CN115733030A - Titanium alloy and glass sealing packaging process and connector - Google Patents
Titanium alloy and glass sealing packaging process and connector Download PDFInfo
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- CN115733030A CN115733030A CN202211370433.7A CN202211370433A CN115733030A CN 115733030 A CN115733030 A CN 115733030A CN 202211370433 A CN202211370433 A CN 202211370433A CN 115733030 A CN115733030 A CN 115733030A
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Abstract
The invention relates to a titanium alloy and glass sealing packaging process and a connector, which mainly comprise the steps of cleaning, workpiece pre-oxidation, workpiece assembly, sintering and post-treatment, wherein the pre-oxidation treatment is carried out by adopting a wet nitrogen method, a guide pin and a titanium alloy shell are pre-oxidized by a wet nitrogen process, the metal guide pin and the titanium alloy shell can carry out oxidation reaction with water under a high-temperature environment, a compact oxide layer is formed on the surface, the adhesion between the oxide layer and glass is also improved, the glass is kept at a standstill temperature during the sintering temperature rise process, the glass is fully contacted with the titanium alloy oxide layer when reaching softening, the temperature is quickly raised to the sintering temperature of the glass after the temperature is raised, the titanium alloy oxide layer can be decomposed at a temperature higher than 700 ℃, more bubbles can be generated when the sintering water resistance exceeds a certain time, the bubbles are discharged through the standstill temperature preservation, the adhesion between the glass and the titanium alloy is improved, the adhesion between the glass and a lead is also improved, and the connector still has stronger pressure resistance under a deep sea high corrosion environment.
Description
Technical Field
The invention belongs to the technical field of connectors, and particularly relates to a titanium alloy and glass sealing packaging process and a connector.
Background
The titanium alloy connector is a plug used in special fields for transmitting information or conducting electricity, and the connector has different use requirements in different fields, for example, the connector is applied to the aviation field and needs to be light, and the connector is applied to a deep water environment and needs to have the characteristics of pressure resistance, water leakage prevention and corrosion resistance, so that the titanium alloy connector and glass sealing process is often applied to a high-pressure and high-corrosion environment in deep sea.
The existing sintering process comprises the following steps: preparing glass powder, cleaning a mould, cleaning, plating a piece, assembling the mould, sintering, cooling and cleaning, wherein the sintering process has the following defects: the titanium alloy has insufficient adhesion with the surface of the glass, poor corrosion resistance and low product yield, is difficult to apply in deep sea environment, and in the sintering process, because the glass is amorphous and has no fixed melting point, tiny bubbles in the contact surface of the glass and the titanium alloy can not be discharged in time during melting, the pressure resistance of the solidified glass is unstable, and the yield is low during testing.
Disclosure of Invention
The invention aims to solve the problems and provide a sealing and packaging process of titanium alloy and glass and a connector.
The invention realizes the purpose through the following technical scheme:
a sealing and packaging process of titanium alloy and glass comprises the following steps:
s1: cleaning: degreasing, cleaning and drying titanium alloy blanks, graphite molds, guide pins and glass blanks required in the sealing process;
s2: pre-oxidation of the workpiece: placing the needle blank in a humidified nitrogen environment, keeping the nitrogen environment at 850-900 ℃ for 15-25 minutes to form a compact oxide layer on the surface of the needle blank to form a needle, placing the titanium alloy blank in a humidified nitrogen and air mixed environment, keeping the nitrogen and air mixed environment at 400-700 ℃ for 15-25 minutes to form a compact oxide layer on the surface of a titanium alloy shell to form a titanium alloy shell;
s3: assembling the workpiece: assembling the titanium alloy shell, the graphite die, the guide pin and the glass blank to form an assembly part;
s4: and (3) sintering: placing the assembly part in a protective gas environment, continuously heating to 590-610 ℃, keeping for 10-15min, then continuously heating to 950-980 ℃, keeping for 25-60min, then cooling to 590-610 ℃, keeping for 10-15min, and finally continuously cooling to form a finished connector;
s5: and (3) post-treatment: and removing graphite residues on the surface of the finished connector, removing redundant oxide layers on the surface of the finished connector, and finally electroplating the finished connector.
