CN102515092B - Method for manufacturing micro-spring - Google Patents
Method for manufacturing micro-spring Download PDFInfo
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- CN102515092B CN102515092B CN201110397334.3A CN201110397334A CN102515092B CN 102515092 B CN102515092 B CN 102515092B CN 201110397334 A CN201110397334 A CN 201110397334A CN 102515092 B CN102515092 B CN 102515092B
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Abstract
The invention relates to a method for manufacturing a micro-spring by using a fracture control method. According to the method disclosed by the invention, the micro-spring is manufactured on the basis of controlling three-dimensional fracture. The method comprises the following steps of: coating a layer of oxide sol on a hard fiber material of which the diameter is of a micron scale; forming a core-shell-structure spindle knot taking the hard fiber material as a core and the oxide sol as a shell by fracturing a liquid membrane of the oxide sol; and forming the core-shell-structure spindle knot taking the oxide sol as the shell when a solvent in an oxide sol shell layer of the spindle knot is volatilized. Because of a special core-shell structure and heterogeneous core-shell components of the spindle knot, the spindle knot not only has a weak core-shell interface, but also has different thermal expansion coefficients. When the spindle knot is subjected to heating treatment, a core-shell material with different thermal expansion coefficients generates a heat stress. Under the action of the heat stress, the weak interface of the spindle knot cracks, and then the regular micro-spring is formed on the shell layer.
Description
Technical field
The invention belongs to chemical, functional material, micron and technical field of nano-processing, be particularly prepared the method for Microspring with Fracture Control method.
Background technology
Along with the development of technology, the microminiaturization of device is to realize its multi-functional and integrated important channel, especially the development of microflow control technique in recent years, undersized MEMS (MEMS) power consumption less, the aspect such as the response time is short, accuracy is high, fast response time demonstrates excellent performance, thereby has broad application prospects in fields such as precision instrument, biologic medical and science and techniques of defence.Growing along with micro element demand, needs ripe process technology low cost to prepare in large quantity micro element at present in a hurry.
As one of most important part drive unit in micro element, the process technology of Microspring receives much concern.At present, traditional Microspring making is mainly based on MEMS technology-MEMS both at home and abroad, comprises chemical corrosion method, photoetching electroforming or plastic casting method, magnetic property method.First two method can only obtain the plane spring of two yardsticks, cannot meet the requirement of rapidoprint diversity, and has processing technology complexity, cycle is long, the deficiency of the aspects such as equipment investment is large, and mask electro-deposition method, although can obtain the spring of three dimension scale, but need to make in advance mask plate, the quality of gained spring depends critically upon the manufacture craft of mask plate, and its preparation process exists processing technology complexity, and the cycle is long, equipment investment is large, prepares the first-class problem of bill of materials.How to seek a kind of method of preparing Microspring simple to operate, with low cost, become one of focal issue of people's concern.
Laser or the laser assisted preparation for processing of Microspring are disclosed in CN101025211A and CN101130196.Although this two method has been broken away from the restriction to rapidoprint, can prepare the three-dimensional spring of different materials, but its manufacturing process need to be made supporting mould, accurate numerical control positioning device and expensive LASER Light Source, still there is processing technology complexity, cycle is long, the problems such as equipment investment is large, thus be unfavorable for preparation in enormous quantities.
Summary of the invention
What the object of the present invention is to provide that a kind of cost is low, speed is fast, simple and convenient is prepared the method for Microspring with Fracture Control method.
The preparation method of Microspring of the present invention comprises the following steps (preparation process can referring to Fig. 2):
(1) the hard fibre material fluid sealant cleaning up is fixed on U-shaped support;
(2) polymer is dissolved in organic solvent, stirs, polymer is dissolved completely, obtain polymer solution, then regulate resulting polymers solution to be acid with acid solution, the pH value of preferred polymers solution is 2.6; And then add the precursor of oxide sol, and stir, make it to form uniform and stable oxide sol;
(3) the U-shaped support that step (1) is fixed with to hard fibre material is impregnated in the oxide sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with hard fibre material is lifted out from oxide sol, dry (the general dry time is 12～24 hours) prepares the oxide gel spinning club with nucleocapsid structure on hard fibre material; Its mesochite is by the dry rear oxide gel forming of oxide sol; Its mesochite is that core is hard fibre material by the dry rear oxide gel forming of oxide sol; Then calcine, make to have oxidized the removing of shell organic matter (containing organic matter in oxide gel) in the oxide gel spinning club of nucleocapsid structure, form inorganic oxide shell, in forming inorganic oxide shell, shell cracking obtains inorganic oxide Microspring.
