CN114481042A - Method for cleaning crucible assembly of electron beam evaporation table - Google Patents

Method for cleaning crucible assembly of electron beam evaporation table Download PDF

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Publication number
CN114481042A
CN114481042A CN202011163179.4A CN202011163179A CN114481042A CN 114481042 A CN114481042 A CN 114481042A CN 202011163179 A CN202011163179 A CN 202011163179A CN 114481042 A CN114481042 A CN 114481042A
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China
Prior art keywords
crucible
cleaning
boron nitride
side wall
baffle
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CN202011163179.4A
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Chinese (zh)
Inventor
徐晓强
程昌辉
吴向龙
闫宝华
王成新
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Shandong Inspur Huaguang Optoelectronics Co Ltd
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Shandong Inspur Huaguang Optoelectronics Co Ltd
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Priority to CN202011163179.4A priority Critical patent/CN114481042A/en
Publication of CN114481042A publication Critical patent/CN114481042A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • C23C14/30Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/243Crucibles for source material

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention relates to a method for cleaning a crucible assembly of an electron beam evaporation table, and belongs to the technical field of semiconductor processing. The operation steps are as follows: (1) preparing a coating: placing a baffle above a crucible, spraying a layer of boron nitride above the baffle by using a boron nitride spray, uniformly distributing the boron nitride spray on the side wall of the crucible, and taking away the baffle after spraying; (2) the crucible is used: metal is evaporated; (3) and (4) cleaning the side wall of the crucible. According to the invention, the boron nitride spray is sprayed on the side wall of the crucible, so that the adhesion degree between the side wall of the crucible and the metal layer is low, a large number of metal layers are conveniently accumulated, the cleaning and removing operation is convenient, the boron nitride spray coating can withstand a high-temperature environment of more than 1000 ℃, the evaporation source in the crucible can be ensured to be normally melted, and meanwhile, the material on the side wall of the crucible can not be melted and flows into the crucible, and the normal evaporation use of the crucible is ensured.

