CN106757275A - Low temperature glass process for sealing after a kind of titanium alloy electrochemical oxidation - Google Patents
Low temperature glass process for sealing after a kind of titanium alloy electrochemical oxidation Download PDFInfo
- Publication number
- CN106757275A CN106757275A CN201611112549.5A CN201611112549A CN106757275A CN 106757275 A CN106757275 A CN 106757275A CN 201611112549 A CN201611112549 A CN 201611112549A CN 106757275 A CN106757275 A CN 106757275A
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- Prior art keywords
- titanium alloy
- sealing
- film
- low temperature
- oxide
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Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
-
- 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
- C03C29/00—Joining metals with the aid 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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
Abstract
The invention discloses low temperature glass process for sealing after a kind of titanium alloy electrochemical oxidation, comprise the following steps:(1)Conventional ungrease treatment is carried out to titanium alloy;(2)From softening temperature be 430 ~ 460 DEG C, sealing temperature be 520 ~ 540 DEG C, thermal coefficient of expansion 8.5 ~ 10.0 × 10‑6/(25~300℃), resistivity be more than 1014The low temperature sealing glass of Ω cm, is prepared into gob according to a conventional method;(3)Using concentration it is the sulfuric acid solution of 150 ~ 200g/L as electrolyte under the conditions of 20 DEG C, the titanium alloy after degreasing carries out electrolytic oxidation as anode, stereotype or graphite cake as negative electrode;(4)Oxidation inner wire workpiece;(5)Glass sealing.The present invention is sintered using glass sealing temperature range is reduced under air atmosphere, and its process for sealing is simple, low cost, and technical process is easy to control.
Description
Technical field
The invention belongs to titanium alloy and glass sealing technical field, and in particular to low temperature glass after a kind of titanium alloy electrochemical oxidation
Glass process for sealing.
Background technology
Space and the electric connector for using under water are usually required that with performances such as hermetic seal, water-stops.Titanium has resistance to sea
Aqueous corrosion performance, it is higher than strong, it is a kind of preferable ship structure material, both at home and abroad to titanium in naval vessel the features such as without magnetic
Using having carried out numerous studies.Particularly the end of the sixties, real ship operational phase is reached, such as former Soviet Union's titanium builds aggressive core
Submarine, is that a typical case applies example, and the titanium alloy of many trades mark such as JIT-IM, JIT-TM, 37,5B and 23A is developed for this, I
The titanium alloy of state's ships mainly has TA2, TA3, TA5 and TA4.In addition, domestic and international many artificial satellites, especially some high scores
Resolution, such as high performance satellite of fine definition, reconnaissance satellite, landsat etc. all use titanium alloy casting.For aviation, space flight
For industry, preferable high-temperature material should have specific strength and specific stiffness high high.Titanium is specific strength highest metal, therefore
It is widely used.
The thermal coefficient of expansion of titanium is (9.41~10.03) × 10-6/℃;Conventional titanium alloy sealing be at 1100 DEG C or so,
Under argon gas protective condition, diffuseed to form with carrying out interface under graphite jig positioning support, with vitreum high temperature.Kovar alloy,
Need to form artificial oxide-film before the materials such as stainless steel and vitreum sealing-in, but titanium alloy is with glass sealing in contrast to this,
There was only several nanometers of natural oxide films before titanium alloy high-temperature glass sealing, sealing-in is relied primarily on during titanium atom under high temperature captures vitreum
Oxygen forms compound interface.Titanium alloy high temperature sintering under argon gas protection, has that energy consumption is big, argon gas consuming cost is high, mould stone
There is chemical reaction and form titanium carbide and be bonded together in ink, destruction mould during pickup and titanium alloy table with titanium alloy contact position
The deficiencies such as face adhesion graphite powder.
Titanium can form the oxide-film for being closely adhered to its surface when less than 800 DEG C in the short time, and then can at high temperature
Form oxide-film that is porous, lacking adhesion;Oxygen is particularly easy to dissolve in titanium under the high temperature conditions as solute, and lacks
The O of amount2Dissolve in the performance that Ti is just may obviously vary in Ti.At 1000 DEG C or so, in extremely low oxygen amount, (pressure of oxygen is titanium
10-30~10-42Individual atmospheric pressure) in the presence of the oxide thickness that is formed reach 1000nm, but easily stripped off from metal surface, even if low
Loose oxidizing process can not be eliminated when 800 DEG C;Even if so being sintered using vacuum drying oven, being prevented under so low partial pressure of oxygen
Over oxidation, be also practically impossible to it is unpractical, this is also the reason for must being protected using argon gas under high temperature.
