CN101377994A - Filament for electromagnetic biprism deflexion electron beam and preparation method thereof - Google Patents

Filament for electromagnetic biprism deflexion electron beam and preparation method thereof Download PDF

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Publication number
CN101377994A
CN101377994A CNA2007101212318A CN200710121231A CN101377994A CN 101377994 A CN101377994 A CN 101377994A CN A2007101212318 A CNA2007101212318 A CN A2007101212318A CN 200710121231 A CN200710121231 A CN 200710121231A CN 101377994 A CN101377994 A CN 101377994A
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China
Prior art keywords
wire rod
electromagnetic
coating
silk
nano wire
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Pending
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CNA2007101212318A
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Chinese (zh)
Inventor
车仁超
杨新安
段晓峰
李建奇
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Institute of Physics of CAS
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Institute of Physics of CAS
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Priority to CNA2007101212318A priority Critical patent/CN101377994A/en
Publication of CN101377994A publication Critical patent/CN101377994A/en
Pending legal-status Critical Current

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Abstract

The invention provides a filament of a deflection electron beam used for an electromagnetic biprism and a manufacturing method thereof. The body of the filament can be a conductive nano wire, or an insulated nano wire; and a metal coating layer is coated on the surface of the insulated nano wire, namely a compound static wire, wherein, the thickness of the metal coating layer is from 5nm to 100nm; the diameter of the nano wire is from 20nm to 1 Mum, and the length thereof is larger than the diameter of a conversion ring.

