CN101311350B - Silicon with three-dimensional depression structure and method for preparing same - Google Patents
Silicon with three-dimensional depression structure and method for preparing same Download PDFInfo
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- CN101311350B CN101311350B CN2008101011900A CN200810101190A CN101311350B CN 101311350 B CN101311350 B CN 101311350B CN 2008101011900 A CN2008101011900 A CN 2008101011900A CN 200810101190 A CN200810101190 A CN 200810101190A CN 101311350 B CN101311350 B CN 101311350B
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Abstract
The invention discloses silicon with a three-dimensional sunken structure and a preparing method thereof, which belongs to the field of semiconductor material and preparation thereof. The three-dimensional sunken structure of the silicon with the three-dimensional sunken structure of the invention is in the shape of a right prism, wherein, the undersurface is a polygon which sequentially consists of side A1, A2, B1, B2, C1 and C2, wherein, side A1 is parallel to A2; side B1 is parallel to B2; side C1 is parallel to C2; triangles formed by three intersections obtained by intersecting of two of straight lines where A1, B1 and C1 or A2, B2 and C2 lie are regular triangles. The inside part of the three-dimensional structure is hollow. Meanwhile, the invention provides a method for preparing the silicon with the three-dimensional sunken structure by a vapor deposition method, wherein, the method is that the silicon with the three-dimensional solid structure grows by the eutectic melting of the sediment of zinc and silicon on the surface of silicon. Compared with the prior art, the invention has the advantages that raw material of the preparation is very cheap; the preparing procedures are simple and easy to be repeated; the preparation parameter is easy to control; the crystallization of a generated product is good; a regular three-dimensional solid structure is provided.
Description
Technical field
The present invention relates to a kind of silicon and preparation method thereof, belong to semiconductor material and preparation field thereof with three-dimensional hollow structure.
Background technology
Silicon is one of of paramount importance material in the semiconductor technology, and growing nano or micrometer structure have great importance on silicon.
The novel character that has the nano material of special construction and show has become the focus of people's research.A lot of physical phenomenons of these materials are foretold and are confirmed.And also be the nearest focus of research in silicon face growing three-dimensional three-dimensional arrangement.This three-dimensional structure that obtains by self-assembled growth has important application prospects in fields such as photoelectric devices.
The 3-D solid structure that the present invention relates to has the right prism profile, and its outside surface can be used as the substrate of other nano material of growth; It still is a hollow simultaneously, and its hollow structure can be used as container again, loads other material.
Study the self-assembly characteristic that this structure can disclose silicon.
At present, this preparation method with silicon of the three-dimensional hollow structure of roof shape yet there are no report.Similarly, people such as GilbertoMedeiros-Ribeiro are by preparing the solid quantum island of Si/Ge [GilbertoMedeiros-Ribeiro at silicon chip surface deposition Ge, et al.Shape Transition of Germanium Nanocrystals on a Silicon (001) Surfacefrom Pyramids to Domes.Scinece 279,353 (1998)].They by under ultrahigh vacuum(HHV) physical vapor deposition (PVD) Ge at Si (001) face.Jeremy T.Robinson etc. use Au as catalyzer [Jeremy T.Robinson, etal.Chemical Nanomachining of Silicon by Gold-Catalyzed Oxidation.Nano Lett.7,2009 (2007)], at the array of the three-dimensional structure of silicon face growth Ge.
Summary of the invention
The object of the present invention is to provide a kind of method that has the silicon of three-dimensional hollow structure and prepare this structure.
Above-mentioned three-dimensional hollow structure with silicon of three-dimensional hollow structure is a vertical prismatic shape, and its bottom surface is a Polygons, comprises limit A1 successively, A2, and B1, B2, C1, C2, wherein A1 is parallel to B2, and B1 is parallel to C2, and C1 is parallel to A2; The trilateral that A1, B1, the straight line at C1 place intersect three intersection points formation that obtain in twos is an equilateral triangle, as shown in Figure 1.The inside of this three-dimensional structure is empty, inner wall shape and outer wall shape approximation.
