CN109807338B - Sectional preparation method of rhenium-niobium composite spray pipe - Google Patents
Sectional preparation method of rhenium-niobium composite spray pipe Download PDFInfo
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- CN109807338B CN109807338B CN201910073664.3A CN201910073664A CN109807338B CN 109807338 B CN109807338 B CN 109807338B CN 201910073664 A CN201910073664 A CN 201910073664A CN 109807338 B CN109807338 B CN 109807338B
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Abstract
The invention relates to a sectional preparation method of a rhenium-niobium composite spray pipe, belonging to the technical field of powder metallurgy preparation of refractory metal materials. The forming sheath at the upper end and the lower end of the invention contains niobium alloy components for forming the rhenium-niobium composite part. The sheath filled with rhenium powder is formed by low-temperature hot isostatic pressing, at the moment, the rhenium component blank has certain strength and the density reaches more than 99 percent after being formed, and the rhenium-niobium transition areas at the upper part and the lower part can be directly processed and formed in the low-temperature area where the spray pipe works; and the middle-end rhenium substrate is further densified by high-temperature sintering to improve the metallurgical bonding strength, so that the mechanical property reaches the service requirement, and then is machined and formed. And finally, welding the upper end, the middle end and the lower end of the machined spray pipe into a complete rhenium-niobium composite spray pipe through vacuum electron beams.
Description
Technical Field
The invention relates to a sectional preparation method of a rhenium-niobium composite spray pipe, belongs to the technical field of powder metallurgy preparation of refractory metal materials, and provides a powder metallurgy preparation method of a rhenium-niobium composite engine spray pipe, which can be used for developing a high-performance rhenium-iridium engine and is applied to a propulsion system of a space vehicle such as a satellite.
Background
The rhenium metal has high melting point (3180 ℃) and good high-low temperature mechanical property, the working temperature of the high-performance rhenium iridium engine combustion chamber taking rhenium as the base iridium as the coating reaches more than 2000 ℃, and the high-performance rhenium iridium engine combustion chamber can be applied to advanced engines of satellites and space vehicles. Generally, a straight line section of the combustion chamber needs to be welded with a titanium alloy injector, an expansion section of the combustion chamber needs to be welded with a niobium alloy extension section, but due to the fact that the melting point of rhenium materials is high, the welding connection difficulty of rhenium metal and other metals is high, and the quality of welding seams is difficult to guarantee, when rhenium is connected with other metals, rhenium and niobium transition connection is generally firstly prepared at the head and the tail of the combustion chamber, and then the rhenium and niobium transition connection is well welded and assembled with the other metals through niobium alloys.
The rhenium-niobium transition connection adopts a Chemical Vapor Deposition (CVD) method at first, a rhenium matrix is formed first, and a niobium layer is chemically vapor deposited on the surface of rhenium. Later, a rhenium-niobium composite combustion chamber is prepared by adopting a traditional powder metallurgy integrated forming process, but due to the high melting point of rhenium materials, generally, the rhenium powder metallurgy Hot Isostatic Pressing (HIP) densification forming needs to be more than 1500 ℃, and the handling performance of niobium alloys is sharply deteriorated at more than 1400 ℃, so that the prepared rhenium-niobium composite combustion chamber is low in connection strength.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a sectional preparation method of the rhenium-niobium composite spray pipe.
The technical solution of the invention is as follows:
the sectional preparation method of the rhenium-niobium composite spray pipe comprises a head part, a straight line section, a convergence section, a throat part, an expansion section and a tail part; the head part is made of niobium alloy, the tail part is made of niobium alloy, and the straight line section, the convergent section, the throat part and the divergent section are made of rhenium; the head part is positioned at the top of the straight line segment, the tail part is positioned at the bottom of the expanding segment, and the rhenium-niobium composite spray pipe is divided into three parts, namely an upper end, a middle end and a lower end, wherein the upper end and the lower end are of a rhenium-niobium composite structure, and the middle end is of a rhenium base material; the upper end is a head part and a part of straight line segment, and the lower end is a tail part and a part of expansion segment; the middle end comprises another part of straight line segment, a convergent section, a throat part and another part of expansion section;
the head part is used for welding, and the tail part is used for welding;
the method comprises the following steps:
(a) carrying out activation treatment on the high-purity rhenium powder;
(b) preparing an upper end near net-shaped mold sheath, a middle end near net-shaped mold sheath and a lower end near net-shaped mold sheath;
(c) preparing an upper end, a middle end and a lower end by using the upper end near-net-shape die sheath, the middle end near-net-shape die sheath and the lower end near-net-shape die sheath prepared in the step (b);
(d) and (c) connecting the upper end and the middle end obtained in the step (c) and connecting the lower end and the middle end by adopting vacuum electron beam welding or laser welding to obtain the rhenium-niobium composite spray pipe.