Description

A kind of filament that is used for electromagnetic biprism deflexion electron beam and preparation method thereof
Technical field
The present invention relates to a kind of manufacture method that is used for the filament of transmission electron microscope electromagnetic biprism, particularly relate to silk of a kind of electromagnetic biprism deflexion electron beam and preparation method thereof.
Background technology
Electromagnetic biprism is the critical component of transmission electron microscope as the electronics beam splitter.Electromagnetic biprism is by two boards shape ground plate and be fixed on the light hurdle, the filament that is in middle position constituted.When feeding electric current in the filament, cause that electron beam deflects, thereby form required interference pattern, so the diameter of filament and conductive capability etc. directly influence the quality of interference pattern.
The filament that is used for electromagnetic biprism at present is comparatively commonly used is Au/SiO 2Filament is (promptly at SiO 2Sputter layer of Au on the filament), its preparation method is the quartz glass bar fully heating and to drawing in oxyhydrogen flame that at first diameter is about 3mm, obtain required diameter after, again with SiO 2Filament places sputter, at its surface plating one deck gold.The prior art has been published in the 2nd phase of April in 2007 " electron microscopic journal " last " making of an ejecting gun transmission electron microscope electronic holographic static biprism silicon dioxide filament " literary composition.But because this preparation technology's operation link complexity is drawing SiO 2During filament, be difficult to keep SiO 2The uniformity of filament thickness and consistency; So poor repeatability, rate of finished products is low, makes the cost of making filament improve, thereby has restricted the use and the development of transmission electron microscope.
Summary of the invention
The objective of the invention is to: overcome the uniformity of the existing filament that is used for the transmission electron microscope electromagnetic biprism and the defective of consistency difference; And preparation technology's complicated operation, the low and defect of high cost of rate of finished products; Thereby provide a kind of filament that is used for the transmission electron microscope electromagnetic biprism that the nanometer wire rod diameter uniformity, that adopt conduction is made that has; And provide a kind of on the nanometer wire rod of insulation, and adopt conventional preparation film process to prepare the simple method of one deck conductive layer, this method can make full use of has the material of uniformity, high conformity as body more.
The objective of the invention is to realize by the following technical solutions:
According to a first aspect of the invention, a kind of silk that is used for the deflection beam of electromagnetic biprism is provided, comprise body, described body is the nanometer wire rod of conduction, perhaps described body is the nanometer wire rod of insulation, and at the surface applied layer of metal coating of nanometer wire rod of insulation, i.e. composite conducting silk (as Fig. 1); Wherein the thickness of metal coating is 5nm~100nm; The diameter of described nanometer wire rod is 20nm~1 μ m, and length is greater than the conversion ring diameter.
According to a second aspect of the invention, the nanometer wire rod of wherein said conduction is room temperature resistivity<1 * 10 -5The nanometer wire rod of Ω m.
According to a third aspect of the present invention, the nanometer wire rod of wherein said conduction is the nano wire or the nanotube of conduction.
According to a fourth aspect of the present invention, the nano wire of wherein said conduction is ZnS nano wire, Al 2O 3Nano wire or ZnO nano wire.
According to a fifth aspect of the present invention, the nanotube of wherein said conduction is carbon nano-tube or carbon-nitrogen nano tube.
According to a sixth aspect of the invention, the nanometer wire rod of wherein said insulation is room temperature resistivity 〉=1 * 10 -5The nanometer wire rod of Ω m.
According to a seventh aspect of the present invention, the nanometer wire rod of wherein said insulation is the nano wire or the nanotube of insulation.
According to an eighth aspect of the present invention, the nano wire of wherein said insulation is MgO nano wire or Si 3N 4Nano wire.
According to a ninth aspect of the present invention, the nanotube of wherein said insulation is a boron nitride nano-tube.
According to a tenth aspect of the present invention, wherein said metal coating is gold plating, platinum coating, spelter coating, nickel coating or copper coating.
According to an eleventh aspect of the present invention, provide a kind of method for preparing the silk of the above-mentioned deflection beam that is used for electromagnetic biprism, specifically comprise the steps:
