CN104152851A - Method for manufacturing tellurium elementary substance nano materials of controllable structure - Google Patents
Method for manufacturing tellurium elementary substance nano materials of controllable structure Download PDFInfo
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- CN104152851A CN104152851A CN201410403628.6A CN201410403628A CN104152851A CN 104152851 A CN104152851 A CN 104152851A CN 201410403628 A CN201410403628 A CN 201410403628A CN 104152851 A CN104152851 A CN 104152851A
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Abstract
The invention provides a method for manufacturing tellurium elementary substance nano materials of a controllable structure. Laser excitation is adopted to enable tellurium elements to be sputtered out from a metal telluride target material in the gas atmosphere, suspended tellurium ions are formed, and under the effects of electric field force and gravitational force, the suspended tellurium ions are deposited on a tellurium nano material deposition target connected with a positive pole to obtain a tellurium nano material array. Incident laser energy, electric field intensity and/or deposition target temperature are controlled to achieve array morphological control over the tellurium elementary substance nano materials. The method overcomes the defects that a tellurium elementary substance nano material array manufactured by a currently-used method is single and cannot be controlled, and has the good market popularization value.
Description
Technical field
The invention belongs to inorganic nano material preparing technical field, the preparation method of the controlled tellurium simple substance nanometer material of a kind of structure is provided especially.
Background technology
Tellurium is a kind of important low-gap semiconductor (direct band gap 0.35eV), not only has the physical propertiess such as good electric conductivity, pyroelectricity, piezoelectricity, polarizability and nonlinear optics, and aspect gas sensing, has good application.Due to the high anisotropy of its crystalline structure itself, can be without template, crystal seed, tensio-active agent auxiliary, just can form one dimension tubular structure, this has excited the research interest of numerous chemosynthesis man.
In in recent years, about the one dimension tubular structure synthetic method of tellurium, there are reports, as physical evaporation method 560 DEG C of evaporation telloys 2 hours under argon shield for: Li Yadong seminar, prepare tellurium micron tube [the J. Mater. Chem. of hexagonal cross-section, 2004,14,244 – 247]; Qian Yitai seminar puts into reactor by hydrothermal method by sodium tellurite and ammoniacal liquor and keeps ~ 180 DEG C, 36 hours, prepares the cylindricality tellurium nanotube [Adv. Mater., 2002,14,1658-1662] of both ends open; Xia Younan seminar by orthotelluric acid and the ethylene glycol 2h that refluxes at 197 DEG C, prepares the solid tellurium nanotube [Adv. Mater., 2002,14,279-282] with hexagonal cross-section in the middle of both ends open by the method for backflow polyvalent alcohol.But these methods mostly, because complicated operation or reaction times are long or temperature of reaction is higher, cause preparation cost high-leveled and difficult with industrialization promotion.
Beijing University of Technology's application number is: the preparation method of a 201110385352.X(high-purity tellurium nanometer powder) invention, adopt the evaporation of noble gas protection-direct current arc, taking the nonmetal high purity tellurium piece of simple substance (purity is as 99.999%) as anode, tungsten is negative electrode, in the atmosphere that is 0.05-0.3MPa at ar pressure, reaction current 30～50A, anode and cloudy voltage across poles are 30～50V, reaction times is 20～40min, it is 20～100nm tellurium nano-powder material that particle diameter is prepared in condensation, but because it requires harsher to starting material, be difficult to realize industrialization.
The Chinese application number that State Nanometer Science Center declares is 201310436069.4 a kind of have the tellurium nano-wire array of field emission characteristic, with and preparation method thereof and application, by the physical vapor precipitator method, taking tellurium as evaporation source, and on silicon chip, deposit tellurium nano-wire and obtain described tellurium nano-wire array.By controlling temperature, base reservoir temperature and the depositing time of tellurium evaporation source in physical vapor precipitation process, can obtain the tellurium nano-wire array with sharp-pointed port; Particularly, it is conical or cylindrical that the top of described tellurium nano-wire array is, or described tellurium nano-wire array is made up of conical tellurium nano-wire.In this invented technology process, use high concentration of hydrofluoric acid, hazardness is very big, can not realize eco-friendly function, and the value that therefore industry is promoted is lower.
