CN114643462B - Titanium alloy/stainless steel composite board and preparation method thereof - Google Patents
Titanium alloy/stainless steel composite board and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of composite material preparation and application, and discloses a titanium alloy/stainless steel composite plate and a preparation method thereof in order to perform smooth and flat treatment on the surfaces of titanium alloy and stainless steel and ensure that the titanium alloy and the stainless steel are tightly connected so as to meet the industrial production and use requirements of the composite plate. The method comprises the steps of firstly, pretreating the surfaces of titanium alloy and stainless steel by an electric spark ultrasonic composite surface finishing technology, removing impurities on the metal surface, reducing the roughness and generating a small amount of metal peaks; and then forming a titanium alloy and stainless steel connecting interface with good bonding strength by a spark plasma sintering technology. The corrosion resistance, high strength and high wear resistance of the titanium alloy are organically combined with the machinability and economy of the stainless steel, and the composite board with good industrial production applicability is obtained.
Description
Technical Field
The invention belongs to the technical field of composite board preparation and application, and particularly relates to a titanium alloy/stainless steel composite board and a preparation method thereof.
Background
With the rapid development of modern industry, the performance of a single material cannot meet the application of industrial production. The titanium alloy has high specific strength, excellent corrosion resistance and certain high-temperature and low-temperature resistance, and is widely applied to high-end parts such as aviation engine blades, compressor discs and the like, but the high cutting processing price and the poor cutting precision and processing performance of the titanium alloy also severely limit the popularization and application development in other fields. On the other hand, stainless steel has good cutting processability and plasticity and toughness, but the development of stainless steel in high-end fields is restricted due to the defects of low hardness, relatively poor wear resistance and the like. If the titanium alloy and the stainless steel can be combined in high quality through an effective connection technology, the advantages of the titanium alloy and the stainless steel can be complemented, and the overall performance is improved.
At present, the compounding of the titanium alloy and the stainless steel is mainly realized by welding, rolling and other methods at home. However, due to the physicochemical properties, the following problems mainly exist in the preparation process:
1) before connection, impurities and surface unevenness possibly exist on the surfaces of the titanium alloy and the stainless steel after common surface treatment, so that the performance of a subsequent connection joint is influenced;
2) the difference between the heat conductivity coefficient and the linear expansion coefficient of the titanium alloy and the stainless steel is large, so that the temperature field and the stress field are unevenly distributed in the connection process, and large residual stress is formed after welding;
3) there may be TiFe and TiFe at the joint interface 2 The formation of intermetallic compounds, which in turn affect the mechanical properties of the joint;
4) the titanium alloy has great chemical activity and reacts with O, N, H, CO and CO in the atmosphere 2 Water vapor, ammonia, etc. produce chemical reactions that form some impurities that form obstacles in connection with stainless steel.
Disclosure of Invention
In order to solve the problems, realize the connection of the titanium alloy and the stainless steel, ensure that a connection interface realizes good metallurgical bonding and meet the requirements of industrial production, the invention provides a titanium alloy/stainless steel composite plate and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a titanium alloy/stainless steel composite plate comprises the following steps:
step 1, performing electric spark ultrasonic composite finishing treatment on the surface of the titanium alloy;
step 3, cleaning and drying the titanium alloy treated in the step 1 and the stainless steel treated in the step 2;
step 4, loading the cleaned and dried titanium alloy and stainless steel into a graphite die;
step 5, prepressing the loaded mould in the step 4;
step 6, after prepressing, performing spark plasma sintering to obtain a composite board;
and 7, cleaning and polishing the composite board obtained after sintering to obtain the titanium alloy/stainless steel composite board.
Further, the electric spark ultrasonic composite finishing treatment on the surface of the titanium alloy in the step 1 specifically comprises the following steps: fixing the titanium alloy on the conductive platform, and connecting the spark output line with the conductive platform; the front end of the H62 brass bar with the phi 5 angle is used as a tool head to be connected with an amplitude transformer, and the amplitude transformer is connected with an ultrasonic generator; grinding paste with the particle size of W5 and kerosene are mixed to be used as grinding diluent, and the proportion is 12 g/L; the ultrasonic vibration frequency of the electrode is 24kHz, and the total ultrasonic grinding time is 14-16 min.
