CN102586880A - Preparation method of oriented ZeTe nanocrystals - Google Patents
Preparation method of oriented ZeTe nanocrystals Download PDFInfo
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- CN102586880A CN102586880A CN2012100808245A CN201210080824A CN102586880A CN 102586880 A CN102586880 A CN 102586880A CN 2012100808245 A CN2012100808245 A CN 2012100808245A CN 201210080824 A CN201210080824 A CN 201210080824A CN 102586880 A CN102586880 A CN 102586880A
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Abstract
The invention discloses a preparation method of oriented ZeTe nanocrystals, which includes the following steps: synthesizing a ZnTe alloy material in vacuum by taking metals Ze and Te having purities higher than 99.99% as raw materials, cleaning the alloy material with deionized water, bonding on an object stage of pulsed laser deposition equipment with conducting silver glue adhesive to obtain a sputtering target material, sputtering the ZeTe target material at a room temperature with a pulsed laser energy density of 2-5J/cm<2>, and carrying out in-situ annealing treatment of the sputtered film at 30-400 DEG C to obtain the oriented ZeTe nanocrystals, wherein the distance between the target material and a substrate is set to be 5cm, the sputtering substrate is glass, sapphire, monocrystalline silicon and the like. The obtained oriented ZeTe nanocrystals have a grain size of about 20-60nm, and have orientations (110, 111). Compared with the traditional preparation method, the preparation method disclosed by the invention can realize oriented growth of the ZeTe nanocrystals through controlling the annealing temperature after sputtering and controlling the substrate.
Description
Technical field
The present invention relates to the brilliant ZnTe crystalline of a kind of orientation nano preparation method, belong to the field of new of nano-crystalline photoelectric material.
Background technology
Zinc telluridse (ZnTe) is a kind of II-VI family wide bandgap compound semiconductor material of excellent performance, and energy gap at room temperature is 2.26eV, and have direct band gap, can heavily doped polygamy etc. advantage.Be with a wide range of applications at aspects such as thin-film solar cells, light emitting semiconductor device, blue green LED, optical waveguides and modulators.
High permeability that the brilliant ZnTe crystal of orientation nano shows because of high relatively anisotropy and stronger excitation spectrum have potential widely application in fields such as photoelectric display and sun power window layer.The brilliant ZnTe crystalline performance of orientation nano and used preparation technology's method have very big relation, and its crystalline quality and anneal environment, temperature are closely related.
Traditional ZnTe crystal growth condition requires high; Temperature is up to 1100 ℃; Because too high growth temperature causes vp and raises that make process of growth set off an explosion easily thereby have influence on, the technology cost increases; Also can there be too high thermal defect in prepared ZnTe crystal, causes optical property to descend.
The present invention proposes the technology of room temperature sputter and in-situ annealing, has both solved the too high difficult problem of crystal growth temperature and vp, for the control of crystal growth orientation condition is provided again.
Summary of the invention
The object of the invention provides the brilliant ZnTe crystalline of a kind of orientation nano preparation method in order to solve above-mentioned technical problem; Promptly through changing substrate material; And sputter at room temperature and in-situ annealing, thereby the nanocrystalline ZnTe crystal that preparation has crystalline orientation property has promptly reached the purpose of controlling the crystal structure quality; Improve its characteristics of luminescence, can effectively control crystal growth direction again.