Description

Method for cleaning crucible assembly of electron beam evaporation table
Technical Field
The invention relates to a method for cleaning a crucible assembly of an electron beam evaporation table, and belongs to the technical field of semiconductor processing.
Background
A light Emitting diode (led) is a semiconductor device. The light emitting diode emits light by the composite radiation of electrons and holes, is a device which performs electroluminescence by depending on a semiconductor P-N node, is made of compounds of nitrogen, arsenic, gallium, phosphorus and the like, and can convert electric energy into light energy. The LED structure mainly comprises two electrodes, namely a P-surface electrode and an N-surface electrode, the general method for manufacturing the electrodes is that metal materials are formed by an electron beam evaporation table through evaporation or sputtering, the specific working principle is that a filament of an electron gun loaded with high voltage emits high-energy electron beams, the electron beams strike the surface of the metal materials to enable the metal materials to be directly changed into gas from solid state, the metal materials are gradually deposited on the surface of a wafer in the form of gas molecules or metal atoms, and finally, a proper electrode structure is obtained through deposition and film forming.
Usually a large amount of metal material hold and preserve inside the crucible, carry out the evacuation to the cavity earlier when the coating by vaporization at every turn, use electron gun heating metal evaporation source to carry out the coating by vaporization. General evaporation system as shown in fig. 1, a crucible assembly is placed at the bottom of a chamber, and materials of the evaporation source are deposited on the surface of a wafer by striking the evaporation source with electrons emitted from an electron gun system below the crucible assembly. However, a large amount of metal materials are evaporated on the side wall of the crucible in the evaporation process, and along with the evaporation heat and the time lengthening, the more the metal on the side wall of the crucible is accumulated, generally, the metal on the side wall of the crucible is accumulated to a certain heat and then is cleaned by opening a cavity, and most of the cleaning methods adopt a physical knocking mode. The adhesion of metal on the side wall of the crucible is very firm, if the metal is cleaned too frequently, a large amount of labor and time are consumed, and the use of equipment is delayed; the frequency of cleaning is too low, and the accumulated excessive metal (the metal is mixed metal of multiple metals) can be re-melted into the crucible, so that the evaporation source is polluted, the evaporation source cannot be used continuously, and particularly, the loss of precious metals is huge.
Chinese patent document CN105039913B discloses a vapor deposition material removing device and a vapor deposition device. Wherein, this coating by vaporization material clearing device includes: a baffle plate arranged above the evaporation source; a displacement member for controlling the baffle plate to move horizontally and vertically relative to the evaporation source; a motor part disposed on the baffle; and a removing member connected to the motor member and driven by the motor, the removing member being capable of removing the evaporation material when the evaporation source has an outlet blocked by the evaporation material. This cleaning device can only carry out preliminary clearance to the choking mouth of crucible, guarantees going on of can normal coating by vaporization, can't accomplish complete clearance to the thick metal on crucible and the crucible lateral wall.
Chinese patent document CN107435132A discloses a method and apparatus for cleaning a crucible opening by laser, wherein the method comprises the following steps: the method comprises the following steps: emitting low-power laser to generate corresponding light spots; moving the light spot to the edge of the crucible opening; generating an annular aperture; adjusting the size of the annular aperture to ensure that the diameter of the inner circle of the annular aperture is equal to or smaller than the diameter of the edge of the crucible opening, and the diameter of the outer circle is larger than the diameter of the edge of the crucible opening; the laser power is increased to heat. . The device is used for cleaning during evaporation, only can clean the surface of the crucible opening and large bulk metal, is not thorough in cleaning, and is additionally provided with a laser light source, so that the cost is high, and the operation is complicated.
Aiming at the defects of the existing cleaning method of the crucible component of the electron beam evaporation table, a cleaning method which can be used for efficiently and thoroughly cleaning, is low in cost and is simple and convenient to operate is needed to be researched.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the method for cleaning the crucible assembly of the electron beam evaporation table, which can efficiently and thoroughly clean the residual metal on the side wall of the crucible, and has the advantages of low cost and simple and convenient operation.
Interpretation of terms:
the crucible assembly: the whole crucible assembly consists of a crucible and a crucible side wall, the crucible side wall and the crucible are separated, the crucible side wall is a fixed part and consists of a cover plate above the idle crucible and a side wall above the used crucible; the crucible can rotate, and a set of crucible subassembly generally loads several to more than ten crucibles, and every crucible all can hold the evaporation source (for the explanation convenience, will be using the crucible of coating by vaporization and call "use the crucible", other crucibles call "idle crucible");
vapor deposition: during evaporation, the crucible containing the material is moved between the side walls of the crucibles according to the requirement of the material, the material is evaporated by electron beam striking, only one crucible is exposed during evaporation, and when other crucibles are used, the other crucibles are rotated to the position (the middle position of the side wall of the crucible in figure 1).
Metal layer: a large amount of metal materials are evaporated on the side wall of the crucible in the evaporation process to form a metal coating layer which needs to be cleaned.
The technical scheme of the invention is as follows:
a method for cleaning a crucible assembly of an electron beam evaporation table comprises the following operation steps:
(1) and (3) coating preparation: placing a baffle above a crucible, spraying a layer of boron nitride above the baffle by using a boron nitride spray, uniformly distributing the boron nitride spray on the side wall of the crucible, and taking away the baffle after spraying;
(2) the crucible is used: placing a metal evaporation source in the crucible coated with the boron nitride spray coating, and carrying out metal evaporation;
(3) cleaning the side wall of the crucible: and scraping the metal layer on the side wall of the crucible by using a tool to finish the cleaning of the side wall of the crucible.
Preferably, the baffle in step (1) is a circular baffle, the diameter of the baffle is larger than that of the crucible, the crucible is completely shielded by the baffle, and sprayed boron nitride spray is prevented from entering the crucible to pollute the evaporation source.
Preferably, the boron nitride spray in the step (1) is a BN-Q type spray, the BN-Q type spray is an anti-bonding protective material, and the content of boron nitride is more than 99 percent.
Preferably, the thickness of the boron nitride spray in the step (1) is less than 1 mm.
It is further preferred that the boron nitride spray coating thickness is 100-300 μm.
Preferably, the tool used in step (3) is a screwdriver or a blade.
The invention has the beneficial effects that:
1. according to the invention, the boron nitride spray is sprayed on the side wall of the crucible, so that the adhesion degree between the side wall of the crucible and the metal layer is low, a large number of metal layers are conveniently accumulated, the cleaning and removing operation is convenient, the boron nitride spray coating can withstand a high-temperature environment of more than 1000 ℃, the evaporation source in the crucible can be ensured to be normally melted, and meanwhile, the material on the side wall of the crucible can not be melted and flows into the crucible, and the normal evaporation use of the crucible is ensured.
