CN105304736A - Method of fabricating Ge/Si quantum dots by magnetron sputtering in combination with rapid annealing technology - Google Patents
Method of fabricating Ge/Si quantum dots by magnetron sputtering in combination with rapid annealing technology Download PDFInfo
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- CN105304736A CN105304736A CN201510421707.4A CN201510421707A CN105304736A CN 105304736 A CN105304736 A CN 105304736A CN 201510421707 A CN201510421707 A CN 201510421707A CN 105304736 A CN105304736 A CN 105304736A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 50
- 238000000137 annealing Methods 0.000 title claims abstract description 18
- 238000001755 magnetron sputter deposition Methods 0.000 title claims abstract description 17
- 238000005516 engineering process Methods 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 42
- 238000004544 sputter deposition Methods 0.000 claims abstract description 37
- 239000000758 substrate Substances 0.000 claims description 23
- 238000000151 deposition Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
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- 230000000149 penetrating effect Effects 0.000 claims 3
- 239000013077 target material Substances 0.000 claims 3
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- 238000004140 cleaning Methods 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 claims 1
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- 238000005477 sputtering target Methods 0.000 claims 1
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- 230000008901 benefit Effects 0.000 abstract description 3
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- 230000007547 defect Effects 0.000 abstract 1
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- 229910021641 deionized water Inorganic materials 0.000 description 10
- 230000008021 deposition Effects 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0352—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions
- H01L31/035209—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures
- H01L31/035218—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures the quantum structure being quantum dots
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic System
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a method of growing Ge quantum dots by magnetron sputtering in combination with rapid annealing technology, which belongs to the technical field of fabrication of semiconductor quantum material. Based on ultrahigh vacuum magnetron sputtering technology, an Ar gas serves as a working gas, when the vacuum degree is smaller than or equal to 2.0*10<-4>Pa, the radio frequency sputtering technology is firstly adopted to grow an intrinsic Si buffer layer with a certain thickness in a high temperature condition, the DC sputtering technology is then adopted to grow a thin Ge atomic layer in conditions of low temperature, low power, low sputtering pressure and the like, and finally, a rapid annealing furnace is used to carry out rapid annealing processing on the Ge atomic thin layer to acquire Ge/Si quantum dots. The method solves defects that quantum dot growth controllability is poor and distribution is uneven at a large sputtering rate, and overcomes shortcomings that in the low-growth rate (MBE, CVD) technology, the growth is slow, and the procedures are relatively complicated when high-density and small-sized quantum dots are fabricated. The acquired quantum dots have advantages of high density, small size, even distribution, good controllability and the like, and the equipment is simple, and the use cost and the maintenance cost are low. The quantum dot fabrication method is simple, high-efficiency, high in finished dot quality and prone to industrialization promotion.
Description
Technical field
The present invention relates to the preparation method of semiconductor quantum material, particularly adopt magnetron sputtering technique, short annealing technology to prepare the method for Ge/Si quantum dot.
Background technology
Semiconductor Ge quantum dot due to have many uniquenesses character (three-dimensional restriction effect, Coulomb blockade effect, phonon bottleneck effect, to vertical incidence photoresponse, can directly and silicon-based electronic circuits integrated) and have huge application potential at photoelectron and field of microelectronic devices, become one of focus of current academic research.
From the angle of quantum dot infrared detector, in order to realize the strong response to vertical incidence light, matter of utmost importance how to obtain the enough little quantum dot of volume, enable the restriction energy level in its athwartship plane control or reduce to 1 to 2 energy levels, this requires that the transverse width of quantum dot is less than or equal to 10nm theoretically; In addition, high-quality can detector must have higher absorption efficiency, this just requires that active area has higher quantum dot density, such as: be obtain the absorptivity suitable with quantum well detector, the carrier density of every layer should be: (1-10) × 10
11cm
-2if the carrier number in each quantum dot is 2, and so quantum dot density should be: (1-5) × 10
11cm
-2, for reaching this density, corresponding quantum dot latter dimensional requirement controls within 30nm; Finally, absorptivity occur saturated before, the absorptivity of detector increases with the increase of the quantum dot number of plies, thus efficiently, quickly grow multi-layer quantum point be also direction very important in element manufacturing.In a word, in order to meet device performance requirements, except improving the order of quantum space of points arrangement, reducing size, improving density, growing efficiently and repeat the importance that active layer is researcher Gonna breakthrough.
