CN104555909A - Method and apparatus for producing silicon germanium core-shell structure nano-particles in laboratory - Google Patents
Method and apparatus for producing silicon germanium core-shell structure nano-particles in laboratory Download PDFInfo
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- CN104555909A CN104555909A CN201410800459.XA CN201410800459A CN104555909A CN 104555909 A CN104555909 A CN 104555909A CN 201410800459 A CN201410800459 A CN 201410800459A CN 104555909 A CN104555909 A CN 104555909A
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Abstract
The invention relates to the fields of production methods and production apparatuses of silicon germanium core-shell structure nano-particles, in particular to a method and an apparatus for producing silicon germanium core-shell structure nano-particles in a laboratory. According to the method, the silicon germanium core-shell structure nano-particles are prepared by adopting a gaseous phase method, and the method has the characteristics of rapid nano-particle production speed and controllable nano-particle size. The apparatus for producing the silicon germanium core-shell structure nano-particles comprises a small-sized glass tube and a large-sized glass tube, wherein the small-sized glass tube is provided with a first cathode and a first anode; the large-sized glass tube is provided with an inner tube and a second anode; a second cathode is arranged in the inner tube. According to the apparatus, the uniform distribution of plasma is realized, and the nano-particles with narrow size distribution are favorably generated. The apparatus has the characteristics that the dispersibility of the nano-particles is good, the surfaces of the nano-particles are uniformly coated, and the like.
Description
Technical field
The present invention relates to production method and the production equipment field of SiGe Core-shell Structure Nanoparticles, spy relates to a kind of method and apparatus of Laboratory Production SiGe Core-shell Structure Nanoparticles.
Background technology
Along with the development of nanometer technology, people have prepared silicon and germanium nano particle by various method.And have been found that many performances that these nano particles have body material and do not possess.Nm-class core-and-shell particles has the nano material of different nature with nuclear structure due to surface coverage, and therefore surface nature is changed to some extent by Shell Materials, often shows the function that core does not have.Research finds that the nucleocapsid structure of SiGe nano wire has excellent Electronic Performance.Because the forbidden band structure of SiGe nano material is different, the nanoparticle structure of the coated germanium of silicon or germanium coated Si may have good optical property.Method at present about the nano particle preparing SiGe nucleocapsid structure there is no relevant report.
Summary of the invention
For the deficiency of background technology, method of the present invention adopts vapor phase method to prepare the nano particle of SiGe nucleocapsid structure, and the method has the controlled feature of the size of nano particle.The equipment of production SiGe Core-shell Structure Nanoparticles of the present invention comprises small-size glass pipe and large glass pipe, and small-size glass pipe is provided with the first negative pole and the first positive pole, and large glass pipe is provided with interior pipe and the second positive pole, and interior pipe is provided with the second negative pole.This device achieves that being uniformly distributed of plasma, be conducive to the nano particle generating narrow size distribution.It is good that this device has nanoparticulate dispersed, and nano grain surface is the feature such as coated evenly.
Technical scheme of the present invention is: the method for the Core-shell Structure Nanoparticles of the coated germanium of a kind of Laboratory Production silicon, is characterized in that:
Step one, vacuumize to system, vacuum reaches below 10 handkerchiefs, by the ratio input GeH between 1:40 to 1:60
4with Ar gas, according to required generation nanometer particle size size adjustment air pressure, mist produces argon plasma in radio frequency plasma, and argon plasma knows from experience shock germane molecule, make germane molecular cleavage and form the nucleus of germanium, and then germanium nucleus is grown up and can be generated germanium nano particle;
Step 2, by between 1:50 to 1:70 ratio input SiH
4with Ar gas, and make argon gas under the exciting of radio-frequency power, and form argon plasma, argon plasma clashes into silane gas makes silane gas cracking;
Generate one deck silicon thin film with the germanium nano grain surface in step one after step 3, silane gas cracking and cover germanium nano grain surface, form the nano particle of the coated germanium of silicon.
A method for the Core-shell Structure Nanoparticles of Laboratory Production germanium coated Si, is characterized in that:
Step one, vacuumize to system, vacuum reaches below 10 handkerchiefs, by the ratio input SiH between 1:50 to 1:70
4with Ar gas, according to required generation nanometer particle size size adjustment air pressure, mist produces argon plasma in radio frequency plasma, and argon plasma knows from experience shock silane molecule, make silane molecule cracking and form the nucleus of silicon, and then silicon wafer core is grown up and can be generated nano silicon particles;
Step 2, by between 1:40 to 1:60 ratio input GeH
4with Ar gas, and make argon gas under the exciting of radio-frequency power, and form argon plasma, argon plasma clashes into Germane gas makes Germane gas cracking;
Cover nano silicon particles surface with the nano silicon particles Surface Creation one deck silicon thin film in step one after step 3, Germane gas cracking, form the nano particle of germanium coated Si.