As a further optimization scheme of the invention, the protective gas in the step S4 is nitrogen or argon, and protective gas is introduced to prevent the protective gas from reacting with gas in the air during high-temperature sintering.
As a further optimization scheme of the invention, in the step S4, the first temperature rise rate is 18-20 ℃/min, the second temperature rise rate is 12-15 ℃/min, the first temperature reduction rate is 5-8 ℃/min, the second temperature reduction rate is 8-10 ℃/min, the intermittence in the temperature rise process is to discharge bubbles at the contact part of the glass and the titanium alloy, and the intermittence in the temperature reduction process is used for eliminating stress.
As a further optimization scheme of the present invention, in step S1, after the graphite mold is cleaned, whether there are scratches and abrasion on the mold surface is checked, and if there are scratches and abrasion, a new graphite mold is replaced, the graphite mold is used because it has a low thermal expansion coefficient, so as to prevent the graphite mold from breaking up the titanium alloy, and if there are scratches on the graphite mold surface, glass in a molten state may overflow during the sintering process.
As a further optimized scheme of the present invention, in the step S5, the manner of removing the residual graphite is to perform acid washing by using an acid washing solution, wherein the acid washing solution is a mixed solution of hydrofluoric acid with a concentration of 5-20% and a 5-20% nitric acid aqueous solution in a volume ratio of 1: 1, and the acid washing process is as follows: and soaking the finished connector in a pickling solution for 5-30S, and then flushing with plasma water to remove the pickling solution.
As a further optimization of the present invention, the method for removing the scale in step S5 is sand blasting.
As a further optimization scheme of the invention, in the step S2, the optimal temperature for pre-oxidizing the titanium alloy blank is 550 ℃, and the optimal time duration is 20min.
In a further optimized scheme of the present invention, in step S4, the optimal temperature for the first temperature rise is 600 ℃, and is maintained for 12min.
The invention also provides a connector which is manufactured by adopting the process.
The invention has the beneficial effects that:
1) According to the invention, a wet nitrogen method is adopted for preoxidation treatment, the lead needle and the titanium alloy shell are preoxidized through a wet nitrogen process, nitrogen gas is passed through a water furnace, the metal lead needle can generate oxidation reaction with water in a high-temperature environment, a compact oxide layer is formed on the surface, the adhesion between glass and the lead needle is increased, and through the above processes, the adhesion between the glass and the titanium alloy is increased, the adhesion between the glass and the lead wire is increased, and the high-corrosion deep sea environment still has strong water pressure resistance;
2) The invention keeps the temperature during the sintering temperature rise process, so that the softening temperature (lower than 700 ℃) of the glass is fully contacted with the titanium alloy oxide layer, the temperature is quickly raised to the sintering temperature of the glass, the titanium alloy oxide layer can be decomposed at the temperature of more than 700 ℃, more bubbles can be generated after the sintering exceeds a certain time, and the bubbles are discharged by keeping the temperature.
Detailed Description
The present application is described in further detail below, and it should be noted that the following detailed description is provided for illustrative purposes only, and is not intended to limit the scope of the present application, which is defined by the appended claims.
