CN101866832A - Method for intermittently growing single-layer Ge quantum dots with high dimensional homogeneity on buffer layer by landfill - Google Patents
Method for intermittently growing single-layer Ge quantum dots with high dimensional homogeneity on buffer layer by landfill Download PDFInfo
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Abstract
The invention relates to a method for intermittently growing single-layer Ge quantum dots with high dimensional homogeneity on a buffer layer by landfill, belonging to the technical field of semiconductor quantum material preparation. In the method, ion beam sputtering technology is adopted and an Si buffer layer with thickness of 20-60nm is intermittently grown on the pretreated silicon substrate material by turning a Ge target and a high-purity Si target, and then the single-layer Ge quantum dots with thickness of 2.0-3.0nm are intermittently grown on the Si buffer layer in a self-assembled manner. Through intermittent growth, the method effectively solves the following problems: multi-layer growth needs to be carried out on the quantum dots to control the dimensional homogeneity of the quantum dots when the quantum dot materials are prepared, the crystallinity and the controllability of the quantum dots are poor, the height-width ratio is low and Ge/Si intermixing is seriously insufficient, and the quantum dot materials used for preparing quantum dot devices are obtained by the method. Besides, the method is low in production cost, good in controllability and easy for industrial production and is simple and efficient.
Description
Technical field:
The present invention relates to a kind of with the high evenly method of individual layer Ge quantum dot of the interrupted growth size of ion beam sputtering technology resilient coating landfill, genus semiconductor quantum technical field of material.
Technical background:
Quantum dot (Quantum Dot, be called for short QD), claim artificial atom again, it is a kind of zero dimension quantum structure freely, when particle size reaches nanometer scale, the size confinement will cause dimensional effect, quantum confinement, macro quanta tunnel effect and skin effect etc., these unique quantum effects, quanta point material is widely studied is applied in the optoelectronic information device, quantum device based on the discrete characteristic of the limited quantum dot of three-dimensional, with its unique excellent electricity, optical property and extremely low power dissipation, in nanoelectronics, optoelectronics, life science, there is extremely application prospects in field such as quantum computer and military and national defense, specifically can be used in quantum dot laser, quantum dot infrared detector, single-photon light source, aspect such as single-electron device and quantum computer.Instantaneous super high power laser, can be used for interception or destroy aircraft (as, guided missile, aircraft, satellite etc.), be a kind of directed intellectual weapon, significant to national defense construction.Therefore, each big state has all launched further investigation to this.Yet, the size of quantum dot, the uniformity of size, shape, density and component distribute and all can produce significant effects to its photoelectric property, and general optoelectronic device applications requires all that quantum dot satisfies the density height, size is little and be evenly distributed, arrange orderly condition.The method of existing silica-based Ge quantum dot self-organizing growth mainly contains chemical vapor deposition (CVD) and molecular beam epitaxy technique (MBE), these two kinds of technology are being applied in the various photodetectors the success of Ge quantum dot, but because when preparing quanta point material with these technology, exist production cost height, complex process, problem that production efficiency is low, be unfavorable for large-scale industrialized production, thereby improved the production cost of quantum dot device.
The inventor's patent 200610048900.9 discloses the method for ion beam sputtering technology self-organizing growth Ge quantum dot under a kind of low growth line first, the Si layer of thickness of having grown less than 80nm, thickness is less than the Ge layer of 20nm, one deck Si and one deck Ge constitute one-period, the sputter periodicity is 5～50 cycles, the Ge layer of last growth quantum point is the block layer, and having obtained diameter is 50nm～90nm, highly is the Ge quantum dot of 2nm～10nm; Another patent 200610048899.X of the inventor discloses a kind of preparation method of low temperature double ion beam sputtered Ge/Si multilayer film self-assembled Ge quantum dot, by two ion beam sputtering rifle alternating sputtering growth Si and Ge multilayer film, the Ge layer of last growth quantum point is as the block layer, having obtained diameter is 10nm～30nm, the Ge quantum dot of height 1nm～2nm.
Summary of the invention:
It is bigger to the objective of the invention is to overcome existing Ge quantum dot size, need the multilayer quantum dot dimensional homogeneity of growing, and in ion beam sputtering quantum dot process crystallinity with the deficiency of size and uniformity and controllability, with interrupted growing method growth individual layer Ge quantum dot, obtain size evenly, the good Ge quantum dot of high density, small size, large ratio of height to width, controllability with the requirement of satisfying the optoelectronic information device simultaneously, improved productivity effect, reduce production costs, satisfy industrial-scale production.
