CN111549313B - Preparation method of high-temperature induced wear-resistant diffusion layer on surface of titanium-zirconium-based alloy - Google Patents
Preparation method of high-temperature induced wear-resistant diffusion layer on surface of titanium-zirconium-based alloy Download PDFInfo
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- CN111549313B CN111549313B CN202010591261.0A CN202010591261A CN111549313B CN 111549313 B CN111549313 B CN 111549313B CN 202010591261 A CN202010591261 A CN 202010591261A CN 111549313 B CN111549313 B CN 111549313B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/12—Oxidising using elemental oxygen or ozone
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
Abstract
The invention belongs to the technical field of preparation of surface protection layers of alloy materials, and particularly relates to a preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy; the oxidation furnace adopted by the preparation method comprises a shell, a motor, a first rotating shaft, a supporting plate and an oxygen injection unit; the first rotating shaft is rotatably connected to the inner side wall of the bottom end of the shell and is fixedly connected with the output end of the motor; the supporting plate is arranged on the side wall of the top end of the first rotating shaft; the oxygen injection unit is arranged on the inner side wall of the shell and comprises a first cam, an air bag, an air storage chamber and a fixing plate; the rotation in-process of a pivot drives the backup pad and rotates simultaneously to area of contact between continuous change square sample and the oxygen realizes that oxygen has guaranteed the thickness homogeneity of square sample surface vacuum diffusion layer at the evenly distributed on square sample surface, thereby has effectively increased the stand wear and tear degree on square sample surface.
Description
Technical Field
The invention belongs to the technical field of preparation of surface protection layers of alloy materials, and particularly relates to a preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy.
Background
The titanium alloy has the excellent characteristics of low density, high strength, good corrosion resistance and the like, and is an important structural material of an aerospace aircraft. The tensile strength of the Ti6Al4V titanium alloy which is widely used at present is 900-1100 MPa, and the elongation at failure is 8-12%. The TiZrAlV alloy is a novel alloy material developed on the basis of Ti6Al4V alloy, and the introduction of zirconium element effectively improves the strength and hardness of the material, so that the TiZrAlV alloy becomes a candidate material of a very potential aerospace craft.
Some technical solutions related to zircaloy also appear in the prior art, for example, a chinese patent with application number 2013105415321 discloses a method for preparing a zircaloy, wherein the zircaloy comprises the following components by mass percent: ti 41-62, Zr 30-51, Al5 and V3, putting various raw materials into a non-consumable electric arc furnace, and smelting to obtain an alloy ingot; coating a high-temperature antioxidant on the surface of the plate-shaped alloy, heating and preserving heat in a furnace, cogging and forging to obtain a plate-shaped alloy, removing the antioxidant on the surface of the plate-shaped alloy, placing the plate-shaped alloy in a heat treatment furnace, heating to 850-870 ℃, preserving heat for 1h, and quenching and cooling with water; cutting the alloy plate into sheets of 3-4 mm, and performing rolling deformation at room temperature, wherein the rolling strain rate is 2.2-3.1 s < -1 >, and the total deformation is more than 80%; then annealing treatment is carried out, and the vacuum degree is 10-4～10-5Pa, the temperature is 740-760 ℃, the temperature is kept for 1h, and then the air cooling is carried out to the room temperature. The titanium-zirconium-based alloy with the microstructure of the special two-state structure is obtained, and the strength of the alloy is effectively improved while the plasticity of the alloy is maintained; however, as the application range of the titanium-zirconium-based alloy is more and more extensive, the application environment of the titanium-zirconium-based alloy becomes worse, and particularly in the application occasions with larger abrasion degree, the application effect and the service life of the titanium-zirconium-based alloy are seriously influenced, so that the improvement of the abrasion resistance of the surface of the titanium-zirconium-based alloy is necessary.