The bottom surface of this right prism is that opposite side is parallel in twos, and interior angle is 120 ° a hexagon.Especially, work as A2, B2, when having a limit to be zero among the C2, this bottom surface is a pentagon, this three-dimensional hollow structure is a pentagonal prism shape; Work as A2, B2, when having two limits to be zero among the C2, this bottom surface is an isosceles trapezoid, this three-dimensional hollow structure is a four prism type; Work as A2, when B2, C2 were zero, this bottom surface was an equilateral triangle, and this three-dimensional hollow structure is regular triangular prism shaped.
According to obtaining scanning electron microscope (SEM) picture, the length of above-mentioned each prismatic bottom surface is all between 1 micron to 50 microns; The height of whole prismatic profile is between 1 micron to 5 microns.
The present invention provides a kind of simultaneously and has prepared above-mentioned method with silicon of three-dimensional hollow structure by CVD (Chemical Vapor Deposition) method, and this method forms the above-mentioned silicon with 3-D solid structure of congruent melting growth by metallic zinc and the silicon that is deposited on silicon face.
This method comprises following step:
(1) silicon chip and the metal zinc with the surfacing cleaning places heatable reaction chamber respectively, and wherein (111) of silicon chip face up, as the above-mentioned substrate with silicon of three-dimensional hollow structure of growth; Preferably, before silicon chip is put into reaction chamber, can use the skin daraf(reciprocal of farad) that silicon chip is carried out clean,, reaction can more successfully be carried out so that its surface is free from foreign meter.Metal zinc can be placed the central position of reaction chamber, but silicon chip centering position then, perhaps near the central position or place tuyere position under the reaction chamber.Here uptake refers to the end that shielding gas enters, and the air port refers to an end of bleeding and exporting down.The consumption of required metal zinc is as the criterion to satisfy two conditions: will guarantee have abundant zinc powder to be evaporated in the chamber on the one hand in temperature-rise period, form zinc fume and contact with silicon face; On the other hand, when heating up end, zinc powder should be evaporated fully, otherwise can form the nanostructure of zinc oxide, interference experiment at silicon chip.
(2) feed shielding gas, remove the air in the reaction chamber, and chamber inner pressure is remained on by force between 0.2 to 0.6MPa; Wherein, described shielding gas is preferably rare gas element, and in actual applications, because cost, commonly used is argon gas.Flow is preferably 30-80sccm.
(3) heating makes the interior temperature of chamber reach 700-1300 ℃, and temperature-rise period continues 60-120 minute, and keeps 30-60 minute under top temperature.Preferably, can be in chamber aerating oxygen improving above-mentioned productive rate with silicon of three-dimensional hollow structure, aerating oxygen during such as the top temperature that reaches setting in temperature, flow is preferably 4-10sccm.
(4) temperature in the chamber is reduced to room temperature naturally, take out sample, obtain having the silicon of three-dimensional hollow structure.
What deserves to be explained is, in above-mentioned steps (3) and (4), all keep feeding shielding gas.
Can find that by the product that obtains being carried out the EDXS analysis major ingredient that the present invention has the silicon of three-dimensional hollow structure is a silicon, contains a spot of oxygen and zinc simultaneously.
Compare with prior art, advantage of the present invention is: the preparation desired raw material is dirt cheap; Preparation process is simple; Be easy to repetition; Preparation parameter is controlled easily; The product well-crystallized who generates, and 3-D solid structure with rule.
Description of drawings
Fig. 1. the present invention has the bottom surface geometrical shape figure of three-dimensional hollow structure of the silicon of three-dimensional hollow structure;
Fig. 2. the present invention has the vertical view of the silicon (equilateral triangle bottom surface) of three-dimensional hollow structure;
Fig. 3. the present invention has the vertical view of the silicon (isosceles trapezoid bottom surface) of three-dimensional hollow structure;
Fig. 4. the present invention has the vertical view of the silicon (hexagon bottom surface) of three-dimensional hollow structure;
Fig. 5. the present invention jaggy has the vertical view of the silicon of three-dimensional hollow structure.
Embodiment
In conjunction with the accompanying drawings the present invention is described in further detail below by embodiment.