Technical scheme of the present invention
The brilliant ZnTe crystalline of a kind of orientation nano preparation method, its preparation process comprises the following steps:
(1), to be higher than 99.999% Metal Zn and Te with purity be raw material, according to the ratio batching of atomic ratio 1:1, adopts high-energy planetary formula ball-grinding machine that raw material is carried out uniform mixing, mixing time is 4h, it is 10 that mixed raw material is placed vacuum
-3In the vacuum melting furnace of Pa, smelting furnace is heated to 1200 ℃ and carries out melting, and melting is cast behind the refining 20min after accomplishing again, promptly obtains the ZnTe alloy material;
(2), the ZnTe alloy material of step (1) gained is cast in the columnar mould that internal diameter is 20mm, furnace cooling forms ZnTe alloy bar to room temperature;
(3), the ZnTe alloy bar with step (2) gained is processed into diameter 20mm, high 10mm, formation ZnTe alloy target material;
(4), the formed ZnTe alloy target material of step (3) is cleaned 60min in deionized water for ultrasonic, dry with blower then;
(5), step (4) handled back ZnTe alloy target material be bonded at conductive silver glue on the target Stage microscope of pulsed laser deposition equipment, behind blower oven dry conductive silver glue, be placed on the pedestal of target Stage microscope of pulsed laser deposition equipment;
(6), the simple glass with 5mm * 5mm, sapphire or silicon single crystal is as substrate, and substrate is put into acetone soln ultrasonic cleaning 15min, rinse the back well with deionized water and use drier;
(7), step (6) handled back substrate be bonded at conductive silver glue on the substrate Stage microscope of pulsed laser deposition equipment, behind blower oven dry conductive silver glue, be placed on the pedestal of substrate Stage microscope of pulsed laser deposition equipment;
(8), after target and substrate place and accomplish, adjustment target and substrate distance are set to 5cm, the vacuum tightness of setting pulse laser deposition equipment is 10
-3Pa is rotated target and substrate with 50 ~ 120r/min;
The preparation of (9), sputter attitude ZnTe film
Target and the substrate that will pass through step (8) adjustment controlled sputter temperature on pulsed laser deposition equipment be room temperature, and pulsed laser energy density is 2～5J/cm
2, preferred 2～3J/cm
2, sputtering time is that 60～120min carries out sputter, obtains sputter attitude ZnTe film;
Described pulsed laser deposition equipment comprises excimer laser and vacuum coating system, and Laser emission route in the adjustment excimer laser makes it pass through the laser incidence window of vacuum coating system, focuses on the target position, and the concrete operations of sputter procedure are following:
Successively start mechanical pump, the molecular pump of vacuum coating system, vacuum tightness reaches 10
-3Pa; Restart the rotation of target and substrate, the adjustment rotating speed; Shutter with vacuum coating system covers substrate, starts laser transmitter, the adjustment pulsed laser energy; Behind the sputtering target material surface contamination layer 5min, remove shutter, begin to carry out sputter, sputtering time is 60 ~ 120min; Close laser transmitter, target and substrate rotation, molecular pump, mechanical pump after the sputter successively; Open the Vakuumkammer of vacuum coating system, take out sputter attitude ZnTe film;
(10), sputter attitude ZnTe film that will be through (9) gained under 30 ~ 400 ℃, preferred 250～400 ℃ are carried out in-situ annealing and handle, can obtain the brilliant ZnTe crystal of orientation nano.
The brilliant ZnTe crystal of a kind of orientation nano of the above-mentioned brilliant ZnTe crystalline of a kind of orientation nano preparation method gained, its grain-size is about 20～60nm, preferred 35～40 nm, the brilliant ZnTe crystal of a kind of orientation nano of gained has < 110>and < 111>orientation.
The brilliant ZnTe crystal of a kind of orientation nano of above-mentioned gained can be used for aspects such as thin-film solar cells, light emitting semiconductor device, blue green LED, optical waveguides and modulator.
Beneficial effect of the present invention
The brilliant ZnTe crystalline of a kind of orientation nano of the present invention preparation method; Owing to adopt pulsed laser deposition and in-situ annealing technology in the preparation process; Therefore; The brilliant ZnTe crystallographic grain of the orientation nano of preparing size can be controlled through the adjustment of in-situ annealing temperature, and its grain size range can be controlled in 20～60nm.
In addition, the brilliant ZnTe crystalline of a kind of orientation nano of the present invention preparation method, owing to, can change the crystalline habit through adjustment to substrate material and growth in situ temperature, thus realize < 110>or < 111>crystals with different orientations.With respect to the brilliant ZnTe crystal of existing orientation nano preparation method, this method has characteristics such as preparation cost is low, the preparation material grains is evenly distributed, and the preparation method is simple efficient.
Description of drawings
Annealing temperature is the XRD figure picture of the ZnTe film of 280 ℃ of preparations among Fig. 1, the embodiment 1.
Embodiment
Below through embodiment and combine accompanying drawing that the present invention is further set forth, but do not limit the present invention.
The model of each used equipment and manufacturer in the embodiments of the invention, specific as follows:
High-energy planetary formula ball-grinding machine: the small-sized planetary ball mill of ND-4L, the Nanjing Lay goes on foot Scientific and Technical Industry Co., Ltd;
Vacuum melting furnace: ZG-10 vacuum induction melting furnace, Shanghai prosperous electric furnace in morning ltd;
Pulsed laser deposition (PLD) equipment: assembled part comprises:
Excimer laser: ThinFilmStar100, Germany's (laser);
Vacuum coating system: PLD-362-S, AOV company.