The hard fibre nuclear material that the present invention can further ftracture shell in the inorganic oxide Microspring obtaining is removed, the described method of removing can ftracture the shell with hard fibre nuclear material the inorganic oxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), removes (as shown in Figure 1) by microoperation arm.
Described being fixed on U-shaped support with fluid sealant, is the opening one end that hard fibre material is fixed on to U-shaped support.
Described fluid sealant preferably uses two-component silicone rubber, and its solidification temperature is normal temperature, and be 0.5～2 hour hardening time, and this kind of fluid sealant can use in temperature is the environment of-200～800 DEG C.
Described cleaning can be cleaned with pure water, acetone, ethanol successively, then uses inert gas (as nitrogen) to dry up.
The diameter of described hard fibre material is 5～80 microns; Hard fibre material is selected from the one in carbon fiber, glass fibre, stainless steel wire, nickel alloy wire, Kafra fiber etc.
The molar ratio of the polymer in the uniform and stable oxide sol of described formation and the presoma of oxide sol is 1: 18～1: 234000.
The mass concentration of described polymer solution is preferably 3～16%.
Described polymer is selected from the one in polyethers (P123, F68 and F127), polyvinylpyrrolidone (PVP), polymethyl methacrylate (PMMA).
Described organic solvent is selected from the one in ethanol, isopropyl alcohol, DMF (DMF), oxolane (THF).
The concentration of described acid solution is preferably 1M; Be selected from the one in hydrochloric acid, sulfuric acid, nitric acid, acetic acid.
The precursor of described oxide sol is selected from the one in the group that isopropyl titanate, tetraethyl orthosilicate, butyl titanate, tetrabutyl zirconate, aluminium isopropoxide, bismuth nitrate and ferric nitrate form.
Described oxide sol is selected from the one in the group that TiO 2 sol, silicon dioxide gel, zirconia sol, alumina sol, iron oxide colloidal sol and bismuthic acid ferrum collosol form.
The temperature of described high-temperature calcination is 450～600 DEG C; The time of described high-temperature calcination is generally 24～48 hours.
The fracture of the Microspring that the inventive method prepares based on controlling three dimension scale obtains, thereby the present invention is by controlling thermal stress controlled fracturing blasting pattern, prepares Microspring shape.Coated one deck oxide sol on the hard fibre material that the present invention is micro-meter scale at diameter, breaking of liquid film by oxide sol formed taking hard fibre material as core, oxide sol is the spindle joint of the nucleocapsid structure of shell, when after the solvent evaporates in the oxide sol shell of this kind of spindle joint, form the spindle joint of the nucleocapsid structure that oxide gel is shell.Due to the special nucleocapsid structure of spindle joint and heterogeneous nucleocapsid composition, this kind of spindle joint not only has weak nucleocapsid interface, and has different thermal coefficient of expansions.Heated when this kind of spindle joint, the core-shell material with different heat expansion coefficient produces thermal stress.Under thermal stress effect, the weak interface place of spindle joint ftractures, at the Microspring of shell formation rule.The present invention is based on Microspring prepared by controlled fracturing blasting method have the controlled regular helical structure of shape, suitable material extensively, without precision instrument, feature cheaply.Spring-like prepared by the present invention, because it is structurally ordered, shape is controlled, and its inside has meso-hole structure, especially it prepares material selection extensively, can be various inorganic oxide materials, ceramic material, metal and polymeric material, so it will have broad application prospects in the fields such as senser element, optics, drive unit, electromagnetic shielding material.
Brief description of the drawings
Fig. 1. method of the present invention is prepared the electron scanning micrograph of gained Microspring.