Embodiment one
In the present embodiment, the reaction raw materials of employing is the silicon chip (111 face) of 10mm * 10mm, the chemical pure metal zinc.
At first use the skin daraf(reciprocal of farad) that silicon chip is cleaned, remove the zone of oxidation on surface and the magazine of surface adsorption.The silicon chip size generally is cut into 10mm * 10mm.
Earlier 3-4 sheet silicon chip is faced up, be arranged in order, place in the middle of the quartz boat, and cover the layer of metal zinc powder on silicon chip, every part quality is 0.2-0.3g.Quartz boat is positioned over the center of tubular type heating furnace, in addition, 3-4 sheet silicon chip is housed equally but the quartz boat that do not cover zinc powder is positioned over apart from the following air port at 15cm place, tubular type heating furnace center.
Sample is packed into after the tubular type heating furnace sealing fully, opens mechanical pump and bleeds, and makes intraductal pressure less than 0.1MPa.Then feeding argon gas reaches about 0.2MPa the interior pressure of stove.And remain on this pressure.In this process, mechanical pump is worked always, reaches running balance.
Set 60 fens clock times and make chamber be warming up to 1200 ℃ of top temperatures, and kept 40 minutes in this temperature from room temperature.In the whole experiment, argon gas feeds as shielding gas always, and flow is 50sccm; Oxygen then is just to feed when rising to 1000 ℃ when temperature.In this process, change as pressure in the stove, adjust rate of air sucked in required and make it to keep original set(ting)value.
After about four or five hours, temperature is reduced to room temperature in the stove, opens vacuum chamber and takes out sample.
In the present embodiment, scanning electronic microscope general image such as accompanying drawing 2 from two resulting silicon chips of quartz boat, shown in 3 and 4, quartz boat at the center, and more pyramid and roof structure have appearred on the silicon chip of covering zinc powder, and a small amount of pyramid and roof structure appear on the silicon chip that does not cover zinc powder in the quartz boat in following air port.
Embodiment two
In the present embodiment, top temperature is made as more than 1300 ℃, and other condition is with embodiment one, and pyramid that obtains on silicon chip or roof structure are also imperfect, many breach occur, as shown in Figure 5.
Embodiment three
In the present embodiment, do not cover on silicon chip or thermal evaporation deposition zinc powder, other condition only heats silicon chip with embodiment one, finally can not obtain the three-dimensional structure of any silicon.
From above three embodiment as can be seen, metal zinc and silicon chip at high temperature react, and obtain having the silicon of three-dimensional hollow structure.Whether other parameter also can influence the growth of the three-dimensional structure of silicon as the feeding of top temperature, pressure and soaking time and oxygen.Wherein, those skilled in the art will appreciate that the size of zinc powder usage quantity, silicon chip and the air flow of oxygen are to decide according to heating installation, do not exceed to scope with the embodiment of the invention.
More than by embodiment the present invention is described in detail, the technology of this area is to be understood that with personnel, in the scope that does not exceed spirit of the present invention and essence, the present invention is made certain modification and distortion, such as replacing the disclosed method of content embodiment of the present invention that silicon chip is carried out clean with additive method, or use and the kin metal of zinc, perhaps the heating installation with other vacuum-pumpings replaces the disclosed tubular type heating furnace of the present invention, still can realize purpose of the present invention.In addition, set different temperature and times, different parameters such as pressure still might be realized result of the present invention.
Claims (12)
1. the silicon with three-dimensional hollow structure is characterized in that, described three-dimensional hollow structure is hollow vertical prismatic shape, and its bottom surface is a Polygons, comprises limit A1 successively, A2, and B1, B2, C1, C2, wherein A1 is parallel to B2, and B1 is parallel to C2, and C1 is parallel to A2; And A1＞0, B1＞0, C1＞0, A2 〉=0, B2 〉=0, C2 〉=0; The trilateral that A1, B1, the straight line at C1 place intersect three intersection points formation that obtain in twos is an equilateral triangle.
2. the silicon with three-dimensional hollow structure as claimed in claim 1 is characterized in that A2, B2, among the C2 only one be zero.