Example 1
The titanium alloy and glass sealing and packaging process in the embodiment comprises the following steps:
s1: cleaning: performing deoiling cleaning and drying on a titanium alloy blank, a graphite die, a guide needle and a glass blank which are required to be used in the sealing process, after the graphite die is cleaned, checking whether scratches and abrasion exist on the surface of the die, and if so, replacing a new graphite die;
s2: pre-oxidation of the workpiece: placing the needle blank in a humidified nitrogen environment, keeping the nitrogen environment at 880 ℃ for 20 minutes to form a compact oxide layer on the surface of the needle blank to form a needle, placing the titanium alloy blank in a humidified nitrogen and air mixed environment, keeping the titanium alloy blank at 550 ℃ for 20 minutes to form a compact oxide layer on the surface of a titanium alloy shell to form a titanium alloy shell;
s3: assembling the workpiece: assembling the titanium alloy shell, the graphite die, the guide pin and the glass blank to form an assembly part;
s4: and (3) sintering: putting the assembly part into a tube furnace, introducing nitrogen or argon, continuously heating to 600 ℃, keeping for 12min, then continuously heating to 960 ℃, keeping for 40min, then cooling to 600 ℃ and keeping for 12min, and finally continuously cooling to form a finished connector, wherein the first heating rate is 19 ℃/min, the second heating rate is 13 ℃/min, the first cooling rate is 6 ℃/min, and the second cooling rate is 9 ℃/min;
s5: and (3) post-treatment: removing graphite residues on the surface of the finished connector by adopting a mixed solution of 12% hydrofluoric acid and 12% nitric acid aqueous solution in a volume ratio of 1: 1, soaking the finished connector in the mixed solution for 20s, then washing by adopting plasma water to remove the mixed solution, carrying out sand blasting treatment on the finished connector to remove an excessive oxide layer on the surface of the finished connector, and finally electroplating the finished connector.
Example 2
The titanium alloy and glass sealing and packaging process in the embodiment comprises the following steps:
s1: cleaning: performing deoiling cleaning and drying on a titanium alloy blank, a graphite die, a guide needle and a glass blank which are required to be used in the sealing process, after the graphite die is cleaned, checking whether scratches and abrasion exist on the surface of the die, and if so, replacing a new graphite die;
s2: pre-oxidation of the workpiece: placing the needle blank in a humidified nitrogen environment, keeping the nitrogen environment at 850 ℃ for 25 minutes to form a compact oxide layer on the surface of the needle blank to form a needle, placing the titanium alloy blank in a humidified nitrogen and air mixed environment, keeping the nitrogen and air mixed environment at 400 ℃ for 25 minutes to form a compact oxide layer on the surface of a titanium alloy shell to form a titanium alloy shell;
s3: assembling a workpiece: assembling the titanium alloy shell, the graphite die, the guide pin and the glass blank to form an assembly part;
s4: and (3) sintering: putting the assembly part into a tube furnace, introducing nitrogen or argon, continuously heating to 590 ℃, keeping for 15min, then continuously heating to 950 ℃, keeping for 60min, then cooling to 590 ℃ and keeping for 15min, and finally continuously cooling to form a finished connector, wherein the first heating rate is 18 ℃/min, the second heating rate is 12 ℃/min, the first cooling rate is 5 ℃/min, and the second cooling rate is 8 ℃/min;
s5: and (3) post-treatment: removing graphite residues on the surface of the finished connector by adopting mixed liquid of hydrofluoric acid with the concentration of 5% and 5% nitric acid aqueous solution in a volume ratio of 1: 1, soaking the finished connector in the mixed liquid for 30s, then flushing the mixed liquid by adopting plasma water to remove the mixed liquid, carrying out sand blasting treatment on the finished connector to remove redundant oxide layers on the surface of the finished connector, and finally electroplating the finished connector.