The method beneficial effect of SiGe Core-shell Structure Nanoparticles of the present invention is: the size of the nano particle of the germanium coated Si that this method is produced or the coated germanium of silicon is controlled, and the even particle size distribution of particle; The size of the particle that this method generates can accomplish below very little so that 10 nanometers.
The invention also discloses a kind of equipment of Laboratory Production SiGe Core-shell Structure Nanoparticles, comprise small-size glass pipe (2), metallic conduit (3), large glass pipe (12), described small-size glass pipe (2) top is connected with air inlet pipe one (10) by glass connector, below is connected with metallic conduit (3) by glass connector, metallic conduit (3) is connected with large glass pipe (12) by glass connector, described metallic conduit (3) is provided with air inlet two (11), it is characterized in that: described small-size glass pipe (2) is provided with the first negative pole (5) and the first positive pole (1), first negative pole (5) and the first positive pole (1) are cylindrical electrode, described large glass pipe (12) is provided with interior pipe (14), large glass pipe (12) is provided with the second positive pole (15), interior pipe (14) is provided with the second negative pole (7), and the second positive pole (15) and the second negative pole (7) are cylindrical electrode.
The equipment of production SiGe Core-shell Structure Nanoparticles as above, it is characterized in that: described the first negative pole (5) is above, first positive pole (1) below, and center line between the first negative pole (5) with the first positive pole (1) and small-size glass pipe (2) center line consistent.
The equipment of production SiGe Core-shell Structure Nanoparticles as above, is characterized in that: the height of described the second negative pole (7) is the same with the height of the second positive pole (15), and is positioned on large glass pipe (12) position of center line.
The equipment of production SiGe Core-shell Structure Nanoparticles as above, is characterized in that: described large glass pipe (12) is concentric with interior pipe (14), and the ratio of large glass pipe (12) internal diameter and interior pipe (14) internal diameter is 1:4.
The equipment of production SiGe Core-shell Structure Nanoparticles as above, is characterized in that: described small-size glass pipe (2) is 1:5 with the ratio of large glass pipe (12) internal diameter.
The equipment of production SiGe Core-shell Structure Nanoparticles as above, it is characterized in that: described interior pipe (14) is provided with a glass pipe (8), there is individual polytetrafluoroethylene (PTFE) lid (9) upper end, glass pipe (8) is connected with glass connector, glass connector and vacuum electrode are connected together, interior pipe (14) the lower end mouth of pipe is closed, and interior pipe (14) and large glass pipe (12) are connected as one by main glass supports (13).
The equipment of production SiGe Core-shell Structure Nanoparticles as above, it is characterized in that: described glass connector is stainless steel material manufacture, it comprises cup-shaped cylinder (16), pipe (17), disc base (18), elastic tape placement section (20) and sealing lid (23); The internal diameter of cup-shaped cylinder (16) is identical with by the external diameter of glass tube that is tightly connected and outer wall that is cup-shaped cylinder has external screw thread, sealing lid (23) has internal thread, hollow circular-tube (17) upper end and cup-shaped cylinder (16) are connected as a single entity, lower end and disc base (18) are connected as a single entity, cup-shaped cylinder is provided with step in (16), and step is elastic tape placement section (20).
The method beneficial effect of SiGe Core-shell Structure Nanoparticles of the present invention is: building of equipment of the present invention is very simple and easy, and cost is low, is conducive to the use in laboratory; Use cylindrical upper/lower electrode in small-size glass pipe of the present invention, being uniformly distributed of the inside plasma can not only be realized, be conducive to the nano particle generating narrow size distribution; Large glass pipe below small-size glass pipe of the present invention makes the nano particle generated in small-size glass pipe above disperse better in larger interval, is more conducive to the coated with uniform of nano particle; And it is more even to use internal and external electrode to make plasma distribute in large glass pipe, also makes coated more even.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention structural representation;
Fig. 2 is glass connector structural representation;
Fig. 3 is sealing lid structural representation.
Detailed description of the invention
Description of reference numerals: the first positive pole 1, small-size glass pipe 2, metallic conduit 3, glass connector 1, glass connector 2 42, glass connector 3 43, glass connector 4 44, glass connector 5 45, first negative pole 5, second negative pole 7, glass pipe 8, polytetrafluoroethylene (PTFE) lid 9, air inlet pipe 1, air inlet 2 11, large glass pipe 12, main glass supports 13, interior pipe 14, second positive pole 15, cup-shaped cylinder 16, pipe 17, disc base 18, clutch disk 19, elastic tape placement section 20, lute 21, vavuum pump 22, metal bellows 1, metal bellows 2 25, collector 26.
