referred to herein as GOI or GeOI, and its structure is shown in FIG. 2, showing more excellent performance.
At present, there are three general methods for manufacturing GeOI: germanium condensation technology (Ge condensation technique), liquid phase epitaxy technology (Liquid phase epitaxy), hydrogen-implanted Smart cut TM. The hydrogen injection intelligent stripping technology gradually becomes a better scheme for manufacturing the GeOI at present, and the main steps comprise: the surface of the germanium sheet a is deposited with a silicon oxide layer (such as PECVD method) and is an insulating layer, a solid black stripe layer is shown in the figure, hydrogen ion implantation is performed, the germanium sheet is reversed, an adhesive is applied on the silicon wafer B (the silicon oxide layer exists on the surface of the silicon wafer B), the hydrogen implantation layer of the germanium sheet a is foamed/separated, and the surface of the germanium left on the GeOI sheet is polished (the flow chart is shown in fig. 3).
However, the intelligent stripping technology for hydrogen injection has obvious defects: firstly, the process is complex, and a plurality of semiconductor process equipment is needed, so that the production cost is increased; secondly, the thickness of the germanium film produced by this method is difficult to control precisely, and requires the cooperation of a polishing process, which is again only suitable for the production of substrate materials (planar structures), and during chip processing, the method is no longer suitable due to the complexity of the surface structure (3D structure).
[ Invention ]
The invention provides a method for preparing a germanium film on an insulator, which can simply and efficiently deposit an elemental germanium film on the insulator through a specific Atomic Layer Deposition (ALD) technology and realize the application of the elemental germanium film in the field of semiconductors.
The specific technical solution is as follows:
a method for preparing germanium film on insulator is characterized by that on insulator substrate first using atomic layer deposition method to deposit And depositing a simple substance germanium film to a required thickness on the transition layer film by using an atomic layer deposition method.
The transition layer film is a buffer layer, and the simple substance germanium layer is effectively deposited and does not fall off due to component buffer, stress buffer or lattice constant buffer, so that the simple substance germanium film can be applied to a complex 3D structure of a chip. A moderate buffer layer thickness, for the effectiveness of the process and the overall properties of the product, may further be preferred
Specifically, the transition layer film comprises at least one of tantalum oxide, titanium oxide, niobium oxide, germanium oxide, cerium oxide and lanthanum oxide.
Specifically, the insulator substrate is silicon oxide, silicon carbide, aluminum oxide, hafnium oxide or zirconium oxide.
Specifically, the atomic layer deposition method is to deposit metal oxide as a transition layer in an oxidizing atmosphere and then deposit a metal Ge simple substance film in a reducing atmosphere.
In one embodiment, the process of depositing elemental germanium film to a desired thickness using an atomic layer deposition process includes: and taking germanium-containing organic molecules as a precursor source, taking plasma with H 2、NH3、N2H4 or H 2/N2 mixed gas as a main body as a reducing agent, and depositing the germanium-containing organic molecules on the transition layer film at the temperature of 100-400 ℃.
In another embodiment, the process of depositing elemental germanium film to a desired thickness using an atomic layer deposition process includes: and depositing the germanium-containing organic molecules on the transition layer film at 100-400 ℃ by taking the germanium-containing organic molecules as a precursor source and taking the precursors of hydrazine, tertiary butyl hydrazine and borane dimethylamine as main bodies as reducing agents.
Specifically, the germanium-containing organic molecules include Ge (NMe 2)4、Ge(iPr2-tBu-amd)2 or Ge (iPr 2-nBu-amd)2) or a combination thereof.
The invention also provides a method for preparing the germanium film on the chip substrate, which can simply and efficiently deposit the simple substance germanium film on the insulator through a specific Atomic Layer Deposition (ALD) technology and realize the application of the simple substance germanium film in the chip manufacturing flow.
The specific technical solution is as follows:
A method for preparing germanium film on chip substrate is characterized by that on silicon or silicon dioxide substrate an insulator base is deposited by atomic layer deposition method or other method (such as physical vapor deposition or chemical vapor deposition), then on the insulator base an atomic layer deposition method is used And depositing a simple substance germanium film to a required thickness on the transition layer dielectric film by using an atomic layer deposition method.
