CN106328466A - Recovery method of sapphire window ceramic sheet of power transmission window - Google Patents

Recovery method of sapphire window ceramic sheet of power transmission window Download PDF

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Publication number
CN106328466A
CN106328466A CN201610783194.6A CN201610783194A CN106328466A CN 106328466 A CN106328466 A CN 106328466A CN 201610783194 A CN201610783194 A CN 201610783194A CN 106328466 A CN106328466 A CN 106328466A
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CN
China
Prior art keywords
ceramics
sapphire window
window
sapphire
delivery
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Pending
Application number
CN201610783194.6A
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Chinese (zh)
Inventor
王鹏康
李金晶
朱刚
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Anhui East China Institute of Optoelectronic Technology
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Anhui East China Institute of Optoelectronic Technology
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Priority to CN201610783194.6A priority Critical patent/CN106328466A/en
Publication of CN106328466A publication Critical patent/CN106328466A/en
Pending legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/50Repairing or regenerating used or defective discharge tubes or lamps
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J23/00Details of transit-time tubes of the types covered by group H01J25/00
    • H01J23/36Coupling devices having distributed capacitance and inductance, structurally associated with the tube, for introducing or removing wave energy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2223/00Details of transit-time tubes of the types covered by group H01J2225/00
    • H01J2223/36Coupling devices having distributed capacitance and inductance, structurally associated with the tube, for introducing or removing wave energy
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/82Recycling of waste of electrical or electronic equipment [WEEE]

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Surface Treatment Of Glass (AREA)
  • Processing Of Stones Or Stones Resemblance Materials (AREA)

Abstract

Provided is a recovery method of a sapphire window ceramic sheet of a power transmission window. The method includes following steps: S01, dissecting the power transmission window; S02, corroding a metal material; S03, grinding and removing a metallization layer; S04, performing chemical cleaning on the sapphire window ceramic sheet, and performing chemical de-oiling cleaning on the sapphire window ceramic sheet obtained in S03 by employing a pickling solution; S05, detecting whether the sapphire window ceramic sheet has a scratch or a gap, S06, detecting whether a residual metallization layer exits; and S07, detecting whether the dimension of the sapphire window ceramic sheet satisfies a design requirement. According to the recovery method of the sapphire window ceramic sheet of the power transmission window, repeated utilization of the sapphire window ceramic sheet can be realized, the production cost is reduced, and the production efficiency is improved; besides, the recovery method is low in cost so that large-scale promotion can be realized.