In the step (a), the method for activating the high-purity rhenium powder comprises the following steps:
selecting high-purity rhenium powder of 100-325 meshes; firstly, reducing rhenium powder in hydrogen with the purity of more than 99.99% for 0.5-4 h at the temperature of 800-1050 ℃, and then, ensuring the vacuum degree to be more than 5 multiplied by 10-3Heat treatment is carried out for 0.5-4 h at the temperature of 900-1200 ℃ under Pa.
In the step (b), the upper-end near-net-shaped die sheath comprises an upper-end outer sheath, an upper-end core die, an upper-end sheath cover and a niobium head, and the upper-end sheath cover is provided with an upper-end air outlet pipe;
the middle-end near-net-shaped mold sheath comprises a middle-end outer sheath, a middle-end core mold and a middle-end sheath cover, and the middle-end sheath cover is provided with a middle-end air outlet pipe;
the lower end near-net-shaped die sleeve comprises a lower end outer sleeve, a lower end core die, a lower end sleeve cover and a niobium tail, and the lower end sleeve cover is provided with a lower end air outlet pipe.
The outer surface of the niobium head is provided with a mechanical connection structure, and the outer surface of the niobium tail is provided with a mechanical connection structure.
The connecting structure is a meshing groove structure, a threaded connecting structure or a pin hole structure.
In the step (b), the upper core die is made of pure niobium or niobium alloy;
the middle core die is made of pure niobium or niobium alloy;
the lower core die is made of pure niobium or niobium alloy;
the material of the upper end outer sheath is steel, titanium, tantalum or niobium;
the upper end covering cover is made of steel, titanium, tantalum or niobium;
the middle-end outer sheath is made of steel, titanium, tantalum or niobium;
the middle-end packing cover is made of steel, titanium, tantalum or niobium;
the material of the outer sheath at the lower end is steel, titanium, tantalum or niobium;
the lower end covering cover is made of steel, titanium, tantalum or niobium;
the assembly of the upper end outer sheath and the upper end sheath cover adopts argon arc welding, electric welding or gas welding;
the assembly of the middle-end outer sheath and the middle-end sheath cover adopts argon arc welding, electric welding or gas welding;
the lower end outer sheath and the lower end sheath cover are assembled by argon arc welding, electric welding or gas welding.
In the step (c), the method for preparing the upper end by using the upper end near net-shaped die sheath comprises the following steps:
(1) installing an upper end core mold at the bottom of the upper end outer sheath, and then sleeving the niobium head on the upper end core mold;
(2) filling the high-purity rhenium powder obtained in the step (a) into a cavity formed by the outer sheath at the upper end, the head part of the niobium material and the core mould at the upper end, and compacting;
(3) welding and fixing an upper-end sheath cover on the top end of the upper-end outer sheath, degassing through an upper-end gas outlet pipe on the upper-end sheath cover, wherein the degassing temperature is 750-900 ℃, the degassing time is 8-48 h, and the vacuum degree during final packaging is less than 5 multiplied by 10-3Pa；
(4) Carrying out hot isostatic pressing treatment on the upper-end near-net-shaped die sheath packaged with the high-purity rhenium powder obtained in the step (3), and removing the upper-end outer sheath, the upper-end core die and the upper-end sheath cover after the hot isostatic pressing treatment is finished to obtain an upper-end blank;
the hot isostatic pressing temperature is 1250-1400 ℃, the hot isostatic pressing time is 1-5 h, and the hot isostatic pressing pressure is not less than 110 MPa;
(5) and (4) machining the upper end blank obtained in the step (4) according to the size requirement of the rhenium-niobium composite spray pipe to obtain the upper end.