Further, the electric spark ultrasonic composite finishing treatment on the stainless steel surface in the step 2 specifically comprises: fixing stainless steel on the conductive platform, and connecting the spark output line with the conductive platform; the front end of the H62 brass bar with the phi 5 angle is used as a tool head to be connected with an amplitude transformer, and the amplitude transformer is connected with an ultrasonic generator; grinding paste with the granularity of W7 and kerosene are mixed to be used as grinding diluent, and the proportion is 12 g/L; the ultrasonic vibration frequency of the electrode is 24kHz, and the total ultrasonic grinding time is 14-16 min.
The surface of titanium alloy and stainless steel is pretreated by using an electric spark ultrasonic composite finishing processing technology. In the processing process, on one hand, the ultrasonic cavitation can soften the surface of the workpiece, which is beneficial to accelerating the stripping of metal; on the other hand, new metal peaks continuously appear on the surface of the workpiece, so that the dispersibility of electric spark discharge is increased, favorable conditions are created for electric discharge machining, impurities on the surface are effectively removed, the roughness is reduced, and the flatness of the surface is increased.
Further, the titanium alloy and stainless steel are cleaned in step 3 by ultrasonic vibration, the ultrasonic frequency is 100khz, and the cleaning time is 4-5 min, so as to remove grinding diluent on the surface; and (3) drying the titanium alloy and the stainless steel at the temperature of 90-100 ℃ for 6-9 min after cleaning, so that high-quality combination of the stainless steel and the titanium alloy in the subsequent sintering process is ensured, and the connection strength of the prepared titanium alloy/stainless steel composite board is further ensured.
Further, the step 4 of putting the dried titanium alloy and the dried stainless steel into a graphite mold is carried out in a vacuum glove box, and the roughness of the inner wall of the graphite mold is Ra 0.07-0.14 mu m. The sequence of putting the graphite grinding tool into the graphite grinding tool is as follows: a piece of graphite paper, stainless steel, titanium alloy, a piece of graphite paper.
Further, the pre-pressing loading pressure in the step 5 is 5 MPa, so that the stainless steel and the titanium alloy are in close contact.
Further, the spark plasma sintering in the step 6 is performed by using a spark plasma sintering furnace, and the sintering process is completed under the conditions of vacuum degree of less than 5Pa, pulse current discharge, self-heat generation in the sample and external water circulation cooling. Keeping the highest current treatment temperature at 850 ℃, and the duty ratio of pulse current at 4:5, so that the connection interface is tighter, and the initial loading pressure in the connection process is 10 MPa, thereby aiming at realizing micro-arc discharge at the connection interface to the maximum extent and further removing a compact oxide film on the surface of the plate; the constant loading pressure in the heat preservation stage is 40 MPa, so that the strength of the connecting joint is increased.
And (4) performing vacuum hot-pressing connection on the pretreated titanium alloy and stainless steel by using discharge plasma sintering equipment. Due to the instantaneous action of the discharge plasma, pulse current is preferentially accumulated in an incomplete metal peak after electric spark ultrasonic composite finishing, a typical micro-arc discharge phenomenon can be generated at the peak, and then melting recrystallization is instantaneously generated in an interface discharge area to form a connection joint with reliable quality.
Further, the process of cleaning and polishing the composite board in the step 7 is as follows: and (3) placing the composite board on a smooth glass plane, gradually grinding the periphery of the composite material from 50-1000# by using sand paper, polishing, wiping the composite material by using an alcohol solution with the volume percentage of 50%, and naturally drying to obtain the silvery white titanium alloy/stainless steel composite board.