Disclosure of Invention
The invention provides a preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy, aiming at improving the wear resistance of the titanium-zirconium-based alloy and prolonging the service life of the titanium-zirconium-based alloy in a use occasion with larger wear degree.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy, which comprises the following steps:
s1: pressing high-purity metals of titanium, zirconium and aluminum with the purity of 99.5 percent and 50Al50V of intermediate alloy into short rod-shaped lump materials to obtain basic raw materials, manufacturing the basic raw materials into electrodes, and then carrying out smelting treatment through a vacuum consumable electrode arc furnace to obtain alloy ingots, wherein the smelting current is 180-260A, and the smelting time is 4-6 min;
s2: carrying out three-pier three-pull turning on the alloy ingot in the S1 to obtain a titanium-zirconium-based alloy bar, cutting a square sample with the shape of 10mm multiplied by 30mm from the bar by using a wire electric discharge machine, and then polishing the titanium-zirconium-based alloy square sample by using SiC abrasive paper to ensure that the surface roughness of the titanium-zirconium-based alloy square sample is 0.1-0.2 mu m;
s3: cleaning the titanium-zirconium-based alloy square sample in the step S2 in an ultrasonic cleaning machine to remove impurity particles on the surface of the titanium-zirconium-based alloy square sample, and drying the surface of the titanium-zirconium-based alloy square sample by using a hot air blower; wherein the heating temperature of the air heater is controlled to be 75-80 ℃, and an included angle of 45 degrees is formed between an air outlet of the air heater and the surface of the titanium-zirconium-based alloy square sample;
s4: carrying out thermal oxidation treatment on the titanium-zirconium-based alloy square sample in the S3 through a muffle furnace, wherein the heating temperature is 650-800 ℃, and the heat preservation time is 12 h; and after the heat preservation is finished, cooling the titanium-zirconium-based alloy square sample along with the furnace, after the titanium-zirconium-based alloy square sample is cooled to room temperature, putting the titanium-zirconium-based alloy square sample into an oxidation furnace for vacuum diffusion treatment, forming an oxygen diffusion layer on the surface of the titanium-zirconium-based alloy square sample, and finishing the preparation of the high-temperature induced titanium-zirconium-based alloy surface wear-resistant diffusion layer.
Preferably, when the base raw material is smelted in a vacuum consumable electrode arc furnace, the smelting current is increased in stages, namely the smelting current is firstly 190A, and smelting is continued for 2 min; then the smelting current is increased to 230A, and smelting is continued for 2 min; and finally, increasing the smelting current to 260A, and finishing the smelting treatment of the basic raw materials after continuously smelting for 2 min.
Preferably, in the vacuum diffusion process of the titanium-zirconium-based alloy square sample, the vacuum diffusion time is 8-10h, and the heating temperature is 400-550 ℃.
Preferably, when the titanium-zirconium-based alloy square sample is cleaned by an ultrasonic cleaning machine, three times of cleaning by different cleaning liquids are required; the method comprises the following steps of firstly cleaning the titanium-zirconium-based alloy square sample by using an acetone solution, cleaning the titanium-zirconium-based alloy square sample by using an alcohol solution after the cleaning is finished, and finally cleaning the titanium-zirconium-based alloy square sample by using deionized water.
Preferably, the oxidation furnace comprises a shell, a motor, a first rotating shaft, a supporting plate and an oxygen injection unit; the top end of the shell is provided with an end cover, and the bottom end of the shell is provided with a bracket; the motor is arranged on the outer side wall of the bottom end of the shell; the first rotating shaft is rotatably connected to the inner side wall of the bottom end of the shell and is fixedly connected with the output end of the motor; the supporting plate is arranged on the side wall of the top end of the first rotating shaft; the oxygen injection unit is arranged on the inner side wall of the shell and comprises a first cam, an air bag, an air storage chamber and a fixing plate; the first cam is fixedly connected to the first rotating shaft; the air bag is arranged on the inner side wall of the shell close to the first cam, and oxygen is filled in the air bag; the air storage chamber is arranged on the outer side wall of the shell, and the air storage chamber is communicated with the air bag through a hose; the fixed plate is arranged on the inner side wall of the shell close to the air storage chamber, and a plurality of air nozzles are arranged on the side wall of the fixed plate and communicated with the air storage chamber; the during operation, when needing to carry out the vacuum diffusion processing with the square sample of titanium zirconium base alloy, place square sample in the backup pad earlier, to the motor circular telegram again this moment, it rotates to drive a pivot after the motor circular telegram, a pivot drives a cam and carries out reciprocal extrusion to the gasbag in the rotation in-process, its inside oxygen passes through the jet orifice blowout after the gasbag pressurized, oxygen is through spouting back and square sample surface contact, thereby form one deck oxygen diffusion layer on its surface, and simultaneously, drive the backup pad and rotate simultaneously at the rotation in-process of a pivot, thereby continuous change the area of contact between square sample and the oxygen, realize the evenly distributed of oxygen on square sample surface, the thickness homogeneity on square sample surface vacuum diffusion layer has been guaranteed, thereby effectively increased the abrasion resistance on square sample surface.
Preferably, a first sliding groove is formed in the fixing plate; the first sliding groove is connected with a clamping plate in a sliding mode through a spring, and a second rotating shaft is rotatably connected to the side wall, close to the air storage chamber, of the first sliding groove; the clamping plate is provided with a plurality of openings, so that the air jet passes through the openings; a second cam is arranged at the end part of the second rotating shaft in the first sliding groove, and blades are arranged at the end part of the second rotating shaft in the air storage chamber; when the pneumatic air injection device works, after the motor is powered on, the first rotating shaft drives the first cam to rotate, the first cam realizes reciprocating extrusion on the air bag when rotating, the oxygen inside the air bag is pressed and enters the air storage chamber through the hose, the fan blade is driven to rotate in the oxygen flowing process, the fan blade drives the second cam to rotate through the second rotating shaft after rotating, the second cam realizes reciprocating extrusion on the clamping plate through matching with the spring in the rotating process, the reciprocating movement in the first sliding groove is realized after the clamping plate is extruded, the clamping plate produces stirring effect on the air injection port through the opening in the moving process, so that the air injection port can swing in a reciprocating mode in the shell, the flow rate and the flow range of the oxygen in the oxidation furnace are further increased, the oxidation effect on a square sample is enhanced, and the oxidation rate on the square sample is improved.