Fig. 2. the preparation process schematic diagram (comprising step (1)～(8)) of the titanium dioxide Microspring of the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but should not regard the restriction to technical solution of the present invention as.
Embodiment 1.
The preparation process of titanium dioxide Microspring shown in Figure 1.
(1) be that the carbon fiber of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the carbon fiber cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to carbon fiber is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with carbon fiber is lifted out from TiO 2 sol, dry 12～24 hours, on carbon fiber, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is carbon fiber; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with carbon fiber nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove (as shown in Figure 1) by microoperation arm.
Embodiment 2
(1) be that the carbon fiber of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the carbon fiber cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL isopropyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 5.1 grams of isopropyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 17.3 grams;
(3) the U-shaped support that step (1) is fixed with to carbon fiber is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with carbon fiber is lifted out from TiO 2 sol, dry 12～24 hours, on carbon fiber, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is carbon fiber; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with carbon fiber nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove (as shown in Figure 1) by microoperation arm.
Embodiment 3.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 4.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 3.2 grams of P123 (molecular weight is 5800) are dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it the even stable dioxy of shape and become homogenizing titanium colloidal sol, its quality is 20.6 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 5.
(1) be that the glass fibre of 10 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 6.
(1) be that the glass fibre of 80 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 7.
(1) be that the stainless steel fibre of 24 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the stainless steel fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to stainless steel fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on stainless steel fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is stainless steel fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with stainless steel fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSSMP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 8.
(1) be that the nickel alloy fiber of 20 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the nickel alloy fiber cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to nickel alloy fiber is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with nickel alloy fiber is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is nickel alloy fiber; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with nickel alloy fiber nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSSMP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 9.
(1) be that the Kafra fiber of 20 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the Kafra fiber cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to Kafra fiber is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with nickel alloy fiber is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is Kafra fiber; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with Kafra fiber nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSSMP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 10.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of F68 (molecular weight is 8350) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, F68 is dissolved completely and obtain F68 ethanolic solution, regulating the pH value of F68 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as F68) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 11.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of F127 (molecular weight is 11500) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, F127 is dissolved completely and obtain F127 ethanolic solution, regulating the pH value of F127 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as F127) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 12.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of PVP (molecular weight is 1300000) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, PVP is dissolved completely and obtain clear solution, regulating the pH value of PVP solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as PVP) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 13.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of PMMA (molecular weight is 350000) is dissolved in 10mL DMF, at room temperature stir, PMMA is dissolved completely and obtain clear solution, regulating the pH value of PMMA solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as PMMA) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 14.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of PMMA (molecular weight is 350000) is dissolved in 10mL THF, at room temperature stir, PMMA is dissolved completely and obtain clear solution, regulating the pH value of PMMA solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as PMMA) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 15.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL isopropyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 aqueous isopropanol, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 16.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL isopropyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 aqueous isopropanol, regulating the pH value of P123 solution with 1M sulfuric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 17.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL isopropyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 aqueous isopropanol, regulating the pH value of P123 solution with 1M nitric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 18.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL isopropyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 aqueous isopropanol, regulating the pH value of P123 solution with 1M acetic acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 19.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL ethanol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 3.74 grams of ethyl orthosilicates to stir 30 minutes, make it to form uniform and stable silicon dioxide gel, its quality is 15.9 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from silicon dioxide gel, dry 12～24 hours, on glass fibre, prepare the silica dioxide gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear silica dioxide gel forming of silicon dioxide gel, contains organic components (as P123) in this kind of silica dioxide gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form silica shell, in forming silica shell, silica shell cracking obtains silica Microspring.