The beneficial effects of the invention are as follows:
The invention can realize the deposition of the germanium film on the insulator, has better adhesiveness, is not easy to fall off, does not influence the overall film performance, has good film uniformity, high step coverage rate and simple process, does not need to use a special substrate, and can be suitable for the chip processing process with complex structure.
[ Description of the drawings ]
FIG. 1 is a schematic diagram of an SOI structure in which SiO 2 is an insulating layer;
FIG. 2 shows a GOI or GeOI structure;
FIG. 3 is a conventional GeOI manufacturing flow;
FIG. 4 is a graph showing the results of ALD method growth of elemental germanium films on silicon and silicon dioxide substrates;
FIG. 5 is a step flow diagram of a deposition process one performed on a silicon substrate;
FIG. 6 is a schematic diagram of the structure of the desired film according to scheme one;
FIG. 7 is a step flow diagram of a deposition process two performed on a silicon substrate;
FIG. 8 is a schematic diagram of the structure of the desired film according to scheme II;
FIG. 9 is a step flow diagram of a deposition process three performed on a silicon substrate;
FIG. 10 is a schematic diagram of the structure of the desired film according to scheme III;
FIG. 11 is a sample point and test result of a process product using an ellipsometer (film thickness above each point in angstroms, 1 angstrom = 0.1 nm; refractive index below each point, fixed refractive index at the time of measurement);
FIG. 12 is a sample point and test result of a flow Cheng Er product using an ellipsometer (film thickness above each point in angstroms, 1 angstrom = 0.1 nm; refractive index below each point, fixed refractive index as measured);
FIG. 13 shows sample points and test results of the three-product process using an ellipsometer (film thickness above each point in angstroms, 1 angstrom = 0.1 nm; refractive index below each point, fixed refractive index at the time of measurement);
FIG. 14 is a TEM section photograph of the film obtained in Process three;
FIG. 15 is a STEM section photograph of the film obtained in Process three;
FIG. 16 is an EDX surface scan photograph (showing the top-down elemental distribution of a sample) of the film obtained in Process three;
FIG. 17 is an EDX scanning element distribution and content of the film obtained in Process three;
Fig. 18 is a raman spectrum example of germanium bulk;
FIG. 19 is a view of the location of a Raman analysis sample on a 4 inch silicon wafer;
FIG. 20 is a Raman spectrum of a film obtained in the third process without heat treatment;
FIG. 21 is a Raman spectrum of a film obtained in the third process after heat treatment at 550 ℃; .
[ Detailed description ] of the invention
The present invention will be described in further detail with reference to the following specific examples, but the present invention is not limited to the following specific examples.
In the processing of chip substrates (base materials), such as Silicon wafer substrates, silicon dioxide wafer substrates, etc., it is becoming mainstream to use Silicon-on-Insulator (or SOI) as a base material to fabricate chips in order to reduce power consumption (particularly mobile devices) of the chips while eliminating a series of parasitic effects unavoidable due to bulk Silicon materials (structure as shown in fig. 1). If germanium is used instead of silicon, the substrate of the chip may be referred to herein as GOI, or GeOI (structure shown in FIG. 2).
A new method of making GeOI is provided herein that primarily utilizes atomic layer deposition techniques. The method can be used for manufacturing GeOI sheets, and can be applied to any occasion in which an elemental germanium film is attempted to be deposited on an insulator in the semiconductor manufacturing process. The method comprises depositing on an insulator substrate by atomic layer depositionAnd depositing a simple substance germanium film to a required thickness on the transition layer film by using an atomic layer deposition method. The transition layer film is a buffer layer, and the simple substance germanium layer is effectively deposited and does not fall off due to component buffer, stress buffer or lattice constant buffer, so that the simple substance germanium film can be applied to a complex 3D structure of a chip. A moderate buffer layer thickness, for the effectiveness of the process and the overall performance of the product, may further be preferred to be/>
Specifically, the transition layer film includes, but is not limited to, tantalum oxide, titanium oxide, niobium oxide, germanium oxide, cerium oxide, lanthanum oxide, and the insulator substrate includes, but is not limited to, silicon oxide, silicon carbide, aluminum oxide, hafnium oxide, or zirconium oxide.
