CN109807338A - A kind of segmented preparation method of rhenium niobium Composite Nozzle - Google Patents
A kind of segmented preparation method of rhenium niobium Composite Nozzle Download PDFInfo
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- CN109807338A CN109807338A CN201910073664.3A CN201910073664A CN109807338A CN 109807338 A CN109807338 A CN 109807338A CN 201910073664 A CN201910073664 A CN 201910073664A CN 109807338 A CN109807338 A CN 109807338A
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Abstract
The present invention relates to a kind of segmented preparation methods of rhenium niobium Composite Nozzle, belong to refractory metal material powder metallurgy preparation technology field.It include niobium alloy component in the forming jacket of top and bottom in the present invention to shape rhenium niobium composite portion.The jacket for being loaded into rhenium powder first passes through Low Temperature Thermal hydrostatic pressing, has some strength after rhenium component blank is shaped at this time and consistency reaches 99% or more, because the rhenium niobium transition region of upper and lower part is in the low-temperature space of jet pipe work, can directly shape；And the rhenium matrix of middle-end, then it is further densified through high temperature sintering post-processing again and improves metallurgical bonding intensity, so that mechanical property is reached service demand, then machined after forming.The jet pipe upper, middle and lower end after machining is finally become into a complete rhenium niobium Composite Nozzle by vacuum electron beam welding.
Description
Technical field
The present invention relates to a kind of segmented preparation methods of rhenium niobium Composite Nozzle, belong to refractory metal material powder metallurgy system
Standby technical field, provides a kind of rhenium niobium hybrid engine jet pipe method for preparing powder metallurgy, can be used for high-performance rhenium iridium and start
The development of machine, the propulsion system applied to spacecrafts such as satellites.
Background technique
Rhenium melting point metal high (3180 DEG C) has good high/low temperature mechanical property, using rhenium as the height of matrix iridium making coatings
Performance rhenium iridium engine chamber operating temperature can be applied to the advanced engine of satellite, spacecraft up to 2000 DEG C or more
On.The straightway needs of usual such combustion chamber are mutually welded with titanium alloy ejector filler, and the expansion segment of combustion chamber needs and niobium alloy
Extended segment is welded, but since rhenium material melting point is high, rhenium metal and the welded connecting difficulty of other metals are big, weldquality
It is difficult to ensure, therefore usually first prepares rhenium niobium transition connection on the head of the combustion chamber and tail portion when rhenium is connect with other metals,
Preferable welding assembly is realized by niobium alloy and other metals again.
Rhenium niobium transition connection uses chemical vapor deposition (CVD) method earliest, rhenium matrix is shaped out, in rhenium surface chemistry gas
Mutually deposition niobium layer, the method long preparation period, costly, production efficiency is low.Later someone uses prior powder metallurgy metallurgy one
Body forming technology prepares rhenium niobium composite combustion chamber, but since rhenium material melting point is high, usual rhenium powder metallurgy hot isostatic pressing (HIP) is caused
Densification forming is needed at 1500 DEG C or more, and niobium alloy can sharply deteriorate in 1400 DEG C or more process performances, causes to prepare
Rhenium niobium bonding strength is low.
Summary of the invention
Technology of the invention solves the problems, such as: overcome the deficiencies in the prior art, proposes a kind of segmentation of rhenium niobium Composite Nozzle
Formula preparation method.
The technical solution of the invention is as follows:
A kind of segmented preparation method of rhenium niobium Composite Nozzle, the rhenium niobium Composite Nozzle includes head, straightway, receipts
Hold back section, throat, expansion segment and tail portion；Head be niobium alloy material, tail portion be niobium alloy material, straightway, converging portion, throat and
Expansion segment is rhenium material；Head is located at the top of straightway, and tail portion is located at the bottom of expansion segment, which is divided into
Three parts, respectively upper end, middle-end and lower end, upper end, lower end are rhenium niobium composite construction, and middle-end is rhenium substrate；Upper end is head
With a part of straightway, lower end is tail portion and a part of expansion segment；Middle-end include another part straightway, converging portion, throat and
Another part expansion segment；
Head is for welding, and tail portion is for welding；
The step of this method includes:
(a) high-purity rhenium powder is activated；
(b) upper end near net-shape mold jacket, middle-end near net-shape mold jacket and lower end near net-shape mold jacket are prepared；
(c) near net-shaped using the upper end near net-shape mold jacket, middle-end near net-shape mold jacket and lower end of step (b) preparation
Mold jacket prepares upper end, middle-end and lower end；
(d) upper end that step (c) obtains is all made of electron-bombardment welding with middle-end, lower end and middle-end or Laser Welding connects
It connects, obtains rhenium niobium Composite Nozzle.
