CN100516285C - Electron beam heating evaporation method as well as device and uses thereof - Google Patents
Electron beam heating evaporation method as well as device and uses thereof Download PDFInfo
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- CN100516285C CN100516285C CNB2007101507850A CN200710150785A CN100516285C CN 100516285 C CN100516285 C CN 100516285C CN B2007101507850 A CNB2007101507850 A CN B2007101507850A CN 200710150785 A CN200710150785 A CN 200710150785A CN 100516285 C CN100516285 C CN 100516285C
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Abstract
The invention relates to a heating and evaporating method of a novel electron beam provided with powdered material with comparatively high melting point and a device thereof. The method combines an electron beam heating evaporating method and a resistance heating evaporating method to provide a filamentose cathode with a negative bias by a high voltage dc power, thus a highfield is formed between the negative bias and an earthing crucible; furthermore, a filamentose hot cathode is provided with an adjustable working current by a low voltage ac power to lead an electron beam current to be emitted by the filamentose hot cathode; the electron beam current bombards and heats the crucible at a high speed under the action of a strong electric field. An electrochromic layer tungsten trioxide WO3 film and an electrolyte layer lithium fluoride LiF film applied to electrochromic equipment can be prepared by using the electron beam heating and evaporating method of the invention; the film material prepared is dense and the charge transport performance is excellent; the film thickness can be precisely controlled when the method is applied to the evaporating preparation of polyimide substrate flexible film and solar cell nickel barrier film, and the device is characterized by simple operation.
Description
Technical field
The present invention relates to vacuum plating/deposition material field, particularly relate to a kind of evaporation and have the higher melt dusty material, and electron beam heating evaporation method and device and the purposes that can accurately control vaporator rate and film thickness.
Background technology
The heat evaporating device of existing vacuum plating/depositing device, resistance-type thermal evaporation and the electron beam heating evaporation dual mode of mainly containing commonly used at present.Wherein the resistance-type evaporation unit uses low-voltage high-current power source directly to drive electric conversion device, and electric conversion device mainly comprises two kinds of boat vaporizer and resistance wires.The boat vaporizer adopts refractory metal such as tungsten, molybdenum etc. to make the boat vaporizer of different shape with punching press or other machining process, the two ends of boat vaporizer link to each other with low-voltage high-current power source, pass to electric current during use, resistance by boat vaporizer self makes source material in the boat body heating evaporation boat, makes it to be deposited on the sample; Resistance wire is around being rolled into spirrillum or other shapes resistance wire, two ends link to each other with low-voltage high-current power source, the normally thread or sheet lodge of source material to be evaporated makes its heating evaporate starting material fusion to be evaporated by pass to big electric current to resistance wire on resistance wire.The evaporation source of electron beam heating generally is designed to e type electron beam gun or straight type electron gun structure.E type electron beam gun partly is made up of electron emission source (hot-cathode of using the tungsten material usually is as emissive source), electronics acceleration components, crucible, magnetic deflection field, watercooling jacket, vacuum environment and control power supply etc.Coating materials to be evaporated is put into the water-cooled crucible, and electronics is sent by accelerating field by electron emission source and forms the line with certain energy, utilizes magnetic field that electronic beam current is focused on and deflection, and coating materials is bombarded heating, makes its fusion evaporation, thereby realizes vacuum plating.
The shortcoming of resistance-type thermal evaporation is that the heating power utilization ratio is low, and main is that vaporator rate is difficult to control etc.; When especially using boat evaporator evaporation metallic substance, because vaporizer is in parallel with evaporating materials formation resistance, evaporating materials is subjected to the restriction of uncertain resistance relation, vaporator rate is difficult to control, can form alloy material at boat body and evaporating materials contact position in addition, reduce the fusing point of boat, increase the fragility of boat, simultaneously evaporating materials original purity that also is hard to keep.It is to adopt the type of heating of tungsten wire loops around quartz crucible that improvement project is also arranged, but is subjected to the restriction of quartzy fusing point, and the use range of evaporation source material has been subjected to certain limitation.
In the electron beam type of heating, under the situation that keeps the crucible water-cooled, can reach high temperature in the part, reach the purpose of evaporation refractory metal and other indissoluble materials, and vaporator rate be controlled with high-power electron beam bombardment heating film material.But electron beam evaporation needs high-intensity magnetic field, high-precision electronic rifle and high power DC high-voltage power supply, equipment input cost height, and its power control system is accurate complicated, and operative technique is also had relatively high expectations.