1) gets a conversion ring and an electrical-conductive nanometer wire rod, after ring and electrical-conductive nanometer wire rod clean up the electrical-conductive nanometer wire rod is placed the top of changing ring with changing, with resin glue or elargol the electrical-conductive nanometer wire rod is fixed on the conversion ring, require the electrical-conductive nanometer wire rod through conversion ring center in the time of fixedly, and under stress, keep rectilinear form;
2) electrical-conductive nanometer wire rod and conversion ring are inverted on the transmission electron microscope electronic holographic light hurdle, the electrical-conductive nanometer wire rod is contacted with surface, light hurdle, the glue that point bonding is used on the two contact position, draw disconnected electrical-conductive nanometer wire rod and the tie point that conversion encircles at last, make a kind of silk of the deflection beam that is used for electromagnetic biprism of electrical-conductive nanometer wire rod.
According to a twelfth aspect of the present invention, provide a kind of method for preparing the composite conducting silk of the above-mentioned deflection beam that is used for electromagnetic biprism, specifically comprise the steps:
1) gets a conversion ring and and thoroughly do away with edge nanometer wire rod, after ring and insulating nano wire rod clean up the insulating nano wire rod is placed the top of changing ring with changing, with resin glue or elargol the insulating nano wire rod is fixed on the becket, require the insulating nano wire rod through the becket center in the time of fixedly, and under stress, keep rectilinear form;
2) utilize sputter coating process, plated film technology, electroplating film technology or vacuum evaporation coating membrane process the gold-plated coating of upper and lower surface, platinum coating, spelter coating, nickel coating or copper coating at insulating nano wire rod and conversion ring;
3) insulating nano wire rod and the conversion ring with the plating coating is inverted on the transmission electron microscope electronic holographic light hurdle, the insulating nano wire rod is contacted with surface, light hurdle, the glue that point bonding is used on the two contact position, draw the insulating nano wire rod of disconnected plating coating and the tie point of conversion ring at last, make a kind of composite conducting silk of the deflection beam that is used for electromagnetic biprism of insulating nano wire rod.
Compared with prior art, advantage of the present invention is:
1. the present invention utilizes the nanometer wire rod of conduction to substitute traditional Au/SiO 2Conductive filament is used for electromagnetic biprism, has reduced the preparation link of follow-up evaporation metal coating, and operating process is oversimplified, and cost reduces, and has avoided the contact berrier between metal and the semi-conducting material simultaneously, more can effectively reach the requirement when using.
2. the present invention uses the nanometer wire rod to substitute traditional need filament to pull-shaped one-tenth in oxyhydrogen flame, therefore can well guarantee the uniformity and the consistency of prepared filament.
The present invention can use insulation the nanometer wire rod as body, make material choice wider of the silk be used to prepare electromagnetic biprism.
Description of drawings
Fig. 1 is to be the composite conducting silk cross-sectional view of body with the insulating nano wire rod.
Embodiment
[embodiment 1]:
1) cut-off directly is 5mm, and thickness is the becket (i.e. conversion ring) of 0.5mm, cleans up, places on the silicon chip.
2) choosing diameter is 20nm, and length is ZnS nano wire, the Al of 5mm 2O 3Nano wire or ZnO nano wire, clean through ultrasonic wave earlier, clamp with tweezers then, under stereomicroscope, the ZnS nano wire placed the conversion ring above, with resin glue or elargol the ZnS nano wire is fixed on the becket, require the ZnS nano wire through the becket center in the time of fixedly, and under stress, keep rectilinear form;
In other embodiment, the diameter of ZnS nano wire can arbitrary selection from 20nm~1 μ m, and its length should be greater than the conversion ring diameter.
3) ZnS nano wire and conversion ring are inverted on the transmission electron microscope electronic holographic light hurdle, the ZnS nano wire is contacted with surface, light hurdle, the glue that point bonding is used on the two contact position toasted 6 hours; Use fine needle to draw the tie point of disconnected ZnS nano wire and becket at last, realization ZnS nano wire separates with becket, thereby makes the silk of the deflection beam that is used for electromagnetic biprism of ZnS nano wire.
[embodiment 2]:
1) cut-off directly is 5mm, and thickness is the becket (i.e. conversion ring) of 0.5mm, cleans up, places on the silicon chip.