The invention also provides a titanium alloy/stainless steel composite plate obtained based on any one of the preparation methods.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts the electric spark ultrasonic composite finishing processing technology to process the surfaces of the titanium alloy and the stainless steel, can effectively remove impurities and pollutants on the titanium alloy and the stainless steel, and obtains a flat and clean surface of the titanium alloy and the stainless steel, so that the interface is more tightly attached in the connecting process and no pollutant exists in the middle.
2. According to the invention, the titanium alloy sheet and the stainless steel sheet are connected by the spark plasma sintering technology, the connecting interface is not like a welding joint which can form a liquid deposited metal and a heat affected zone, and only a thin layer of the interface is locally melted and is connected together under the action of pressure. And after the electric spark ultrasonic composite surface finishing treatment, the wettability between the interfaces is good, the tip is quickly melted by the electric spark, and the tip is pressurized and solidified. The final residual stress is lower and the connection joint is more reliable because the phase change of the connection joint is less.
3. When the traditional welding is adopted as the connection mode of the titanium alloy and the stainless steel, because the surface needs to be heated to a high temperature, remelted and recrystallized, the titanium alloy and the stainless steel can react at the interface to generate TiFe and TiFe of brittle phases 2 And the like. However, when the connection is carried out by the spark plasma sintering technology, the whole connection process has high speed, high temperature rise, high cooling speed and low temperature, and the condition of generating compounds by reaction cannot be achieved. The connection interface is cleaner and has no storageThe brittle phase and the precipitated phase affect the bonding properties at the interface.
4. The method of the invention utilizes the spark plasma sintering technology to ensure that the titanium alloy and the stainless steel are in vacuum in the whole connecting process and cannot contact with the atmosphere. The connecting interface has no oxidation and the like, and the formed connecting interface is firmer.
5. The method of the invention creatively combines the electric spark ultrasonic composite finishing treatment and the discharge plasma sintering technology to prepare the titanium alloy/stainless steel laminated composite board with good mechanical property. Before the application, the electric spark ultrasonic composite finishing processing technology is generally used for processing the surface after the preparation of the material is finished, so that the effects of cleaning and reducing the surface roughness are achieved; the spark plasma sintering technique is generally used in powder metallurgy because micro-discharge phenomenon can be directly generated in the powder sintering process, and for the connection of metal sheets, the metal sheets cannot be tightly combined because the discharge phenomenon cannot be generated between the sheets. The invention creatively applies the electric spark ultrasonic composite finishing processing technology to material preparation. Through the electric spark ultrasonic composite finishing processing technology, impurities and oxide films on the surface are removed, metal micro tips with different heights are generated on the metal surface through the interaction of electric sparks and ultrasonic vibration, and the metal micro tips can unexpectedly make good preparation for tightly connecting a titanium alloy sheet and a stainless steel sheet in the subsequent discharge plasma sintering process. Meanwhile, the layered composite board is prepared by the spark plasma sintering technology for the first time, so that the interface reaches the metallurgical-grade combination, and the combination strength is good.
6. The preparation method of the titanium alloy/stainless steel composite board is simple and feasible, and is a feasible way for industrial preparation of the titanium alloy/stainless steel composite board.
Drawings
FIG. 1 is a scanning micrograph of a titanium alloy/stainless steel composite plate according to the present invention.
FIG. 2 is a graphical representation of nanoindentation microhardness of the titanium alloy/stainless steel composite sheet of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be specifically and specifically described below with reference to the embodiments of the present invention and the accompanying drawings.
Example 1
The embodiment is a preparation method of a titanium alloy/stainless steel composite plate, which comprises the following steps:
step 1, performing electric spark ultrasonic composite finishing treatment on the surface of the titanium alloy: fixing the titanium alloy of phi 15 mm multiplied by 1 mm on the conductive platform, and connecting the spark output line with the conductive platform. The front end of the H62 brass bar of phi 5 is used as a tool head at an angle of 45 degrees and is connected with an amplitude transformer, and the amplitude transformer is connected with an ultrasonic generator. Grinding paste with the granularity of W5 and kerosene are mixed to be used as grinding diluent, and the proportion is 12 g/L. The ultrasonic vibration frequency of the electrode is 24kHz, and the total ultrasonic grinding time is 14 min.