Summary of the invention
Purpose of the present invention is intended to overcome defective of the prior art, and the new vacuum electron beam heating evaporation method and device and uses thereof of a kind of vacuum plating/deposition usefulness are provided.The present invention combines the electron beam source of electron beam evaporation and the vaporizer of resistance heating evaporation, draws the advantage of two kinds of evaporation coating technology, has simplified experimental installation, falls low power consume, saves cost.
For achieving the above object, the invention discloses a kind of electron beam heating evaporation method.It is characterized in that: described method is in conjunction with electron beam heating evaporation and two kinds of evaporation modes of resistance heating evaporation, by high-voltage DC power supply for the filament hot-cathode provides negative bias, make it and the ground connection crucible between form highfield; In addition provide the working current of an adjustable size by low-voltage alternating current power supply for the filament hot-cathode, the filament hot-cathode after the heating is in order to divergent bundle; The electron beam line bombards crucible at a high speed under the highfield effect, with the crucible heating, in order to the evaporation coating material.
The invention also discloses a kind of device that is exclusively used in above-mentioned electron beam heating evaporation method, comprise: filament hot-cathode, Wehnelt electrode, crucible, watercooling jacket and electron-optical system circuit, it is characterized in that: described crucible is supported by conducting bracket, and its below is provided with the Wehnelt electrode of upper shed; Described Wehnelt electrode is provided with watercooling jacket outward, and portion is provided with the filament hot-cathode within it.
Electron beam heating evaporation method of the present invention can be used for preparing the tungsten oxide film and the lithium fluoride film of electrochromic device, and prepares polyimide substrate flexible thin-film solar cell metal nickel film material.
Superiority of the present invention is: the electron beam heating evaporation method and the device of vacuum plating/deposition usefulness that the present invention proposes, improve the electron-optical system and the circuit control system of the electron beam type of heating of routine.Evaporation unit after the improvement can accurately be controlled the film thickness of vaporator rate and preparation by meticulous adjusting heater current and negative bias size, can evaporate the high-melting-point dusty material.For example: can prepare the photochromic layer tungstic oxide WO3 film and the dielectric substrate lithium fluoride LiF film that are used for electrochromic device, the thin-film material densification of preparation, charge transport properties are good.When being used for polyimide substrate flexible thin-film solar cell nickel barrier material evaporation preparation, thickness can be precisely controlled, and operation of equipment is simple.
Description of drawings
Fig. 1: the electron-optical system synoptic diagram of electron beam heating evaporation device of the present invention;
Fig. 2: the electron-optical system electrical block diagram of electron beam heating evaporation device of the present invention;
Fig. 3: the electron-optical system schematic circuit diagram of electron beam heating evaporation device of the present invention.
Embodiment
Electron beam heating evaporation method of the present invention is in conjunction with electron beam heating evaporation and two kinds of evaporation modes of resistance heating evaporation, by conventional high-voltage DC power supply for the filament hot-cathode provides negative bias, make it and the ground connection crucible between form highfield.In addition provide the working current of an adjustable size by conventional low-voltage alternating current power supply for the filament hot-cathode, the filament hot-cathode after the heating is in order to divergent bundle.With the electric field controls filament hot-cathode divergent bundle line size between Wehnelt electrode and the filament hot-cathode.The electron beam line bombards crucible at a high speed under the highfield effect, with the crucible heating, in order to evaporate different Coating Materials.
Wehnelt electrode current potential of the present invention is generally a little less than filament hot-cathode current potential 0-30V, by regulating Wehnelt electrode current potential modulated electron beam line size.Change strength of electric field by regulating negative bias, thereby change electronic beam current capacity control crucible temperature.And electron beam line size is by placed in-line electronic beam current monitor monitoring between crucible 1 and the ground.
The device that the present invention is used for above-mentioned electron beam heating evaporation method is seen shown in Figure 1, comprising: filament hot-cathode 4, Wehnelt electrode 3, crucible 1, watercooling jacket 5 and electron-optical system circuit etc.Wherein: filament is to make incense coil shape with the tungsten material, and through adding heat setting type; Crucible is supported by crucible conducting bracket 2, and its below is provided with the Wehnelt electrode of upper shed; Described Wehnelt electrode is provided with watercooling jacket outward, and portion is provided with the filament hot-cathode within it.
Crucible: select fusing point to make crucible than higher tungsten or Mo.