The preparation of quantum dot has multiple means, comprise the technology such as molecular beam epitaxy (MBE), chemical vapor deposition (CVD), physical vapor deposition (PVD) and atomic layer epitaxy (ALE), in recent years, in order to overcome too low, the oversize difficult problem of density, many researchers have carried out a large amount of trials and have achieved breakthrough progress, such as: first make figure on a si substrate, then carry out Ge deposition; Utilize super thin oxide layer design window, deposition Ge forms quantum dot; Utilize molecular beam epitaxial device, by depositing appropriate B atom or C atom, induction preparation Ge quantum dot.Particularly induce into method a little by foreign atom, lateral dimension is less than 10nm, is highly less than 1nm, and density is up to 10
11cm
-2ge quantum dot aobviously have report.The method that the routine more than introduced prepares Ge quantum dot is generally low deposition rate (speed is 0.001-0.004nm/s) technology, growth rate is slow, meanwhile, for realizing high density, small size, have to pass through again relative complex or meticulous modification or impurity induced process.A kind ofly have that equipment is simple, operation and maintenance cost is low so find or explore, growing method simple and fast, become point mass quantum dot preparation method that is high, that be easy to the advantages such as Industry Promotion to be urgent need to solve the problem in this field.
Summary of the invention
Adopting low deposition rate to prepare small size, high density Ge/Si quantum dot speed is slow, process is complicated, cost of equipment maintenance is high deficiency by substrate modification or impurity induced to overcome, the invention provides a kind of method utilizing magnetron sputtering technique to carry out the research of Ge/Si Quantum Dots Growth.The method not only cost of equipment maintenance is low, simple to operate and can grow and prepare the high-quality quantum dot that density is high, size is little, uniformity is good efficient quick (sputter deposition rate is 0.18nm/s).
The technical solution adopted for the present invention to solve the technical problems is: adopt FJL560
type superhigh vacuum magnetron sputtering instrument is growth apparatus, with the low-doped Si(100 of N-shaped) single-sided polishing crystal is for substrate, and substrate thickness is 0.50mm, and resistivity is 1-3 Ω .cm.Standard Shiraki method is used to clean to substrate, then in HF acid solution rinsing to remove the natural oxidizing layer of substrate surface, complete the H passivation to substrate surface simultaneously, after drying up with high pure nitrogen, substrate is put into rapidly the growth that magnetron sputtering vacuum chamber carries out Ge point.
Before deposited on substrates Ge, first evacuation process is carried out to magnetron sputtering chamber, treat that base vacuum reaches 2.0 × 10
-4heat Si substrate during Pa, temperature arrives 800
obe incubated 600s during C and carry out degassed process, in order to reduce surface state impact, reducing surface roughness simultaneously, reducing blemish, first underlayer temperature being reduced to 700
oc, then grows the Si resilient coating of 50nm, to resilient coating insulation 1800s, its percent crystallization in massecuite is maximized.Reduce substrate temperature subsequently to 600
oc is incubated 300s, deposits the Ge atom film of 3.4nm thickness after temperature stabilization, and Temperature fall obtains initial sample, then initial sample is put into the short annealing process acquisition quantum dot final sample that RTP-1000D4 type quick anneal oven carries out suitable temperature.The quantum dot surface pattern of sample adopts SPA-400SPM type atomic force microscope (AFM) to characterize, and it is carry out on the burnt micro-Raman spectroscopy of invia copolymerization that Raman analyzes.All tests all at room temperature complete.
With the common MBE preparing quantum dot low-dimensional materials, CVD (deposition rate is 0.001-0.004nm/s) compares, magnetron sputtering apparatus (deposition rate is 0.1-0.8nm/s) has higher deposition rate, the advantage of its Ultra-High Efficiency obtains accreditation in coating technique field, achieve Industry Promotion, but too high deposition rate is preparing in quanta point material the difficult problem existing and can not ignore, sufficient migration has been had insufficient time at deposition process Atom, if improve underlayer temperature obtain system capacity by it and then cross over dynamics confinement barrier, Ge-Si can be aggravated so again mix mutually, the large-sized often alloy island obtained.For taking into account efficiency and effect, the present invention adopts low sputtering power (for 35w), low sputtering pressure (for 0.3pa), low Ar throughput (for 5sccm) to obtain the growth course that relatively low deposition rate (for 0.18nm/s) carrys out " simulation " MBE and CVD, for the Ge-Si reduced in growth course mixes mutually, take into account the percent crystallization in massecuite of material, underlayer temperature during deposition Ge is set to 600 simultaneously
oc.In addition, for obtaining high density, undersized Ge quantum dot, need raising annealing temperature to allow more Ge atom carry out surface migration on the one hand and enter Ge island, meet in transition process simultaneously and form new core, the maturing process that annealing time suppresses Ge island will be controlled on the other hand accurately, the present invention is by the trial of different annealing time and annealing temperature, and the final argument of acquisition is 700
oc, 600s.