As shown in Figure 1, small-size glass pipe 2 is air inlet pipe 1 above, air inlet pipe 1 is welded on clutch disk 19, the disc base 18 of clutch disk and glass connector 1 by rubber sealing ring together with clamp connection, glass connector 1 and small-size glass pipe 2 are tightly connected, and are imported to by reacting gas among small-size glass pipe 2.Small-size glass pipe 2 is also provided with two cylindrical electrodes, these two cylindrical electrodes are all as in figure 1 around small-size glass pipe 2, and the first negative pole 5 is above, and the first positive pole 1 below.Center line between first negative pole 5 with the first positive pole 1 is best and small-size glass pipe 2 center line is consistent, and the spacing between the two poles of the earth is 20mm, small-size glass pipe 2 and metallic conduit 3 is coupled together below small-size glass pipe 2 by glass connector 2 42.
Metallic conduit 3 is provided with air inlet 2 11, and be a large-scale glass connector 3 43 below air inlet 2 11, metallic conduit 3 and large glass pipe 12 below couple together by glass connector 3 43.The structure of large glass pipe 12 and above small-size glass pipe 2 are different, small-size glass pipe 2 is large comparatively above for first large-scale glass tube 12, the middle-size and small-size glass tube 2 of the present invention is 1:5 with the ratio of large glass pipe 12 internal diameter, internal diameter as small-size glass pipe 2 is 40mm, the internal diameter of large glass pipe 12 is 200mm, this is in order to the particle of generation in small-size glass pipe 2 better can disperse in large glass pipe 12, contributes to carrying out coated at particle surface.The second, large glass pipe 12 is concentric glass cylinder with interior pipe 14, and large glass pipe 12 internal diameter is 1:4 with the ratio of interior pipe 14 internal diameter, and the internal diameter as large glass pipe is 200mm, and inner tube diameter is 50mm.Interior pipe 14 has a glass pipe 8, and glass pipe 8 is connected with glass connector 4 44 again.Then glass connector 4 44 and vacuum electrode are connected together.Then the second negative pole 7 is stuck on the tube wall of interior pipe 14, and the height of the second negative pole 7 is the same with the height of the second positive pole 15, and is preferably positioned at pipe 14 position of center line, and the second negative pole 7 is connected with vacuum electrode by wire.The interior pipe 14 lower end mouth of pipe is closed, there is individual polytetrafluoroethylene (PTFE) lid 9 upper end, interior pipe 14 is connected as one by main glass supports 13 with large glass pipe 12, main glass supports 13 is glass bars, one end and the large glass pipe 12 of glass bar are integrated, the other end and interior pipe 14 are integrated, and large glass pipe 12 and interior pipe 14 are connected as a single entity like this, play the effect of pipe 14 in supporting.Large glass pipe 12 is connected with metal bellows 24 by glass connector 5 45.Metal bellows 24 couples together with collector 26 again, and collector 26 is connected with metal bellows 25 again again, and metal bellows 25 is connected with vavuum pump 22 again.
Fig. 2 is glass connector structural representation of the present invention, and glass connector is stainless steel material manufacture.Glass connector comprises cup-shaped cylinder 16, pipe 17, disc base 18, elastic tape placement section 20 and sealing lid 23.The internal diameter of cup-shaped cylinder 16 is identical with by the external diameter of glass tube (small-size glass pipe 2 or large glass pipe 12) that is tightly connected and outer wall that is cup-shaped cylinder has external screw thread, sealing lid 23 has internal thread, hollow circular-tube 17 upper end and cup-shaped cylinder are connected as a single entity, and lower end and disc base 18 are connected as a single entity.Be provided with step in cup-shaped cylinder 16, step is elastic tape placement section 20.The bottom of cup-shaped cylinder is placed on by the one end of the glass tube sealed, rubber sealing ring 21 is placed on elastic tape placement section 20, such rubber sealing ring is just centered around by the outer wall of the glass tube sealed, metallic gasket placed by lute, the internal thread of lid 23 and the external screw thread of cup-shaped cylinder 16 agree with, rotatory sealing lid 23, sealing lid 23 just compresses metallic gasket, metallic gasket is pressed on lute 21, lute 21 is out of shape, tightly be attached to by the glass tube that seals, such glass tube just and glass connector be sealed connected together.Disk 18 can dock mutually with the clutch disk 19 of device, realizes being tightly connected of device, and clutch disk 19 only shows in air inlet pipe 1 and small-size glass pipe 2 junction by accompanying drawing of the present invention, and other junctions all need to do identical encapsulation process.The structure of glass connector 1 of the present invention, glass connector 2 42, glass connector 3 43, glass connector 4 44, glass connector 5 45 is identical, and the size of each glass connector is determined according to the actual situation of use that makes.