Embodiment 1
Its preparation process of the brilliant ZnTe crystalline of a kind of < 110>of the present invention orientation nano preparation technology method comprises the following steps:
(1), to be higher than 99.999% Metal Zn and Te with purity be raw material, according to the ratio batching of atomic ratio 1:1, adopts high-energy planetary formula ball-grinding machine that raw material is carried out uniform mixing, mixing time is 4h, it is 10 that mixed raw material is placed vacuum tightness
-3In the vacuum melting furnace of Pa, smelting furnace is heated to 1200 ℃ and carries out melting, and melting is cast behind the refining 20min after accomplishing again, promptly obtains the ZnTe alloy material;
(2), the ZnTe alloy material of step (1) gained is cast in the columnar mould that internal diameter is 20mm, furnace cooling forms ZnTe alloy bar to room temperature;
(3), the ZnTe alloy bar with step (2) gained is processed into diameter 20mm, high 10mm, formation ZnTe alloy target material;
(4), the formed ZnTe alloy target material of step (3) was cleaned 60 minutes in deionized water for ultrasonic, dry with blower then;
(5), step (4) handled back ZnTe alloy target material be bonded on pulsed laser deposition (PLD) the equipment target Stage microscope with conductive silver glue, behind blower oven dry conductive silver glue, be placed on the pedestal of target Stage microscope of PLD;
(6), with the simple glass of 5mm * 5mm as substrate, substrate is put into acetone soln ultrasonic cleaning 15min, rinse the back well with deionized water and use drier;
(7), step (6) handled back substrate be bonded at conductive silver glue on the substrate Stage microscope of pulsed laser deposition (PLD) equipment, behind blower oven dry conductive silver glue, be placed on the pedestal of substrate Stage microscope of PLD;
(8), after target and substrate place and accomplish, the adjustment target is set to 5cm with substrate distance, controlling PLD equipment vacuum tightness is 10
-3Pa is rotated target and the substrate speed with 50r/min;
The preparation of (9) sputter attitude ZnTe film
Target and the substrate that will pass through step (8) adjustment controlled sputter temperature on pulsed laser deposition equipment be room temperature, and pulsed laser energy density is 3J/cm
2, sputtering time is that 60min carries out sputter, obtains sputter attitude ZnTe film;
(10), will under 280 ℃, carry out in-situ annealing through the sputter attitude ZnTe film of (9) gained handles; Can obtain the brilliant ZnTe crystal of orientation nano, the XRD figure of anneal rear film is as as shown in Figure 1, as can be seen from Figure 1; The brilliant ZnTe crystal of a kind of orientation nano of gained; Its grain-size is about 40nm, and its crystal grain is evenly distributed, and has < 110>orientation.
Embodiment 2
Its preparation process of the brilliant ZnTe crystalline of a kind of < 100>of the present invention orientation nano preparation technology method comprises the following steps:
(1), to be higher than 99.999% Metal Zn and Te with purity be raw material, according to the ratio batching of atomic ratio 1:1, adopts high-energy planetary formula ball-grinding machine that raw material is carried out uniform mixing, mixing time is 4h, it is 10 that mixed raw material is placed vacuum tightness
-3In the vacuum melting furnace of Pa, smelting furnace is heated to 1200 ℃ and carried out melting, and melting is cast behind the refining 20min after accomplishing again, promptly obtains the ZnTe alloy material;
(2), the ZnTe alloy material of step (1) gained is cast in the columnar mould that internal diameter is 20mm, furnace cooling forms ZnTe alloy bar to room temperature;
(3), the ZnTe alloy bar with step (2) gained is processed into diameter 20mm, high 10mm, formation ZnTe alloy target material;
(4), the formed ZnTe alloy target material of step (3) is cleaned 60min in deionized water for ultrasonic, dry with blower then;
(5), step (4) handled back ZnTe alloy target material be bonded at conductive silver glue on the target Stage microscope of pulsed laser deposition (PLD) equipment, behind blower oven dry conductive silver glue, be placed on the pedestal of target Stage microscope of PLD;
(6), with the sapphire of 5mm * 5mm as substrate, substrate is put into acetone soln ultrasonic cleaning 15min, rinse the back well with deionized water and use drier;
(7), step (6) handled back substrate be bonded at conductive silver glue on the substrate Stage microscope of pulsed laser deposition (PLD) equipment, behind blower oven dry conductive silver glue, be placed on the pedestal of substrate Stage microscope of PLD;
(8), after target and substrate place and accomplish, the adjustment target is set to 5cm with substrate distance, controlling PLD equipment vacuum tightness is 10
-3Pa is rotated target and the substrate speed with 60r/min;
The preparation of (9), sputter attitude ZnTe film
Target and the substrate that will pass through step (8) adjustment controlled sputter temperature on pulsed laser deposition equipment be room temperature, and pulsed laser energy density is 3J/cm
2, sputtering time is that 60min carries out sputter, obtains sputter attitude ZnTe film;
(10), will under 250 ℃, carry out in-situ annealing through the sputter attitude ZnTe film of (9) preparation and handle, can obtain grain-size and be about 35nm, its crystal grain is evenly distributed, and has the brilliant ZnTe crystal of orientation nano of < 100>orientation.