The combination of titanium oxide and its underlying metal is clearly dependent on the chemical bond formed between oxide and metal;Titanium exists
Loose TiO is formed during high temperature2Film, oxygen and titanium ion can be continued to aoxidize, be caused by this membrane diffusion, the metal surface under oxide-film
Thicken oxide-film.Cation is metal inside lattice defect is occurred to the result of external diffusion by oxide-film, if not preventing
The formation of these lattice defects, oxide-film will then be stripped off.Therefore, the growth of stress is the knot of this process in oxide
Really, and cation by oxide-film to external diffusion along with the formation of metal inside lattice defect, cause oxide layer deterioration
True cause.So, it is most important to form an oxide-film for determination and stablize during sealing-in to the sealing-in of titanium alloy
's.
The content of the invention
For above-mentioned deficiency of the prior art, sealed the invention provides low temperature glass after a kind of titanium alloy electrochemical oxidation
Technique is connect, can effectively solve that sealing temperature in the prior art is high, the oxidation binding force of membrane that titanium alloy is formed before sealing-in is not enough, easily de-
The problems such as falling.
To achieve the above object, the technical solution adopted for the present invention to solve the technical problems is:
Low temperature glass process for sealing, comprises the following steps after a kind of titanium alloy electrochemical oxidation:
(1) conventional ungrease treatment is carried out to titanium alloy;
(2) it is 520~540 DEG C, thermal coefficient of expansion 8.5~10.0 for 430~460 DEG C, sealing temperature to select softening temperature
×10-6/ (25~300 DEG C), resistivity are more than 1014The low temperature sealing glass of Ω cm, is prepared into glass according to a conventional method
Base;
(3) under the conditions of 20 DEG C, using sulfuric acid solution that concentration is 150~200g/L as electrolyte, the titanium after degreasing is closed
Used as anode, stereotype or graphite cake under the DC voltage of 18~30V, are electrolysed 25~35min to gold as negative electrode, make titanium alloy
Surface forms one layer of uniform oxide-film;
(4) will 4J50 materials inner wire workpiece routine degreasing after be placed in 650~700 DEG C under the conditions of air oxidation 10~
20min, makes inner wire workpiece surface form one layer of uniform oxide-film;
(5) it is titanium alloy shell by the titanium alloy for forming oxide-film, forms inner wire workpiece and the gob peace of oxide-film
Loaded in graphite jig, sealed graphite box is subsequently placed in 640~660 DEG C of Muffle furnace, is incubated 60~80min, closes power supply
Open after burner hearth is cooled to room temperature and take out closing graphite.
Further, sulfuric acid solution concentration is 180g/L in step (3).
Further, electrolytic condition is under the DC voltage of 24V, to be electrolysed 30min in step (3).
Further, air oxidizing temperature is 680~690 DEG C in step (4), and oxidization time is 10min.
Further, in step (5) by formed oxide-film titanium alloy be titanium alloy shell, formed oxide-film inner wire
Workpiece and gob are installed in graphite jig, sealed graphite box, are subsequently placed in 650~660 DEG C of Muffle furnace, insulation
60min。
Low temperature glass process for sealing after the titanium alloy electrochemical oxidation that the present invention is provided, has the advantages that:
(1) oxide-film of densification is formed before titanium alloy and glass sealing by electrochemical method, replaces traditional high-temperature atmosphere
Middle oxidation, with superior process consistency and repeatability, finer and close compared to high temperature oxide film, oxide-film is combined with Titanium base
Intensity is higher.
(2) present invention is sintered using glass sealing temperature range is reduced under air atmosphere, the letter of its process for sealing
It is single, low cost, and technical process is easy to control.
(3) this process for sealing is used, when seal interface highly reaches 1.2mm, the airtight gas leakage of titanium alloy sealing-in product
Rate≤1 × 10-9Pa·m3/ s, titanium alloy shell and inner wire are higher than glass shear strength in itself with glass sealing intensity.