In the step (c), the method for preparing the middle end by using the middle end near net-shaped mold sheath comprises the following steps:
(1) mounting the middle-end core mold at the bottom of the middle-end outer sheath;
(2) filling the high-purity rhenium powder obtained in the step (a) into a cavity formed by the middle-end outer sheath and the middle-end core mold, and compacting;
(3) welding and fixing the middle-end sheath cover on the top end of the middle-end outer sheath, degassing through a middle-end air outlet pipe on the middle-end sheath cover, wherein the degassing temperature is 750-900 ℃, the degassing time is 8-48 h, and the vacuum degree in final packaging is less than 5 multiplied by 10- 3Pa；
(4) Carrying out hot isostatic pressing treatment on the middle-end near-net-shaped die sheath packaged with the high-purity rhenium powder obtained in the step (3), and removing the middle-end outer sheath, the middle-end core die and the middle-end sheath cover by using a mechanical processing or chemical milling method after the hot isostatic pressing treatment is finished to obtain a middle-end pure rhenium blank;
the hot isostatic pressing temperature is 1250-1400 ℃, the hot isostatic pressing time is 1-5 h, and the hot isostatic pressing pressure is not less than 110 MPa;
(5) performing high-temperature heat treatment on the medium-end rhenium blank obtained in the step (4), and then performing high-temperature hot isostatic pressing treatment, wherein the high-temperature heat treatment atmosphere is vacuum or hydrogen atmosphere, the high-temperature heat treatment temperature is 1800-2600 ℃, the high-temperature heat treatment time is 0.5-6 h, the high-temperature hot isostatic pressing treatment temperature is 1600-2000 ℃, the high-temperature hot isostatic pressing treatment time is 1-4 h, and the high-temperature hot isostatic pressing treatment pressure is 130-200 MPa;
(6) machining the middle-end pure rhenium blank treated in the step (5) according to the size requirement of the rhenium-niobium composite spray pipe to obtain a middle end;
in the step (c), the method for preparing the lower end by using the lower end near net-shaped die sheath comprises the following steps:
(1) mounting a lower end core mold at the bottom of the lower end outer sheath, and then sleeving the tail part of the niobium material on the lower end core mold;
(2) filling the high-purity rhenium powder obtained in the step (a) into a cavity formed by the lower-end outer sheath, the niobium tail and the lower-end core mold, and compacting;
(3) welding and fixing the lower-end sheath cover on the top end of the lower-end outer sheath, degassing through a lower-end gas outlet pipe on the lower-end sheath cover, wherein the degassing temperature is 750-900 ℃, the degassing time is 8-48 h, and the vacuum degree in final packaging is less than 5 multiplied by 10- 3Pa；
(4) Carrying out hot isostatic pressing treatment on the lower end near-net-shaped die sheath packaged with the high-purity rhenium powder obtained in the step (3), and removing the lower end outer sheath, the lower end core die and the lower end sheath cover after the hot isostatic pressing treatment is finished to obtain a lower end blank;
the hot isostatic pressing temperature is 1250-1400 ℃, the hot isostatic pressing time is 1-5 h, and the hot isostatic pressing pressure is not less than 110 MPa;
(5) and (4) machining the lower end blank obtained in the step (4) according to the size requirement of the rhenium-niobium composite spray pipe to obtain the lower end.
In the step (d), the welding speed is 0.5-3 m/min.
Advantageous effects
(1) The rhenium-niobium composite spray pipe prepared by the powder metallurgy sectional forming process can obtain a high-strength rhenium matrix, overcomes various problems of transition connection of rhenium and niobium prepared by a chemical vapor deposition method and a traditional powder metallurgy process, and has high forming efficiency and low cost.
(2) The invention relates to a forming method for preparing a rhenium component of a rhenium-niobium composite combustion chamber, which comprises the following steps: firstly, removing surface oxides of high-purity rhenium powder through hydrogen activation treatment, and then filling the treated rhenium powder into a near-net forming sheath, wherein the forming sheaths at the upper end and the lower end comprise niobium alloy components for forming a rhenium-niobium composite part. The sheath filled with rhenium powder is formed by low-temperature hot isostatic pressing, at the moment, the rhenium component blank has certain strength and the density reaches more than 99 percent after being formed, and the rhenium-niobium transition areas at the upper part and the lower part can be directly processed and formed in the low-temperature area where the spray pipe works; and the middle-end rhenium substrate is further densified by high-temperature sintering to improve the metallurgical bonding strength, so that the mechanical property reaches the service requirement, and then is machined and formed. And finally, welding the upper end, the middle end and the lower end of the machined spray pipe into a complete rhenium-niobium composite spray pipe through vacuum electron beams. The rhenium-niobium composite spray pipe prepared by the scheme has a high-strength rhenium matrix, and avoids the damage of high-temperature treatment to the rhenium-niobium transition connection area and the performance of niobium alloy.
Drawings
FIG. 1 is a schematic structural view of a rhenium-niobium composite lance wherein a 101-niobium alloy region, a 102-rhenium alloy region, a 103-rhenium-niobium transition region, an upper end of a 104-rhenium-niobium composite lance, a middle end of a 105-rhenium-niobium composite lance, and a lower end of a 106-rhenium-niobium composite lance;
FIG. 2 is a schematic view of a mold jacket structure with a near-net-shaped upper end; wherein, 201-niobium alloy head, 202-upper core mold, 203-upper outer sheath, 204-upper sheath cover, 205-upper outlet pipe;
FIG. 3 is a schematic diagram of a middle near net shape mold jacket structure; wherein, 301-middle end outer sheath, 302-middle end core mold, 303-middle end sheath cover and 304-middle end air outlet pipe;
FIG. 4 is a schematic diagram of a jacket structure of a lower-end near-net-shape die, wherein 401-niobium alloy tail, 402-lower-end core die, 403-lower-end outer jacket, 404-lower-end jacket cover and 405-lower-end air outlet pipe.