Embodiment 3
Its preparation process of the brilliant ZnTe crystalline of a kind of < 110>of the present invention orientation nano preparation technology method comprises the following steps:
(1), to be higher than 99.999% Metal Zn and Te with purity be raw material, according to the ratio batching of atomic ratio 1:1, adopts high-energy planetary formula ball-grinding machine that raw material is carried out uniform mixing, mixing time is 4h, it is 10 that mixed raw material is placed vacuum tightness
-3In the vacuum melting furnace of Pa, smelting furnace is heated to 1200 ℃ and carries out melting, and melting is cast behind the refining 20min after accomplishing again, promptly obtains the ZnTe alloy material;
(2), the ZnTe alloy material of step (1) gained is cast in the columnar mould that internal diameter is 20mm, furnace cooling forms ZnTe alloy bar to room temperature;
(3), the ZnTe alloy bar with step (2) gained is processed into diameter 20mm, high 10mm, formation ZnTe alloy target material;
(4), the formed ZnTe alloy target material of step (3) was cleaned 60 minutes in deionized water for ultrasonic, dry with blower then;
(5), step (4) handled back ZnTe alloy target material be bonded on pulsed laser deposition (PLD) the equipment target Stage microscope with conductive silver glue, behind blower oven dry conductive silver glue, be placed on the pedestal of target Stage microscope of PLD;
(6), the silicon single crystal of 5mm * 5mm (110 orientation) as substrate, is put into acetone soln ultrasonic cleaning 15min with substrate, rinse the back well with deionized water and use drier;
(7), step (6) handled back substrate be bonded at conductive silver glue on the substrate Stage microscope of pulsed laser deposition (PLD) equipment, behind blower oven dry conductive silver glue, be placed on the pedestal of substrate Stage microscope of PLD;
(8), after target and substrate place and accomplish, the adjustment target is set to 5cm with substrate distance, controlling PLD equipment vacuum tightness is 10
-3Pa is rotated target and the substrate speed with 120r/min;
The preparation of (9), sputter attitude ZnTe film
Target and the substrate that will pass through step (8) adjustment controlled sputter temperature on pulsed laser deposition equipment be room temperature, and pulsed laser energy density is 2J/cm
2, sputtering time is that 120min carries out sputter, obtains sputter attitude ZnTe film;
(10), will under 400 ℃, carry out in-situ annealing through the sputter attitude ZnTe film of (9) gained and handle, can obtain grain-size and be about 40nm, have the brilliant ZnTe crystal of orientation nano of < 110>orientation.