Specific embodiment
Embodiment 1
Low temperature glass process for sealing, comprises the following steps after a kind of titanium alloy electrochemical oxidation:
(1) after TC4 titanium alloy workpieces machining, spray glass ball or chemical polishing to remove burr etc., Ran Houjin
Row routine ungrease treatment;
(2) it is 520 DEG C, thermal coefficient of expansion 8.96 × 10 for 430 DEG C, sealing temperature to select softening temperature-6/ (25~300
DEG C), resistivity be more than 1014The low temperature sealing glass of Ω cm, is prepared into gob according to a conventional method;
(3) under the conditions of 20 DEG C, sulfuric acid solution using concentration as 180g/L is used as electrolyte, the titanium alloy conduct after degreasing
Anode, stereotype under the DC voltage of 24V, is electrolysed 30min as negative electrode, titanium alloy surface is formed one layer of uniform blueness
Oxide-film;
(4) inner wire is processed with half-hard state 4J50, air oxygen under the conditions of 680 DEG C will be placed in after the routine degreasing of inner wire workpiece
Change 10min, inner wire workpiece surface forms one layer of uniform Slate grey oxide-film;
(5) glass sealing:By formed oxide-film titanium alloy be titanium alloy shell, formed oxide-film inner wire workpiece and
Gob is installed in graphite jig, places into graphite, sealing, and (graphite conducts heat to form one to be finally placed in 650 DEG C of Muffle furnaces
Determine thermograde, sealing temperature of the furnace temperature higher than glass) in close power supply after insulation 60min, after Muffle furnace is cooled to room temperature
Closing graphite is taken out, the titanium alloy shell after sealing-in is changed into yellowish slightly general coloured appearance, 4J50 inner wires are still grey black.
Connector inner wire needs plating cupro-nickel gold, electroplates preceding technical hydrochloric acid and adds corrosion inhibiter, and immersion is removed to be led in 4J50
The oxide-film in body surface face, soak time about 5~10min, inner wire is presented metallic luster completely;Activation electricity is carried out after to be cleaned
Plating, can be by titanium alloy shell jointed anode during plating, and used as a part for anode, and inner wire is processed as negative electrode, plating
Process uses copper facing, nickel plating and gold-plated electroplating solution.
After plating completion, glass ball (air pressure 3atm) is sprayed to titanium alloy shell, removal titanium alloy surface is uneven
Oxide-film, obtains the titanium alloy true qualities of matt, and shot-peening process is that inner conductors and glass do suitably protecting.Products obtained therefrom air-tightness
Well, inner wire hardness is not substantially reduced with respect to original state, and product electric property is qualified.
4J50 inner wires and titanium alloy shell are pre-oxidized respectively under conditions of being each adapted to and then in atmosphere
650 DEG C of low temperature glass sealing-in is carried out, the oxidation of metal will not be serious, and slightly processing just can be electroplated, so both ensured envelope
Intensity is connect, the oxidized surface of 4J50 is reduced to metal true qualities again, it is more convenient to carry out electroplating processes.
Embodiment 2
Low temperature glass process for sealing, comprises the following steps after a kind of titanium alloy electrochemical oxidation:
(1) after TC4 titanium alloy workpieces machining, spray glass ball or chemical polishing to remove burr etc., Ran Houjin
Row routine ungrease treatment;
(2) it is 540 DEG C, thermal coefficient of expansion 8.96 × 10 for 460 DEG C, sealing temperature to select softening temperature-6/ (25~300
DEG C), resistivity be more than 1014The low temperature sealing glass of Ω cm, is prepared into gob according to a conventional method;
(3) under the conditions of 20 DEG C, sulfuric acid solution using concentration as 180g/L is used as electrolyte, the titanium alloy conduct after degreasing
Anode, stereotype under the DC voltage of 24V, is electrolysed 30min as negative electrode, titanium alloy surface is formed one layer of uniform blueness
Oxide-film;
(4) inner wire is processed with semihard 4J50, is aoxidized under the conditions of 680 DEG C will be placed in after the routine degreasing of inner wire workpiece
10min, inner wire workpiece surface forms one layer of uniform Slate grey oxide-film;
(5) glass sealing:By formed oxide-film titanium alloy be titanium alloy shell, formed oxide-film inner wire workpiece and
Gob is installed in graphite jig, places into graphite, sealing, is then placed in being sintered in nitrogen (hydrogenation) continuous tunnel furnace, tunnel
Stove is divided into preheating, sintering, slow cooling workshop section, and preheating time is 20min, makes its temperature close to sintering temperature, sintering temperature
It is set as 650 DEG C, then sinters Temperature fall after 60min, taken out after being down to room temperature, the titanium alloy shell after sealing-in is changed into yellowish
Slightly general coloured appearance, 4J50 inner wires are reduced to metal true qualities.
Connector inner wire needs plating cupro-nickel gold, electroplates preceding technical hydrochloric acid and adds corrosion inhibiter, and immersion is removed to be led in 4J50
The slight subsidiary oxide-film in body surface face, soak time about 120s, inner wire is presented metallic luster completely;Lived after to be cleaned
Change plating, can be by titanium alloy shell jointed anode during plating, used as a part for anode, and inner wire is processed as negative electrode,
Electroplating process uses copper facing, nickel plating, gold-plated solution.