2. According to the invention, with the increase of the evaporation heat, the thickness of the metal on the crucible wall is gradually increased, the metal layer and the boron nitride coating form a separation gap after reaching a certain thickness, the large metal layer is easily torn off directly by inserting the hard material into the gap, and the crucible wall does not need to be knocked in the cleaning process.
3. The process method disclosed by the invention is simple and convenient to operate, low in cost, quick and effective, and free of physical damage to parts such as the crucible, is not only suitable for cleaning the side wall of the crucible, but also applicable to parts with thicker accumulated metal in evaporation or sputtering, such as small shower, electron beam absorption plates, parts such as craters at the connection part of an electron gun and the crucible, and is also suitable for other processing processes for covering high-temperature metal on the surface.
4. The spraying thickness of the boron nitride spraying agent is too thick in the cleaning process of the crucible assembly, a complete isolation layer can be formed, and when less metal is evaporated, the boron nitride isolation layer can fall off, so that the cleaning frequency is increased, and the use cost of the boron nitride spraying agent is increased; the spraying is too thin, effective isolation cannot be formed, part of metal still contacts with the crucible wall, complete massive metal cannot be formed during cleaning, knocking cleaning is needed, and damage is caused to the crucible wall.
Drawings
FIG. 1 is a schematic view of an evaporation station evaporation system;
FIG. 2 is a schematic view of the boron nitride spray of the present invention;
FIG. 3 is a schematic view of a crucible assembly of the present invention;
wherein: 1. a cover plate; 2. a crucible assembly; 3. using a crucible; 4. idling the crucible; 5. a crucible side wall; 6. a baffle plate; 7. the spraying direction; 8. an evaporation rack; 9. an evaporation table cavity; 10. an evaporation source.
Detailed Description
The present invention will be further described by way of examples, but not limited thereto, with reference to the accompanying drawings.
Example 1:
the embodiment provides a method for cleaning a crucible assembly of an electron beam evaporation table, which comprises the following operation steps:
(1) and (3) coating preparation: placing a baffle 6 above a crucible 3, spraying a layer of boron nitride above the baffle by using a boron nitride spray, wherein the spraying direction 7 is shown in figure 2, so that the boron nitride spray is uniformly distributed on the side wall of the crucible, and taking away the baffle 6 after the spraying is finished;
(2) the crucible is used: placing a metal evaporation source in the crucible coated with the boron nitride spray coating, and carrying out metal evaporation;
(3) cleaning a crucible: and scraping the metal layer on the side wall 5 of the crucible by using a tool to finish the cleaning of the crucible.
In the step (1), the baffle 6 is a circular baffle, the diameter of the baffle is larger than that of the crucible, the crucible is completely shielded by the baffle, the sprayed boron nitride spray is prevented from entering the crucible to pollute the evaporation source, the evaporation table is a large-scale integral assembly system, the crucible is difficult to disassemble and assemble, and a large amount of labor time can be consumed if the sprayed boron nitride spray is prevented from entering the crucible by disassembling the crucible.
The thickness of the boron nitride spray coating in the step (1) is 100 mu m.
The tool used in the step (3) is a screwdriver.
The crucible side wall 5 is a fixed part and is composed of a cover plate 1 above an idle crucible 4 and a side wall of a used crucible 3, and a schematic view of a crucible assembly 2 is shown in FIG. 3.
After the cleaning method of the embodiment cleans, the residual amount of the metal layer on the side wall of the crucible is 0.
Example 2:
a method for cleaning a crucible assembly of an electron beam evaporation station comprises the following operation steps of example 1, except that the thickness of a boron nitride spray coating in the step (1) is 300 μm.
The tool used in step (3) is a blade.
After the cleaning method of the embodiment cleans, the residual amount of the metal layer on the side wall of the crucible is 0.
Example 3:
the operation steps of the method for cleaning the crucible component of the electron beam evaporation table are as described in embodiment 1, and the difference is that the boron nitride spray in the step (1) is a BN-Q type spray, the BN-Q type spray is an anti-bonding protective material, and the content of boron nitride is more than 99%.
Comparative example 1:
comparative example 1 provides a method for cleaning a crucible assembly of an electron beam evaporation station, which comprises the following steps of 1, wherein the boron nitride spray coating is 50 μm thick, and the residual amount of a metal layer on the side wall of the crucible after cleaning by the cleaning method of comparative example 1 is 5-20%.
Comparative example 2:
comparative example 2 provides a method for cleaning a crucible assembly of an electron beam evaporation station, which comprises the following steps as described in example 1, except that the thickness of the boron nitride spray coating is 600 μm, the boron nitride spray coating is too thick, a metal layer warping layer is formed by less evaporated metal, and the metal layer falls off in the crucible during evaporation to influence the subsequent evaporation.
Comparative example 3:
comparative example 3 provides a cleaning method of a crucible assembly of an electron beam evaporation station, the operation steps are as described in example 1, except that a high temperature resistant adhesive tape is used to make a coating on the side wall of the crucible in the step (1), after the cleaning method of the comparative example 3 is used for cleaning, the residual quantity of a metal layer on the side wall of the crucible is more than 30%, and the melting quantity of the coating is more than 50%. The high-temperature resistant adhesive tape cannot bear the high temperature during evaporation, most of the high-temperature resistant adhesive tape can be melted and mixed with metal, and the high-temperature resistant adhesive tape is difficult to clean.
Comparative example 4:
comparative example 4 provides a method for cleaning a crucible assembly of an electron beam evaporation station, which comprises the following steps of 1, wherein the insulating teflon material is used for preparing a coating on the side wall of the crucible in the step (1), and after the cleaning method of the comparative example 4 is used for cleaning, the residual quantity of the metal layer on the side wall of the crucible is more than 30%, and the melting quantity of the coating is more than 50%. The insulating teflon material cannot bear the high temperature during evaporation, most of the insulating teflon material is melted and doped with metal, and the insulating teflon material is difficult to clean.
To sum up, the boron nitride spray coating thickness of comparative example 1 is too thin, leads to the metal level of crucible lateral wall to remain the volume too high, and the boron nitride spraying of comparative example 2 is too thick, and the less metal of coating by vaporization can form the metal level and stick up the layer, and this part metal level of coating by vaporization process will drop and influence follow-up coating by vaporization in falling into the crucible. The high-temperature-resistant adhesive tape of the comparative example 3 and the insulating Teflon material of the comparative example 4 can not bear the high temperature during evaporation, most of the high-temperature-resistant adhesive tape can be melted and mixed with metal, and the cleaning is difficult. After the cleaning methods described in examples 1 and 2, the residual amount of the metal layer on the side wall of the crucible was 0, and the cleaning effect was the best.