Detailed Description
The sectional preparation method of the rhenium-niobium composite spray pipe comprises a head part, a straight line section, a convergence section, a throat part, an expansion section and a tail part; the head part is made of niobium alloy, the tail part is made of niobium alloy, and the straight line section, the convergent section, the throat part and the divergent section are made of rhenium; the head part is positioned at the top of the straight line segment, the tail part is positioned at the bottom of the expanding segment, and the rhenium-niobium composite spray pipe is divided into three parts, namely an upper end, a middle end and a lower end, wherein the upper end and the lower end are of a rhenium-niobium composite structure, and the middle end is of a rhenium base material; the upper end is a head part and a part of straight line segment, and the lower end is a tail part and a part of expansion segment; the middle end comprises another part of straight line segment, a convergent section, a throat part and another part of expansion section;
the head part is used for welding, and the tail part is used for welding;
the method comprises the following steps:
(a) carrying out activation treatment on the high-purity rhenium powder;
selecting high-purity rhenium powder of 100-325 meshes; firstly, reducing rhenium powder in hydrogen with the purity of more than 99.99% for 0.5-4 h at the temperature of 800-1050 ℃, and then, ensuring the vacuum degree to be more than 5 multiplied by 10-3Heat treatment is carried out for 0.5-4 h at the temperature of 900-1200 ℃ under Pa;
(b) preparing an upper end near net-shaped mold sheath, a middle end near net-shaped mold sheath and a lower end near net-shaped mold sheath;
the upper-end near-net-shaped mold sheath comprises an upper-end outer sheath 203, an upper-end core mold 202, an upper-end sheath cover 204 and a niobium head 201, wherein an upper-end air outlet pipe 205 is arranged on the upper-end sheath cover 204;
the middle-end near-net-shaped mold sheath comprises a middle-end outer sheath 301, a middle-end core mold 302 and a middle-end sheath cover 303, wherein a middle-end air outlet pipe 304 is arranged on the middle-end sheath cover 303;
the lower end near-net-shaped mold jacket comprises a lower end outer jacket 403, a lower end core mold 402, a lower end jacket cover 404 and a niobium tail 401, wherein a lower end air outlet pipe 405 is arranged on the lower end jacket cover 404;
the outer surface of the niobium head 201 is provided with a mechanical connection structure, such as a meshing groove structure, a threaded connection structure or a pin hole structure, i.e., the connection part of the niobium head 201 and the straight line section is provided with a mechanical connection structure for increasing the connection strength of the niobium head 201 and the straight line section;
the outer surface of the niobium tail 401 has a mechanical connection structure, such as a meshing groove structure, a threaded connection structure or a pin hole structure, i.e., the connection part of the niobium tail 401 and the expansion section has a mechanical connection structure for increasing the connection strength of the niobium tail 401 and the expansion section;
(c) preparing an upper end, a middle end and a lower end;
the preparation method of the upper end comprises the following steps:
(1) installing an upper end core mold 202 at the bottom of an upper end outer sheath 203, and then sleeving a niobium head 201 on the upper end core mold 202;
(2) filling the high-purity rhenium powder obtained in the step (a) into a cavity formed by the outer sheath 203 at the upper end, the head 201 made of niobium and the core mould 202 at the upper end, and compacting;
(3) welding and fixing an upper end sheath cover 204 on the top end of the upper end outer sheath 203, degassing through an upper end air outlet pipe 205 on the upper end sheath cover 204 at the temperature of 750-900 ℃ for 8-48 h, and finally packaging under the vacuum degree of less than 5 multiplied by 10-3Pa；
(4) Performing hot isostatic pressing treatment on the upper-end near-net-shaped die sheath packaged with the high-purity rhenium powder obtained in the step (3), and removing the upper-end outer sheath 203, the upper-end core die 202 and the upper-end sheath cover 204 after the hot isostatic pressing treatment is finished to obtain an upper-end blank;
the hot isostatic pressing temperature is 1250-1400 ℃, the hot isostatic pressing time is 1-5 h, and the hot isostatic pressing pressure is not less than 110 MPa;
(5) and (4) machining the upper end blank obtained in the step (4) according to the size requirement of the rhenium-niobium composite spray pipe to obtain the upper end.