Device of the present invention can produce the nano particle of the coated germanium of silicon, also can produce the nano particle of germanium coated Si simultaneously.
The course of work of the equipment of Laboratory Production SiGe Core-shell Structure Nanoparticles of the present invention is: when producing the nano particle of the coated germanium of silicon, vacuumize to system, vacuum reaches below 10 handkerchiefs, passes into G from air inlet pipe 1
eh
4(germane) and Ar(argon gas) mist, GeH
4with the flow rate ratio of Ar is traditionally arranged to be between 1:40 to 1:60, and carry out adjustable pressure by control vavuum pump valve regulated or gas flow, in internal diameter one timing of small-size glass pipe 2, air pressure determines the particle size of the germanium core of the nucleocapsid structure of preparation.Radio frequency plasma is by connection first negative pole 5 and the first positive pole 1 also input power, argon plasma can be produced between the two poles of the earth, argon plasma knows from experience shock germane molecule, make germane molecular cleavage and form the nucleus of germanium, germanium nucleus is grown up and can generate germanium nano particle in small-size glass pipe 2, the nano particle generated in small-size glass pipe 2 flows to large glass pipe 12 through metallic conduit 3, large glass pipe 12 provides larger space for silicon nanoparticle, particle is dispersed in wherein better, be conducive to germanium nano grain surface coated of silicon in dispersion, the coaxal electrode structure of large glass pipe 12 more contributes to forming uniform plasma between interior pipe 14 and large glass pipe 12 compared with the top-bottom electrode structures of small-size glass pipe 2 simultaneously, just the internal diameter little employing upper/lower electrode structure of small-size glass pipe enough provides more uniform plasma to distribute, do not need to adopt internal and external electrode structure.Then the air inlet 2 11 above large glass pipe 12 passes into SiH
4the mist of (silane) and Ar, SiH
4with the gas flow ratio of Ar controls, between 1:50 to 1:70, to note SiH simultaneously
4geH in air inlet pipe 1 had better not be greater than with the flow sum of Ar
4flow sum with Ar, prevents gas backstreaming.Argon gas under the exciting of radio-frequency power between the second negative pole 7 of below and the second positive pole 15, and can form argon plasma.Argon plasma clashes into silane gas makes silane gas cracking, can cover germanium nano grain surface by the Surface Creation one deck silicon thin film at Ge particle between large glass pipe 12 and interior pipe 14, form the nano particle of the coated germanium of silicon after silane cracking.
When generating the nano particle of germanium coated Si, general principle is identical with the nano particle of the coated germanium of silicon, just the plasma passing into silane and argon gas in air inlet pipe 1, in air inlet 2 11, then pass into the plasma of germane and argon gas, its ratio is consistent with above-mentioned.So just first in small-size glass pipe 2, generate nano silicon particles, then in large glass pipe 12, remove coated Si nano particle with germanium thus the nano particle of formation germanium coated Si.
Claims (9)
1. a method for Laboratory Production SiGe Core-shell Structure Nanoparticles, is characterized in that:
Step one, vacuumize to system, vacuum reaches below 10 handkerchiefs, by the ratio input GeH between 1:40 to 1:60
4with Ar gas, according to required generation nanometer particle size size adjustment air pressure, mist produces argon plasma in radio frequency plasma, and argon plasma knows from experience shock germane molecule, make germane molecular cleavage and form the nucleus of germanium, and then germanium nucleus is grown up and can be generated germanium nano particle;
Step 2, by between 1:50 to 1:70 ratio input SiH
4with Ar gas, and make argon gas under the exciting of radio-frequency power, and form argon plasma, argon plasma clashes into silane gas makes silane gas cracking;
Generate one deck silicon thin film with the germanium nano grain surface in step one after step 3, silane gas cracking and cover germanium nano grain surface, form the nano particle of the coated germanium of silicon.