Claims (6)

1. A method for cleaning a crucible assembly of an electron beam evaporation table is characterized by comprising the following operation steps:
(1) and (3) coating preparation: placing a baffle above a crucible, spraying a layer of boron nitride above the baffle by using a boron nitride spray, uniformly distributing the boron nitride spray on the side wall of the crucible, and taking away the baffle after spraying;
(2) the crucible is used: placing a metal evaporation source in the crucible coated with the boron nitride spray coating, and carrying out metal evaporation;
(3) cleaning the side wall of the crucible: and scraping the metal layer on the side wall of the crucible by using a tool to finish the cleaning of the side wall of the crucible.
2. The method for cleaning the crucible assembly of the electron beam evaporation station as claimed in claim 1, wherein the baffle in step (1) is a circular baffle, and the diameter of the baffle is larger than that of the crucible.
3. The method for cleaning the crucible assembly of the electron beam evaporation table as claimed in claim 1, wherein the boron nitride spray in the step (1) is a BN-Q type spray.
4. The method for cleaning the crucible assembly of the electron beam evaporation station as claimed in claim 1, wherein the thickness of the boron nitride spray in step (1) is less than 1 mm.
5. The method for cleaning the crucible assembly of the electron beam evaporation station as claimed in claim 4, wherein the thickness of the boron nitride spray coating in the step (1) is 100-300 μm.
6. The method for cleaning the crucible assembly of the electron beam evaporation station as claimed in claim 1, wherein the tool used in the step (3) is a screwdriver or a blade.
CN202011163179.4A 2020-10-27 2020-10-27 Method for cleaning crucible assembly of electron beam evaporation table Pending CN114481042A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103290355A (en) * 2012-02-14 2013-09-11 金文焕 Cleaning method of part of physical vapor deposition reaction chamber
CN106756805A (en) * 2016-12-28 2017-05-31 京东方科技集团股份有限公司 Evaporation crucible and deposition system
JP2019081949A (en) * 2017-10-31 2019-05-30 キヤノントッキ株式会社 Evaporation source device, film deposition apparatus, film deposition method, and manufacturing method of electronic device
CN209522904U (en) * 2018-11-24 2019-10-22 苏州佑伦真空设备科技有限公司 A kind of protective cover for the crucible easy to clean evaporating aluminum material
CN210287491U (en) * 2019-07-05 2020-04-10 苏州普京真空技术有限公司 Conveniently take and abluent crucible

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103290355A (en) * 2012-02-14 2013-09-11 金文焕 Cleaning method of part of physical vapor deposition reaction chamber
CN106756805A (en) * 2016-12-28 2017-05-31 京东方科技集团股份有限公司 Evaporation crucible and deposition system
JP2019081949A (en) * 2017-10-31 2019-05-30 キヤノントッキ株式会社 Evaporation source device, film deposition apparatus, film deposition method, and manufacturing method of electronic device
CN209522904U (en) * 2018-11-24 2019-10-22 苏州佑伦真空设备科技有限公司 A kind of protective cover for the crucible easy to clean evaporating aluminum material
CN210287491U (en) * 2019-07-05 2020-04-10 苏州普京真空技术有限公司 Conveniently take and abluent crucible

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