In one embodiment, the process of depositing elemental germanium film to a desired thickness using an atomic layer deposition process includes: and taking germanium-containing organic molecules as a precursor source, taking plasma with H 2、NH3、N2H4 or H 2/N2 mixed gas as a main body as a reducing agent, and depositing the germanium-containing organic molecules on the transition layer film at the temperature of 100-400 ℃.
In another embodiment, the process of depositing elemental germanium film to a desired thickness using an atomic layer deposition process includes: and depositing the germanium-containing organic molecules on the transition layer film at 100-400 ℃ by taking the germanium-containing organic molecules as a precursor source and taking the precursors of hydrazine, tertiary butyl hydrazine and borane dimethylamine as main bodies as reducing agents.
The germanium film grown by ALD method can be directly grown on the surface of silicon wafer, but has a certain problem of poor adhesion on insulators such as silicon oxide, aluminum oxide, hafnium oxide and the like. In one embodiment, we deposit germanium films directly by ALD using silicon and silicon dioxide as substrates, respectively. Taking Ge (iPr 2 -tBu-amd) as an example of a precursor, the temperature of a source bottle is 140 ℃, the temperature of a cavity is 250 ℃, and the pulse time, the purging time, the hydrogen plasma pulse time and the purging time of the precursor are respectively as follows: 3s, 15s, 10s, deposition rate ofTotal 200 cycles, thickness approximately/>The results are shown in FIG. 4. The above results demonstrate that a germanium film with silicon as a substrate can be grown, but the germanium film with silicon dioxide as a substrate is exfoliated.
When the solution of the invention is adopted, namely before the elemental germanium is grown, the ALD method is adopted to deposit(The step of ALD depositing an excessive dielectric film in FIG. 7) other insulating films such as tantalum oxide, titanium oxide, germanium oxide, cerium oxide, etc., then growing an elemental germanium film by ALD method, and using silicon dioxide as a substrate, the elemental germanium film is not peeled off, the physical and chemical properties are consistent with those of the film directly grown on the surface of the silicon wafer, and the deposition rate is/>The film composition has a germanium atomic percentage higher than 70at.%
In another embodiment, we illustrate the invention using silicon wafer as the substrate, alumina as the insulating layer, and ALD method to grow Ge film. For convenience of explanation, we selected 3 different deposition schemes for comparison. All three deposition runs used Ge (iPr 2 -tBu-amd) as precursor, source bottle temperature 140℃and chamber temperature 250 ℃.
The process is shown in fig. 5, and the simple substance germanium film is directly deposited on the silicon surface by ALD, and the preparation method comprises the following specific steps: precursor pulse time, purge time, hydrogen plasma pulse time, purge time are respectively: 3s, 15s, 10s, deposition rate ofA total of 40 cycles. The resulting schematic structural model is shown in fig. 6.
As shown in fig. 7, the process for preparing the elemental germanium film is carried out by depositing an alumina insulator on the silicon surface by ALD, and then the elemental germanium film is deposited as follows: firstly, depositing alumina, wherein a TMA source bottle is at room temperature, the cavity temperature is 250 ℃, and the precursor pulse time, the purging time, the oxygen plasma pulse time and the purging time are respectively as follows: 0.02s,10s,1s,10s, deposition rate ofAfter the cycle is finished, depositing an elemental germanium film, wherein the pulse time, the purge time, the pulse time of hydrogen plasma and the purge time of the precursor are respectively as follows: 3s, 15s, 10s, deposition rate/>A total of 40 cycles and the resulting schematic structural model is shown in figure 8.
As shown in fig. 9, the process is that after depositing alumina insulator on the silicon surface by ALD, depositing dielectric transition film layer and depositing simple substance germanium film, the specific process is as follows: firstly, depositing aluminum oxide, wherein a TMA source bottle is at room temperature, the cavity temperature is 250 ℃, the precursor pulse time, the purging time and the oxygen plasma pulse time are respectively as follows: 0.02s,10s,1s,10s, deposition rate ofAnd (3) performing total circulation for 100 times, and after the circulation is finished, depositing a GeO2 film, wherein the precursor pulse time, the purging time and the ozone pulse time are respectively as follows: 6s,10s, deposition rate is/>Cycling 20 times in total; and finally depositing an elemental germanium film, wherein the pulse time, the purging time and the hydrogen plasma pulse time of the precursor are respectively as follows: 3s,15s,10 s, deposition rate is/>A total of 40 cycles, the resulting schematic structural model is shown in fig. 10.