Shell with glass fibre nuclear material is ftractureed to the silica Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 20.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL ethanol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 3.67 grams of aluminium isopropoxides to stir 30 minutes, make it to form uniform and stable alumina sol, its quality is 15.9 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the alumina sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from alumina sol, dry 12～24 hours, on glass fibre, prepare the alumina gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear alumina gel forming of alumina sol, contains organic components (as P123) in this kind of alumina gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the alumina gel spindle joint of nucleocapsid structure, form aluminium oxide shell, in forming aluminium oxide shell, aluminium oxide shell cracking obtains aluminium oxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the aluminium oxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 21.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL ethanol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.9 grams of tetrabutyl zirconates to stir 30 minutes, make it to form uniform and stable zirconia sol, its quality is 19.1 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the alumina sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from zirconia sol, dry 12～24 hours, on glass fibre, prepare the zirconia pick gel spinning club with nucleocapsid structure; Its mesochite is by the dry rear zirconia gel forming of zirconia sol, contains organic components (as P123) in this kind of zirconia gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the zirconia gel spinning club of nucleocapsid structure, form zirconia shell, in forming zirconia shell, zirconia shell cracking obtains zirconia Microspring.
Shell with glass fibre nuclear material is ftractureed to the zirconia Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 22.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 7.23 grams of ferric nitrates to stir 30 minutes, make it to form uniform and stable iron oxide colloidal sol, its quality is 19.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the iron oxide colloidal sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from iron oxide colloidal sol, dry 12～24 hours, on glass fibre, prepare the iron oxide gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear iron oxide gel forming of iron oxide colloidal sol, contains organic components (as P123) in this kind of iron oxide gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the iron oxide gel spindle joint of nucleocapsid structure, form iron oxide shell, in forming iron oxide shell, iron oxide shell cracking obtains iron oxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the iron oxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 23.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 7.2 grams of ferric nitrates and 8.7 grams of bismuth nitrates, stir 30 minutes, make it to form uniform and stable bismuthic acid ferrum collosol, its quality is 28.1 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the bismuthic acid ferrum collosol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from bismuthic acid ferrum collosol, dry 12～24 hours, on glass fibre, prepare the bismuthic acid iron gel spinning club with nucleocapsid structure; Its mesochite is by the dry rear bismuthic acid iron gel forming of bismuthic acid ferrum collosol, contains organic components (as P123) in this kind of bismuthic acid iron gel; Core is glass fibre; Then be at 450 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the bismuthic acid iron gel spinning club of nucleocapsid structure, form bismuthic acid iron-clad layer, in forming bismuthic acid iron-clad layer, bismuthic acid iron-clad layer cracking obtains iron oxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the bismuthic acid iron Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 24.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 500 DEG C, to carry out high-temperature calcination 24 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Embodiment 25.
(1) be that the glass fibre of 5 microns cleans with pure water, acetone, ethanol successively by diameter, nitrogen dries up; Then the glass fibre cleaning up being fixed on to a base length with two-component silicone rubber is 5 centimetres, and height is 2 centimetres, on the U-shaped support that material is stainless steel alloy;
(2) 1 gram of P123 (molecular weight is 5800) is dissolved in 10mL absolute ethyl alcohol, at room temperature stir, P123 is dissolved completely and obtain P123 ethanolic solution, regulating the pH value of P123 solution with 1M hydrochloric acid is 2.6, add again 6.2 grams of butyl titanates to stir 30 minutes, make it to form uniform and stable TiO 2 sol, its quality is 18.4 grams;
(3) the U-shaped support that step (1) is fixed with to glass fibre is impregnated in the TiO 2 sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with glass fibre is lifted out from TiO 2 sol, dry 12～24 hours, on glass fibre, prepare the titania gel spindle joint with nucleocapsid structure; Its mesochite is by the dry rear titania gel forming of TiO 2 sol, contains organic components (as P123) in this kind of titania gel; Core is glass fibre; Then be at 600 DEG C, to carry out high-temperature calcination 48 hours in temperature, make to have oxidized the removing of shell organic matter in the titania gel spindle joint of nucleocapsid structure, form titanium dioxide shell, in forming titanium dioxide shell, titanium dioxide shell cracking obtains titanium dioxide Microspring.
Shell with glass fibre nuclear material is ftractureed to the titanium dioxide Microspring that obtains in SuSS MP5 analysis probe platform (Karl Suss company), remove by microoperation arm.