In the step (a), method that high-purity rhenium powder is activated are as follows:
Select 100 mesh~325 mesh high-purity rhenium powder；First by rhenium powder purity greater than 99.99% hydrogen in 800 DEG C~
1050 DEG C of 0.5~4h of reduction treatment, then it is higher than 5 × 10 in vacuum degree-3Lower 900 DEG C~1200 DEG C 0.5~4h of heat treatment of Pa.
In the step (b), upper end near net-shape mold jacket includes jacket outside upper end, upper end core model, upper end jacket lid
With niobium material head, upper end jacket is covered with upper end escape pipe；
Middle-end near net-shape mold jacket includes middle-end outer jacket, middle-end core model, middle-end jacket lid, and middle-end jacket, which covers, to be had
Middle-end escape pipe；
Lower end near net-shape mold jacket includes jacket outside lower end, lower end core model, lower end jacket lid and niobium material tail portion, lower end
Jacket is covered with lower end escape pipe.
The outer surface on niobium material head has mechanical connecting structure, and the outer surface of niobium material tail portion is with mechanical connection knot
Structure.
Connection structure is ratcheting groove structure, screw connection structure or pin pore structure.
In the step (b), the material of upper end core model is pure niobium or niobium alloy；
The material of middle-end core model is pure niobium or niobium alloy；
The material of lower end core model is pure niobium or niobium alloy；
The material of jacket is steel, titanium, tantalum or niobium material outside upper end；
The material of upper end jacket lid is steel, titanium, tantalum or niobium material；
The material of the outer jacket of middle-end is steel, titanium, tantalum or niobium material；
The material of middle-end jacket lid is steel, titanium, tantalum or niobium material；
The material of jacket is steel, titanium, tantalum or niobium material outside lower end；
The material of lower end jacket lid is steel, titanium, tantalum or niobium material；
The assembling of jacket and upper end jacket lid uses argon arc welding, electric welding or gas welding outside upper end；
The assembling of the outer jacket of middle-end and middle-end jacket lid uses argon arc welding, electric welding or gas welding；
Assembling argon arc welding, electric welding or the gas welding of jacket and lower end jacket lid outside lower end.
In the step (c), the method for upper end near net-shape mold jacket preparation upper end is utilized are as follows:
(1) upper end core model is mounted on to the bottom of jacket outside upper end, then covers on niobium material head on the core model of upper end；
(2) high-purity rhenium powder for obtaining step (a) is packed full with jacket and niobium material head, upper end core model outside upper end and is formed
In cavity, and jolt ramming；
(3) upper end jacket lid is weldingly fixed on to the top of jacket outside upper end, the upper end outlet covered by upper end jacket
Pipe carries out degasification, and outgassing temperature is 750~900 DEG C, and the degasification time is 8~48h, and vacuum degree when final encapsulation is less than 5 ×
10-3Pa；
(4) the upper end near net-shape mold jacket for being packaged with high-purity rhenium powder for obtaining step (3) carries out hip treatment,
Jacket, upper end core model, upper end jacket lid outside upper end are removed after hip treatment, obtain upper end blank；
Hip treatment temperature is 1250 DEG C~1400 DEG C, and the hip treatment time is 1~5h, hip treatment
Pressure >=110MPa；
(5) the upper end blank that step (4) obtains is machined by the size requirement of rhenium niobium Composite Nozzle, is obtained
End.