Crucible holder: crucible holder 2 requires conduction good, and thermal insulation is good.Consider that its function selects the stainless material support crucible that is suitable for vacuum system for use.Good for guaranteeing its conduction, have certain heat-proof quality simultaneously, the crucible conducting bracket is designed to two sections, and support is made up of horizontal tray and longitudinal carrier, and the junction of horizontal tray and longitudinal carrier uses vacuum ceramic piece 6 heat insulation, with joint bolt conducting electric current.Support is mainly considered good current lead-through with being connected of crucible except that considering physical strength.
The circuit control system of electron-optical system of the present invention comprises following major portion shown in Fig. 2,3:
1. high-voltage DC power supply B1: for providing, filament stablizes adjustable negative bias, crucible ground connection, the two forms highfield.Electron beam at a high speed bombards crucible under the highfield effect, be heated, can be according to the high-voltage value of the different adjustment needs of evaporation source material.
2. filament low-voltage alternating current power supply B2:, regulate electric current by potentiometer and make filament hot-cathode heating emitting electrons line for the filament hot-cathode provides an adjustable working current.
3, between crucible and ground, the milliampere meter M1 that connects is as electronic beam current measuring instrument monitoring electron beam line size.By regulating negative high voltage and heater current, can realize the control of electronic beam current size, can effectively control vaporator rate and thickness.
4, the Wehnelt electrode power supply is used to control filament hot-cathode divergent bundle line size.
The experimental implementation process is as follows:
1. vacuum system adopts mechanical pump to make forepump, and molecular pump is as high-vacuum pump, in order to obtain the high vacuum experimental situation.
(1). open mechanical pump, the preevacuated chamber makes the system vacuum degree be better than 10Pa;
(2). logical water coolant cools off, opens molecular pump to crucible system and molecular pump, treats to open high valve after the molecular pump works better, and this moment, mechanical pump was as the molecular pump forepump;
(3) substrate begins heating, 120 ℃ of temperature controls;
(4). preheating vacuumometer 10 minutes, measuring system vacuum tightness;
(5). when vacuum tightness reaches 3 * 10
-3During Pa, satisfied requirement of experiment.
2. voltage-regulation
(1). connect high-voltage power supply;
(2). regulate high-voltage power supply, gradually high pressure is added to-4kV;
(3). regulate the about 20V of Wehnelt electrode voltage;
(4) connect heater supply;
(5). regulate heater supply, strengthen heater current gradually, little red up to crucible, the about 4mA of electronic beam current.
3. evaporation coating
(1) regulate the about 14V of Wehnelt electrode voltage, electronic beam current is stabilized in 6mA, makes coating materials distillation or fusing and begins gasification;
(2). after steaming 1 minute in advance, open baffle plate, evaporation picks up counting;
(3). after treating that the substrate lower surface has evenly plated satisfactory film, close baffle plate;
(4). slowly reduce and close filament voltage and high pressure, close the high valve of vacuum system, stop molecular pump, stop mechanical pump and water coolant subsequently.
The photochromic layer tungstic oxide WO that uses electron beam heating evaporation device of the present invention to prepare to be used for electrochromic device
3Film and dielectric substrate lithium fluoride LiF film, the thin-film material densification of preparation, charge transport properties are good; When being used for polyimide substrate flexible thin-film solar cell nickel barrier film evaporation preparation, by meticulous adjusting heater current and negative bias size, film thickness and vaporator rate can be precisely controlled, and operation of equipment is simple.
Prepare WO with electron beam heating evaporation method of the present invention
3The experimental data of film is as shown in table 1.Wherein: pressure 3 * 10
-3Pa; The substrate ito glass; Evaporation time 12 minutes.
| Experimentation | Underlayer temperature T (℃) | Negative bias (kV) | Filament voltage (V) | Wehnelt electrode voltage (V) | Electronic beam current Ie (mA) | Observed phenomenon |
| Processing parameter adjustment before the evaporation | Room temperature → 120 | 0→-4 | 0→40 | 0→20 | 0→4 | The incandescent crucible of filament is little red |
| Evaporation | 120 | -4 | 40 | 20→14 | 4→6 | The material evaporation |
| Evaporation finishes | 120 → room temperature | -4→0 | 40→0 | 14→0 | 6→0 | / |
Claims (9)
1, a kind of electron beam heating evaporation method is characterized in that: described method is in conjunction with electron beam heating evaporation and two kinds of evaporation modes of resistance heating evaporation, by high-voltage DC power supply for the filament hot-cathode provides negative bias, make it and the ground connection crucible between form highfield; In addition provide the working current of an adjustable size by low-voltage alternating current power supply for the filament hot-cathode, the filament hot-cathode after the heating is in order to divergent bundle; Described electron beam line bombards crucible at a high speed under the highfield effect, with the crucible heating, in order to the evaporation coating material.