The preparation method of the middle-end comprises the following steps:
(1) mounting a middle-end core mould 302 at the bottom of the middle-end outer sheath 301;
(2) filling the high-purity rhenium powder obtained in the step (a) into a cavity formed by the middle-end outer sheath 301 and the middle-end core mold 302, and compacting;
(3) welding and fixing the middle-end sheath cover 303 on the top end of the middle-end outer sheath 301, degassing through the middle-end air outlet pipe 304 on the middle-end sheath cover 303, wherein the degassing temperature is 750-900 ℃, the degassing time is 8-48 h, and the vacuum degree in final packaging is less than 5 multiplied by 10-3Pa；
(4) Performing hot isostatic pressing treatment on the middle-end near-net-shaped die sheath encapsulated with the high-purity rhenium powder obtained in the step (3), and removing the middle-end outer sheath 301, the middle-end core die 302 and the middle-end sheath cover 303 by using a machining or chemical milling method after the hot isostatic pressing treatment is finished to obtain a middle-end pure rhenium blank;
the hot isostatic pressing temperature is 1250-1400 ℃, the hot isostatic pressing time is 1-5 h, and the hot isostatic pressing pressure is not less than 110 MPa;
(5) performing high-temperature heat treatment on the medium-end rhenium blank obtained in the step (4), and then performing high-temperature hot isostatic pressing treatment, wherein the high-temperature heat treatment atmosphere is vacuum or hydrogen atmosphere, the high-temperature heat treatment temperature is 1800-2600 ℃, the high-temperature heat treatment time is 0.5-6 h, the high-temperature hot isostatic pressing treatment temperature is 1600-2000 ℃, the high-temperature hot isostatic pressing treatment time is 1-4 h, and the high-temperature hot isostatic pressing treatment pressure is 130-200 MPa;
(6) machining the middle-end pure rhenium blank treated in the step (5) according to the size requirement of the rhenium-niobium composite spray pipe to obtain a middle end;
the preparation method of the lower end comprises the following steps:
(1) mounting a lower-end mandrel 402 at the bottom of a lower-end outer sheath 403, and then sleeving a niobium tail 401 on the lower-end mandrel 402;
(2) filling the high-purity rhenium powder obtained in the step (a) into a cavity formed by the outer sheath 403 at the lower end, the tail 401 of the niobium material and the mandrel 402 at the lower end, and compacting;
(3) welding and fixing a lower end cover 404 on the top end of the lower end outer sheath 403, and degassing through a lower end air outlet pipe 405 on the lower end cover 404 at the degassing temperature of 750-900 ℃ for 8-48 h, wherein the vacuum degree in final packaging is less than 5 multiplied by 10-3Pa；
(4) Performing hot isostatic pressing treatment on the lower end near-net-shaped die sheath packaged with the high-purity rhenium powder obtained in the step (3), and removing the lower end outer sheath 403, the lower end core die 402 and the lower end sheath cover 404 after the hot isostatic pressing treatment is finished to obtain a lower end blank;
the hot isostatic pressing temperature is 1250-1400 ℃, the hot isostatic pressing time is 1-5 h, and the hot isostatic pressing pressure is not less than 110 MPa;
(5) and (4) machining the lower end blank obtained in the step (4) according to the size requirement of the rhenium-niobium composite spray pipe to obtain the lower end.
(d) And (c) connecting the upper end and the middle end obtained in the step (c) and connecting the lower end and the middle end by adopting vacuum electron beam welding or laser welding at the welding speed of 0.5-3 m/min to obtain the rhenium-niobium composite spray pipe.
In the step (b), the material of the upper end core mold 202 is pure niobium or a niobium alloy (such as a niobium hafnium alloy or a niobium tungsten alloy);
the material of the middle core mold 302 is pure niobium or niobium alloy (such as niobium hafnium alloy or niobium tungsten alloy);
the material of the lower mandrel 402 is pure niobium or a niobium alloy (such as a niobium hafnium alloy or a niobium tungsten alloy);
the upper end outer sheath 203 is made of steel, titanium, tantalum or niobium;
the upper end sheathing cap 204 is made of steel, titanium, tantalum or niobium;
the middle-end outer sheath 301 is made of steel, titanium, tantalum or niobium;
the middle-end packing cover 303 is made of steel, titanium, tantalum or niobium;
the lower end outer sheath 403 is made of steel, titanium, tantalum or niobium;
the lower end ladle cover 404 is made of steel, titanium, tantalum or niobium;
the upper end outer sheath 203 and the upper end sheath cover 204 are assembled by argon arc welding, electric welding or gas welding;
the middle-end outer sheath 301 and the middle-end sheath cover 303 are assembled by argon arc welding, electric welding or gas welding;
the assembly of the lower end outer jacket 403 and the lower end jacket cover 404 is performed by argon arc welding, electric welding or gas welding.
The invention is further illustrated by the following figures and examples.
Example 1
To manufacture a profile size of
The rhenium-niobium composite nozzle (as shown in figure 1) is taken as an example to illustrate the specific implementation mode of the method.