After the above deposition was completed according to the first, second and third procedures, film thickness measurement was performed by ellipsometry with a corresponding model (the test results only showed the uppermost film thickness, the refractive index of the measuring chamber was fixed to the lower numerical value of the figure), and the results are shown in table 1, and the film thickness distribution is shown in fig. 11, 12 and 13.
TABLE 1
From the above results, it can be seen that the elemental germanium film of the second process has not grown successfullyThe left and right film thickness can be ignored); the simple substance germanium film is prepared in the first process and the third process, and the simple substance germanium film in the third process successfully grows on the alumina insulation film.
The film obtained in the third procedure was subjected to one-step performance analysis by Transmission Electron Microscopy (TEM), scanning tunneling microscopy (STEM) and energy spectrum (EDX), and the results are shown in fig. 14, 15, 16 and 17.
In FIG. 14, since the GeOx film is too thinNot evident at the magnification of fig. 14, the upper Al 2O3 layer is a protective layer that protects the Ge film from oxidation. It can be seen from FIG. 15 that the first deposition/>After the GeOx buffer layer, a20 nm Ge simple substance layer successfully grows on the surface of the alumina 30nm film; as can be seen from the EDX surface scans of fig. 16 and 17, it was shown that the Ge elemental substance was successfully grown on the surface of the alumina film.
From the TEM/STEM/EDX characterization results, it can be determined that procedure three successfully grows a germanium film on the 30nm Al 2O3 insulator surface using ALD.
The thin film structure obtained in the third procedure was further characterized by Raman (Raman) spectroscopy. Fig. 18 is a raman spectrum example of a germanium bulk, showing a crystalline germanium peak at 301cm -1. We performed Raman analysis samples on 4 inch silicon wafers at the points marked in FIG. 19, and it can be seen from FIGS. 20 and 21 that the as-deposited germanium film was partially crystallized and after heat treatment at 550℃for 5 hours, the 15nm germanium film was completely crystallized.
The above examples are not intended to limit the scope of the invention, nor the order of execution of the steps described, and the directions described are limited to the accompanying drawings. The present invention is obviously modified by those skilled in the art in combination with the prior common general knowledge, and also falls within the scope of protection claimed by the present invention.

Claims (5)

1. A method for preparing germanium film on insulator is characterized by that,
Depositing a transition layer film of 3-20A on an insulator substrate by an atomic layer deposition method, and depositing a simple substance germanium film to a required thickness on the transition layer film by an atomic layer deposition method; the transition layer is germanium oxide; the insulator substrate is alumina.
2. The method for producing a germanium film on an insulator according to claim 1, wherein,
The atomic layer deposition method is that firstly, metal oxide is deposited in an oxidizing atmosphere to serve as a transition layer, and then, a metal Ge simple substance film is deposited in a reducing atmosphere.
3. The method for producing a germanium film on an insulator according to claim 2, wherein,
The process for depositing the elemental germanium film to the required thickness by using the atomic layer deposition method comprises the following steps: and taking germanium-containing organic molecules as a precursor source, taking plasma with H 2 or H 2/N2 mixed gas as a main body as a reducing agent, and depositing the germanium-containing organic molecules on the transition layer film at the temperature of 100-400 ℃.
4. A method for fabricating a germanium film on an insulator according to claim 3,
The germanium-containing organic molecules include one or more of Ge (NMe 2)4、Ge(iPr2-tBu-amd)2 or Ge (iPr 2-nBu-amd)2).
5. A method for preparing germanium film on chip substrate is characterized by that,
Depositing an insulator substrate on a silicon or silicon dioxide substrate by using an atomic layer deposition method or a physical vapor deposition method or a chemical vapor deposition method, depositing a transition layer dielectric film of 3-20A on the insulator substrate by using an atomic layer deposition method, and depositing an elemental germanium film to a required thickness on the transition layer film by using an atomic layer deposition method; the transition layer film is germanium oxide; the insulator substrate is alumina.
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