Example 3
The titanium alloy and glass sealing and packaging process in the embodiment comprises the following steps:
s1: cleaning: performing deoiling cleaning and drying on a titanium alloy blank, a graphite die, a guide needle and a glass blank which are required to be used in the sealing process, after the graphite die is cleaned, checking whether scratches and abrasion exist on the surface of the die, and if so, replacing a new graphite die;
s2: pre-oxidation of the workpiece: placing the needle blank in a humidified nitrogen environment, keeping the nitrogen environment at 900 ℃ for 15 minutes to form a compact oxide layer on the surface of the needle blank to form a needle, placing the titanium alloy blank in a humidified nitrogen and air mixed environment, keeping the titanium alloy blank at 700 ℃ for 15 minutes to form a compact oxide layer on the surface of a titanium alloy shell to form a titanium alloy shell;
s3: assembling the workpiece: assembling the titanium alloy shell, the graphite die, the guide pin and the glass blank to form an assembly part;
s4: and (3) sintering: putting the assembly part into a tube furnace, introducing nitrogen or argon, continuously heating to 610 ℃, keeping for 10min, then continuously heating to 980 ℃, keeping for 25min, then cooling to 610 ℃ and keeping for 10min, and finally continuously cooling to form a finished connector, wherein the first heating rate is 20 ℃/min, the second heating rate is 15 ℃/min, the first cooling rate is 8 ℃/min, and the second cooling rate is 10 ℃/min;
s5: and (3) post-treatment: removing graphite residues on the surface of the finished connector by adopting a mixed solution of hydrofluoric acid with the concentration of 20% and a 20% nitric acid aqueous solution in a volume ratio of 1: 1, soaking the finished connector in the mixed solution for 5s, then washing the mixed solution by adopting plasma water to remove the mixed solution, carrying out sand blasting treatment on the finished connector to remove redundant oxide layers on the surface of the finished connector, and finally electroplating the finished connector.
Comparative example 1
The sealing and packaging process of the titanium alloy and the glass in the comparative example comprises the following steps:
s1: cleaning: performing deoiling cleaning and drying on a titanium alloy blank, a graphite die, a guide needle and a glass blank which are required to be used in the sealing process, after the graphite die is cleaned, checking whether scratches and abrasion exist on the surface of the die, and if so, replacing a new graphite die;
s2: pre-oxidation of the workpiece: placing the needle blank in a humidified nitrogen environment, keeping the nitrogen environment at 880 ℃ for 20 minutes to form a compact oxide layer on the surface of the needle blank to form a needle, placing the titanium alloy blank in a humidified nitrogen and air mixed environment, keeping the titanium alloy blank at 550 ℃ for 20 minutes to form a compact oxide layer on the surface of a titanium alloy shell to form a titanium alloy shell;
s3: assembling a workpiece: assembling the titanium alloy shell, the graphite die, the guide pin and the glass blank to form an assembly part;
s4: and (3) sintering: placing the assembly part into a tube furnace, introducing nitrogen or argon, continuously heating to 960 ℃, keeping for 60min, then cooling to 600 ℃ and keeping for 12min, and finally continuously cooling to form a finished connector, wherein the heating rate is 19 ℃/min, the first cooling rate is 6 ℃/min, and the second cooling rate is 9 ℃/min;
s5: and (3) post-treatment: removing graphite residues on the surface of the finished connector by adopting a mixed solution of hydrofluoric acid with the concentration of 12% and a 12% nitric acid aqueous solution in a volume ratio of 1: 1, soaking the finished connector in the mixed solution for 20s, then washing the mixed solution by adopting plasma water to remove the mixed solution, carrying out sand blasting treatment on the finished connector to remove redundant oxide layers on the surface of the finished connector, and finally electroplating the finished connector.
Comparative example 2
The sealing and packaging process of the titanium alloy and the glass in the comparative example comprises the following steps:
s1: cleaning: performing deoiling cleaning and drying on a titanium alloy blank, a graphite die, a guide needle and a glass blank which are required to be used in the sealing process, after the graphite die is cleaned, checking whether scratches and abrasion exist on the surface of the die, and if so, replacing a new graphite die;
s2: pre-oxidation of the workpiece: placing the needle blank in the air, keeping the temperature at 880 ℃ for 20 minutes to form an oxide layer on the surface of the needle blank to form a needle, placing the titanium alloy blank in the air, keeping the temperature at 550 ℃ for 20 minutes to form an oxide layer on the surface of the titanium alloy shell to form a titanium alloy shell;
s3: assembling the workpiece: assembling the titanium alloy shell, the graphite die, the guide pin and the glass blank to form an assembly part;
s4: and (3) sintering: putting the assembly part into a tube furnace, introducing nitrogen or argon, continuously heating to 600 ℃, keeping for 12min, then continuously heating to 960 ℃, keeping for 40min, then cooling to 600 ℃ and keeping for 12min, and finally continuously cooling to form a finished connector, wherein the first heating rate is 19 ℃/min, the second heating rate is 13 ℃/min, the first cooling rate is 6 ℃/min, and the second cooling rate is 9 ℃/min;
s5: and (3) post-treatment: removing graphite residues on the surface of the finished connector by adopting a mixed solution of hydrofluoric acid with the concentration of 12% and a 12% nitric acid aqueous solution in a volume ratio of 1: 1, soaking the finished connector in the mixed solution for 20s, then washing the mixed solution by adopting plasma water to remove the mixed solution, carrying out sand blasting treatment on the finished connector to remove redundant oxide layers on the surface of the finished connector, and finally electroplating the finished connector.