Preferably, the supporting plate is provided with a positioning plate; the surface of the positioning plate is provided with a second sliding groove which is communicated with the air bag through a hose; a plurality of first sliding blocks and second sliding blocks are connected in the second sliding groove in a sliding mode; the first sliding block is symmetrically and slidably connected to two ends of the second sliding groove, and elastic sealing cloth is connected between the first sliding block and the inner side wall of the second sliding groove; the second sliding block is connected in a second sliding groove between the first sliding blocks in a sliding manner, and elastic sealing cloth is connected between the second sliding block and the first sliding block; air holes are formed in the first sliding block and the second sliding block, and the first sliding block and the second sliding block are connected through a V-shaped elastic plate; when the device works, when a titanium-zirconium-based alloy square sample needs to be subjected to vacuum diffusion treatment, the square sample is placed on the V-shaped elastic plate, after the air bag is pressed, gas in the air bag enters the second sliding groove to generate thrust to the first sliding block, the first sliding block is stressed to slide in the second sliding groove in a reciprocating manner, in the sliding process of the first sliding block, the second sliding block is simultaneously thrust to the second sliding block through the V-shaped elastic plate, so that the second sliding block also slides in the second sliding groove, the V-shaped elastic plate is also correspondingly bent and elastically deformed, when the V-shaped elastic plate is bent and elastically deformed, the square sample generates jacking force and thrust, so that the square sample rolls back and forth on the surface of the V-shaped elastic plate, the side face of the square sample, which is in contact with the V-shaped elastic plate, is continuously replaced, and the side face of the square sample, which is in contact with the V-shaped elastic plate, cannot be fully contacted with oxygen, affecting the quality of the vacuum diffusion layer on the surface of the square sample.
Preferably, a through hole is formed in the side wall of the top end of the second sliding block, so that the through hole is communicated with the air vent; a rubber plug is connected in the through hole in a sliding manner; the V-shaped elastic plate is connected to the side wall of the top end of the rubber plug; the during operation, after oxygen gets into No. two spouts, make a slider and No. two sliders take place to slide under the effect of atmospheric pressure, thereby make V-arrangement elastic plate also take place corresponding elastic deformation, at the deformation in-process of V-arrangement elastic plate, V-arrangement elastic plate moves the rubber stopper and carries out reciprocal slip in the through-hole, thereby make and realize discontinuous intercommunication and jam between through-hole and the bleeder vent, when through-hole and bleeder vent intercommunication, oxygen in No. two spouts to the bottom surface of square sample through-hole and bleeder vent, further strengthen the oxidation effect to the square sample, guarantee the quality on square sample surface vacuum diffusion layer.
The invention has the following beneficial effects:
1. according to the preparation method of the high-temperature induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy, the oxidation treatment of the surface of the square titanium-zirconium-based alloy sample is realized through the cooperation of the shell, the motor, the first rotating shaft, the supporting plate and the oxygen injection unit, the quality of the vacuum diffusion layer on the surface of the square sample is enhanced, and the oxidation rate of the square sample is accelerated by improving the oxygen concentration on the surface of the square sample.