Description

A kind of recovery method of delivery of energy window sapphire window ceramics
Technical field
The present invention relates to the recovery method of a kind of delivery of energy window sapphire window ceramics, belong to sapphire and recycle field.
Background technology
In travelling-wave tube, the Main Function of delivery of energy window is transmission microwave energy.Sapphire has good heat conductivity and high frequency Can, it is applied to high power travelling wave tube output window.During travelling-wave tube makes, the gas leakage of delivery of energy window often occurs or stays Ripple is unsatisfactory for the situation of design requirement and produces and cause window to be scrapped, and secondly also has the travelling-wave tube life-span to end or electrical quantity degenerates and causes Pipe is scrapped, and the most also has substantial amounts of window of scrapping and produces.Due to sapphire function admirable, price comparison costliness, if can have A kind of sapphire window ceramics recovery method, can reuse after being passed through processing is significantly.
Summary of the invention
The technical problem to be solved in the present invention is to provide one and can realize the recycling of sapphire window ceramics, save life Produce cost and improve the recovery method of delivery of energy window sapphire window ceramics of production efficiency;Further, the present invention provides a kind of The recovery method of the delivery of energy window sapphire window ceramics that cost recovery is cheap.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
The recovery method of a kind of delivery of energy window sapphire window ceramics, comprises the following steps:
S01, dissects delivery of energy window, according to the practical structures of delivery of energy window, by mechanical cutting method by sapphire window ceramics from delivery of energy Window dissects out;
S02, metallic material corrosion, the sapphire window ceramics obtained by S01 is immersed in the etch chemistries solution prepared and carries out Corrosiveness, clean so that the metal material of sealing-in sapphire window ceramics is etched;
S03, metal layer grinds to be removed, and the sapphire window ceramics obtained by S02 carries out accurate polishing on surface grinding machine, with will On sapphire window ceramics, the metal layer of residual is removed;
S04, sapphire window ceramics Chemical cleaning, the sapphire window ceramics obtained by S03 uses Acidwash solution to carry out chemical deoiling and degreasing Clean;
S05, whether detection sapphire window ceramics exists cut or breach, and the sapphire window ceramics that if it is S04 obtains is straight It is informed of a case useless, if otherwise continuing the next one to process step;
S06, detects whether to exist remaining metal layer, amplifies whether 24 times check sapphire window ceramics surface under the microscope There is remaining metal layer, if it is forward S03 to and re-operate, if otherwise continuing the next one to process step;
S07, whether detection sapphire window ceramics size meets design requirement, if the sapphire window ceramics size otherwise obtained is not Qualified, if it is judge that the sapphire window ceramics obtained is certified products, be successfully completed the recovery operation of sapphire window ceramics.
Described recovery method is to use Activated Molybdenum manganese method metallization process for sapphire, and sealing of metal is kovar alloy material The delivery of energy window of material processing.
In S04, Acidwash solution includes ammonia and the mixed solution of formic acid of hydrogen peroxide, 20%~25% of 30%~35%, its The volume of middle hydrogen peroxide, ammonia and formic acid is 300 ± 10mL.
The number of times of described sapphire window ceramics Chemical cleaning is more than or equal to 1 time.
The time of described corrosiveness is more than 24h.
Described etch chemistries solution includes following components sulphuric acid, nitric acid and deionized water, according to volume ratio sulphuric acid: nitric acid: Deionized water=(3~4): (5~6): (2~5) proportional arrangement forms, described sulphuric acid includes that concentrated sulphuric acid, described nitric acid include dense nitre Acid.
Described etch chemistries solution includes the mixed solution of sulphuric acid and nitric acid, and wherein the volume fraction of sulphuric acid and nitric acid is respectively It is 30% and 50%.
Described mechanical cutting method includes turning or fast silk cutting.
Beneficial effects of the present invention: the recovery method of a kind of delivery of energy window sapphire window ceramics that the present invention provides, including 7 Implement step easily, it is possible to realize the recycling of sapphire window ceramics, while saving production cost, also improve production Efficiency;Described Acidwash solution and etch chemistries solution composition are simple, and effect is notable, cheap, it is possible to reduce delivery of energy window indigo plant precious The cost recovery of stone window ceramics.
Accompanying drawing explanation
Fig. 1 is the flow chart of the present invention;
Fig. 2 is the structural representation of delivery of energy window in the present invention.
Detailed description of the invention
The invention will be further described below in conjunction with the accompanying drawings, and following example are only used for clearly illustrating the present invention Technical scheme, and can not limit the scope of the invention with this.
Embodiment 1
As it is shown in figure 1, the recovery method of a kind of delivery of energy window sapphire window ceramics, comprise the following steps:
S01, dissects delivery of energy window, according to the practical structures of delivery of energy window, by turning or fast silk cutting method by sapphire window ceramics Dissect out from delivery of energy window;
S02, metallic material corrosion, the sapphire window ceramics obtained by S01 is immersed in the etch chemistries solution prepared and carries out Corrosiveness, clean so that the metal material of sealing-in sapphire window ceramics is etched;
S03, metal layer grinds to be removed, and the sapphire window ceramics obtained by S02 carries out accurate polishing on surface grinding machine, with will On sapphire window ceramics, the metal layer of residual is removed;