Step 3, cleaning the titanium alloy and the stainless steel: and respectively putting the titanium alloy and the stainless steel into an ultrasonic vibration cleaning machine, wherein the ultrasonic frequency is 100khz, and the cleaning time is 4 min. And drying the titanium alloy and the stainless steel after cleaning, wherein the drying temperature is 90 ℃, and the drying time is 6 min.
Step 4, loading of titanium alloy and stainless steel: the titanium alloy and the stainless steel are put into a graphite mold with the inner wall roughness of Ra0.07 mu m and the cavity size of phi 15 mm multiplied by 60 mm. The sequence of putting into graphite grinding apparatus is: one piece of graphite paper with phi 15 mm, stainless steel, titanium alloy and one piece of graphite paper with phi 15 mm.
And 5, loading 5 MPa pressure to pre-press the loaded die.
Step 6, performing spark plasma sintering on the titanium alloy and the stainless steel: and putting the pre-pressed die into a discharge plasma sintering device for discharge plasma sintering to obtain the composite board. Setting sintering conditions as follows: the vacuum degree is less than 5Pa, the highest current processing temperature is kept at 850 ℃, the duty ratio of the pulse current is 4:5, in order to enable the connection interface to be more compact, the small pressure of 10 MPa is loaded in the initial stage of the connection process, and the constant pressure of 40 MPa is loaded in the subsequent heat preservation stage.
And 7, cleaning and polishing the composite board: and (3) placing the composite board on a smooth glass plane, sequentially and progressively grinding the periphery of the composite material by using abrasive paper from 50-1000# and polishing, then wiping the composite material by using an alcohol solution with the volume percentage of 50%, and naturally drying to obtain the final titanium alloy/stainless steel composite board.
Example 2
The embodiment is a preparation method of a titanium alloy/stainless steel composite plate, which comprises the following steps:
step 1, performing electric spark ultrasonic composite finishing treatment on the surface of the titanium alloy: fixing the titanium alloy of phi 30 mm multiplied by 1 mm on the conductive platform, and connecting the spark output line with the conductive platform. The front end of the H62 brass bar of phi 5 is used as a tool head at an angle of 45 degrees and is connected with an amplitude transformer, and the amplitude transformer is connected with an ultrasonic generator. Grinding paste with the granularity of W5 and kerosene are mixed to be used as grinding diluent, and the proportion is 12 g/L. The ultrasonic vibration frequency of the electrode is 24kHz, and the total ultrasonic grinding time is 15 min.
Step 3, cleaning the titanium alloy and the stainless steel: and respectively putting the titanium alloy and the stainless steel into an ultrasonic vibration cleaning machine, wherein the ultrasonic frequency is 100khz, and the cleaning time is 5 min. And drying the cleaned titanium alloy and stainless steel at the drying temperature of 95 ℃ for 7 min.
Step 4, loading of titanium alloy and stainless steel: the titanium alloy and the stainless steel are put into a graphite mold with the roughness of the inner wall of Ra0.12 mu m and the size of the cavity of phi 30 mm multiplied by 60 mm. The sequence of putting the graphite grinding tool into the graphite grinding tool is as follows: one piece of graphite paper with phi 30 mm, stainless steel, titanium alloy and one piece of graphite paper with phi 30 mm.
And 5, loading 5 MPa pressure to pre-press the loaded die.
Step 6, performing spark plasma sintering on the titanium alloy and the stainless steel: and putting the pre-pressed die into a discharge plasma sintering device for discharge plasma sintering to obtain the composite board. The sintering conditions are that the vacuum degree is less than 5Pa, the highest current processing temperature is kept at 850 ℃, the duty ratio of pulse current is 4:5, in order to enable a connecting interface to be more compact, the initial loading pressure in the connecting process is less than 10 MPa, and the subsequent loading pressure in the heat preservation stage is 40 MPa.