2. According to the preparation method of the high-temperature induced titanium-zirconium-based alloy surface wear-resistant diffusion layer, the air jet port can swing back and forth in the shell through the cooperation of the fixing plate, the clamping plate, the second rotating shaft, the fan blades and the second cam, the flow rate and the flow range of oxygen in the oxidation furnace are further increased, the oxidation effect on a square sample is enhanced, and the oxidation rate on the square sample is increased.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a perspective view of an oxidation oven used in the present invention;
FIG. 3 is a sectional view of an oxidation oven used in the present invention;
FIG. 4 is an enlarged view of a portion of FIG. 3 at A;
FIG. 5 is a partial enlarged view at B in FIG. 3;
FIG. 6 is a surface topography of example 1 of the present invention;
FIG. 7 is a surface topography of example 2 of the present invention;
FIG. 8 is a surface topography of example 3 of the present invention;
in the figure: the oxygen injection device comprises a shell 1, an end cover 11, a support 12, a motor 2, a first rotating shaft 3, a support plate 4, a positioning plate 41, a second sliding groove 411, a first sliding block 412, a second sliding block 413, elastic sealing cloth 414, an air hole 415, a V-shaped elastic plate 416, a through hole 417, a rubber plug 418, an oxygen injection unit 5, a first cam 51, an air bag 52, an air storage chamber 53, a fixing plate 54, a first sliding groove 541, a clamping plate 542, a second rotating shaft 543, an opening 544, a second cam 545, fan blades 546 and an air jet 55.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
S1: pressing high-purity metals of titanium, zirconium and aluminum with the purity of 99.5 percent and 50Al50V of a master alloy into short rod-shaped lump materials to obtain basic raw materials, manufacturing the basic raw materials into electrodes, and then carrying out smelting treatment through a vacuum consumable electrode arc furnace to obtain alloy ingots, wherein the smelting current is 220A, and the smelting time is 5 min;
s2: carrying out three-pier three-pull turning on the alloy ingot in the S1 to obtain a titanium-zirconium-based alloy bar, cutting a square sample with the shape of 10mm multiplied by 30mm from the bar by using a wire electric discharge machine, and then polishing the titanium-zirconium-based alloy square sample by using SiC abrasive paper to ensure that the surface roughness of the titanium-zirconium-based alloy square sample is 0.15 mu m;
s3: cleaning the titanium-zirconium-based alloy square sample in the step S2 in an ultrasonic cleaning machine to remove impurity particles on the surface of the titanium-zirconium-based alloy square sample, and drying the surface of the titanium-zirconium-based alloy square sample by using a hot air blower; wherein the heating temperature of the air heater is controlled to be 75 ℃, and an included angle of 45 degrees is formed between an air outlet of the air heater and the surface of the titanium-zirconium-based alloy square sample;
s4: carrying out thermal oxidation treatment on the titanium-zirconium-based alloy square sample in the S3 through a muffle furnace, wherein the heating temperature is 750 ℃, and the heat preservation time is 12 hours; and after the heat preservation is finished, cooling the titanium-zirconium-based alloy square sample along with the furnace, after the titanium-zirconium-based alloy square sample is cooled to room temperature, putting the titanium-zirconium-based alloy square sample into an oxidation furnace for vacuum diffusion treatment, wherein the vacuum diffusion time is 9 hours, the temperature is 450 ℃, and an oxygen diffusion layer is formed on the surface of the titanium-zirconium-based alloy square sample to finish the preparation of the high-temperature induced titanium-zirconium-based alloy surface wear-resistant diffusion layer.
Example 2
S1: pressing high-purity metals of titanium, zirconium and aluminum with the purity of 99.5 percent and 50Al50V of a master alloy into short rod-shaped lump materials to obtain basic raw materials, manufacturing the basic raw materials into electrodes, and then carrying out smelting treatment through a vacuum consumable electrode arc furnace to obtain alloy ingots, wherein the smelting current is 220A, and the smelting time is 5 min;
s2: carrying out three-pier three-pull turning on the alloy ingot in the S1 to obtain a titanium-zirconium-based alloy bar, cutting a square sample with the shape of 10mm multiplied by 30mm from the bar by using a spark wire cutting machine, and then polishing the titanium-zirconium-based alloy square sample by using SiC abrasive paper to ensure that the surface roughness of the titanium-zirconium-based alloy square sample is 0.15 mu m;
s3: cleaning the titanium-zirconium-based alloy square sample in the step S2 in an ultrasonic cleaning machine to remove impurity particles on the surface of the titanium-zirconium-based alloy square sample, and drying the surface of the titanium-zirconium-based alloy square sample by using a hot air blower; wherein the heating temperature of the air heater is controlled to be 75 ℃, and an included angle of 45 degrees is formed between an air outlet of the air heater and the surface of the titanium-zirconium-based alloy square sample;
s4: carrying out thermal oxidation treatment on the titanium-zirconium-based alloy square sample in the S3 through a muffle furnace, wherein the heating temperature is 750 ℃, and the heat preservation time is 12 hours; and after the heat preservation is finished, cooling the titanium-zirconium-based alloy square sample along with the furnace, after the titanium-zirconium-based alloy square sample is cooled to room temperature, putting the titanium-zirconium-based alloy square sample into an oxidation furnace for vacuum diffusion treatment, wherein the vacuum diffusion time is 9 hours, the temperature is 500 ℃, and an oxygen diffusion layer is formed on the surface of the titanium-zirconium-based alloy square sample to finish the preparation of the high-temperature induced titanium-zirconium-based alloy surface wear-resistant diffusion layer.