After plating completion, glass ball (air pressure 3atm) is sprayed to titanium alloy shell, removal titanium alloy surface is uneven
Oxide-film, obtains the titanium alloy true qualities of matt, and shot-peening process is that inner conductors and glass do suitably protecting.Products obtained therefrom air-tightness
Well, inner wire hardness is not substantially reduced with respect to original state, and product electric property is qualified.
Embodiment 3
Low temperature glass process for sealing, comprises the following steps after a kind of titanium alloy electrochemical oxidation:
(1) after TA2 titanium alloy workpieces machining, spray glass ball or chemical polishing to remove burr etc., Ran Houjin
Row routine ungrease treatment;
(2) it is 530 DEG C, thermal coefficient of expansion 8.96 × 10 for 450 DEG C, sealing temperature to select softening temperature-6/ (25~300
DEG C), resistivity be more than 1014The low temperature sealing glass of Ω cm, is prepared into gob according to a conventional method;
(3) under the conditions of 20 DEG C, sulfuric acid solution using concentration as 170g/L is used as electrolyte, the titanium alloy conduct after degreasing
Anode, stereotype under the DC voltage of 23V, is electrolysed 30min as negative electrode, titanium alloy surface is formed one layer of uniform blueness
Oxide-film;
(4) inner wire is processed with semihard 4J50, is aoxidized under the conditions of 680 DEG C will be placed in after the routine degreasing of inner wire workpiece
10min, inner wire workpiece surface forms one layer of uniform Slate grey oxide-film;
(5) glass sealing:By formed oxide-film titanium alloy be titanium alloy shell, formed oxide-film inner wire workpiece and
Gob is installed in graphite jig, places into graphite, sealing, is then placed in being sintered in nitrogen (hydrogenation) continuous tunnel furnace, tunnel
Stove is divided into preheating, sintering, slow cooling workshop section, and preheating time is 20min, makes its temperature close to sintering temperature, sintering temperature
It is set as 650 DEG C, then sinters Temperature fall after 60min, taken out after being down to room temperature, the titanium alloy shell after sealing-in is changed into yellowish
Slightly general coloured appearance, 4J50 inner wires are reduced to metal true qualities.
Connector inner wire needs plating cupro-nickel gold, electroplates preceding technical hydrochloric acid and adds corrosion inhibiter, and immersion is removed to be led in 4J50
The slight subsidiary oxide-film in body surface face, soak time about 120s, inner wire is presented metallic luster completely;Lived after to be cleaned
Change plating, can be by titanium alloy shell jointed anode during plating, used as a part for anode, and inner wire is processed as negative electrode,
Sulfuric acid solution is used as electrolyte.
After plating completion, low-intensity spray sandblasting is carried out to titanium alloy shell, sandblasting particle diameter is 600 mesh, is closed for removing titanium
The uneven oxide-film of gold surface, obtains the titanium alloy true qualities of matt, and sandblasting procedures are that inner conductors and glass do suitably protecting.
Products obtained therefrom air-tightness is good, and inner wire hardness is not substantially reduced with respect to original state, and product electric property is qualified.
Embodiment 4
The difference from Example 1 of embodiment 4 is:The concentration of sulfuric acid solution is 150g/L in step (3), and electrolytic condition is
Under the DC voltage of 18V, 25min is electrolysed.
Embodiment 5
The difference from Example 1 of embodiment 5 is:The concentration of sulfuric acid solution is 200g/L in step (3), and electrolytic condition is
Under the DC voltage of 30V, 35min is electrolysed.
Embodiment 6
The difference from Example 1 of embodiment 6 is:Sintering temperature is 640 DEG C in step (5), sinters 80min.
Embodiment 7
The difference from Example 1 of embodiment 7 is:Sintering temperature is 660 DEG C in step (5), sinters 60min.
Embodiment 1-3, when the process for sealing seal interface provided using the present invention highly reaches 1.2mm, titanium alloy sealing-in
Airtight released gas rate≤1 × 10 of product-9Pa·m3/ s, the breakdown pressure that can be born is the shear strength of glass;Titanium alloy shell
Body and inner wire and glass sealing intensity are higher than glass shear strength in itself, and the products obtained therefrom performance of embodiment 1 is optimal.