And 7, cleaning and polishing the composite board: and (3) placing the composite board on a smooth glass plane, sequentially and progressively grinding the periphery of the composite material by using abrasive paper from 50-1000# and polishing, then wiping the composite material by using an alcohol solution with the volume percentage of 50%, and naturally drying to obtain the final titanium alloy/stainless steel composite board.
Example 3
The embodiment is a preparation method of a titanium alloy/stainless steel composite plate, which comprises the following steps:
step 1, performing electric spark ultrasonic composite finishing treatment on the surface of the titanium alloy: fixing the titanium alloy of phi 20 mm multiplied by 1 mm on the conductive platform, and connecting the spark output line with the conductive platform. The front end of the H62 brass bar of phi 5 is used as a tool head at an angle of 45 degrees and is connected with an amplitude transformer, and the amplitude transformer is connected with an ultrasonic generator. Grinding paste with the granularity of W5 and kerosene are mixed to be used as grinding diluent, and the proportion is 12 g/L. The ultrasonic vibration frequency of the electrode is 24kHz, and the total ultrasonic grinding time is 16 min.
Step 3, cleaning the titanium alloy and the stainless steel: and respectively putting the titanium alloy and the stainless steel into an ultrasonic vibration cleaning machine, wherein the ultrasonic frequency is 100khz, and the cleaning time is 5 min. And drying the titanium alloy and the stainless steel after cleaning, wherein the drying temperature is 100 ℃, and the drying time is 9 min.
Step 4, loading of titanium alloy and stainless steel: the titanium alloy and the stainless steel are put into a graphite mold with the roughness of the inner wall of Ra 0.14 mu m and the size of the cavity of phi 20 mm multiplied by 60 mm. The sequence of putting the graphite grinding tool into the graphite grinding tool is as follows: one piece of graphite paper with phi 20 mm, stainless steel, titanium alloy and one piece of graphite paper with phi 20 mm.
And step 5, loading 5 MPa pressure to pre-press the loaded die.
Step 6, performing spark plasma sintering on the titanium alloy and the stainless steel: and putting the pre-pressed die into a discharge plasma sintering device for discharge plasma sintering to obtain the composite board. The sintering conditions are that the vacuum degree is less than 5Pa, the highest current processing temperature is kept at 850 ℃, the duty ratio of pulse current is 4:5, in order to enable a connecting interface to be more compact, the initial loading pressure in the connecting process is less than 10 MPa, and the subsequent loading pressure in the heat preservation stage is 40 MPa.
And 7, cleaning and polishing the composite board: and (3) placing the composite board on a smooth glass plane, sequentially and progressively grinding the periphery of the composite material by using abrasive paper from 50-1000# and polishing, then wiping the composite material by using an alcohol solution with the volume percentage of 50%, and naturally drying to obtain the final titanium alloy/stainless steel composite board.
The connection interface of the titanium alloy/stainless steel composite plate prepared in example 2 of the present invention was analyzed.
(1) Firstly, SEM microscopic structure observation is carried out on the appearance of the connecting interface.
A distinct interfacial layer can be seen at the interface where the titanium alloy and stainless steel join (see fig. 1), indicating that the titanium alloy and stainless steel have reacted at the interface. Once the reaction occurs at the interface, a stronger joint is formed at the interface. It can also be seen from the SEM scan that the structure of the interface layer is relatively uniform and dense without significant defects and voids.
(2) And testing the micro-nano mechanical property at the interface through the nano indentation.
It can be seen that the hardness at the interface is higher than that of titanium alloy and stainless steel (see fig. 2). This also demonstrates that the connection joints of titanium alloy/stainless steel composite plates prepared by the method of the present invention are very reliable.