The above content is merely the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (6)
1. the brilliant ZnTe crystalline of an orientation nano preparation method is characterized in that comprising the steps:
(1), to be higher than 99.999% Metal Zn and Te with purity be raw material, according to the ratio batching of atomic ratio 1:1, adopts high-energy planetary formula ball-grinding machine that raw material is carried out uniform mixing, mixing time is 4h, it is 10 that mixed raw material is placed vacuum
-3In the vacuum melting furnace of Pa, smelting furnace is heated to 1200 ℃ and carries out melting, and melting is cast behind the refining 20min after accomplishing again, promptly obtains the ZnTe alloy material;
(2), the ZnTe alloy material of step (1) gained is cast in the columnar mould that internal diameter is 20mm, furnace cooling forms ZnTe alloy bar to room temperature;
(3), the ZnTe alloy bar with step (2) gained is processed into diameter 20mm, high 10mm, formation ZnTe alloy target material;
(4), the formed ZnTe alloy target material of step (3) is cleaned 60min in deionized water for ultrasonic, dry with blower then;
(5), step (4) handled back ZnTe alloy target material be bonded at conductive silver glue on the target Stage microscope of pulsed laser deposition equipment, behind blower oven dry conductive silver glue, be placed on the pedestal of target Stage microscope of pulsed laser deposition equipment;
(6), the simple glass with 5mm * 5mm, sapphire or silicon single crystal is as substrate, and substrate is put into acetone soln ultrasonic cleaning 15min, rinse the back well with deionized water and use drier;
(7), step (6) handled back substrate be bonded at conductive silver glue on the substrate Stage microscope of pulsed laser deposition equipment, behind blower oven dry conductive silver glue, be placed on the pedestal of substrate Stage microscope of pulsed laser deposition equipment;
(8), after target and substrate place and accomplish, adjustment target and substrate distance are set to 5cm, the vacuum tightness of setting pulse laser deposition equipment is 10
-3Pa is rotated target and substrate with 50 ~ 120r/min;
The preparation of (9), sputter attitude ZnTe film
Target and the substrate that will pass through step (8) adjustment controlled sputter temperature on pulsed laser deposition equipment be room temperature, and pulsed laser energy density is 2～5J/cm
2, preferred 2～3 J/cm
2, sputtering time is that 60～120min carries out sputter, obtains sputter attitude ZnTe film;
Described pulsed laser deposition equipment comprises excimer laser and vacuum coating system, and Laser emission route in the adjustment excimer laser makes it pass through the laser incidence window of vacuum coating system, focuses on the target position, and the concrete operations of sputter procedure are following:
Successively start mechanical pump, the molecular pump of vacuum coating system, vacuum tightness reaches 10
-3Pa; Restart the rotation of target and substrate, the adjustment rotating speed; Shutter with vacuum coating system covers substrate, starts laser transmitter, the adjustment pulsed laser energy; Behind the sputtering target material surface contamination layer 5min, remove shutter, begin to carry out sputter, sputtering time is 60 ~ 120min; Close laser transmitter, target and substrate rotation, molecular pump, mechanical pump after the sputter successively; Open the Vakuumkammer of vacuum coating system, take out sputter attitude ZnTe film;
(10), will under 30 ~ 400 ℃, carry out in-situ annealing through the sputter attitude ZnTe film of (9) gained and handle, can obtain the brilliant ZnTe crystal of orientation nano.
2. the brilliant ZnTe crystalline of a kind of orientation nano as claimed in claim 1 preparation method is characterized in that the described pulsed laser energy density of step (9) is 2 ~ 3J/cm
2
3. the brilliant ZnTe crystalline of a kind of orientation nano as claimed in claim 2 preparation method is characterized in that the described in-situ annealing temperature of step (10) is 250 ~ 400 ℃.
4. like the brilliant ZnTe crystal of orientation nano of claim 1, the brilliant ZnTe crystalline of 2 or 3 described a kind of orientation nanos preparation method gained, it is characterized in that the nanocrystalline ZnTe crystalline of gained is oriented to < 110>and < 111 >.
5. the brilliant ZnTe crystal of a kind of orientation nano as claimed in claim 4 is characterized in that the brilliant ZnTe crystalline of described orientation nano grain-size is 20～60nm.
6. the brilliant ZnTe crystal of a kind of orientation nano as claimed in claim 4 is characterized in that the brilliant ZnTe crystalline of described orientation nano grain-size is 30～40nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103754836A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院合肥物质科学研究院 | Method for preparing tellurium colloid solution with high chemical activity and telluride nanometer material |
| CN103950904A (en) * | 2014-05-12 | 2014-07-30 | 广东先导稀材股份有限公司 | Preparation method of zinc telluride |
| CN113451447A (en) * | 2021-06-30 | 2021-09-28 | 南方科技大学 | Deep ultraviolet amorphous gallium oxide photoelectric detector and preparation method and application thereof |
| WO2022032733A1 (en) * | 2020-08-14 | 2022-02-17 | 南京公诚节能新材料研究院有限公司 | Method for maintaining stability of znte crystal |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103754836A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院合肥物质科学研究院 | Method for preparing tellurium colloid solution with high chemical activity and telluride nanometer material |
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| CN103950904A (en) * | 2014-05-12 | 2014-07-30 | 广东先导稀材股份有限公司 | Preparation method of zinc telluride |
| WO2022032733A1 (en) * | 2020-08-14 | 2022-02-17 | 南京公诚节能新材料研究院有限公司 | Method for maintaining stability of znte crystal |
| CN113451447A (en) * | 2021-06-30 | 2021-09-28 | 南方科技大学 | Deep ultraviolet amorphous gallium oxide photoelectric detector and preparation method and application thereof |
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Application publication date: 20120718 |