The invention has the beneficial effects as follows, equipment operating is simple, be easy to safeguard, the preparation growth efficient quick of quantum dot, becoming point mass, high (density is up to 1.02 × 10
11cm
-2, transverse width is contracted to 22nm, longitudinal height reduction is to 5nm), this provides possibility scheme for growth multi-layer quantum point fast realizes Industry Promotion.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the integrated artistic flow process adopting magnetron sputtering method to prepare high density, small size Ge/Si quantum dot;
Fig. 2 is the AFM testing result characterizing quantum dot sample two-dimensional appearance;
Fig. 3 is the AFM testing result characterizing quantum dot sample three-dimensional appearance;
Fig. 4 is the statistic histogram of quantum dot sample diameter and height;
Fig. 5 is for characterizing the crystalline Raman spectrogram of quantum dot.
Embodiment
In Fig. 1, the operating process of embodiment A is as follows:
1. with analyzing pure acetone at room temperature ultrasonic 5min, deionized water rinsing.This step repeats 3 times;
2. with absolute ethyl alcohol at room temperature ultrasonic 5min, deionized water rinsing.This step repeats 3 times;
3. first dense H
2sO
4(98%): H
2o
23-5min is boiled, deionized water rinsing 2-3 time, rear HF (10%): H in the mixed solution of=2:1
2the mixed solution of O=1:10 soaks 30s, deionized water rinsing 2-3 time;
4. first dense HNO
3boil 3min, deionized water rinsing 2-3 time, rear HF (10%): H
2the mixed solution of O=1:10 soaks 30s, deionized water rinsing 2-3 time.This step repeats 2 times;
5. first dense HNO
3: H
2o
2: H
2the mixed solution of O=1:1:4 boils 5min, deionized water rinsing 2-3 time, rear HF (10%): H
2the mixed solution of O=1:10 soaks 30s, deionized water rinsing 2-3 time;
6. use HCL:H
2add and H after the mixed solution of O=3:1 boils
2the isopyknic H of O
2o
2transparent to solution, deionized water rinsing 2-3 time;
7. with HF (10%): H
2the mixed solution rinsing 30-60s of O=1:40, deionized water rinsing 2-3 time;
8. after drying up with nitrogen, be placed in sample carrier, send into magnetron sputtering apparatus vacuum chamber.
In Fig. 1, the operation scheme of Embodiment B is as follows:
1. magnetron sputtering chamber vacuum degree is evacuated to 2 × 10
-4pa;
2. pair substrate is first heated to 800
oc is incubated 600s, rear Temperature fall to 700
oc is incubated 300s;
3. pass into the Ar gas that purity is 99.999% in sputtering chamber, flow is 10sccm, and start Si target radio frequency sputtering device, sputtering pressure is adjusted to 3-5Pa, and sputtering power is set to 50-60w, carries out pre-sputtering 600s;
4. regulate operating air pressure to 0.3Pa, sputtering power is 50w, sputtering 700s, to sample insulation 1800s;
5. reduce underlayer temperature to 600
oc, insulation 300s;
6. start Ge target DC sputtering device, sputtering pressure is adjusted to 3-5Pa, and sputtering power is set to 50-60w, carries out pre-sputtering 600s;
7. regulate operating air pressure to 0.3Pa, sputtering power is 35w, sputtering 16s, Temperature fall.
In Fig. 1, the execution details of Embodiment C is as follows:
1. pass into N in quick anneal oven
20Mpa is reached to air pressure;
2. open furnace chamber, put into sample, first vacuumize, after pass into N
2;
3. heating curve is set, is heated to 700
oc, annealing time is 600s;
4. water-cooled cooling, takes out sample after shutdown.
In Fig. 1, embodiment D is sample characterization conventional method.
Fig. 2 provides the AFM two-dimensional appearance figure of quantum dot sample, and through statistics, density reaches 1.02 × 10
11cm
-2.
Fig. 3, Fig. 4 show the fluctuation distribution of the concrete three-dimensional appearance of quantum dot and transverse direction, longitudinal size, and easily find out from statistic histogram, the transverse width of quantum dot is about 22nm, and is highly longitudinally about 5nm, depth-width ratio is close to 1:4.