Example 3
S1: pressing high-purity metals of titanium, zirconium and aluminum with the purity of 99.5 percent and 50Al50V of a master alloy into short rod-shaped lump materials to obtain basic raw materials, manufacturing the basic raw materials into electrodes, and then carrying out smelting treatment through a vacuum consumable electrode arc furnace to obtain alloy ingots, wherein the smelting current is 220A, and the smelting time is 5 min;
s2: carrying out three-pier three-pull turning on the alloy ingot in the S1 to obtain a titanium-zirconium-based alloy bar, cutting a square sample with the shape of 10mm multiplied by 30mm from the bar by using a wire electric discharge machine, and then polishing the titanium-zirconium-based alloy square sample by using SiC abrasive paper to ensure that the surface roughness of the titanium-zirconium-based alloy square sample is 0.15 mu m;
s3: cleaning the titanium-zirconium-based alloy square sample in the step S2 in an ultrasonic cleaning machine to remove impurity particles on the surface of the titanium-zirconium-based alloy square sample, and drying the surface of the titanium-zirconium-based alloy square sample by using a hot air blower; wherein the heating temperature of the air heater is controlled to be 75 ℃, and an included angle of 45 degrees is formed between an air outlet of the air heater and the surface of the titanium-zirconium-based alloy square sample;
s4: carrying out thermal oxidation treatment on the titanium-zirconium-based alloy square sample in the S3 through a muffle furnace, wherein the heating temperature is 750 ℃, and the heat preservation time is 12 hours; and after the heat preservation is finished, cooling the titanium-zirconium-based alloy square sample along with the furnace, after the titanium-zirconium-based alloy square sample is cooled to room temperature, putting the titanium-zirconium-based alloy square sample into an oxidation furnace for vacuum diffusion treatment, wherein the vacuum diffusion time is 9 hours, the temperature is 550 ℃, and an oxygen diffusion layer is formed on the surface of the titanium-zirconium-based alloy square sample to finish the preparation of the high-temperature induced titanium-zirconium-based alloy surface wear-resistant diffusion layer.
Carrying out an abrasion test on a sample (namely, the embodiment 1-3) subjected to thermal oxidation on a multifunctional tribology testing machine, and measuring abrasion marks through an optical topography instrument to measure abrasion volume; the samples of each example were tested in 3 sets of replicates; after the abrasion test, sequentially adopting acetone, distilled water and absolute ethyl alcohol to carry out ultrasonic cleaning and scrubbing, then drying and weighing; the results are shown in Table 1.
TABLE 1
Note: sources of the reference
1.L.Q.Yang,H.Zhong,G.Lv,et al.Dry Sliding Behavior of a TiZr-Based Alloy under Air and Vacuum Conditions.Journal of Materials Engineering and Performance.2019,28:3402-3412.
It can be seen from examples 1 to 3 that the vacuum diffusion layer on the surface of the titanium-zirconium-based alloy has a wear-resistant effect, and the quality of the vacuum diffusion layer on the surface of the titanium-zirconium-based alloy is gradually enhanced with the increase of the oxidation temperature of the titanium-zirconium-based alloy, so that the overall wear-resistant effect of the titanium-zirconium-based alloy is improved, the service effect of the titanium-zirconium-based alloy is improved, and the service life of the titanium-zirconium-based alloy is prolonged.
As a specific embodiment of the invention, when the base raw material is smelted in a vacuum consumable electrode arc furnace, the smelting current is increased in stages, that is, the smelting current is firstly 190A, and smelting is continued for 2 min; then the smelting current is increased to 230A, and smelting is continued for 2 min; and finally, increasing the smelting current to 260A, and finishing the smelting treatment of the basic raw materials after continuously smelting for 2 min.
As a specific embodiment of the present invention, when the square titanium-zirconium-based alloy sample is cleaned by an ultrasonic cleaning machine, the square titanium-zirconium-based alloy sample needs to be cleaned by three different cleaning solutions; the method comprises the following steps of firstly cleaning the titanium-zirconium-based alloy square sample by using an acetone solution, cleaning the titanium-zirconium-based alloy square sample by using an alcohol solution after the cleaning is finished, and finally cleaning the titanium-zirconium-based alloy square sample by using deionized water.
