CN101724819A - Method for preparing Er2O3 coating - Google Patents
Method for preparing Er2O3 coating Download PDFInfo
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- CN101724819A CN101724819A CN200910243034A CN200910243034A CN101724819A CN 101724819 A CN101724819 A CN 101724819A CN 200910243034 A CN200910243034 A CN 200910243034A CN 200910243034 A CN200910243034 A CN 200910243034A CN 101724819 A CN101724819 A CN 101724819A
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- sputtering
- water vapour
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Abstract
The invention belongs to the technical field of reactive sputtering, and more particularly relates to a method for preparing Er2O3 coating, comprising: putting a quartz substrate on a heater, installing target material, and adjusting the target substrate distance; vacuumizing until the vacuum degree is not more than 3.0*10-3Pa, and heating the substrate to be 700-800 DEG C; filling argon and steam, and adjusting the atmospheric pressure to be 0.1-0.8Pa, wherein the water pressure is 0.04-0.08Pa; sputtering, and increasing the sputtering power to be 80-100W; after stabilizing glow, moving a baffle away, and starting deposition; and after depositing for 20-40min, closing the baffle, stopping sputtering, disconnecting the argon and the steam, cutting off a heating power supply, turning off a vacuum system, and obtaining the Er2O3 coating. The reactive sputtering of the method improves the sputtering efficiency, taking the steam as reactant gas, prevents the surface of the target material from being oxidized, and improves the controllability of the rate of deposition. The method preparing the Er2O3 coating is rapid and controllable in the rate of deposition.
Description
Technical field
The invention belongs to technical field of reactive sputtering, particularly a kind of preparation Er
2O
3The method of coating.
Background technology
Er
2O
3Have higher dielectric properties, excellent photoelectric performance and good corrosion resistance, it is had a wide range of applications in fields such as microelectronics, photoelectron, corrosion and protection and nuclear application.Preparation well-crystallized, densification, the high quality Er that bonding force is strong
2O
3Coating has great importance.
At present, the method for various system films all can be used to prepare Er
2O
3Coating is as PLD, sputter, electron beam evaporation, sol-gel, chemical vapour deposition, original position liquid immersion plating growth etc.Magnetron sputtering has a wide range of applications as the method for manufacturing thin film of routine, can use Er
2O
3Ceramic target adopts the rf magnetron sputtering preparation, also can use the Er metallic target to adopt direct current or rf magnetron sputtering preparation.But Er
2O
3The ceramic target sputtering yield is low excessively, is unfavorable for sizable application; The metallic target reaction magnetocontrol sputtering generates oxide compound at target material surface easily, makes that the coating sedimentation rate is wayward.
Summary of the invention
The purpose of this invention is to provide a kind of preparation Er
2O
3The method of coating is characterized in that, is target with pure metal Er target, adopts reactive sputtering to prepare Er
2O
3Coating may further comprise the steps:
(1) quartz substrate is placed on the well heater, target is installed, the adjusting target-substrate distance is 30～50mm;
(2) be evacuated to vacuum tightness and be not more than 3.0 * 10
-3Pa opens heater power source, and substrate is heated to 700～800 ℃;
(3) feed argon gas and water vapour, air pressure is transferred to 0.1～0.8Pa, wherein water partial pressure is 0.04～0.08Pa, opens sputter, and sputtering power is increased to 80～100W, after aura is stable, removes baffle plate, begins deposition;
(4) deposition is after 20～40 minutes, and the pass baffle plate closes sputter, disconnects argon gas and water vapour, cuts off heating power supply, closes vacuum system, gets Er
2O
3Coating.
Described pure metal Er target purity is 99.9%.
Described water vapour is provided by the vacuum water tank, and the vacuum water tank keeps constant temperature, to keep the constant of water vapour steam output.
At above-mentioned Er
2O
3Among the preparation method of coating, in the step (2), require back of the body end vacuum high as far as possible, to avoid the remaining O of cavity
2Experimental result is impacted, improve the controllability of experimental result.
At above-mentioned Er
2O
3Among the preparation method of coating, in the step (3), water vapour provides reaction requisite oxygen atom as reactant gases; Hydrogen atom is provided simultaneously, reduces the target material surface degree of oxidation, so steam vapour amount is one of key parameters of experiment.Water vapour is provided by the vacuum water tank, and water vapour enters cavity by evaporation through pipeline by the vacuum water tank, therefore requires the water tank temperature stable as far as possible, preferably can keep constant temperature, to keep the constant of water vapour steam output.