(a) Rhenium powder activation treatment
Selecting 100-mesh high-purity rhenium powder; firstly, reducing rhenium powder in hydrogen with the purity of more than 99.99% for 2 hours at 1000 ℃; then the vacuum is higher than 5 multiplied by 10-3Heat treatment at 1000 ℃ under Pa for 1 hour;
(b) jacket design and assembly
Respectively designing and processing an upper end near-net-shaped die sheath, a middle end near-net-shaped die sheath and a lower end near-net-shaped die sheath of the rhenium-niobium composite spray pipe according to the shape and the size of a pre-prepared rhenium-niobium composite spray pipe (shown in figure 1), wherein the structures of the upper end near-net-shaped die sheath, the middle end near-net-shaped die sheath and the lower end near-net-shaped die sheath are respectively shown in figures 2, 3 and 4;
(c) powder filling and degassing package
Respectively filling the high-purity rhenium powder obtained in the step (a) into the upper end near-net-shaped die sheath, the middle end near-net-shaped die sheath and the lower end in the step (b)After the near-net-shaped mold is fully filled in the sheath and compacted, the sheath cover is covered and welded and fixed; degassing at 750 deg.C for 10 hr via the gas outlet pipe on the cover, and final packaging with vacuum degree higher than 5 × 10-3Pa。
(d) Low temperature hot isostatic pressing
Respectively carrying out hot isostatic pressing on the upper end near-net-shape die sheath, the middle end near-net-shape die sheath and the lower end near-net-shape die sheath obtained in the step (c) at 1250 ℃ for 2 hours and under the pressure of 120MPa, and removing the upper end outer sheath, the upper end core die and the upper end sheath cover to obtain an upper end blank; removing the lower end outer sheath, the lower end core mold and the lower end sheath cover to obtain a lower end blank;
(e) machining the upper and middle ends of the spray pipe
Machining the upper end blank piece and the lower end blank piece obtained in the step (d) according to the size requirement of the spray pipe to obtain the rhenium-niobium composite upper end and the rhenium-niobium composite lower end of the spray pipe;
(f) middle end sheath removal
Sheathing the middle-end near-net-shaped die after the hot isostatic pressing treatment in the step (d), and removing all the middle-end outer sheathing, the middle-end core die and the middle-end sheathing covers by using a machining method to obtain a pure rhenium blank, namely a middle-end blank;
(g) carrying out high-temperature heat treatment and hot isostatic pressing treatment on the middle-end blank;
carrying out heat treatment on the pure rhenium blank obtained in the step (f) for 3 hours at the temperature of 1800 ℃ in a vacuum atmosphere; and hot isostatic pressing the obtained rhenium blank at 1600 ℃ for 2h and under 130 MPa.
(h) Middle end machining
And (g) performing finish machining on the pure rhenium blank obtained in the step (g) according to the external dimension requirement of the rhenium spray pipe to obtain a middle end.
(i) Welding the upper, middle and lower ends
And (e) welding and connecting the upper end and the lower end of the rhenium-niobium composite spray pipe obtained in the step (e) and the middle end obtained in the step (h) through a vacuum electron beam at the welding speed of 0.6m/min, and finally obtaining the required complete rhenium-niobium composite spray pipe.
Example 2
To manufacture a profile size of
The rhenium-niobium composite nozzle (as shown in figure 1) is taken as an example to illustrate the specific implementation mode of the method.
(a) Rhenium powder activation treatment
Selecting high-purity rhenium powder of-100 meshes; firstly, reducing rhenium powder in hydrogen with the purity of more than 99.99% at 900 ℃ for 2.5 hours; then the vacuum is higher than 5 multiplied by 10-3Heat treatment at 1000 ℃ under Pa for 1 hour;
(b) jacket design and assembly
Respectively designing and processing near-net-shaped die jackets at the upper end, the middle end and the lower end of the rhenium-niobium composite spray pipe and niobium alloy components according to the shape and the size of a pre-prepared rhenium-niobium composite spray pipe (as shown in figure 1); the upper, middle and lower die sleeve structures and niobium alloy components required by the rhenium-niobium composite nozzle pipe (shown in figure 1) are respectively shown in figures 2, 3 and 4;
(c) powder filling and degassing package
Filling the high-purity rhenium powder obtained in the step (a) into upper, middle and lower end die casings assembled in the step (b), and covering a casing cover for welding and fixing after the casing cover is fully compacted; degassing the sheath at 800 deg.C for 8 hr via the gas outlet pipe on the sheath cover, and final packaging with vacuum degree higher than 5 × 10-3Pa。
(d) Low temperature hot isostatic pressing
Sheathing the upper, middle and lower ends obtained in the step (c) at 1250 ℃, and hot isostatic pressing for 3 hours at 130 MPa.
(e) Machining the upper and middle ends of the spray pipe
Machining the upper end and the middle end of the rhenium spray pipe obtained in the step (d) according to the size requirement of the spray pipe to obtain the rhenium-niobium composite upper end and the rhenium-niobium composite lower end of the spray pipe;
(f) middle end sheath removal
And (d) removing all sheath materials of the medium-end rhenium spray pipe subjected to the hot isostatic pressing treatment in the step (d) by using a machining method to obtain a pure rhenium blank.
(g) Intermediate ultra high temperature heat treatment and hot isostatic pressing
Carrying out heat treatment on the pure rhenium blank obtained in the step (f) for 2 hours at the temperature of 2000 ℃ in a vacuum atmosphere; and hot isostatic pressing the obtained rhenium blank at 1700 ℃ for 2h and under 130 MPa.
(h) Middle end machining
And (g) carrying out finish machining on the pure rhenium blank obtained in the step (g) according to the external dimension requirement of the rhenium spray pipe.