2) choosing diameter is 20nm, length is carbon nano-tube or the carbon-nitrogen nano tube of 5mm, clean through ultrasonic wave earlier, clamp with tweezers then, under stereomicroscope, carbon nano-tube placed the conversion ring above, with resin glue or elargol carbon nano-tube is fixed on the becket, requires carbon nano-tube through the becket center in the time of fixedly, and under stress, keep rectilinear form;
In other embodiment, the diameter of carbon nano-tube can arbitrary selection from 20nm~1 μ m, and its length should be greater than the conversion ring diameter.
3) carbon nano-tube and conversion ring are inverted on the transmission electron microscope electronic holographic light hurdle, carbon nano-tube is contacted with surface, light hurdle, the glue that point bonding is used on the two contact position toasted 6 hours; Use fine needle to draw the tie point of disconnected carbon nano-tube and becket at last, the realization carbon nano-tube is separated with becket, thereby makes the silk of the deflection beam that is used for electromagnetic biprism of carbon nano-tube.
[embodiment 3]:
1) cut-off directly is 5mm, and thickness is the becket (i.e. conversion ring) of 0.5mm, cleans up, places on the silicon chip.
2) choosing diameter is 20nm, and length is MgO nano wire or the Si of 5mm 3N 4Nano wire, clean through ultrasonic wave earlier, clamp with tweezers then, under stereomicroscope, the MgO nano wire placed the conversion ring above, with resin glue or elargol the MgO nano wire is fixed on the becket, require the MgO nano wire through the becket center in the time of fixedly, and under stress, keep rectilinear form;
In other embodiment, the diameter of MgO nano wire can arbitrary selection from 20nm~1 μ m, and its length should be greater than the conversion ring diameter.
3) utilize sputter coating process, plated film technology, electroplating film technology or vacuum evaporation coating membrane process to take front, reverse side and inclination miter angle, totally 6 angles are in MgO nano wire and becket surface plated with gold coating, make its circumferential outer surface that evenly covers MgO nano wire and becket, coating layer thickness is 50nm;
In other embodiment, coating can also be platinum coating, spelter coating, nickel coating or copper coating, and wherein coating layer thickness can arbitrary selection from 5nm~100nm.
4) gold-plated MgO nano wire and conversion ring are inverted on the transmission electron microscope electronic holographic light hurdle, gold-plated MgO nano wire is contacted with surface, light hurdle, the glue that point bonding is used on the two contact position toasted 6 hours; Use fine needle to draw the tie point of disconnected gold-plated MgO nano wire and becket at last, realize separating of gold-plated MgO nano wire and becket, thereby make the composite conducting silk of the deflection beam that is used for electromagnetic biprism of MgO nano wire.
[embodiment 4]:
1) cut-off directly is 5mm, and thickness is the becket (i.e. conversion ring) of 0.5mm, cleans up, places on the silicon chip.
2) choosing diameter is 20nm, length is the boron nitride nano-tube of 5mm, clean through ultrasonic wave earlier, clamp with tweezers then, under stereomicroscope, boron nitride nano-tube placed the conversion ring above, with resin glue or elargol boron nitride nano-tube is fixed on the becket, requires boron nitride nano-tube through the becket center in the time of fixedly, and under stress, keep rectilinear form;
In other embodiment, the diameter of boron nitride nano-tube can arbitrary selection from 20nm~1 μ m, and its length should be greater than the conversion ring diameter.
3) utilize sputter coating process, plated film technology, electroplating film technology or vacuum evaporation coating membrane process to take front, reverse side and inclination miter angle, totally 6 angles are in boron nitride nano-tube and becket surface plated with gold coating, make its circumferential outer surface that evenly covers boron nitride nano-tube and becket, coating layer thickness is 50nm;
In other embodiment, coating can be platinum coating, spelter coating, nickel coating or copper coating, and wherein metal coating thickness can arbitrary selection from 5nm~100nm.
4) gold-plated boron nitride nano-tube and conversion ring are inverted on the transmission electron microscope electronic holographic light hurdle, gold-plated boron nitride nano-tube is contacted with surface, light hurdle, the glue that point bonding is used on the two contact position toasted 6 hours; Use fine needle to draw the tie point of disconnected gold-plated boron nitride nano-tube and becket at last, realize separating of gold-plated boron nitride nano-tube and becket, thereby make the composite conducting silk of the deflection beam that is used for electromagnetic biprism of boron nitride nano-tube.