The present invention realizes by following technical proposal:
The present invention with ion beam sputtering by rotating the position of high-purity Ge target and high-purity Si target, sputtering sedimentation Ge and Si film on the silicon base material.The present invention's ion beam vacuum sputtering as working gas, is 600eV～1400eV at the argon ion energy with argon gas, and discharge voltage is 75V～80V, and growth temperature is 500 ℃～700 ℃, and the growth line is 14mA～20mA, and sputter pressure is 2.0 * 10
-2Under the condition of Pa, interrupted growth thickness is the Si resilient coating of 20nm～60nm on the silicon base material, and interrupted self-organizing growth thickness is the individual layer Ge quantum dot of 2.0nm～3.0nm on the Si resilient coating then.
Described ion beam sputtering, with prior art the silicon base material is handled in advance:
A, selection crystal orientation are the Si base material of (100), clean 15min respectively successively with toluene, acetone, absolute ethyl alcohol, remove substrate surface organic substance and inorganic matter impurity;
B, the Si base material that will clean are used H earlier
2SO
4: H
2O
2=4: 1 solution boils 10min, uses HF: H again
2O
2=1: 9 solution soaks 20s～40s;
C, the Si base material after above-mentioned B step process are used NH earlier
3OH: H
2O
2: H
2O=1: 1: 4 solution boils 10min, uses HF: H again
2O
2=1: 9 solution soaks 20s～40s;
D, the Si base material after above-mentioned C step process are used earlier dense HNO
3Boil 3min, use HF: H again
2O
2=1: 9 solution soaks 20s～40s;
E, the Si base material after above-mentioned D step process are used earlier HCl: H
2O
2: H
2O=3: 1: 1 solution boils 5min, uses HF: H again
2O=1: 20 solution soaks 30s～60s
Following concrete grammar self-organizing growth individual layer Ge quantum dot is passed through in described ion beam sputtering:
A, pretreated silicon base material is dried up with high pure nitrogen, place in the sputtering chamber, treat that sputtering chamber base vacuum degree is less than 2.0 * 10
-4Pa, adjusting growth temperature is 500 ℃～700 ℃, keeps 10min～30min, makes the H key desorption of silicon face, obtains clean surface; Charging into purity subsequently in sputtering chamber is the Ar gas of 5N, and regulating pressure is 2.0 * 10
-2Pa;
B, be 500 ℃～700 ℃ of chambers in temperature, the argon ion energy is 600eV～1400eV, line is 14mA～20mA, discharge voltage is 75V～80V, sputter thickness is the Si resilient coating of 10nm～30nm, and original position keeps 5min～15min, the Si resilient coating of continued growth 10nm～30nm more then, original position keeps 5min～15min behind the growth ending, to improve the crystallinity and the surface smoothness of resilient coating; The first Ge layer of growth 0.7nm～0.9nm in 500 ℃～700 ℃ scopes then, original position keeps 3min～5min, and the Ge layer of regrowth 1.30nm～2.0nm cools to room temperature at last naturally.
The present invention is by interrupted growth, efficiently solving the preparation quanta point material exists quantum dot to need the multilayer quantum dot dimensional homogeneity of growing, and the crystallization of quantum dot, poor controllability, depth-width ratio are low, and Ge/Si mix wretched insufficiency mutually, acquisition can be used to make the quanta point material of quantum dot device, and production cost is low, controllability is good, is easy to industrialization production, is a kind of simple and efficient method of preparation quantum dot.
Description of drawings:
Fig. 1 is the AFM testing result figure of the embodiment of the invention 1 gained sample;
Fig. 2 is the AFM testing result figure of the embodiment of the invention 2 gained samples;
Fig. 3 is the AFM testing result figure of the embodiment of the invention 3 gained samples
Embodiment:
Below by embodiment the present invention is described further.
Embodiment 1:
Device therefor is the ion beam sputtering chamber of FJL560III type ultra high vacuum many targets magnetic control and ion beam associating sputtering equipment, settles a Kaufman ion gun in the growth room.Used target is square target of high-purity Ge and the square target of HIGH-PURITY SILICON of 5N (more than 99.999%), and sputter gas is the high-purity argon gas of 5N (more than 99.999%).It is the N type single crystalline Si sheet of (100) that used Si base material adopts the crystal orientation, single-sided polishing, and resistivity is 0.001 Ω m～0.005 Ω m.Commercial ultrasonic cleaning machine is used in ultrasonic cleaning.Specifically:
One, the processing of silicon base material
A, selection crystal orientation are the Si base material of (100), clean 15min respectively successively with toluene, acetone, absolute ethyl alcohol, remove substrate surface organic substance and inorganic matter impurity;
B, the Si base material that will clean are used H earlier
2SO
4: H
2O
2=4: 1 solution boils 10min, uses HF: H again
2O
2=1: 9 solution soaks 20s～40s;
C, the Si base material after above-mentioned B step process are used NH earlier
3OH: H
2O
2: H
2O=1: 1: 4 solution boils 10min, uses HF: H again
2O
2=1: 9 solution soaks 20s～40s;
D, the Si base material after above-mentioned C step process are used earlier dense HNO
3Boil 3min, use HF: H again
2O
2=1: 9 solution soaks 20s～40s;
E, the Si base material after above-mentioned D step process are used earlier HCl: H
2O
2: H
2O=3: 1: 1 solution boils 5min, uses HF: H again
2O=1: 20 solution soaks 30s～60s.