3. the silicon with three-dimensional hollow structure as claimed in claim 1 is characterized in that A2, and B2 has two to be zero among the C2.
4. the silicon with three-dimensional hollow structure as claimed in claim 1 is characterized in that A2, and B2, C2 are zero.。
5. the silicon with three-dimensional hollow structure as claimed in claim 1 is characterized in that, A1, and A2, B1, B2, C1, the base length of side non-vanishing among the C2 is between 1 micron to 50 microns.
6. the silicon with three-dimensional hollow structure as claimed in claim 1 is characterized in that, the height of described three-dimensional hollow structure is between 1 micron to 5 microns.
7. preparation method with silicon of three-dimensional hollow structure, its step comprises:
(1) silicon chip and the zinc powder with the surfacing cleaning places heatable reaction chamber respectively, and (111) face of silicon chip is as reaction interface;
(2) feed shielding gas, remove the air in the reaction chamber, and make that pressure remains between 0.2 to 0.6MPa in the chamber;
(3) heating makes the reaction chamber room temp reach 700-1300 ℃, and temperature-rise period continues 60-120 minute, and keeps 30-60 minute under top temperature;
(4) temperature in the chamber is reduced to room temperature naturally, obtain having the silicon of three-dimensional hollow structure.
8. method as claimed in claim 7 is characterized in that, the described zinc powder of step (1) places the central position in the reaction chamber, and silicon chip can place the central position of reaction chamber and be positioned under the zinc powder, also can place down the air port.
9. method as claimed in claim 7 is characterized in that, the quality of the described zinc powder of step (1) satisfies following condition: guaranteeing in temperature-rise period has abundant zinc powder to be evaporated in the reaction chamber, makes the zinc fume that forms contact with silicon face; When heating up end, zinc powder is evaporated fully simultaneously.
10. method as claimed in claim 7 is characterized in that, the described reaction chamber of step (1) is the tubular type heating furnace, and perhaps other can provide the heatable equipment of vacuum chamber.
11. method as claimed in claim 7 is characterized in that, the described shielding gas of step (2) is a rare gas element.
12. method as claimed in claim 7 is characterized in that, in step (3), also be included in the temperature-rise period or under top temperature in chamber aerating oxygen.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5719741A (en) * | 1994-10-07 | 1998-02-17 | Oji Paper Co., Ltd. | Zinc-deposited base material for metallized capacitors and method of manufacture thereof |
| CN1396300A (en) * | 2002-07-17 | 2003-02-12 | 清华大学 | Process for preparing large-area zinc oxide film with nano lines by physical gas-phase deposition |
| CN1789139A (en) * | 2005-12-29 | 2006-06-21 | 大连理工大学 | Method for directional growth of zinc oxide nano-belt |
| CN101311347A (en) * | 2008-02-29 | 2008-11-26 | 北京大学 | Silicon with three-dimensional depression structure and method for preparing same |
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2008
- 2008-02-29 CN CN2008101011900A patent/CN101311350B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5719741A (en) * | 1994-10-07 | 1998-02-17 | Oji Paper Co., Ltd. | Zinc-deposited base material for metallized capacitors and method of manufacture thereof |
| CN1396300A (en) * | 2002-07-17 | 2003-02-12 | 清华大学 | Process for preparing large-area zinc oxide film with nano lines by physical gas-phase deposition |
| CN1789139A (en) * | 2005-12-29 | 2006-06-21 | 大连理工大学 | Method for directional growth of zinc oxide nano-belt |
| CN101311347A (en) * | 2008-02-29 | 2008-11-26 | 北京大学 | Silicon with three-dimensional depression structure and method for preparing same |
Non-Patent Citations (3)
| Title |
|---|
| L Vescan等.Self-assembling of Ge on finite Si 001 areas comparable withthe island size.Applied Physics Letters8 2.2003,8(2),3517. |
| L Vescan等.Self-assembling of Ge on finite Si 001 areas comparable withthe island size.Applied Physics Letters8 2.2003,8(2),3517. * |
| Shyh-shin Ferng等.Growth behaviour of Ge nano-islands on the nanosized Si(111) facets bordering on two (100) planes.Nanotechnology17.2006,175207. * |
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