Beneficial effect of the present invention is: the invention provides a kind of preparation Er
2O
3The possible technique of coating.Reactive sputtering has improved sputtering yield, and water vapour has prevented the oxidation of target material surface simultaneously as reactant gases, has improved the controllability of sedimentation rate.The present invention is the not only fast but also controlled Er of a kind of sedimentation rate
2O
3Coating production.
Description of drawings
Fig. 1 is a device structure synoptic diagram used herein;
Fig. 2 is the prepared Er of the embodiment of the invention 1
2O
3Coating x ray θ-2 θ scintigram;
Fig. 3 is the prepared Er of the embodiment of the invention 1
2O
3Coating SEM scans shape appearance figure;
Fig. 4 is the prepared Er of the embodiment of the invention 2
2O
3Coating x ray θ-2 θ scintigram;
Fig. 5 is the prepared Er of the embodiment of the invention 2
2O
3Coating SEM scans shape appearance figure;
Fig. 6 is the prepared Er of the embodiment of the invention 3
2O
3Coating x ray θ-2 θ scintigram;
Fig. 7 is the prepared Er of the embodiment of the invention 3
2O
3Coating SEM scans shape appearance figure;
Fig. 8 is the prepared Er of the embodiment of the invention 3
2O
3The coating cross-section morphology.
Number in the figure: 1-Ar makings amount under meter; The 2-stopping valve; The 3-sputtering target; The 4-baffle plate; The 5-well heater; The 6-molecular pump; The 7-mechanical pump; The 8-vacuumometer; The 9-slide valve; The 10-water tank; The 11-control valve; The 12-mixing chamber.
Embodiment
The invention will be further described below in conjunction with accompanying drawing:
Following examples are all carried out in device as shown in Figure 1.Device structure synoptic diagram used herein as shown in Figure 1, this equipment is mainly by Ar makings amount under meter 1, stopping valve 2, sputtering target 3, baffle plate 4, well heater 5, molecular pump 6, mechanical pump 7, vacuumometer 8, slide valve 9, water tank 10, control valve 11 and mixing chamber 12 are formed, adopt molecular pump 6 and 7 pairs of systems of mechanical pump to vacuumize, all adopt this equipment in following examples.The used water vapour of reactive sputtering is provided by water tank, and the water tank temperature keeps 25 ℃, to keep the constant of water vapour steam output.
Adopt reactive sputtering to prepare Er
2O
3Coating is a target with the pure metal Er target (purity is 99.9%) of Φ 75 * 5mm, may further comprise the steps:
(1) quartz substrate is put into alcohol earlier and carried out ultrasonic cleaning 2 minutes, remove the moisture on surface; Put into acetone then and carried out ultrasonic cleaning 3 minutes, remove the greasy dirt on surface; Dry up with hair dryer at last; Quartz substrate is placed on the well heater, target is installed, the adjusting target-substrate distance is 40mm;
(2) be evacuated to vacuum tightness and be not more than 3.0 * 10
-3Pa opens heater power source, and substrate is heated to 750 ℃;
(3) feed argon gas, regulate the water vapour control valve, water vapour is provided by water tank, and the water tank temperature keeps 25 ℃, and to keep the constant of water vapour steam output, vacuumometer shows that water vapour is 4.0 * 10
-2Pa, regulator plate valve to air pressure is 0.5Pa, opens sputter, and sputtering power is increased to 100W, after aura is stable, removes baffle plate, begins deposition;
(4) deposition is after 20 minutes, and the pass baffle plate closes sputter, disconnects argon gas and water vapour, cuts off heating power supply, closes vacuum system, gets Er
2O
3Coating.
Er
2O
3Fig. 2 is seen in coating x ray θ-2 θ scanning, and Fig. 3 prepares Er for present embodiment
2O
3Coating SEM figure shows the coating well-crystallized, and continuous, smooth, fine and close, the flawless in surface, and coating is a cube phase.
Adopt reactive sputtering to prepare Er
2O
3Coating is a target with the pure metal Er target (purity is 99.9%) of Φ 75 * 5mm, may further comprise the steps:
(1) quartz substrate is put into alcohol earlier and carried out ultrasonic cleaning 2 minutes, remove the moisture on surface; Put into acetone then and carried out ultrasonic cleaning 3 minutes, remove the greasy dirt on surface; Dry up with hair dryer at last; Quartz substrate is placed on the well heater, target is installed, the adjusting target-substrate distance is 40mm;
(2) be evacuated to vacuum tightness and be not more than 3.0 * 10
-3Pa opens heater power source, and substrate is heated to 750 ℃;
(3) feed argon gas, regulate the water vapour control valve, water vapour is provided by water tank, and the water tank temperature keeps 25 ℃, and to keep the constant of water vapour steam output, vacuumometer shows that water vapour is 8.0 * 10
-2Pa, regulator plate valve to air pressure is 0.5Pa, opens sputter, and sputtering power is increased to 80～100W, after aura is stable, removes baffle plate, begins deposition;
(4) deposition is after 20 minutes, and the pass baffle plate closes sputter, disconnects argon gas and water vapour, cuts off heating power supply, closes vacuum system, gets Er
2O
3Coating.