Fig. 5 is the Raman spectrogram of quantum dot sample, is not difficult to find out from figure, frequency displacement 520cm
-2there is obvious peak position in place, is lateral optical (TO) peak of Si, the crystallinity that the strong and narrower halfwidth display Si substrate in higher peak is good.Meanwhile, at 300cm
-2near also there is the crystalline state peak of Ge, the measuring accuracy of the peak position of comprehensive frequency displacement, the thickness of Ge film and Raman (is 1cm
-1), in quantum dot sample, Ge component also obtain good crystallinity.On the other hand, at frequency displacement 400cm
-1place does not find peak crystallization, and do not occur in interpret sample that obvious Si-Ge mixes mutually, this result achieves suppression slaking mentioned above, avoids occurring the object on large scale alloy island.
Claims (10)
1.
a kind ofmagnetron sputtering associating short annealing technology prepares the method for Ge/Si quantum dot, the method with superhigh vacuum magnetron sputtering instrument for growth apparatus, purity be 99.999% Ar gas be working gas, purity be 99.999% high-purity intrinsic Si and intrinsic Ge be sputtering target material, it is characterized in that adopting single-sided polishing low-doped n type single crystalline Si to be substrate, first evacuation process and the heat de-airing process before sputtering the substrate after cleaning are carried out to magnetron sputtering cavity, then on substrate, first sputtering grows the Si resilient coating of 20-50nm, the Ge film of rear growth 2.3-4nm, obtain initial sample, finally initial sample is put into quick anneal oven and carry out short annealing process acquisition quantum dot final sample.
2. the method preparing Ge/Si quantum dot according to claim 1, is characterized in that the single-sided polishing low-doped n type single crystalline Si that the growth substrates of described quantum dot be high preferred orientation is 110, thickness is 0.3-0.6mm, resistivity is 1-8 Ω .cm.
3. the method preparing Ge/Si quantum dot according to claim 1, before it is characterized in that sputter-deposited thin films, sputtering cavity low vacuum is in 2.0 × 10
-4pa.
4. the method preparing Ge/Si quantum dot according to claim 1, before it is characterized in that sputter-deposited thin films, heats to 800 to substrate
oc-900
oc completes degassed process.
5. the method preparing Ge/Si quantum dot according to claim 1, to is characterized in that in magnetron sputtering technique, in the vertical mode sputtered between target with substrate, by rotating substrate location, substrate first depositing Si, then depositing Ge.
6. the method preparing Ge/Si quantum dot according to claim 1, before it is characterized in that depositing Si resilient coating in described step, start the radio frequency sputtering of Si target in advance, remove target material surface impurity by pre-sputtering, actual conditions is as follows: Ar throughput is 10-15sccm; Sputtering pressure is 3-5Pa; Penetrating power is 50-60w; Sputtering time is 600s.
7. method according to claim 1, is characterized in that first substrate being cooled to 700 when depositing Si resilient coating in described step
oc, be depositional mode with radio frequency sputtering, actual conditions is as follows: Ar throughput is 10-15sccm; Sputtering pressure is 0.3-0.4Pa; Penetrating power is 45-60w; Deposit thickness is 20-50nm; Temperature retention time is 30-60min.
8. method according to claim 1, before it is characterized in that depositing Ge film in described step, start Ge target direct current sputtering in advance, remove target material surface impurity by pre-sputtering, actual conditions is as follows: Ar throughput is 10-15sccm; Sputtering pressure is 3-5Pa; Penetrating power is 50-60w; Sputtering time is 600s.
9. method according to claim 1, is characterized in that first substrate being cooled to 600-650 when depositing Ge in described step
oc, be depositional mode with direct current sputtering, actual conditions is as follows: Ar throughput is 5-8sccm; Sputtering pressure is 0.3-0.4Pa; Sputtering power is 30-40w; Deposit thickness is 2.3-4.0nm; After sputtering, Temperature fall obtains initial sample at once.
10. method according to claim 1, it is characterized in that carrying out short annealing process to the process of initial sample for sample is put into quick anneal oven in described step, annealing parameter is as follows: with N
2for protective gas, annealing temperature is 700
oc-750
oc, annealing time is 600-650s.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112071926A (en) * | 2020-08-27 | 2020-12-11 | 深圳市奥伦德元器件有限公司 | Infrared detector and preparation method thereof |
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| CN108899756B (en) * | 2018-06-06 | 2020-04-28 | 青岛海信宽带多媒体技术有限公司 | Method for depositing metal electrode |
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|---|---|---|---|---|
| CN101866832A (en) * | 2010-05-25 | 2010-10-20 | 云南大学 | Method for intermittently growing single-layer Ge quantum dots with high dimensional homogeneity on buffer layer by landfill |
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