As shown in fig. 1 to 8, as an embodiment of the present invention, the oxidation furnace includes a housing 1, a motor 2, a first rotating shaft 3, a support plate 4, and an oxygen injection unit 5; an end cover 11 is arranged at the top end of the shell 1, and a support 12 is arranged at the bottom end of the shell 1; the motor 2 is arranged on the outer side wall of the bottom end of the shell 1; the first rotating shaft 3 is rotatably connected to the inner side wall of the bottom end of the shell 1, and the first rotating shaft 3 is fixedly connected with the output end of the motor 2; the supporting plate 4 is arranged on the side wall of the top end of the first rotating shaft 3; the oxygen injection unit 5 is arranged on the inner side wall of the shell 1, and the oxygen injection unit 5 comprises a first cam 51, an air bag 52, an air storage chamber 53 and a fixing plate 54; the first cam 51 is fixedly connected to the first rotating shaft 3; the air bag 52 is arranged on the inner side wall of the shell 1 close to the first cam 51, and oxygen is filled in the air bag 52; the air storage chamber 53 is arranged on the outer side wall of the shell 1, and the air storage chamber 53 is communicated with the air bag 52 through a hose; the fixing plate 54 is mounted on the inner side wall of the shell 1 close to the air storage chamber 53, a plurality of air nozzles 55 are arranged on the side wall of the fixing plate 54, and the air nozzles 55 are communicated with the air storage chamber 53; when the device works, when a titanium-zirconium-based alloy square sample needs to be subjected to vacuum diffusion treatment, the square sample is placed on the supporting plate 4, the motor 2 is powered on, the motor 2 drives the first rotating shaft 3 to rotate after being powered on, the first rotating shaft 3 drives the first cam 51 to extrude the air bag 52 in a reciprocating manner in the rotating process, oxygen in the air bag 52 is sprayed out through the air spraying port 55 after being pressed, the oxygen is contacted with the surface of the square sample after being sprayed out, so that an oxygen diffusion layer is formed on the surface of the square sample, and meanwhile, drive backup pad 4 and rotate simultaneously at the rotation in-process of a pivot 3 to continuous change area of contact between square sample and the oxygen, realize the evenly distributed of oxygen on square sample surface, guaranteed the thickness homogeneity of square sample surface vacuum diffusion layer, thereby effectively increased the stand wear and tear degree on square sample surface.
As a specific embodiment of the present invention, a first sliding groove 541 is formed in the fixing plate 54; a clamping plate 542 is slidably connected in the first sliding groove 541 through a spring, and the first sliding groove 541 is rotatably connected with a second rotating shaft 543 on the side wall close to the air storage chamber 53; a plurality of openings 544 are formed in the clamping plate 542, so that the air jet 55 passes through the openings 544; a second cam 545 is installed at the end part of the second rotating shaft 543 in the first sliding groove 541, and fan blades 546 are installed at the end part of the second rotating shaft 543 in the air storage chamber 53; when the air bag type oxidation furnace is in work, after the motor 2 is powered on, the first rotating shaft 3 drives the first cam 51 to rotate, the first cam 51 realizes reciprocating extrusion on the air bag 52 when rotating, oxygen in the air bag 52 enters the air storage chamber 53 through the hose after being compressed, the fan blade 546 is driven to rotate in the flow process of the oxygen, the fan blade 546 drives the second cam 545 to rotate through the second rotating shaft 543 after rotating, the second cam 545 realizes reciprocating extrusion on the clamping plate 542 through matching with the spring in the rotating process, the clamping plate 542 realizes reciprocating movement in the first sliding groove 541 after being extruded, the clamping plate 542 generates a stirring effect on the air jet 55 through the opening 544 in the moving process, so that the air jet 55 can perform reciprocating swing in the shell 1, the flow rate and the flow range of the oxygen in the oxidation furnace are further increased, and the oxidation effect on a square sample is enhanced, the oxidation rate of the square sample is increased.
As a specific embodiment of the present invention, a positioning plate 41 is mounted on the supporting plate 4; a second sliding groove 411 is formed in the surface of the positioning plate 41, and the second sliding groove 411 is communicated with the air bag 52 through a hose; a plurality of first sliding blocks 412 and second sliding blocks 413 are connected in the second sliding groove 411 in a sliding mode; the first sliding block 412 is symmetrically and slidably connected to two ends of the second sliding groove 411, and an elastic sealing cloth 414 is connected between the inner side walls of the first sliding block 412 and the second sliding groove 411; the second sliding block 413 is connected in a second sliding groove 411 between the first sliding blocks 412 in a sliding manner, and an elastic sealing cloth 414 is connected between the second sliding block 413 and the first sliding blocks 412; the first sliding block 412 and the second sliding block 413 are both provided with air holes 415, and the first sliding block 412 and the second sliding block 413 are connected through a V-shaped elastic plate 416; when the device works, when the titanium-zirconium-based alloy square sample needs to be subjected to vacuum diffusion treatment, the square sample is placed on the V-shaped elastic plate 416, after the air bag 52 is pressed, gas in the air bag 52 enters the second sliding groove 411 to generate thrust on the first sliding block 412, the first sliding block 412 is stressed and then slides in the second sliding groove 411 in a reciprocating manner, in the sliding process of the first sliding block 412, the second sliding block 413 is simultaneously thrust on the second sliding block 413 through the V-shaped elastic plate 416, so that the second sliding block 413 also slides in the second sliding groove 411, the V-shaped elastic plate 416 is also correspondingly bent and elastically deformed, when the V-shaped elastic plate 416 is bent and elastically deformed, jacking force and thrust are generated on the square sample, the square sample rolls back and forth on the surface of the V-shaped elastic plate 416, the side face of the square sample, which is in contact with the V-shaped elastic plate 416, is continuously replaced, and the side face of the square sample, which is in contact with the V-shaped elastic plate 416, cannot be fully contacted with oxygen, affecting the quality of the vacuum diffusion layer on the surface of the square sample.