Dalian University of Technology's application number is a kind of method use coating by pulse electrochemical deposition technology of preparing tellurium-lead telluride nano crystal assembling superlattice nano line array of 201410000512.8, the electrolytic solution that contains plumbous and tellurium element is carried out to coating by pulse electrochemical deposition, obtain Te-PbTe crystal assembling superlattice nano line.Because the method needs first obtain porous anodic alumina template by anonizing, then sputter gold evaporation film is electrode, more loaded down with trivial details, is unfavorable for producing in enormous quantities.
In sum, the exhaust system of general sputter equipment is all used oil diffusion pump system substantially, the operating pressure higher (usually above 1Pa) of diode sputtering, in this pressure range, diffusion pump works hardly, main valve is in closing condition, and exhaust velocity is little, and in base vacuum and argon gas, residual atmosphere on sputter coating impact greatly.
Secondly, the sedimentation rate of diode sputtering plated film is low, and thick films more than 10 μ m should not adopt this method to be coated with.Why lower diode sputtering speed is, is to be determined by its discharge type.Distance between diode sputtering negative electrode and anode is conventionally in 2 ~ 6 ㎝ left and right, and spacing is excessive, and sedimentation rate declines too fast.Spacing is excessively near, and secondary electron is too short at the move distance of two interpolars, sustain discharge difficulty.It is also to hinder the reason that sputter rate improves that the heat dissipation of target surface is not gone out.Diode sputtering target voltage high (several kilovolts), target current is low, and the heat dissipation power of target has become to improve the obstacle of target power output.
Finally, a large amount of secondary electrons directly bombards substrate, and making substrate temperature too high is the another obvious shortcoming of diode sputtering.This can make substrate cause the radiation injury of some performance irreversible change.
Summary of the invention
The object of the invention is to overcome the preparation process complexity that prior art exists, influence factor is many, the tellurium structure preparing is single, be unfavorable for the problem of industrialization, the preparation method of the controlled laser tellurium of a kind of structure simple substance nanometer material is provided, this laser tellurium simple substance nanometer material preparation method, there is preparation process simple, tellurium nano material array process of growth is controlled, and because laser excitation is sputtered to the advantages such as local heating growing environment temperature is controlled, fundamentally address the above problem, be specially adapted to Industry Promotion.
For achieving the above object, technical scheme of the present invention is to comprise the following steps:
(1) adopt the laser incident metal telluride target that sends of LASER Light Source, utilize laser excitation sputter principle, tellurium element is gone out from the metal telluride target as sputter in atmosphere, become suspension tellurium ion;
(2) on positive pole and tellurium nano material deposition targets, negative pole is collected target with impurity and is connected, tellurium nano material deposition targets and impurity are collected under the electrical forces and action of gravity producing between target, and by suspension tellurium ion deposition, on tellurium nano material deposition targets, deposition obtains tellurium nano material array;
By the step to described (1) and step, (control of incident laser energy, strength of electric field and/or deposition targets carried charge and/or temperature in 2 realizes the array morphology control of tellurium simple substance nanometer material.
Further arranging is that described LASER Light Source is the adjustable LASER Light Source of pulse that gas, solid, liquid excite, and the energy of described LASER Light Source is 10W ~ 1000W.
Further arranging is in described step (1) to be 5 ~ 90 ° by laser incident and metal telluride target angle, and the middle laser excitation working hour of described step (1) is 1 ~ 1000s.
Further arranging is that described metal telluride target is lath or the powder that any metal telluride is made.
Further arranging is that the described middle work climate electric field of step (2) is DC electric field, and strength of electric field scope is: 100 ~ 1000N/C.
Further arranging is that the substrate material of described tellurium nano material deposition targets is silicon chip, and described silicon chip pre-treatment is to carry out surface cleaning through TruMicro7050 laser equipment.
Further arrange is that described step (1) and step (2) work climate is the gas that argon gas, helium or its arbitrary proportion mix.
Further arrange is that described metal telluride target pre-treatment mode is as follows:
Under normal temperature condition, metal telluride plate or powder are placed in to dehydrated alcohol, dipping 5 ~ 30min, takes out, dry under 60 ~ 150 DEG C of environment.
The temperature that further setting is tellurium nano material deposition targets is controlled, and its span of control is: 0 ~ 300 DEG C.
The carried charge that further setting is tellurium nano material deposition targets and impurity collecting board is controlled by impressed voltage.