Embodiment 4-7 products obtained therefroms, its airtight released gas rate is higher than embodiment 1-3, although embodiment 4-7 products obtained therefroms
It is more slightly worse than embodiment 1-3 products obtained therefrom performances, but compared with prior art, its sealing temperature is low, the oxide-film that titanium alloy is formed
Good bonding strength, difficult for drop-off, low cost, easily-controlled operation.
The airtight released gas rate of embodiment 1-7 products obtained therefroms is shown in Table 1:
In sum, it is more excellent using properties of product obtained in the process for sealing for providing of the invention.
Claims (5)
1. low temperature glass process for sealing after a kind of titanium alloy electrochemical oxidation, it is characterised in that comprise the following steps:
(1)Conventional ungrease treatment is carried out to titanium alloy;
(2)From softening temperature be 430 ~ 460 DEG C, sealing temperature be 520 ~ 540 DEG C, thermal coefficient of expansion 8.5 ~ 10.0 × 10-6/
(25~300℃), resistivity be more than 1014The low temperature sealing glass of Ω cm, is prepared into gob according to a conventional method;
(3)Using concentration it is the sulfuric acid solution of 150 ~ 200g/L as electrolyte, the titanium alloy conduct after degreasing under the conditions of 20 DEG C
Anode, stereotype or graphite cake under the DC voltage of 18 ~ 30V, are electrolysed 25 ~ 35min as negative electrode, form titanium alloy surface
One layer of uniform oxide-film;
(4)10 ~ 20min of air oxidation under the conditions of 650 ~ 700 DEG C will be placed in after the inner wire workpiece routine degreasing of 4J50 materials, makes
Inner wire workpiece surface forms one layer of uniform oxide-film;
(5)It is that titanium alloy shell, the inner wire workpiece of formation oxide-film and gob are installed on by the titanium alloy for forming oxide-film
In graphite jig, sealed graphite box is subsequently placed in 640 ~ 660 DEG C of Muffle furnace, is incubated 60 ~ 80min, is incited somebody to action after being cooled to room temperature
Closing graphite takes out.
2. low temperature glass process for sealing after titanium alloy electrochemical oxidation according to claim 1, it is characterised in that step
(3)Middle sulfuric acid solution concentration is 180g/L.
3. low temperature glass process for sealing after titanium alloy electrochemical oxidation according to claim 1, it is characterised in that step
(3)Middle electrolytic condition is under the DC voltage of 24V, to be electrolysed 30min.
4. low temperature glass process for sealing after titanium alloy electrochemical oxidation according to claim 1, it is characterised in that step
(4)Middle air oxidizing temperature is 680 ~ 690 DEG C, and oxidization time is 10min.
5. low temperature glass process for sealing after titanium alloy electrochemical oxidation according to claim 1, it is characterised in that step
(5)Middle is that titanium alloy shell, the inner wire workpiece of formation oxide-film and gob are installed on stone by the titanium alloy for forming oxide-film
In black mould, sealed graphite box is subsequently placed in 650 ~ 660 DEG C of Muffle furnace, is incubated 60min.
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Cited By (4)
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CN110615624A (en) * | 2019-08-22 | 2019-12-27 | 遵义玉波电子玻璃有限公司 | Titanium alloy glass sintering process |
CN110911940A (en) * | 2018-09-17 | 2020-03-24 | 北京首量科技股份有限公司 | Preparation method of glass sealing socket |
CN110911939A (en) * | 2018-09-17 | 2020-03-24 | 北京首量科技股份有限公司 | Preparation method of glass sealing socket |
CN111018352A (en) * | 2019-12-06 | 2020-04-17 | 西安赛尔电子材料科技有限公司 | Glass material for titanium and titanium alloy-kovar sealing and preparation method and application thereof |
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CN110911940A (en) * | 2018-09-17 | 2020-03-24 | 北京首量科技股份有限公司 | Preparation method of glass sealing socket |
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CN110911939B (en) * | 2018-09-17 | 2021-07-16 | 北京首量科技股份有限公司 | Preparation method of glass sealing socket |
CN110615624A (en) * | 2019-08-22 | 2019-12-27 | 遵义玉波电子玻璃有限公司 | Titanium alloy glass sintering process |
CN111018352A (en) * | 2019-12-06 | 2020-04-17 | 西安赛尔电子材料科技有限公司 | Glass material for titanium and titanium alloy-kovar sealing and preparation method and application thereof |
CN111018352B (en) * | 2019-12-06 | 2022-05-20 | 西安赛尔电子材料科技有限公司 | Glass material for titanium and titanium alloy-kovar sealing and preparation method and application thereof |
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