S04, sapphire window ceramics Chemical cleaning, the sapphire window ceramics obtained by S03 uses Acidwash solution to carry out chemical deoiling and degreasing Clean;
S05, whether detection sapphire window ceramics exists cut or breach, and the sapphire window ceramics that if it is S04 obtains is straight It is informed of a case useless, if otherwise continuing the next one to process step;
S06, detects whether to exist remaining metal layer, amplifies whether 24 times check sapphire window ceramics surface under the microscope There is remaining metal layer, if it is forward S03 to and re-operate, if otherwise continuing the next one to process step;
S07, whether detection sapphire window ceramics size meets design requirement, if the sapphire window ceramics size otherwise obtained Defective, if it is judge that the sapphire window ceramics obtained is certified products, be successfully completed the recovery operation of sapphire window ceramics.
In Fig. 2, delivery of energy window mainly includes sapphire window ceramics 1, delivery of energy window upper flange 2 and delivery of energy window upper flange 3.
Described mechanical cutting method includes turning or fast silk cutting, as preferably, by fast silk cutting method by described defeated Energy window upper flange 1 and described delivery of energy window lower flange are respectively cut at close described sapphire window ceramics 2mm and remove.
Described recovery method is to use Activated Molybdenum manganese method metallization process for sapphire, and sealing of metal is kovar alloy material The delivery of energy window of material processing.
In S04, Acidwash solution includes the hydrogen peroxide of 30%, the ammonia of 20% and the mixed solution of formic acid, wherein peroxidating The volume of hydrogen, ammonia and formic acid is 300 ± 10mL.
The number of times of described sapphire window ceramics Chemical cleaning is more than or equal to 1 time, as preferably selecting Chemical cleaning Number of times is 3 times.
The time of described corrosiveness is more than 24h, it is therefore an objective to by clean for sealing-in sapphire window ceramics metal material etching.
Described etch chemistries solution includes following components sulphuric acid, nitric acid and deionized water, according to volume ratio sulphuric acid: nitric acid: Deionized water=3:5:2 proportional arrangement forms, and described sulphuric acid includes that concentrated sulphuric acid, described nitric acid include concentrated nitric acid.
Described etch chemistries solution includes the mixed solution of sulphuric acid and nitric acid, and wherein the volume fraction of sulphuric acid and nitric acid is respectively It is 30% and 50%.
Embodiment 2
As it is shown in figure 1, the recovery method of a kind of delivery of energy window sapphire window ceramics, comprise the following steps:
S01, dissects delivery of energy window, according to the practical structures of delivery of energy window, by turning or fast silk cutting method by sapphire window ceramics Dissect out from delivery of energy window;
S02, metallic material corrosion, the sapphire window ceramics obtained by S01 is immersed in the etch chemistries solution prepared and carries out Corrosiveness, clean so that the metal material of sealing-in sapphire window ceramics is etched;
S03, metal layer grinds to be removed, and the sapphire window ceramics obtained by S02 carries out accurate polishing on surface grinding machine, with will On sapphire window ceramics, the metal layer of residual is removed;
S04, sapphire window ceramics Chemical cleaning, the sapphire window ceramics obtained by S03 uses Acidwash solution to carry out chemical deoiling and degreasing Clean;
S05, whether detection sapphire window ceramics exists cut or breach, and the sapphire window ceramics that if it is S04 obtains is straight It is informed of a case useless, if otherwise continuing the next one to process step;
S06, detects whether to exist remaining metal layer, amplifies whether 24 times check sapphire window ceramics surface under the microscope There is remaining metal layer, if it is forward S03 to and re-operate, if otherwise continuing the next one to process step;
S07, whether detection sapphire window ceramics size meets design requirement, if the sapphire window ceramics size otherwise obtained Defective, if it is judge that the sapphire window ceramics obtained is certified products, be successfully completed the recovery operation of sapphire window ceramics.
In Fig. 2, delivery of energy window mainly includes sapphire window ceramics 1, delivery of energy window upper flange 2 and delivery of energy window upper flange 3.
Described mechanical cutting method includes turning or fast silk cutting, as preferably, by fast silk cutting method by described defeated Energy window upper flange 1 and described delivery of energy window lower flange are respectively cut at close described sapphire window ceramics 2mm and remove.
Described recovery method is to use Activated Molybdenum manganese method metallization process for sapphire, and sealing of metal is kovar alloy material The delivery of energy window of material processing.
In S04, Acidwash solution includes the hydrogen peroxide of 35%, the ammonia of 25% and the mixed solution of formic acid, wherein peroxidating The volume of hydrogen, ammonia and formic acid is 300 ± 10mL.
The number of times of described sapphire window ceramics Chemical cleaning is more than or equal to 1 time, as preferably selecting Chemical cleaning Number of times is 3 times.
The time of described corrosiveness is more than 24h, it is therefore an objective to by clean for sealing-in sapphire window ceramics metal material etching.
Described etch chemistries solution includes following components sulphuric acid, nitric acid and deionized water, according to volume ratio sulphuric acid: nitric acid: Deionized water=4:6:5 proportional arrangement forms, and described sulphuric acid includes that concentrated sulphuric acid, described nitric acid include concentrated nitric acid.
Described etch chemistries solution includes the mixed solution of sulphuric acid and nitric acid, and wherein the volume fraction of sulphuric acid and nitric acid is respectively It is 30% and 50%.
The above is only the preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (7)