Claims (9)
1. A preparation method of a titanium alloy/stainless steel composite board is characterized by comprising the following steps: the method comprises the following steps:
step 1, performing electric spark ultrasonic composite finishing treatment on the surface of the titanium alloy;
step 2, performing electric spark ultrasonic composite finishing treatment on the surface of the stainless steel;
step 3, cleaning and drying the titanium alloy treated in the step 1 and the stainless steel treated in the step 2;
step 4, putting the cleaned and dried titanium alloy and stainless steel into a graphite die;
step 5, prepressing the loaded mould in the step 4;
step 6, after prepressing, performing spark plasma sintering to obtain a composite board;
and 7, cleaning and polishing the composite board obtained after sintering to obtain the titanium alloy/stainless steel composite board.
2. The method for preparing a titanium alloy/stainless steel composite plate according to claim 1, wherein: in the step 1, the surface of the titanium alloy is subjected to electric spark ultrasonic composite finishing treatment, specifically, the titanium alloy is fixed on a conductive platform, and a spark output line is connected with the conductive platform; the front end of the H62 brass bar with the phi 5 angle is used as a tool head to be connected with an amplitude transformer, and the amplitude transformer is connected with an ultrasonic generator; grinding paste with the granularity of W5 and kerosene are mixed to be used as grinding diluent, and the proportion is 12 g/L; the ultrasonic vibration frequency of the electrode is 24kHz, and the total ultrasonic grinding time is 14-16 min.
3. The method for preparing a titanium alloy/stainless steel composite plate according to claim 1, wherein: in the step 2, the electric spark ultrasonic composite finishing treatment is carried out on the surface of the stainless steel, specifically, the stainless steel is fixed on a conductive platform, and a spark output line is connected with the conductive platform; the front end of the H62 brass bar with the phi 5 angle is used as a tool head to be connected with an amplitude transformer, and the amplitude transformer is connected with an ultrasonic generator; grinding paste with the particle size of W7 and kerosene are mixed to be used as grinding diluent, and the proportion is 12 g/L; the ultrasonic vibration frequency of the electrode is 24kHz, and the total time of ultrasonic grinding is 14-16 min.
4. The method for preparing a titanium alloy/stainless steel composite plate according to claim 1, wherein: and 3, cleaning the titanium alloy and the stainless steel by ultrasonic vibration, wherein the ultrasonic frequency is 100khz, the cleaning time is 4-5 min, the temperature for drying the titanium alloy and the stainless steel after cleaning is 90-100 ℃, and the drying time is 6-9 min.
5. The method for preparing a titanium alloy/stainless steel composite plate according to claim 1, wherein: the step 4 of putting the dried titanium alloy and the dried stainless steel into a graphite mold is carried out in a vacuum glove box, and the roughness of the inner wall of the graphite mold is Ra 0.07-0.14 mu m; the sequence of putting the graphite grinding tool into the graphite grinding tool is as follows: a piece of graphite paper, stainless steel, titanium alloy, a piece of graphite paper.
6. The method for preparing a titanium alloy/stainless steel composite plate according to claim 1, wherein: and the pre-pressing loading pressure in the step 5 is 5 MPa.
7. The method for preparing a titanium alloy/stainless steel composite plate according to claim 1, wherein: the spark plasma sintering in the step 6 is performed by using a spark plasma sintering furnace, and the sintering process is completed under the conditions that the vacuum degree is less than 5Pa, pulse current discharge, self-heat generation in the sample and external water circulation cooling are performed; keeping the highest current processing temperature at 850 ℃, the duty ratio of the pulse current at 4:5, and the initial loading pressure in the connection process at 10 MPa; the loading constant pressure in the heat preservation stage is 40 MPa.
8. The method for preparing a titanium alloy/stainless steel composite plate according to claim 1, wherein: the cleaning and polishing process of the composite board in the step 7 is as follows: and (3) placing the composite board on a smooth glass plane, gradually grinding the periphery of the composite material from 50-1000# by using sand paper, polishing, wiping the composite material by using an alcohol solution with the volume percentage of 50%, and naturally drying to obtain the silvery white titanium alloy/stainless steel composite board.
9. A titanium alloy/stainless steel composite plate obtained by the preparation method of any one of claims 1 to 8.
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