As a specific embodiment of the present invention, a through hole 417 is formed on a side wall of a top end of the second slider 413, so that the through hole 417 is communicated with the air hole 415; a rubber plug 418 is slidably connected in the through hole 417; the V-shaped elastic plate 416 is connected to the side wall of the top end of the rubber plug 418; during operation, after oxygen enters the second sliding groove 411, the first sliding block 412 and the second sliding block 413 slide under the action of air pressure, so that the V-shaped elastic plate 416 also generates corresponding elastic deformation, in the deformation process of the V-shaped elastic plate 416, the V-shaped elastic plate 416 drives the rubber plug 418 to slide in the through hole 417 in a reciprocating mode, so that intermittent communication and blockage between the through hole 417 and the air holes 415 are achieved, when the through hole 417 is communicated with the air holes 415, the oxygen in the second sliding groove 411 is sprayed out to the bottom surface of the square sample through the through hole 417 and the air holes 415, the oxidation effect of the square sample is further enhanced, and the quality of a vacuum diffusion layer on the surface of the square sample is guaranteed.
When the device works, when a titanium-zirconium-based alloy square sample needs to be subjected to vacuum diffusion treatment, the square sample is placed on the supporting plate 4, the motor 2 is powered on, the motor 2 drives the first rotating shaft 3 to rotate after being powered on, the first rotating shaft 3 drives the first cam 51 to extrude the air bag 52 in a reciprocating manner in the rotating process, oxygen in the air bag 52 is sprayed out through the air spraying port 55 after being pressed, the oxygen is contacted with the surface of the square sample after being sprayed out, so that an oxygen diffusion layer is formed on the surface of the square sample, and meanwhile, the supporting plate 4 is driven to rotate simultaneously in the rotating process of the first rotating shaft 3, so that the contact area between the square sample and oxygen is continuously changed, the uniform distribution of the oxygen on the surface of the square sample is realized, the thickness uniformity of a vacuum diffusion layer on the surface of the square sample is ensured, and the wear resistance of the surface of the square sample is effectively increased; after the motor 2 is electrified, the first cam 51 is driven to rotate through the first rotating shaft 3, the first cam 51 realizes reciprocating extrusion on the air bag 52 when rotating, oxygen in the air bag 52 enters the air storage chamber 53 through the hose after being pressed, the fan blades 546 are driven to rotate in the flowing process of oxygen, the fan blades 546 are driven to rotate through the second rotating shaft 543 after rotating, the second cam 545 realizes reciprocating extrusion on the clamping plate 542 through cooperation with the spring in the rotating process, the clamping plate 542 realizes reciprocating movement in the first sliding groove 541 after being extruded, the clamping plate 542 generates a stirring effect on the air jet 55 through the opening 544 in the moving process, thereby, the air jet 55 swings in the housing 1 in a reciprocating manner, the flow rate and the flow range of oxygen in the oxidation furnace are further increased, the oxidation effect on the square sample is enhanced, and the oxidation rate on the square sample is improved.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy is characterized by comprising the following steps: the preparation method comprises the following steps:
s1: pressing high-purity metals of titanium, zirconium and aluminum with the purity of 99.5 percent and 50Al50V of intermediate alloy into short rod-shaped lump materials to obtain basic raw materials, manufacturing the basic raw materials into electrodes, and then carrying out smelting treatment through a vacuum consumable electrode arc furnace to obtain alloy ingots, wherein the smelting current is 180-260A, and the smelting time is 4-6 min;
s2: carrying out three-pier three-pull turning on the alloy ingot in the S1 to obtain a titanium-zirconium-based alloy bar, cutting a square sample with the shape of 10mm multiplied by 30mm from the bar by using a wire electric discharge machine, and then polishing the titanium-zirconium-based alloy square sample by using SiC abrasive paper to ensure that the surface roughness of the titanium-zirconium-based alloy square sample is 0.1-0.2 mu m;
s3: cleaning the titanium-zirconium-based alloy square sample in the step S2 in an ultrasonic cleaning machine to remove impurity particles on the surface of the titanium-zirconium-based alloy square sample, and drying the surface of the titanium-zirconium-based alloy square sample by using a hot air blower; wherein the heating temperature of the air heater is controlled to be 75-80 ℃, and an included angle of 45 degrees is formed between an air outlet of the air heater and the surface of the titanium-zirconium-based alloy square sample;
s4: carrying out thermal oxidation treatment on the titanium-zirconium-based alloy square sample in the S3 through a muffle furnace, wherein the heating temperature is 650-800 ℃, and the heat preservation time is 12 h; after the heat preservation is finished, cooling the titanium-zirconium-based alloy square sample along with the furnace, after the titanium-zirconium-based alloy square sample is cooled to room temperature, putting the titanium-zirconium-based alloy square sample into an oxidation furnace for vacuum diffusion treatment, forming an oxygen diffusion layer on the surface of the titanium-zirconium-based alloy square sample, and finishing the preparation of the high-temperature induced titanium-zirconium-based alloy surface wear-resistant diffusion layer;