Claims (10)
1. a preparation method for Microspring, is characterized in that, described method comprises the following steps:
(1) the hard fibre material fluid sealant cleaning up is fixed on U-shaped support;
(2) polymer is dissolved in organic solvent, stirs, polymer is dissolved completely, obtain polymer solution, then regulate resulting polymers solution to be acid with acid solution, and then add the precursor of oxide sol, stir, make it to form uniform and stable oxide sol;
(3) the U-shaped support that step (1) is fixed with to hard fibre material is impregnated in the oxide sol that step (2) obtains, adopt czochralski method, the U-shaped support that is fixed with hard fibre material is lifted out from oxide sol, dry, on hard fibre material, prepare the oxide gel spinning club with nucleocapsid structure; Its mesochite is that core is hard fibre material by the dry rear oxide gel forming of oxide sol; Then calcine, make to have oxidized the removing of shell organic matter in the oxide gel spinning club of nucleocapsid structure, form inorganic oxide shell, in forming inorganic oxide shell, shell cracking obtains inorganic oxide Microspring.
2. preparation method according to claim 1, is characterized in that: the shell with hard fibre nuclear material is ftractureed to the inorganic oxide Microspring that obtains in SuSS MP5 analysis probe platform, remove hard fibre nuclear material by microoperation arm.
3. preparation method according to claim 1, is characterized in that: the diameter of described hard fibre material is 5～80 microns;
Described hard fibre material is selected from the one in carbon fiber, glass fibre, stainless steel wire, nickel alloy wire, Kafra fiber.
4. preparation method according to claim 1, is characterized in that: the molar ratio of the polymer in the uniform and stable oxide sol of described formation and the presoma of oxide sol is 1:18～1:234000.
5. according to the preparation method described in claim 1 or 4, it is characterized in that: described polymer is selected from the one in polyethers, polyvinylpyrrolidone, polymethyl methacrylate.
6. preparation method according to claim 1, is characterized in that: described organic solvent is selected from the one in DMF, ethanol, isopropyl alcohol, oxolane.
7. preparation method according to claim 1, is characterized in that: described acid solution is selected from the one in hydrochloric acid, sulfuric acid, nitric acid, acetic acid.
8. according to the preparation method described in claim 1 or 4, it is characterized in that: the precursor of described oxide sol is selected from least one in the group that isopropyl titanate, tetraethyl orthosilicate, butyl titanate, tetrabutyl zirconate, aluminium isopropoxide, bismuth nitrate, ferric nitrate form.
9. according to the preparation method described in claim 1 or 4, it is characterized in that: described oxide sol is selected from the one in the group that TiO 2 sol, silicon dioxide gel, zirconia sol, alumina sol, iron oxide colloidal sol and bismuthic acid ferrum collosol form.
10. preparation method according to claim 1, is characterized in that: the temperature of described calcining is 450～600 DEG C.
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| CN1948143A (en) * | 2006-11-13 | 2007-04-18 | 南京大学 | Method of symmetrically growing spiral carbon tube |
| CN100999315A (en) * | 2006-12-26 | 2007-07-18 | 华东理工大学 | Method of preparing spiral nanometer carbon fiber |
| CN101007632A (en) * | 2007-01-19 | 2007-08-01 | 中国科学院山西煤炭化学研究所 | Method for preparing spiral nanometre carbon tube |
| CN101200283A (en) * | 2007-12-14 | 2008-06-18 | 天津理工大学 | Simple method for preparing large-area metal or metal-oxide nano ring |
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| US6636676B1 (en) * | 1998-09-30 | 2003-10-21 | Optomec Design Company | Particle guidance system |
| KR20100075341A (en) * | 2008-12-24 | 2010-07-02 | 실버레이 주식회사 | Micro-spring manufacturing method and micro-spring manufacturing apparatus |
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| CN1948143A (en) * | 2006-11-13 | 2007-04-18 | 南京大学 | Method of symmetrically growing spiral carbon tube |
| CN100999315A (en) * | 2006-12-26 | 2007-07-18 | 华东理工大学 | Method of preparing spiral nanometer carbon fiber |
| CN101007632A (en) * | 2007-01-19 | 2007-08-01 | 中国科学院山西煤炭化学研究所 | Method for preparing spiral nanometre carbon tube |
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