Claims (12)

1. a silk that is used for the deflection beam of electromagnetic biprism comprises body, it is characterized in that, described body is the nanometer wire rod of conduction, perhaps described body is the nanometer wire rod of insulation, and at the surface applied layer of metal coating of nanometer wire rod of insulation, i.e. composite conducting silk; Wherein the thickness of metal coating is 5nm~100nm; The diameter of described nanometer wire rod is 20nm~1 μ m, and length is greater than the conversion ring diameter.
2. the silk that is used for the deflection beam of electromagnetic biprism according to claim 1 is characterized in that: the nanometer wire rod of described conduction is room temperature resistivity<1 * 10 -5The nanometer wire rod of Ω m.
3. the silk that is used for the deflection beam of electromagnetic biprism according to claim 1 is characterized in that: the nanometer wire rod of described conduction is the nano wire or the nanotube of conduction.
4. the silk that is used for the deflection beam of electromagnetic biprism according to claim 3 is characterized in that: the nano wire of described conduction is ZnS nano wire, Al 2O 3Nano wire or ZnO nano wire.
5. the silk that is used for the deflection beam of electromagnetic biprism according to claim 3 is characterized in that: the nanotube of described conduction is carbon nano-tube or carbon-nitrogen nano tube.
6. the silk that is used for the deflection beam of electromagnetic biprism according to claim 1 is characterized in that: the nanometer wire rod of described insulation is room temperature resistivity 〉=1 * 10 -5The nanometer wire rod of Ω m.
7. the silk that is used for the deflection beam of electromagnetic biprism according to claim 1 is characterized in that: the nanometer wire rod of described insulation is the nano wire or the nanotube of insulation.
8. the silk that is used for the deflection beam of electromagnetic biprism according to claim 7 is characterized in that: the nano wire of described insulation is MgO nano wire or Si 3N 4Nano wire.
9. the silk that is used for the deflection beam of electromagnetic biprism according to claim 7 is characterized in that: the nanotube of described insulation is a boron nitride nano-tube.
10. the silk that is used for the deflection beam of electromagnetic biprism according to claim 1 is characterized in that: described metal coating is gold plating, platinum coating, spelter coating, nickel coating or copper coating.
11. a method for preparing the silk of the described deflection beam that is used for electromagnetic biprism of claim 1 is characterized in that comprising the steps:
1) gets a conversion ring and a nanometer wire rod, after ring and nanometer wire rod clean up the nanometer wire rod is placed the top of changing ring with changing, with resin glue or elargol the nanometer wire rod is fixed on the conversion ring, require the nanometer wire rod through conversion ring center in the time of fixedly, and under stress, keep rectilinear form;
2) electrical-conductive nanometer wire rod and conversion ring are inverted on the transmission electron microscope electronic holographic light hurdle, the electrical-conductive nanometer wire rod is contacted with surface, light hurdle, the glue that point bonding is used on the two contact position, draw disconnected electrical-conductive nanometer wire rod and the tie point of changing ring at last, thereby make a kind of silk of the deflection beam that is used for electromagnetic biprism of electrical-conductive nanometer wire rod.
12. a method for preparing the composite conducting silk of the described deflection beam that is used for electromagnetic biprism of claim 1 is characterized in that comprising the steps:
1) gets a conversion ring and and thoroughly do away with edge nanometer wire rod, after ring and insulating nano wire rod clean up the insulating nano wire rod is placed the top of changing ring with changing, with resin glue or elargol the insulating nano wire rod is fixed on the becket, require the insulating nano wire rod through the becket center in the time of fixedly, and under stress, keep rectilinear form;
2) utilize sputter coating process, plated film technology, electroplating film technology or vacuum evaporation coating membrane process the gold-plated coating of upper and lower surface, platinum coating, spelter coating, nickel coating or copper coating at insulating nano wire rod and conversion ring;
3) insulating nano wire rod and the conversion ring with the plating coating is inverted on the transmission electron microscope electronic holographic light hurdle, the insulating nano wire rod is contacted with surface, light hurdle, the glue that point bonding is used on the two contact position, draw the insulating nano wire rod of disconnected plating coating and the tie point of conversion ring at last, thereby make a kind of composite conducting silk of the deflection beam that is used for electromagnetic biprism of insulating nano wire rod.
CNA2007101212318A 2007-08-31 2007-08-31 Filament for electromagnetic biprism deflexion electron beam and preparation method thereof Pending CN101377994A (en)

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CNA2007101212318A CN101377994A (en) 2007-08-31 2007-08-31 Filament for electromagnetic biprism deflexion electron beam and preparation method thereof

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Application Number Priority Date Filing Date Title
CNA2007101212318A CN101377994A (en) 2007-08-31 2007-08-31 Filament for electromagnetic biprism deflexion electron beam and preparation method thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101976594A (en) * 2010-08-31 2011-02-16 中国科学院苏州纳米技术与纳米仿生研究所 Composite conductor application of carbon nano tube fiber and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101976594A (en) * 2010-08-31 2011-02-16 中国科学院苏州纳米技术与纳米仿生研究所 Composite conductor application of carbon nano tube fiber and preparation method thereof

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Open date: 20090304