Principle of the present invention and advantage are:
Telluride target is in atmosphere of inert gases, impact through high energy laser beam, moment distillation becomes telluride steam, under the electric field action of working spaces, tellurium ion moves to the tellurium simple substance nano-precipitation target direction of positively charged, and be finally deposited on this target, reasonably adjust by the temperature to laser beam energy, deposition targets and carried charge, can obtain the tellurium simple substance nanometer material of any array structure.
Tellurium simple substance nanometer material preparation method involved in the present invention, preparation process is simple, because laser excitation is sputtered to local heating, by the Temperature Setting of deposition targets, can further improve the purity of tellurium simple substance nanometer material, therefore relatively low to the purity requirement of sputter material, be specially adapted to suitability for industrialized production.
Below in conjunction with specification drawings and specific embodiments, the present invention is described further.
Brief description of the drawings
Fig. 1 is tellurium simple substance nanometer material preparation process schematic diagram.
Embodiment
Below by embodiment, the present invention is specifically described; only be used to further illustrate the present invention; can not be interpreted as limiting the scope of the present invention, the technician in this field can make some nonessential improvement and adjustment to the present invention according to the content of foregoing invention.
Embodiment 1
Telluride target is tellurium copper, and the LASER Light Source of use is CO
2laser apparatus, power 10W, the angle of laser incident and target is 5 °, firing time is 1s, strength of electric field is 100N/C, and tellurium nano material deposition targets temperature is 150 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtain point-like tellurium nano material array, granularity size 1 μ m.
Embodiment 2
Telluride target is tellurium copper, and the LASER Light Source of use is CO
2laser apparatus, power 50W, the angle of laser incident and target is 5 °, firing time is 10s, strength of electric field is 100N/C, and tellurium nano material deposition targets temperature is 150 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtain bar shaped tellurium nano material array, crystal grain length is 10 μ m.
Embodiment 3
Telluride target is tellurium copper, and the LASER Light Source of use is CO
2laser apparatus, power 50W, the angle of laser incident and target is 45 °, firing time is 1000s, strength of electric field is 100N/C, tellurium nano material deposition targets temperature is 150 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtains hexagonal array structure tellurium nano material.
Embodiment 4
Telluride target is tellurium copper, and the LASER Light Source of use is CO
2laser apparatus, power 500W, the angle of laser incident and target is 30 °, firing time is 100s, and strength of electric field is 200N/C, and tellurium nano material deposition targets temperature is 50 DEG C, extremely be applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtain needle-like array structure tellurium nano material.
Embodiment 5
Telluride target is lead telluride, and the LASER Light Source of use is CO
2laser apparatus, power 500W, the angle of laser incident and target is 60 °, firing time is 150s, strength of electric field is 1000N/C, and tellurium nano material deposition targets temperature is 300 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtain ball array structure tellurium nano material, grain-size is 50 μ m.
Embodiment 6
Telluride target is lead telluride, and the LASER Light Source of use is CO
2laser apparatus, power 500W, the angle of laser incident and target is 60 °, firing time is 150s, strength of electric field is 1000N/C, tellurium nano material deposition targets temperature is 100 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtains lath array structure tellurium nano material.
Embodiment 7
Telluride target is tellurium potassium, and the LASER Light Source of use is CO
2laser apparatus, power 500W, the angle of laser incident and target is 90 °, firing time is 150s, strength of electric field is 1000N/C, tellurium nano material deposition targets temperature is 100 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtains sheet-like array structure tellurium nano material.
Embodiment 8
Telluride target is tellurium potassium, and the LASER Light Source of use is CO
2laser apparatus, power 50W, the angle of laser incident and target is 90 °, firing time is 150s, strength of electric field is 1000N/C, tellurium nano material deposition targets temperature is 100 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtains line array structure tellurium nano material.
Embodiment 9
Telluride target is tellurium potassium, and the LASER Light Source of use is CO
2laser apparatus, power 200W, the angle of laser incident and target is 90 °, firing time is 150s, strength of electric field is 1000N/C, tellurium nano material deposition targets temperature is 100 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtains conical array array structure tellurium nano material.
Embodiment 10
Telluride target is tellurium potassium, and the LASER Light Source of use is CO
2laser apparatus, power 1000W, the angle of laser incident and target is 45 °, firing time is 150s, strength of electric field is 1000N/C, tellurium nano material deposition targets temperature is 300 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtains whole crystalline array structure tellurium nano material.