Er
2O
3Fig. 4 is seen in coating x ray θ-2 θ scanning, and Fig. 5 prepares Er for present embodiment
2O
3Coating SEM figure shows the coating well-crystallized, and continuous, smooth, fine and close, the flawless in surface, and coating is a cube phase, and is (222) orientation preferential growth.
Adopt reactive sputtering to prepare Er
2O
3Coating is a target with the pure metal Er target (purity is 99.9%) of Φ 75 * 5mm, may further comprise the steps:
(1) quartz substrate is put into alcohol earlier and carried out ultrasonic cleaning 2 minutes, remove the moisture on surface; Put into acetone then and carried out ultrasonic cleaning 3 minutes, remove the greasy dirt on surface; Dry up with hair dryer at last; Quartz substrate is placed on the well heater, target is installed, the adjusting target-substrate distance is 40mm;
(2) be evacuated to vacuum tightness and be not more than 3.0 * 10
-3Pa opens heater power source, and substrate is heated to 800 ℃;
(3) feed argon gas, regulate the water vapour control valve, water vapour is provided by water tank, and the water tank temperature keeps 25 ℃, and to keep the constant of water vapour steam output, vacuumometer shows that water vapour is 4.0 * 10
-2Pa, regulator plate valve to air pressure is 0.5Pa, opens sputter, and sputtering power is increased to 80～100W, after aura is stable, removes baffle plate, begins deposition;
(4) deposition is after 20 minutes, and the pass baffle plate closes sputter, disconnects argon gas and water vapour, cuts off heating power supply, closes vacuum system, gets Er
2O
3Coating.
Er
2O
3Fig. 6 is seen in coating x ray θ-2 θ scanning, and Fig. 7 prepares Er for present embodiment
2O
3Coating SEM figure shows the coating well-crystallized, and continuous, smooth, fine and close, the flawless in surface, and coating is a cube phase, and is (222) orientation preferential growth.Fig. 8 prepares Er for present embodiment
2O
3Coating cross-section morphology figure shows that coating combines with substrate well, coating is fine and close, is the column crystal growth, and the coating growth velocity is 50nm/min.
Claims (3)
1. one kind prepares Er
2O
3The method of coating is characterized in that, is target with pure metal Er target, adopts reactive sputtering to prepare Er
2O
3Coating may further comprise the steps:
(1) quartz substrate is placed on the well heater, target is installed, the adjusting target-substrate distance is 30～50mm;
(2) be evacuated to vacuum tightness and be not more than 3.0 * 10
-3Pa opens heater power source, and substrate is heated to 700～800 ℃;
(3) feed argon gas and water vapour, air pressure is transferred to 0.1～0.8Pa, wherein water partial pressure is 0.04～0.08Pa, opens sputter, and sputtering power is increased to 80～100W, after aura is stable, removes baffle plate, begins deposition;
(4) deposition is after 20～40 minutes, and the pass baffle plate closes sputter, disconnects argon gas and water vapour, cuts off heating power supply, closes vacuum system, gets Er
2O
3Coating.
2. a kind of preparation Er according to claim 1
2O
3The method of coating is characterized in that, described pure metal Er target purity is 99.9%.
3. a kind of preparation Er according to claim 1
2O
3The method of coating is characterized in that, described water vapour is provided by the vacuum water tank, and the vacuum water tank keeps constant temperature, to keep the constant of water vapour steam output.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102430342A CN101724819B (en) | 2009-12-22 | 2009-12-22 | Method for preparing Er2O3 coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102430342A CN101724819B (en) | 2009-12-22 | 2009-12-22 | Method for preparing Er2O3 coating |
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|---|---|
| CN101724819A true CN101724819A (en) | 2010-06-09 |
| CN101724819B CN101724819B (en) | 2011-08-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111155052A (en) * | 2019-12-06 | 2020-05-15 | 中国工程物理研究院核物理与化学研究所 | Er2O3Preparation method and application of coating |
-
2009
- 2009-12-22 CN CN2009102430342A patent/CN101724819B/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111155052A (en) * | 2019-12-06 | 2020-05-15 | 中国工程物理研究院核物理与化学研究所 | Er2O3Preparation method and application of coating |
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|---|---|
| CN101724819B (en) | 2011-08-31 |
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Effective date of registration: 20190402 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Research Institute of engineering and Technology Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |