CN110330238A - A kind of quartz glass optical window and preparation method thereof - Google Patents
A kind of quartz glass optical window and preparation method thereof Download PDFInfo
- Publication number
- CN110330238A CN110330238A CN201910575985.3A CN201910575985A CN110330238A CN 110330238 A CN110330238 A CN 110330238A CN 201910575985 A CN201910575985 A CN 201910575985A CN 110330238 A CN110330238 A CN 110330238A
- Authority
- CN
- China
- Prior art keywords
- quartz glass
- preparation
- optical window
- titanium valve
- glass optical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0075—Cleaning of glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0085—Drying; Dehydroxylation
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/04—Joining glass to metal by means of an interlayer
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/04—Joining glass to metal by means of an interlayer
- C03C27/042—Joining glass to metal by means of an interlayer consisting of a combination of materials selected from glass, glass-ceramic or ceramic material with metals, metal oxides or metal salts
- C03C27/046—Joining glass to metal by means of an interlayer consisting of a combination of materials selected from glass, glass-ceramic or ceramic material with metals, metal oxides or metal salts of metals, metal oxides or metal salts only
-
- E—FIXED CONSTRUCTIONS
- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
- E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
- E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
- E06B3/54—Fixing of glass panes or like plates
- E06B3/58—Fixing of glass panes or like plates by means of borders, cleats, or the like
- E06B3/60—Fixing of glass panes or like plates by means of borders, cleats, or the like of clamping cleats of metal
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Joining Of Glass To Other Materials (AREA)
Abstract
The invention discloses a kind of preparation methods of quartz glass optical window, the preparation method is quartz glass is successively cleaned, drying, after sealing surface metalized, then by after sealing surface metalized quartz glass and metal parts assembling after carry out vacuum brazing sealing-in.The disposable sealing-in success of quartz glass and metal parts may be implemented in the present invention, has very high physical bonds intensity and air-tightness, while good process repeatability, may be implemented to produce in batches.
Description
Technical field
The invention belongs to optical window technical fields, and in particular to a kind of quartz glass optical window and preparation method thereof.
Background technique
Quartz glass has high temperature resistant, low dielectric loss, can resist electron bombardment and atomic radiation, and have very high
Electric breakdown strength is the more satisfactory energy output window material of certain UHF electronic devices；In addition, quartz glass has well
The transparency has very high transmissivity to infrared ray and ultraviolet light, and chemical stabilization is good, can be used in electric light source and laser device；Together
When, quartz glass is also the high-temperature material of good heat stability, and can make space vehicle pries through optical window etc..
But the coefficient of expansion of quartz glass is very low, can match with it without any one metal, the anti-tensile of quartz glass
Intensity is again very low, this just makes the sealing-in of quartz glass and metal become very difficult.Currently, the sealing-in of quartz glass and metal is normal
Frequently with epoxy bonding, transitional glass connector, directly the methods of sealing.Although the gas that these methods can reache a certain level
Close property sealing-in, but respectively have disadvantage.It is easy aging as epoxy is bonded, it cannot be guaranteed that long-term airtight；Transitional glass connector, essence
Low, intensity difference is spent, cumbersome is difficult to grasp；It directly seals, the geometric dimension of metalwork is very limited, air-tightness and resistance to
Thermal shock resistance properties is all poor.In this way if the method that a kind of new quartz glass and metalwork sealing-in can be invented, it is clear that be significant
's.
Summary of the invention
Present invention seek to address that the technical problems existing in the prior art.For this purpose, the present invention provides a kind of quartz glass light
Window and preparation method thereof, it is therefore an objective to realize the disposable sealing-in success of quartz glass and metal parts, while there is very high object
Manage adhesive strength and air-tightness.
To achieve the goals above, the technical scheme adopted by the invention is as follows:
A kind of preparation method of quartz glass optical window, the preparation method are quartz glass is successively cleaned, drying, envelope
After junction metalized, then by the quartz glass after sealing surface metalized and progress vacuum pricker after metal parts assembling
Sealing connects.
The method of the sealing surface metalized is to coat titanium valve paste in quartz glass sealing surface, is carried out after coating is good
Drying and processing, the temperature of drying are 80~100 DEG C, and the titanium valve paste is the mixture of titanium valve and cotton solution, titanium valve and nitre
The mass volume ratio of cotton solution is 1g:13~15ml.
Preferably, the purity of titanium valve reaches 99.7% or more, and for granularity between 270~360 mesh, fine size is a little, is conducive to
Paste coating.
The preparation method of the titanium valve paste is the guncotton for pouring into ball grinder the titanium valve of formula ratio, and measuring formula ratio
Solution imports in ball grinder, in ball grinder lid, will be arranged 250~300 revs/min of drum's speed of rotation, ball milling 1~2 hour i.e.
It can.Cotton solution prepares the method configuration being referred in electrovacuum technique document.
Quartz glass sealing surface coating titanium valve paste with a thickness of 20~50 μm.
The method of the cleaning is that quartz glass is first successively soaked in gasoline, is deoiled in acetone, later by quartz glass
Surface acid-washing is carried out, then the acid solution of washing removal Quartz glass surfaces.
The method of the pickling is that quartz glass is impregnated to 1~2min in hydrofluoric acid.
The drying is that baking oven drying will be put into after quartz glass dehydration of alcohol, and the temperature setting of baking oven is 80~100
℃。
The material selection of metal parts has the metal or the lower ceramic sealing alloy metal of the coefficient of expansion of good plasticity.It is excellent
Choosing, the material of the metal parts uses oxygen-free copper or kovar alloy.The oxygen-free copper trade mark is Tu1, and the kovar alloy trade mark is
4J34。
After the quartz glass and metal parts assembling, silver-copper solder, the vacuum are placed at gap to be welded
The process of soldering is that quartz glass and the assembled component of metal parts are put into vacuum drying oven, when vacuum reaches 3 × 10- 5When mmHg or more, starting to warm up, heating rate is controlled at 6~15 DEG C/min, when sealing temperature reaches 820~830 DEG C, heat preservation
3~5 minutes.
Quartz glass optical window quality testing: the brazing quality of quartz glass optical window, stone are examined with helium mass spectrum leak detection instrument
English glass optical window air-tightness reaches leakage rate Q≤10-10MmHg liter/second, and can be hot three times to room temperature by 200~500 DEG C
Impact test can determine whether that quartz glass optical window is up-to-standard.
A kind of quartz glass optical window is made using above-mentioned preparation method, including metal parts and quartz glass, the quartz
The sealing surface of glass is coated with titanium valve layer of paste, is placed with silver-at the gap to be welded after quartz glass and metal parts assembling
Spelter solder.
Beneficial effects of the present invention: the disposable sealing-in success of quartz glass and metal parts, tool may be implemented in the present invention
There are very high physical bonds intensity and air-tightness, while good process repeatability, may be implemented to produce in batches.
Detailed description of the invention
This specification includes the following drawings, and shown content is respectively:
Fig. 1 is the process step of the invention flow diagram；
Fig. 2 is quartz glass optical window structural schematic diagram of the invention.
In the figure, it is marked as
1, quartz glass, 2, metal parts, 3, silver-copper solder.
Specific embodiment
Below against attached drawing, by the description of the embodiment, making to a specific embodiment of the invention further details of
Explanation, it is therefore an objective to those skilled in the art be helped to have more complete, accurate and deep reason to design of the invention, technical solution
Solution, and facilitate its implementation.
Metal parts herein is for the metal sealing part with quartz glass sealing-in.
As shown in Figure 1 to Figure 2, a kind of quartz glass optical window, including metal parts 2 and quartz glass 1, quartz glass 1
Sealing surface is coated with titanium valve layer of paste, is placed with silver-copper weldering at the gap to be welded after quartz glass 1 and the assembling of metal parts 2
Material 3.
The preparation method of above-mentioned quartz glass optical window is quartz glass is successively cleaned, drying, at sealing surface metallization
After reason, then by the quartz glass after sealing surface metalized and progress vacuum brazing sealing-in after metal parts assembling.
The method of sealing surface metalized is to coat titanium valve paste in quartz glass sealing surface, is dried after coating is good
Processing, the temperature of drying are 80~100 DEG C, and the titanium valve paste is the mixture of titanium valve and cotton solution, and titanium valve is molten with guncotton
The mass volume ratio of liquid is 1g:13~15ml.Preferably, the purity of titanium valve reaches 99.7% or more, and granularity is in 270~360 mesh
Between, fine size is a little, is conducive to paste coating.Metal parts material selection have good plasticity metal or the coefficient of expansion compared with
Low ceramic sealing alloy metal, preferential to select oxygen-free copper or kovar alloy, the oxygen-free copper trade mark is Tu1, and the kovar alloy trade mark is 4J34.
It is illustrated for below using kovar alloy as the material of metal parts:
Embodiment 1
A kind of preparation method of quartz glass optical window, concrete operations processing step are as follows:
A), the pre-processing of quartz glass: the quartz glass to sealing-in being deoiled, is cleaned, process be by
Quartz glass is soaked in gasoline and acetone respectively deoils in order, soaking time with Quartz glass surfaces greasy dirt situation and
Fixed, general soaking time is 30~45min；Quartz glass is impregnated to 1~2min after deoiling in hydrofluoric acid, carries out surface acid
It washes；Deionized water scouring stone English 3~5min of glass is used later, so that the hydrofluoric acid of glass surface is rinsed completely；Finally will
Until being put into 80~100 DEG C of baking oven drying after quartz glass dehydration of alcohol.
B), the preparation of titanium valve paste: the process by titanium valve and cotton solution modulation paste making agent is according to titanium powder
(g): guncotton (ml)=1:15 proportion, the titanium valve for weighing requirement pour into ball grinder, and measure said ratio with graduated cylinder
The cotton solution of volume pours into ball grinder, by ball grinder lid, is arranged 250~300 revs/min of drum's speed of rotation, ball milling 1
Hour.
C), quartz glass coats titanium valve paste: the paste that step (b) prepares uniformly is coated in quartzy glass with writing brush
On the sealing surface of glass, quartz glass is entered 80~100 DEG C of drying paste coatings of baking oven after coating is good in 35um by thickness control.
D), the assembling of quartz glass and metal parts: sealing surface has been coated titanium valve paste by structure according to Fig.2,
Quartz glass assembled with metal parts, at gap to be welded place one circle specification be Ф 0.8 silver-copper solder.
E), assembled component is put into vacuum drying oven and carries out high temperature brazing, specifically executed by following technique: when vacuum reaches
3×10-5When mmHg or more, start slowly to heat up, heating rate is controlled at 6~15 DEG C/min, and sealing temperature reaches 820~830
DEG C when, keep the temperature 3~5 minutes.
F), quartz glass optical window quality testing: examining the brazing quality of quartz glass optical window with helium mass spectrum leak detection instrument,
Guarantee that quartz glass optical window air-tightness reaches leakage rate Q≤10-10MmHg liter/second, and can by 200 DEG C to room temperature three times
Thermal shock test can determine whether that quartz glass optical window is up-to-standard.
Comparative example 1
This comparative example and embodiment 1 the difference lies in that prepare paste making agent using molybdenum powder and cotton solution, it is final obtained
The thermal shock effect of quartz glass optical window is not so good as embodiment 1.
Comparative example 2
This comparative example and embodiment 1 the difference lies in that prepare paste making agent using tungsten powder and cotton solution, it is final obtained
The thermal shock effect of quartz glass optical window is not so good as embodiment 1.
Comparative example 3
This comparative example and embodiment 1 the difference lies in that in the preparation of titanium valve paste, titanium powder (g): guncotton (ml)=1:
17, the thermal shock effect of final quartz glass optical window obtained is not so good as embodiment 1, and air-tightness is relatively poor.
Comparative example 4
This comparative example and embodiment 1 the difference lies in that in the preparation of titanium valve paste, titanium powder (g): guncotton (ml)=1:
12, the thermal shock effect of final quartz glass optical window obtained is not so good as embodiment 1, and air-tightness is relatively poor.
Comparative example 5
Quartz glass, the difference lies in that after quartz glass coating titanium valve paste, is entered baking oven with embodiment 1 by this comparative example
The thermal shock effect of 150 DEG C of drying paste coatings, final quartz glass optical window obtained is not so good as embodiment 1.
Comparative example 6
This comparative example is with embodiment 1 the difference lies in that the temperature of vacuum seal rises in temperature-rise period at 830 DEG C or more
For warm rate control at 15 DEG C/min or more, the thermal shock effect of final quartz glass optical window obtained is not so good as embodiment 1, airtight
Property is relatively poor.
Comparative example 7
This comparative example and embodiment 1 the difference lies in that the temperature of vacuum seal at 820 DEG C hereinafter, being risen in temperature-rise period
Warm rate control is at 6 DEG C/min hereinafter, the thermal shock effect of final quartz glass optical window obtained is not so good as embodiment 1, air-tightness
It is relatively poor.
The present invention is exemplarily described in conjunction with attached drawing above.Obviously, present invention specific implementation is not by above-mentioned side
The limitation of formula.As long as using the improvement for the various unsubstantialities that the inventive concept and technical scheme of the present invention carry out；Or not
It is improved, above-mentioned conception and technical scheme of the invention are directly applied into other occasions, in protection scope of the present invention
Within.
Claims (10)
1. a kind of preparation method of quartz glass optical window, which is characterized in that the preparation method is successively to pass through quartz glass clearly
It washes, dry, after sealing surface metalized, after then assembling the quartz glass after sealing surface metalized with metal parts
Carry out vacuum brazing sealing-in.
2. the preparation method of quartz glass optical window according to claim 1, which is characterized in that the sealing surface metalized
Method be to coat titanium valve paste in quartz glass sealing surface, drying and processing is carried out after coating is good, the temperature of drying is 80~100
DEG C, the titanium valve paste is the mixture of titanium valve and cotton solution, the mass volume ratio of titanium valve and cotton solution be 1g:13~
15ml。
3. the preparation method of quartz glass optical window according to claim 2, which is characterized in that the preparation side of the titanium valve paste
Method is to pour into the titanium valve of formula ratio in ball grinder, and the cotton solution for measuring formula ratio imports in ball grinder, by ball milling tank mouth
It covers, is arranged 250~300 revs/min of drum's speed of rotation, ball milling 1~2 hour.
4. the preparation method of quartz glass optical window according to claim 2, which is characterized in that the quartz glass sealing surface applies
Cover titanium valve paste with a thickness of 20~50 μm.
5. the preparation method of quartz glass optical window according to claim 1, which is characterized in that the method for the cleaning is first will
Quartz glass is successively soaked in gasoline, deoils in acetone, and quartz glass is carried out surface acid-washing later, then washing removal quartz
The acid solution of glass surface.
6. the preparation method of quartz glass optical window according to claim 5, which is characterized in that the method for the pickling is by stone
English glass impregnates 1~2min in hydrofluoric acid.
7. the preparation method of quartz glass optical window according to claim 1, which is characterized in that the drying is by quartz glass
With baking oven drying is put into after dehydration of alcohol, the temperature setting of baking oven is 80~100 DEG C.
8. the preparation method of quartz glass optical window according to claim 1, which is characterized in that the material of the metal parts is adopted
With oxygen-free copper or kovar alloy.
9. the preparation method of quartz glass optical window according to claim 1, which is characterized in that the quartz glass and metal zero
After part assembling, be placed with silver-copper solder at gap to be welded, the process of the vacuum brazing be by quartz glass with
The assembled component of metal parts is put into vacuum drying oven, when vacuum reaches 3 × 10-5It when mmHg or more, starts to warm up, heating rate
Control is at 6~15 DEG C/min, when sealing temperature reaches 820~830 DEG C, keeps the temperature 3~5 minutes.
10. a kind of quartz glass optical window, which is characterized in that including metal parts and quartz glass, the sealing-in of the quartz glass
Face is coated with titanium valve layer of paste, is placed with silver-copper solder at the gap to be welded after quartz glass and metal parts assembling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910575985.3A CN110330238A (en) | 2019-06-28 | 2019-06-28 | A kind of quartz glass optical window and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910575985.3A CN110330238A (en) | 2019-06-28 | 2019-06-28 | A kind of quartz glass optical window and preparation method thereof |
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| Publication Number | Publication Date |
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| CN110330238A true CN110330238A (en) | 2019-10-15 |
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ID=68144571
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| CN201910575985.3A Pending CN110330238A (en) | 2019-06-28 | 2019-06-28 | A kind of quartz glass optical window and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004063793A (en) * | 2002-07-29 | 2004-02-26 | Kyocera Corp | Package for housing infrared ray sensor element and infrared ray sensor device |
| CN203466158U (en) * | 2013-08-13 | 2014-03-05 | 安徽华东光电技术研究所 | Ceramic-to-metal seal structure for boron-nitride energy delivery window of travelling wave tube |
| CN109742221A (en) * | 2018-12-07 | 2019-05-10 | 湖北深紫科技有限公司 | A kind of full-inorganic LED encapsulation method and encapsulating structure |
| CN109926748A (en) * | 2019-03-22 | 2019-06-25 | 中国科学院上海光学精密机械研究所 | A kind of vacuum observation window of brazing metal sealing-in and preparation method thereof |
-
2019
- 2019-06-28 CN CN201910575985.3A patent/CN110330238A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004063793A (en) * | 2002-07-29 | 2004-02-26 | Kyocera Corp | Package for housing infrared ray sensor element and infrared ray sensor device |
| CN203466158U (en) * | 2013-08-13 | 2014-03-05 | 安徽华东光电技术研究所 | Ceramic-to-metal seal structure for boron-nitride energy delivery window of travelling wave tube |
| CN109742221A (en) * | 2018-12-07 | 2019-05-10 | 湖北深紫科技有限公司 | A kind of full-inorganic LED encapsulation method and encapsulating structure |
| CN109926748A (en) * | 2019-03-22 | 2019-06-25 | 中国科学院上海光学精密机械研究所 | A kind of vacuum observation window of brazing metal sealing-in and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张启运 等: "《钎焊手册》", 31 January 1999, 机械工业出版社 * |
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