Comparative example 3
The sealing and packaging process of the titanium alloy and the glass in the comparative example comprises the following steps:
s1: cleaning: degreasing, cleaning and drying titanium alloy blanks, graphite molds, guide pins and glass blanks required in the sealing process, cleaning the graphite molds, then checking whether scratches and abrasion exist on the surfaces of the molds, and if so, replacing new graphite molds;
s2: pre-oxidation of the workpiece: placing the needle blank in air, keeping the temperature at 880 ℃ for 20 minutes to form an oxide layer on the surface of the needle blank to form a needle, placing the titanium alloy blank in air, keeping the temperature at 550 ℃ for 20 minutes to form an oxide layer on the surface of the titanium alloy shell to form a titanium alloy shell;
s3: assembling a workpiece: assembling the titanium alloy shell, the graphite die, the guide pin and the glass blank to form an assembly part;
s4: and (3) sintering: putting the assembly part into a tube furnace, introducing nitrogen or argon, continuously heating to 960 ℃, keeping for 60min, then cooling to 600 ℃, keeping for 12min, and finally continuously cooling to form a finished connector, wherein the heating rate is 19 ℃/min, the first cooling rate is 6 ℃/min, and the second cooling rate is 9 ℃/min;
s5: and (3) post-treatment: removing graphite residues on the surface of the finished connector by adopting a mixed solution of hydrofluoric acid with the concentration of 12% and a 12% nitric acid aqueous solution in a volume ratio of 1: 1, soaking the finished connector in the mixed solution for 20s, then washing the mixed solution by adopting plasma water to remove the mixed solution, carrying out sand blasting treatment on the finished connector to remove redundant oxide layers on the surface of the finished connector, and finally electroplating the finished connector.
In the comparative example 1, the temperature stopping reservation in the sintering temperature rising process is cancelled, and the temperature is directly raised to 960 ℃ at one time; in comparative example 2, the pre-oxidation process of the workpiece employed a heat treatment method common in the prior art; in comparative example 3, the shutdown hold was eliminated and the pre-oxidation process employed a common heat treatment.
The finished connectors in examples 1-3 and comparative examples 1-3 were subjected to qualification rate detection of pressure resistance, insulation and airtightness respectively using a pressure resistance tester (purchased from Qingdao Inuo Intelligent instruments Co., ltd.), an insulation tester (purchased from Shanxi high electric Co., ltd.), and a helium mass spectrometer leak detector (purchased from Beijing Zhongke instruments Co., ltd.), in a detection scene simulating a deep sea high corrosion environment, and the following experimental data were obtained:
from the above table data, the following conclusions can be drawn: 1) The titanium alloy blank is subjected to pre-oxidation treatment by a wet nitrogen method, nitrogen is used as protective gas, the humidified nitrogen carries water vapor, part of oxygen atoms are obtained on the surface of the titanium alloy blank along with water molecules in the environment of 550 ℃, an oxidation reaction is generated, a compact oxide layer is formed, the compact oxide layer has better cohesiveness when being combined with glass, and the qualification rate of the air tightness of a sealing part can be greatly improved; 2) The temperature is stopped and maintained in the sintering and heating process, so that residual bubbles on the contact surface of the glass and the titanium alloy are discharged, the tightness of the bonding surface is improved, and the glass still has stronger water pressure resistance under the deep-sea high-corrosion environment.