Two, the interrupted sputter self-organizing growth of ion beam individual layer Ge quantum dot
A, pretreated silicon base material is dried up with high pure nitrogen, place in the sputtering chamber, treat that sputtering chamber base vacuum degree is less than 2.0 * 10
-4Pa, adjusting temperature is to keep 10min after 700 ℃, and charging into purity in sputtering chamber is the Ar gas of 5N, and making pressure is 2.0 * 10
-2Pa;
B, be 500 ℃ in temperature, line is 17mA, and the argon ion energy is 1400eV, and discharge voltage is 75V, and sputter pressure is 2.0 * 10
-2Under the condition of Pa, at first sputter thickness is the Si resilient coating of 30nm.Original position keeps the Si resilient coating that sputter 30nm is thick again behind the 10min, keep 15min behind the Si growth ending, the Ge layer of the 0.7nm that under 500 ℃ of temperature, at first grows then, the Ge of regrowth 2nm behind the original position maintenance 5min, at last cool to room temperature naturally, obtain Ge quantum dot thin-film material.
The sample detection result of present embodiment 1 is shown in Fig. 1 stereogram, and the average height of Ge quantum dot is 11nm among the figure, and average diameter is 30nm, and average depth-width ratio is 0.36, and density is 9.97 * 10
9Cm
-2, this moment, lateral size of dots was little and even and density is higher, and it is also relatively more orderly to distribute.
Embodiment 2:
Device therefor and material are all identical with embodiment 1.Concrete steps are:
One, the processing of silicon base material:
Identical with embodiment 1.
Two, the interrupted sputter self-organized quantum dot of ion beam
A, pretreated silicon base material is dried up with high pure nitrogen, place in the sputtering chamber, treat that sputtering chamber base vacuum degree is less than 2.0 * 10
-4Pa, adjusting temperature is to keep 30min after 500 ℃, and charging into purity in sputtering chamber is the Ar gas of 5N, and making pressure is 2.0 * 10
-2Pa;
B, be 700 ℃ in temperature, line is 14mA, and the argon ion energy is 1100eV, and discharge voltage is 80V, and sputter pressure is 2.0 * 10
-2Under the condition of Pa, at first sputter thickness is the Si resilient coating of 15nm.Original position keeps the Si resilient coating that sputter 15nm is thick again behind the 5min, keep 10min behind the Si growth ending, the Ge layer of the 0.8nm that under 700 ℃ of temperature, at first grows then, the Ge of regrowth 1.5nm behind the original position maintenance 4min, at last cool to room temperature naturally, obtain Ge quantum dot thin-film material.
The sample detection result of present embodiment 2 is shown in Fig. 2 stereogram, and the average height of Ge quantum dot is 15.62nm among the figure, and average diameter is 52.44nm,, average depth-width ratio is 0.30, density is 1.58 * 10
10Cm
-2This moment, density was big, and highly higher, distribution of sizes is more even.
Embodiment 3:
Device therefor and material are all identical with embodiment 1.Concrete steps are:
One, the processing of silicon base material:
Identical with embodiment 1.
Two, the interrupted sputter self-organized quantum dot of ion beam
A, pretreated silicon base material is dried up with high pure nitrogen, place in the sputtering chamber, treat that sputtering chamber base vacuum degree is less than 2.0 * 10
-4Pa, adjusting temperature is to keep 20min after 650 ℃, and charging into purity in sputtering chamber is the Ar gas of 5N, and making pressure is 2.0 * 10
-2Pa;
B, be 650 ℃ in temperature, line is 20mA, and the argon ion energy is 600eV, and discharge voltage is 78V, and sputter pressure is 2.0 * 10
-2Under the condition of Pa, at first sputter thickness is the Si resilient coating of 10nm.Original position keeps the Si resilient coating that sputter 10nm is thick again behind the 8min, keep 5min at 650 ℃ behind the Si growth ending, the Ge layer of the 0.9nm that under 650 ℃ of temperature, at first grows then, the Ge of regrowth 1.0nm behind the original position maintenance 3min, at last cool to room temperature naturally, obtain Ge quantum dot thin-film material.