Embodiment 11
Telluride target is lead telluride, and the LASER Light Source of use is CO
2laser apparatus, power 500W, the angle of laser incident and target is 90 °, firing time is 700s, strength of electric field is 500N/C, tellurium nano material deposition targets temperature is 100 DEG C, is extremely applicable to scope by carried charge, the angle of controlling tellurium nano material deposition targets, obtains cylindrical array array structure tellurium nano material.
Claims (10)
1. a preparation method for the controlled tellurium simple substance nanometer material of structure, is characterized in that comprising the following steps:
(1) adopt the laser incident metal telluride target that sends of LASER Light Source, utilize laser excitation sputter principle, tellurium element is gone out from the metal telluride target as sputter in atmosphere, become suspension tellurium ion;
(2) on positive pole and tellurium nano material deposition targets, negative pole is collected target with impurity and is connected, tellurium nano material deposition targets and impurity are collected under the electrical forces and action of gravity producing between target, and by suspension tellurium ion deposition, on tellurium nano material deposition targets, deposition obtains tellurium nano material array;
By the control of incident laser energy, strength of electric field and/or deposition targets carried charge and/or temperature in the step to described (1) and step (2), realize the array morphology control of tellurium simple substance nanometer material.
2. according to described in claim 1, it is characterized in that: described LASER Light Source is the adjustable LASER Light Source of pulse that gas, solid, liquid excite, and the energy of described LASER Light Source is 10W ~ 1000W.
3. according to described in claim 1, it is characterized in that: in described step (1), be 5 ~ 90 ° by laser incident and metal telluride target angle, in described step (1), the laser excitation working hour is 1 ~ 1000s.
4. according to described in claim 1, it is characterized in that: described metal telluride target is lath or the powder that any metal telluride is made.
5. according to described in claim 1, it is characterized in that: in described step (2), work climate electric field is DC electric field, and strength of electric field scope is: 100 ~ 1000N/C.
6. according to described in claim 1, it is characterized in that: the substrate material of described tellurium nano material deposition targets is silicon chip, and described silicon chip pre-treatment is to carry out surface cleaning through TruMicro7050 laser equipment.
7. according to described in claim 1, it is characterized in that: described step (1) and step (2) work climate are the gas that argon gas, helium or its arbitrary proportion mix.
8. according to described in claim 1, it is characterized in that: described metal telluride target pre-treatment mode is as follows:
Under normal temperature condition, metal telluride plate or powder are placed in to dehydrated alcohol, dipping 5 ~ 30min, takes out, dry under 60 ~ 150 DEG C of environment.
9. according to described in claim 1, it is characterized in that: the temperature of tellurium nano material deposition targets is controlled, and its span of control is: 0 ~ 300 DEG C.
10. according to described in claim 1, it is characterized in that: the carried charge of tellurium nano material deposition targets and impurity collecting board is controlled by impressed voltage.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117588A (en) * | 2017-05-03 | 2017-09-01 | 清远先导材料有限公司 | The preparation method of tellurium target |
| CN108998766A (en) * | 2018-07-26 | 2018-12-14 | 望江县天长光学科技有限公司 | A kind of coating of optical lens machine |
| CN116443823A (en) * | 2023-03-17 | 2023-07-18 | 南昌大学 | Preparation method of tellurium alkene nano structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103451599A (en) * | 2013-10-10 | 2013-12-18 | 南京清航新材料科技有限公司 | Cadmium telluride/bismuth telluride integrated nano structure material with photo-thermal synergic electric generation and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103451599A (en) * | 2013-10-10 | 2013-12-18 | 南京清航新材料科技有限公司 | Cadmium telluride/bismuth telluride integrated nano structure material with photo-thermal synergic electric generation and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117588A (en) * | 2017-05-03 | 2017-09-01 | 清远先导材料有限公司 | The preparation method of tellurium target |
| CN108998766A (en) * | 2018-07-26 | 2018-12-14 | 望江县天长光学科技有限公司 | A kind of coating of optical lens machine |
| CN116443823A (en) * | 2023-03-17 | 2023-07-18 | 南昌大学 | Preparation method of tellurium alkene nano structure |
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Effective date of registration: 20211229 Address after: 323010 No. 553, Xiushan Road, Liandu District, Lishui City, Zhejiang Province Patentee after: Zhejiang Core Microelectronics Co.,Ltd. Address before: 325000 No. 717 Fudong Road, Wenzhou City, Zhejiang Province Patentee before: ZHEJIANG INDUSTRY & TRADE VACATIONAL College |