The method used in this example is a conventional method known to those skilled in the art unless otherwise specified, and the materials used are commercially available unless otherwise specified.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (9)
1. A sealing and packaging process of titanium alloy and glass is characterized in that: the method comprises the following steps:
s1: cleaning: degreasing, cleaning and drying titanium alloy blanks, graphite molds, guide pins and glass blanks required in the sealing process;
s2: pre-oxidation of the workpiece: placing the needle guiding blank in a humidified nitrogen environment, keeping the nitrogen environment at 850-900 ℃ for 15-25 minutes to form a compact oxide layer on the surface of the needle guiding blank to form a needle guiding, placing the titanium alloy blank in a humidified nitrogen and air mixed environment, keeping the nitrogen and air mixed environment at 400-700 ℃ for 15-25 minutes to form a compact oxide layer on the surface of a titanium alloy shell to form a titanium alloy shell;
s3: assembling the workpiece: assembling the titanium alloy shell, the graphite die, the guide pin and the glass blank to form an assembly part;
s4: and (3) sintering: placing the assembly in a protective gas environment, continuously heating to 590-610 ℃, keeping for 10-15min, then continuously heating to 950-980 ℃, keeping for 25-60min, then cooling to 590-610 ℃, keeping for 10-15min, and finally continuously cooling to form a finished connector;
s5: and (3) post-treatment: and removing graphite residues on the surface of the finished connector, removing redundant oxide layers on the surface of the finished connector, and finally electroplating the finished connector.
2. The process of claim 1, wherein the sealing and packaging process comprises: and the protective gas in the step S4 is nitrogen or argon.
3. The process of claim 1, wherein the sealing and packaging process comprises: in the step S4, the first temperature rise rate is 18-20 ℃/min, the second temperature rise rate is 12-15 ℃/min, the first temperature reduction rate is 5-8 ℃/min, and the second temperature reduction rate is 8-10 ℃/min.
4. A titanium alloy and glass sealing and packaging process according to claim 1, wherein: in the step S1, the graphite mold is cleaned and then inspected for scratches and abrasion on the mold surface, and if so, a new graphite mold is replaced.
5. The process of claim 1, wherein the sealing and packaging process comprises: in the step S5, the residual graphite is removed by adopting a pickling solution for pickling, wherein the pickling solution is a mixed solution of hydrofluoric acid with the concentration of 5-20% and nitric acid aqueous solution with the volume ratio of 5-20% of 1: 1, and the pickling process is as follows: and soaking the finished connector in a pickling solution for 5-30S, and then flushing with plasma water to remove the pickling solution.
6. The process of claim 1, wherein the sealing and packaging process comprises: the method for removing the oxide skin in the step S5 is sand blasting.
7. The process of claim 1, wherein the sealing and packaging process comprises: in the step S2, the optimal temperature for pre-oxidizing the titanium alloy blank is 550 ℃, and the optimal time duration is 20min.
8. The process of claim 1, wherein the sealing and packaging process comprises: in the step S4, the optimal temperature for the first temperature rise is 600 ℃, and the temperature is kept for 12min.
9. A connector made by the process of any one of claims 1-8.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211370433.7A CN115733030A (en) | 2022-11-03 | 2022-11-03 | Titanium alloy and glass sealing packaging process and connector |
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| CN202211370433.7A CN115733030A (en) | 2022-11-03 | 2022-11-03 | Titanium alloy and glass sealing packaging process and connector |
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| CN115733030A true CN115733030A (en) | 2023-03-03 |
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| CN202211370433.7A Pending CN115733030A (en) | 2022-11-03 | 2022-11-03 | Titanium alloy and glass sealing packaging process and connector |
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