The sample detection result of present embodiment 3 is shown in Fig. 3 stereogram, and the average height of Ge quantum dot is 14.35nm among the figure, and average diameter is 55.74nm,, average depth-width ratio is 0.26, density is 9.76 * 10
9Cm
-2
Claims (3)
1. the high evenly method of individual layer Ge quantum dot of the interrupted growth size of resilient coating landfill is used ion beam sputtering technology, by rotating the position of high-purity Ge target and high-purity Si target, sputtering sedimentation Ge and Si film on pretreated silicon base material; The method elder generation interrupted growth thickness on pretreated silicon base material that it is characterized in that individual layer Ge quantum dot of the present invention is the Si resilient coating of 20nm～60nm, and interrupted self-organizing growth thickness is the individual layer Ge quantum dot of 2.0nm～3.0nm on the Si resilient coating again.
2. method according to claim 1, the condition of work that it is characterized in that described ion beam sputtering is: the ion beam vacuum sputtering, and use argon gas as working gas, the argon ion energy is 600eV～1400eV, discharge voltage is 75V～80V, growth temperature is 500 ℃～700 ℃, operating room's base vacuum degree 8.0 * 10
-5Pa～2.0 * 10
-4Pa,, the growth line is 14mA～20mA, sputter pressure is 2.0 * 10
-2Pa.
3. method according to claim 1 is characterized in that described ion beam sputtering is by following concrete grammar self-organizing growth individual layer Ge quantum dot:
A, pretreated silicon base material is dried up with high pure nitrogen, place in the sputtering chamber, treat that sputtering chamber base vacuum degree is less than 2.0 * 10
-4Pa, adjusting growth temperature is 500 ℃～700 ℃, keeps 10min～30min; Charging into purity subsequently in sputtering chamber is the Ar gas of 5N, and regulating pressure is 2.0 * 10
-2Pa;
B, be 500 ℃～700 ℃ in temperature, the argon ion energy is 600eV～1400eV, and discharge voltage is 75V～80V, and the growth line is 14mA～20mA, and sputter pressure is 2.0 * 10
-2Under the condition of Pa, growth thickness is the Si resilient coating of 10nm～30nm; Original position keeps 5min～15min, the Si resilient coating of regrowth 10nm～30nm; Original position keeps 5min～15min behind the growth ending; The first Ge layer of growth 0.7nm～0.9nm in 500 ℃～700 ℃ scopes then, original position keeps 3min～5min, the Ge layer of regrowth 1.0nm～2.0nm; The last room temperature that cools to naturally.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103903966A (en) * | 2014-03-11 | 2014-07-02 | 复旦大学 | Method for manufacturing ultrahigh-density germanium silicon quantum dots based on obliquely-cut silicon substrate |
| CN105304736A (en) * | 2015-07-18 | 2016-02-03 | 云南大学 | Method of fabricating Ge/Si quantum dots by magnetron sputtering in combination with rapid annealing technology |
| CN105652516A (en) * | 2016-01-04 | 2016-06-08 | 合肥京东方显示光源有限公司 | Lateral entrance type backlight module and making method and display device thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050051861A1 (en) * | 2003-09-09 | 2005-03-10 | Industrial Technology Research Institute | Avalanche photo-detector with high saturation power and high gain-bandwidth product |
| CN1974837A (en) * | 2006-12-11 | 2007-06-06 | 云南大学 | Prepn process of low temperature double ion beam sputtered multilayer Ge/Si film with self-organized Ge quantum dots |
-
2010
- 2010-05-25 CN CN2010101819341A patent/CN101866832B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050051861A1 (en) * | 2003-09-09 | 2005-03-10 | Industrial Technology Research Institute | Avalanche photo-detector with high saturation power and high gain-bandwidth product |
| CN1974837A (en) * | 2006-12-11 | 2007-06-06 | 云南大学 | Prepn process of low temperature double ion beam sputtered multilayer Ge/Si film with self-organized Ge quantum dots |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103903966A (en) * | 2014-03-11 | 2014-07-02 | 复旦大学 | Method for manufacturing ultrahigh-density germanium silicon quantum dots based on obliquely-cut silicon substrate |
| CN105304736A (en) * | 2015-07-18 | 2016-02-03 | 云南大学 | Method of fabricating Ge/Si quantum dots by magnetron sputtering in combination with rapid annealing technology |
| CN105652516A (en) * | 2016-01-04 | 2016-06-08 | 合肥京东方显示光源有限公司 | Lateral entrance type backlight module and making method and display device thereof |
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