2. a method for Laboratory Production SiGe Core-shell Structure Nanoparticles, is characterized in that:
Step one, vacuumize to system, vacuum reaches below 10 handkerchiefs, by the ratio input SiH between 1:50 to 1:70
4with Ar gas, according to required generation nanometer particle size size adjustment air pressure, mist produces argon plasma in radio frequency plasma, and argon plasma knows from experience shock silane molecule, make silane molecule cracking and form the nucleus of silicon, and then silicon wafer core is grown up and can be generated nano silicon particles;
Step 2, by between 1:40 to 1:60 ratio input GeH
4with Ar gas, and make argon gas under the exciting of radio-frequency power, and form argon plasma, argon plasma clashes into Germane gas makes Germane gas cracking;
Cover nano silicon particles surface with the nano silicon particles Surface Creation one deck silicon thin film in step one after step 3, Germane gas cracking, form the nano particle of germanium coated Si.
3. the equipment of a Laboratory Production SiGe Core-shell Structure Nanoparticles, comprise small-size glass pipe (2), metallic conduit (3), large glass pipe (12), described small-size glass pipe (2) top is connected with air inlet pipe one (10) by glass connector, below is connected with metallic conduit (3) by glass connector, metallic conduit (3) is connected with large glass pipe (12) by glass connector, described metallic conduit (3) is provided with air inlet two (11), it is characterized in that: described small-size glass pipe (2) is provided with the first negative pole (5) and the first positive pole (1), first negative pole (5) and the first positive pole (1) are cylindrical electrode, described large glass pipe (12) is provided with interior pipe (14), large glass pipe (12) is provided with the second positive pole (15), interior pipe (14) is provided with the second negative pole (7), and the second positive pole (15) and the second negative pole (7) are cylindrical electrode.
4. the equipment producing SiGe Core-shell Structure Nanoparticles as above, it is characterized in that: described the first negative pole (5) is above, first positive pole (1) below, and center line between the first negative pole (5) with the first positive pole (1) and small-size glass pipe (2) center line consistent.
5. the equipment producing SiGe Core-shell Structure Nanoparticles as above, is characterized in that: the height of described the second negative pole (7) is the same with the height of the second positive pole (15), and is positioned on large glass pipe (12) position of center line.
6. the equipment producing SiGe Core-shell Structure Nanoparticles as above, it is characterized in that: described large glass pipe (12) is concentric with interior pipe (14), the ratio of large glass pipe (12) internal diameter and interior pipe (14) internal diameter is 1:4.
7. the equipment producing SiGe Core-shell Structure Nanoparticles as above, is characterized in that: described small-size glass pipe (2) is 1:5 with the ratio of large glass pipe (12) internal diameter.
8. the equipment producing SiGe Core-shell Structure Nanoparticles as above, it is characterized in that: described interior pipe (14) is provided with a glass pipe (8), there is individual polytetrafluoroethylene (PTFE) lid (9) upper end, glass pipe (8) is connected with glass connector, glass connector and vacuum electrode are connected together, interior pipe (14) the lower end mouth of pipe is closed, and interior pipe (14) and large glass pipe (12) are connected as one by main glass supports (13).
9. the equipment producing SiGe Core-shell Structure Nanoparticles as above, it is characterized in that: described glass connector is stainless steel material manufacture, it comprises cup-shaped cylinder (16), pipe (17), disc base (18), elastic tape placement section (20) and sealing lid (23); The internal diameter of cup-shaped cylinder (16) is identical with by the external diameter of glass tube that is tightly connected and outer wall that is cup-shaped cylinder has external screw thread, sealing lid (23) has internal thread, hollow circular-tube (17) upper end and cup-shaped cylinder (16) are connected as a single entity, lower end and disc base (18) are connected as a single entity, cup-shaped cylinder is provided with step in (16), and step is elastic tape placement section (20).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559946A (en) * | 2009-04-27 | 2009-10-21 | 浙江大学 | Method and device for preparing silicon nanoparticles by utilizing plasma body |
| US20090317557A1 (en) * | 2008-06-20 | 2009-12-24 | Toyota Motor Engineering & Manufacturing North America, Inc. | Process To Make Core-Shell Structured Nanoparticles |
| CN102144275A (en) * | 2008-09-03 | 2011-08-03 | 陶氏康宁公司 | Low pressure high frequency pulsed plasma reactor for producing nanoparticles |
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2014
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090317557A1 (en) * | 2008-06-20 | 2009-12-24 | Toyota Motor Engineering & Manufacturing North America, Inc. | Process To Make Core-Shell Structured Nanoparticles |
| CN102144275A (en) * | 2008-09-03 | 2011-08-03 | 陶氏康宁公司 | Low pressure high frequency pulsed plasma reactor for producing nanoparticles |
| CN101559946A (en) * | 2009-04-27 | 2009-10-21 | 浙江大学 | Method and device for preparing silicon nanoparticles by utilizing plasma body |
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