2, according to the described electron beam heating evaporation method of claim 1, it is characterized in that: adjust the Wehnelt electrode current potential a little less than filament hot-cathode current potential, modulated electron beam line size.
3, according to the described electron beam heating evaporation method of claim 1, it is characterized in that: regulate negative bias and change strength of electric field, change electronic beam current capacity control crucible temperature.
4, according to claim 2 or 3 described electron beam heating evaporation methods, it is characterized in that: described electron beam line size is by placed in-line electronic beam current monitor monitoring between crucible 1 and the ground.
5, the employed device of electron beam heating evaporation method as claimed in claim 1, comprise: filament hot-cathode, Wehnelt electrode, crucible, watercooling jacket and electron-optical system circuit, it is characterized in that: described crucible is supported by conducting bracket, and its below is provided with the Wehnelt electrode of upper shed; Described Wehnelt electrode is provided with watercooling jacket outward, and portion is provided with the filament hot-cathode within it; Described electron-optical system circuit comprises high-voltage DC power supply B1, low-voltage alternating current power supply B2 and electron beam beam monitoring instrument A; Wherein: described high-voltage DC power supply B1 provides stable negative bias for the filament hot-cathode,
Crucible ground connection, the two forms highfield, and electron beam bombards crucible at a high speed under the highfield effect; Described low-voltage alternating current power supply B2 provides an adjustable working current for the filament hot-cathode, regulates electric current by potentiometer and makes filament hot-cathode heating emitting electrons line.
6, according to the described electron beam heating evaporation device of claim 5, it is characterized in that: the milliampere meter of connecting between described crucible and the ground, as electron beam beam monitoring instrument A.
7, according to the described electron beam heating evaporation device of claim 5, it is characterized in that: described crucible conducting bracket is made up of horizontal tray and longitudinal carrier, and the junction of horizontal tray and longitudinal carrier uses the vacuum ceramic piece heat insulation, with joint bolt conducting electric current.
8, according to the described electron beam heating evaporation device of claim 5, it is characterized in that: described filament is to make incense coil shape with the tungsten material, and through adding heat setting type.
9, the purposes of the described electron beam heating evaporation method of claim 1 is characterized in that being used to prepare the tungsten oxide film or the lithium fluoride film of electrochromic device, or is used to prepare polyimide substrate flexible thin-film solar cell metal nickel film material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101507850A CN100516285C (en) | 2007-12-06 | 2007-12-06 | Electron beam heating evaporation method as well as device and uses thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101507850A CN100516285C (en) | 2007-12-06 | 2007-12-06 | Electron beam heating evaporation method as well as device and uses thereof |
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| CN101177777A CN101177777A (en) | 2008-05-14 |
| CN100516285C true CN100516285C (en) | 2009-07-22 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102965624B (en) * | 2011-08-31 | 2016-08-17 | 深圳光启高等理工研究院 | A kind of Meta Materials and preparation method thereof |
| JP5557817B2 (en) * | 2011-09-30 | 2014-07-23 | 株式会社日立ハイテクノロジーズ | Evaporation source and film forming apparatus |
| CN105555994B (en) * | 2013-12-20 | 2018-05-29 | 株式会社爱发科 | Electron gun arrangements and vacuum deposition apparatus |
| CN105632745A (en) * | 2014-10-27 | 2016-06-01 | 国家电网公司 | Production technology of semiconductor conductive material for transformer |
| CN106676480B (en) * | 2017-03-10 | 2019-11-08 | 南京大学 | A kind of electron beam evaporation source that evaporation rate is controllable |
| CN107068514A (en) * | 2017-04-18 | 2017-08-18 | 江苏圣亚有色金属材料有限公司 | A kind of preparation method of electron gun filament |
| KR102319130B1 (en) * | 2020-03-11 | 2021-10-29 | 티오에스주식회사 | Metal-Oxide semiconductor evaporation source equipped with variable temperature control module |
| CN113388884A (en) * | 2021-06-18 | 2021-09-14 | 北京理工大学 | Double-crucible evaporation source |
| CN115786857B (en) * | 2022-12-06 | 2023-07-28 | 安徽其芒光电科技有限公司 | Vacuum deposition film forming apparatus |
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