1. the recovery method of a delivery of energy window sapphire window ceramics, it is characterised in that comprise the following steps:
S01, dissects delivery of energy window, according to the practical structures of delivery of energy window, by mechanical cutting method by sapphire window ceramics from delivery of energy Window dissects out;
S02, metallic material corrosion, the sapphire window ceramics obtained by S01 is immersed in the etch chemistries solution prepared and carries out Corrosiveness, clean so that the metal material of sealing-in sapphire window ceramics is etched;
S03, metal layer grinds to be removed, and the sapphire window ceramics obtained by S02 carries out accurate polishing on surface grinding machine, with will On sapphire window ceramics, the metal layer of residual is removed;
S04, sapphire window ceramics Chemical cleaning, the sapphire window ceramics obtained by S03 uses Acidwash solution to carry out chemical deoiling and degreasing Clean;
S05, whether detection sapphire window ceramics exists cut or breach, and the sapphire window ceramics that if it is S04 obtains is straight It is informed of a case useless, if otherwise continuing the next one to process step;
S06, detects whether to exist remaining metal layer, amplifies whether 24 times check sapphire window ceramics surface under the microscope There is remaining metal layer, if it is forward S03 to and re-operate, if otherwise continuing the next one to process step;
S07, whether detection sapphire window ceramics size meets design requirement, if the sapphire window ceramics size otherwise obtained is not Qualified, if it is judge that the sapphire window ceramics obtained is certified products, be successfully completed the recovery operation of sapphire window ceramics.
The recovery method of a kind of delivery of energy window sapphire window ceramics the most according to claim 1, it is characterised in that: described recovery Method is to use Activated Molybdenum manganese method metallization process for sapphire, and sealing of metal is the delivery of energy window of kovar alloy materials processing.
The recovery method of a kind of delivery of energy window sapphire window ceramics the most according to claim 1, it is characterised in that: acid in S04 Dilution includes ammonia and the mixed solution of formic acid that hydrogen peroxide that concentration is 30%~35%, concentration are 20%~25%, wherein The volume of hydrogen peroxide, ammonia and formic acid is 300 ± 10mL.
The recovery method of a kind of delivery of energy window sapphire window ceramics the most according to claim 1, it is characterised in that: described blue precious The number of times of stone window ceramics Chemical cleaning is more than or equal to 1 time.
The recovery method of a kind of delivery of energy window sapphire window ceramics the most according to claim 1, it is characterised in that: described corrosion The time of effect is more than 24h.
The recovery method of a kind of delivery of energy window sapphire window ceramics the most according to claim 1, it is characterised in that: described corrosion Chemical solution includes following components sulphuric acid, nitric acid and deionized water, according to volume ratio sulphuric acid: nitric acid: deionized water=(3~4): (5~6): (2~5) proportional arrangement forms, described sulphuric acid includes that concentrated sulphuric acid, described nitric acid include concentrated nitric acid.
The recovery method of a kind of delivery of energy window sapphire window ceramics the most according to claim 1, it is characterised in that: described machinery Cutting method includes turning or fast silk cutting.
CN201610783194.6A 2016-08-31 2016-08-31 Recovery method of sapphire window ceramic sheet of power transmission window Pending CN106328466A (en)

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Application Number Priority Date Filing Date Title
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004186600A (en) * 2002-12-05 2004-07-02 Mitsubishi Heavy Ind Ltd Optical characteristics recovery method of optical system and its device
CN101875886A (en) * 2009-04-29 2010-11-03 重庆川仪自动化股份有限公司 Sapphire infrared window cleaning agent and preparation method
CN104708724A (en) * 2015-03-09 2015-06-17 江苏苏博瑞光电设备科技有限公司 Sapphire diaphragm producing technology
CN104868020A (en) * 2014-02-21 2015-08-26 山东浪潮华光光电子股份有限公司 Method for recovering sapphire substrate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004186600A (en) * 2002-12-05 2004-07-02 Mitsubishi Heavy Ind Ltd Optical characteristics recovery method of optical system and its device
CN101875886A (en) * 2009-04-29 2010-11-03 重庆川仪自动化股份有限公司 Sapphire infrared window cleaning agent and preparation method
CN104868020A (en) * 2014-02-21 2015-08-26 山东浪潮华光光电子股份有限公司 Method for recovering sapphire substrate
CN104708724A (en) * 2015-03-09 2015-06-17 江苏苏博瑞光电设备科技有限公司 Sapphire diaphragm producing technology

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