(i) Welding the upper, middle and lower ends
And (e) connecting the upper end and the lower end of the rhenium-niobium composite spray pipe obtained in the step (e) with the middle end of the spray pipe obtained in the step (h) through vacuum electron beam welding at the welding speed of 1.2m/min, and finally obtaining the required complete rhenium-niobium composite spray pipe.
The rhenium-niobium composite spray pipe prepared by the method is welded with the titanium alloy injector and the niobium alloy extension section to form a body part, and the test run requirement of the product at 2000 ℃ can be met.
The above description is only for the best mode of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Those skilled in the art will appreciate that the invention may be practiced without these specific details.
Claims (8)
1. A sectional preparation method of a rhenium-niobium composite spray pipe is characterized by comprising the following steps: the rhenium-niobium composite spray pipe comprises a head part, a straight line section, a convergence section, a throat part, an expansion section and a tail part; the head part is made of niobium alloy, the tail part is made of niobium alloy, the straight line section, the convergent section, the throat part and the expansion section are made of rhenium, and the rhenium is pure rhenium; the head part is positioned at the top of the straight line segment, the tail part is positioned at the bottom of the expanding segment, and the rhenium-niobium composite spray pipe is divided into three parts, namely an upper end, a middle end and a lower end, wherein the upper end and the lower end are of a rhenium-niobium composite structure, and the middle end is of a rhenium base material; the upper end is a head part and a part of straight line segment, and the lower end is a tail part and a part of expansion segment; the middle end comprises another part of straight line segment, a convergent section, a throat part and another part of expansion section;
the head part is used for welding, and the tail part is used for welding;
the method comprises the following steps:
(a) carrying out activation treatment on the high-purity rhenium powder;
(b) preparing an upper end near net-shaped mold sheath, a middle end near net-shaped mold sheath and a lower end near net-shaped mold sheath;
(c) preparing an upper end, a middle end and a lower end by using the upper end near-net-shape die sheath, the middle end near-net-shape die sheath and the lower end near-net-shape die sheath prepared in the step (b);
(d) connecting the upper end and the middle end obtained in the step (c) and connecting the lower end and the middle end by adopting vacuum electron beam welding or laser welding to obtain a rhenium-niobium composite spray pipe;
in the step (b), the upper-end near-net-shaped die sheath comprises an upper-end outer sheath, an upper-end core die, an upper-end sheath cover and a niobium head, and the upper-end sheath cover is provided with an upper-end air outlet pipe;
the middle-end near-net-shaped mold sheath comprises a middle-end outer sheath, a middle-end core mold and a middle-end sheath cover, and the middle-end sheath cover is provided with a middle-end air outlet pipe;
the lower end near-net-shaped die sleeve comprises a lower end outer sleeve, a lower end core die, a lower end sleeve cover and a niobium tail, and the lower end sleeve cover is provided with a lower end air outlet pipe;
the upper core die is made of pure niobium or niobium alloy;
the middle core die is made of pure niobium or niobium alloy;
the lower core die is made of pure niobium or niobium alloy;
the material of the upper end outer sheath is steel, titanium, tantalum or niobium;
the upper end covering cover is made of steel, titanium, tantalum or niobium;
the middle-end outer sheath is made of steel, titanium, tantalum or niobium;
the middle-end packing cover is made of steel, titanium, tantalum or niobium;
the material of the outer sheath at the lower end is steel, titanium, tantalum or niobium;
the lower end covering cover is made of steel, titanium, tantalum or niobium;
the assembly of the upper end outer sheath and the upper end sheath cover adopts argon arc welding, electric welding or gas welding;
the assembly of the middle-end outer sheath and the middle-end sheath cover adopts argon arc welding, electric welding or gas welding;
the lower end outer sheath and the lower end sheath cover are assembled by argon arc welding, electric welding or gas welding.
2. The sectional preparation method of a rhenium-niobium composite lance according to claim 1, characterized in that: in the step (a), the method for activating the high-purity rhenium powder comprises the following steps:
selecting high-purity rhenium powder of 100-325 meshes; firstly, reducing rhenium powder in hydrogen with the purity of more than 99.99% for 0.5-4 h at the temperature of 800-1050 ℃, and then, ensuring the vacuum degree to be more than 5 multiplied by 10-3Heat treatment is carried out for 0.5-4 h at the temperature of 900-1200 ℃ under Pa.
3. The sectional preparation method of a rhenium-niobium composite lance according to claim 1, characterized in that: the outer surface of the niobium head is provided with a mechanical connection structure, and the outer surface of the niobium tail is provided with a mechanical connection structure.
4. The sectional preparation method of the rhenium-niobium composite nozzle according to claim 3, characterized in that: the connecting structure is a meshing groove structure, a threaded connecting structure or a pin hole structure.