the oxidation furnace comprises a shell (1), a motor (2), a first rotating shaft (3), a supporting plate (4) and an oxygen injection unit (5); an end cover (11) is arranged at the top end of the shell (1), and a support (12) is arranged at the bottom end of the shell (1); the motor (2) is arranged on the outer side wall of the bottom end of the shell (1); the first rotating shaft (3) is rotatably connected to the inner side wall of the bottom end of the shell (1), and the first rotating shaft (3) is fixedly connected with the output end of the motor (2); the supporting plate (4) is arranged on the side wall of the top end of the first rotating shaft (3); the oxygen injection unit (5) is arranged on the inner side wall of the shell (1), and the oxygen injection unit (5) comprises a first cam (51), an air bag (52), an air storage chamber (53) and a fixing plate (54); the first cam (51) is fixedly connected to the first rotating shaft (3); the air bag (52) is arranged on the inner side wall of the shell (1) close to the first cam (51), and oxygen is filled in the air bag (52); the air storage chamber (53) is arranged on the outer side wall of the shell (1), and the air storage chamber (53) is communicated with the air bag (52) through a hose; the fixing plate (54) is arranged on the inner side wall of the shell (1) close to the air storage chamber (53), a plurality of air nozzles (55) are arranged on the side wall of the fixing plate (54), and the air nozzles (55) are communicated with the air storage chamber (53);
a first sliding groove (541) is formed in the fixing plate (54); a clamping plate (542) is connected in the first sliding groove (541) in a sliding manner through a spring, and a second rotating shaft (543) is rotatably connected on the side wall of the first sliding groove (541) close to the air storage chamber (53); a plurality of openings (544) are arranged on the clamping plate (542) so that the air jet (55) penetrates through the openings (544); a second cam (545) is installed at the end part of the second rotating shaft (543) positioned in the first sliding groove (541), and a fan blade (546) is installed at the end part of the second rotating shaft (543) positioned in the air storage chamber (53);
a positioning plate (41) is arranged on the supporting plate (4); a second sliding groove (411) is formed in the surface of the positioning plate (41), and the second sliding groove (411) is communicated with the air bag (52) through a hose; a plurality of first sliding blocks (412) and second sliding blocks (413) are connected in the second sliding groove (411) in a sliding mode; the first sliding block (412) is symmetrically connected to two ends of the second sliding groove (411) in a sliding mode, and elastic sealing cloth (414) is connected between the first sliding block (412) and the inner side wall of the second sliding groove (411); the second sliding block (413) is connected in a second sliding groove (411) between the first sliding blocks (412) in a sliding mode, and elastic sealing cloth (414) is connected between the second sliding block (413) and the first sliding blocks (412); the first sliding block (412) and the second sliding block (413) are internally provided with air holes (415), and the first sliding block (412) is connected with the second sliding block (413) through a V-shaped elastic plate (416).
2. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 1, wherein the method comprises the following steps: when the basic raw materials are smelted through a vacuum consumable electrode arc furnace, the smelting current is increased in stages, namely the smelting current is firstly 190A, and smelting is continued for 2 min; then the smelting current is increased to 230A, and smelting is continued for 2 min; and finally, increasing the smelting current to 260A, and finishing the smelting treatment of the basic raw materials after continuously smelting for 2 min.
3. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 1, wherein the method comprises the following steps: in the vacuum diffusion process of the titanium-zirconium-based alloy square sample, the vacuum diffusion time is 8-10h, and the heating temperature is 400-550 ℃.
4. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 1, wherein the method comprises the following steps: when the titanium-zirconium-based alloy square sample is cleaned by an ultrasonic cleaning machine, the titanium-zirconium-based alloy square sample needs to be cleaned by different cleaning liquids for three times; the method comprises the following steps of firstly cleaning the titanium-zirconium-based alloy square sample by using an acetone solution, cleaning the titanium-zirconium-based alloy square sample by using an alcohol solution after the cleaning is finished, and finally cleaning the titanium-zirconium-based alloy square sample by using deionized water.
5. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 1, wherein the method comprises the following steps: a through hole (417) is formed in the side wall of the top end of the second sliding block (413), so that the through hole (417) is communicated with the air hole (415); a rubber plug (418) is connected in the through hole (417) in a sliding way; the V-shaped elastic plate (416) is connected to the side wall of the top end of the rubber plug (418).
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