5. The sectional preparation method of a rhenium-niobium composite lance according to claim 1, characterized in that: in the step (c), the method for preparing the upper end by using the upper end near net-shaped die sheath comprises the following steps:
(1) installing an upper end core mold at the bottom of the upper end outer sheath, and then sleeving the niobium head on the upper end core mold;
(2) filling the high-purity rhenium powder obtained in the step (a) into a cavity formed by the outer sheath at the upper end, the head part of the niobium material and the core mould at the upper end, and compacting;
(3) welding and fixing an upper-end sheath cover on the top end of the upper-end outer sheath, degassing through an upper-end gas outlet pipe on the upper-end sheath cover, wherein the degassing temperature is 750-900 ℃, the degassing time is 8-48 h, and the vacuum degree during final packaging is less than 5 multiplied by 10- 3Pa；
(4) Carrying out hot isostatic pressing treatment on the upper-end near-net-shaped die sheath packaged with the high-purity rhenium powder obtained in the step (3), and removing the upper-end outer sheath, the upper-end core die and the upper-end sheath cover after the hot isostatic pressing treatment is finished to obtain an upper-end blank;
the hot isostatic pressing temperature is 1250-1400 ℃, the hot isostatic pressing time is 1-5 h, and the hot isostatic pressing pressure is not less than 110 MPa;
(5) and (4) machining the upper end blank obtained in the step (4) according to the size requirement of the rhenium-niobium composite spray pipe to obtain the upper end.
6. The sectional preparation method of a rhenium-niobium composite lance according to claim 1, characterized in that: in the step (c), the method for preparing the middle end by using the middle end near net-shaped mold sheath comprises the following steps:
(1) mounting the middle-end core mold at the bottom of the middle-end outer sheath;
(2) filling the high-purity rhenium powder obtained in the step (a) into a cavity formed by the middle-end outer sheath and the middle-end core mold, and compacting;
(3) welding and fixing the middle-end sheath cover on the top end of the middle-end outer sheath, degassing through a middle-end air outlet pipe on the middle-end sheath cover, wherein the degassing temperature is 750-900 ℃, the degassing time is 8-48 h, and the vacuum degree in final packaging is less than 5 multiplied by 10-3Pa；
(4) Carrying out hot isostatic pressing treatment on the middle-end near-net-shaped die sheath packaged with the high-purity rhenium powder obtained in the step (3), and removing the middle-end outer sheath, the middle-end core die and the middle-end sheath cover by using a mechanical processing or chemical milling method after the hot isostatic pressing treatment is finished to obtain a middle-end pure rhenium blank;
the hot isostatic pressing temperature is 1250-1400 ℃, the hot isostatic pressing time is 1-5 h, and the hot isostatic pressing pressure is not less than 110 MPa;
(5) performing high-temperature heat treatment on the medium-end rhenium blank obtained in the step (4), and then performing high-temperature hot isostatic pressing treatment, wherein the high-temperature heat treatment atmosphere is vacuum or hydrogen atmosphere, the high-temperature heat treatment temperature is 1800-2600 ℃, the high-temperature heat treatment time is 0.5-6 h, the high-temperature hot isostatic pressing treatment temperature is 1600-2000 ℃, the high-temperature hot isostatic pressing treatment time is 1-4 h, and the high-temperature hot isostatic pressing treatment pressure is 130-200 MPa;
(6) and (4) machining the medium-end pure rhenium blank treated in the step (5) according to the size requirement of the rhenium-niobium composite spray pipe to obtain the medium end.
7. The sectional preparation method of a rhenium-niobium composite lance according to claim 1, characterized in that: in the step (c), the method for preparing the lower end by using the lower end near net-shaped die sheath comprises the following steps:
(1) mounting a lower end core mold at the bottom of the lower end outer sheath, and then sleeving the tail part of the niobium material on the lower end core mold;
(2) filling the high-purity rhenium powder obtained in the step (a) into a cavity formed by the lower-end outer sheath, the niobium tail and the lower-end core mold, and compacting;
(3) welding and fixing the lower-end sheath cover on the top end of the lower-end outer sheath, and degassing through a lower-end gas outlet pipe on the lower-end sheath cover at the degassing temperature of 750-900 ℃ for 8-48 h, wherein the vacuum degree during final packaging is less than 5 multiplied by 10-3Pa；
(4) Carrying out hot isostatic pressing treatment on the lower end near-net-shaped die sheath packaged with the high-purity rhenium powder obtained in the step (3), and removing the lower end outer sheath, the lower end core die and the lower end sheath cover after the hot isostatic pressing treatment is finished to obtain a lower end blank;
the hot isostatic pressing temperature is 1250-1400 ℃, the hot isostatic pressing time is 1-5 h, and the hot isostatic pressing pressure is not less than 110 MPa;
(5) and (4) machining the lower end blank obtained in the step (4) according to the size requirement of the rhenium-niobium composite spray pipe to obtain the lower end.
8. The sectional preparation method of a rhenium-niobium composite lance according to claim 1, characterized in that: in the step (d), the welding speed is 0.5-3 m/min.
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