In the step (c), the method for middle-end near net-shape mold jacket preparation middle-end is utilized are as follows:
(1) middle-end core model is mounted on to the bottom of jacket outside middle-end；
(2) high-purity rhenium powder for obtaining step (a) is packed full in the cavity that the outer jacket of middle-end and middle-end core model are formed, and is shaken
It is real；
(3) middle-end jacket lid is weldingly fixed on to the top of jacket outside middle-end, the middle-end outlet covered by middle-end jacket
Pipe carries out degasification, and outgassing temperature is 750~900 DEG C, and the degasification time is 8~48h, and vacuum degree when final encapsulation is less than 5 × 10- 3Pa；
(4) the middle-end near net-shape mold jacket for being packaged with high-purity rhenium powder for obtaining step (3) carries out hip treatment,
Method removal middle-end outer jacket, middle-end core model, the middle-end jacket of machining or chemistry milling are utilized after hip treatment
Lid, obtains the pure rhenium blank of middle-end；
Hip treatment temperature is 1250 DEG C~1400 DEG C, and the hip treatment time is 1~5h, hip treatment
Pressure >=110MPa；
(5) the middle-end rhenium blank that step (4) obtains is subjected to high-temperature heat treatment again, is then carried out at high temperature hot isostatic pressing again
Reason, high-temperature heat treatment atmosphere are in vacuum or hydrogen atmosphere, at 1800 DEG C~2600 DEG C of high-temperature heat treatment temperature, high-temperature heat treatment
0.5~6h of time, 1600 DEG C~2000 DEG C of high temperature hip treatment temperature, 1~4h of high temperature hip treatment time, high temperature
Hip treatment pressure is 130MPa~200MPa；
(6) step (5) treated the pure rhenium blank of middle-end is machined out by the size requirement of rhenium niobium Composite Nozzle, is obtained
To middle-end；
In the step (c), the method for lower end near net-shape mold jacket preparation lower end is utilized are as follows:
(1) lower end core model is mounted on to the bottom of jacket outside lower end, then covers niobium material tail portion on the core model of lower end；
(2) high-purity rhenium powder for obtaining step (a) is packed full with jacket and niobium material tail portion, lower end core model outside lower end and is formed
In cavity, and jolt ramming；
(3) lower end jacket lid is weldingly fixed on to the top of jacket outside lower end, the lower end outlet covered by lower end jacket
Pipe carries out degasification, and outgassing temperature is 750~900 DEG C, and the degasification time is 8~48h, and vacuum degree when final encapsulation is less than 5 × 10- 3Pa；
(4) the lower end near net-shape mold jacket for being packaged with high-purity rhenium powder for obtaining step (3) carries out hip treatment,
Jacket, lower end core model, lower end jacket lid outside lower end are removed after hip treatment, obtain lower end blank；
Hip treatment temperature is 1250 DEG C~1400 DEG C, and the hip treatment time is 1~5h, hip treatment
Pressure >=110MPa；
(5) the lower end blank that step (4) obtains is machined by the size requirement of rhenium niobium Composite Nozzle, is obtained down
End.
In the step (d), speed of welding is 0.5~3m/min.
Beneficial effect
(1) present invention, which prepares rhenium niobium Composite Nozzle both using powder metallurgy segmented forming technology, can obtain high intensity
Rhenium matrix, and chemical vapour deposition technique and prior powder metallurgy technique is overcome to prepare the problems that rhenium niobium transition connects, and its
Forming efficiency is high, at low cost.
(2) the present invention relates to a kind of manufacturing process for preparing rhenium niobium composite combustion chamber rhenium component, comprising steps of first will be high
Pure rhenium powder handles removal oxide on surface by Hydrogen activation, then will it is processed after rhenium powder be fitted into near-net-shape jacket,
It include niobium alloy component in the forming jacket of middle top and bottom to shape rhenium niobium composite portion.It is loaded into the jacket of rhenium powder
First pass through Low Temperature Thermal hydrostatic pressing, have after rhenium component blank is shaped at this time some strength and consistency reach 99% with
On, because the rhenium niobium transition region of upper and lower part is in the low-temperature space of jet pipe work, can directly shape；And the rhenium base of middle-end
Body then further densifies again through high temperature sintering post-processing and improves metallurgical bonding intensity, mechanical property is made to reach service demand,
It is machined after forming again.The jet pipe upper, middle and lower end after machining is finally become into a complete rhenium by vacuum electron beam welding
Niobium Composite Nozzle.The rhenium niobium Composite Nozzle of this programme preparation, that is, have high-intensitive rhenium matrix, in turn avoid high-temperature process to rhenium
The destruction of niobium transition region and niobium alloy performance.
Detailed description of the invention
Fig. 1 is rhenium niobium Composite Nozzle structural schematic diagram, wherein 101- niobium alloy area, 102- rhenium alloys area, 103- rhenium niobium mistake
Cross area, 104- rhenium niobium Composite Nozzle upper end, 105- rhenium niobium Composite Nozzle middle-end, 106- rhenium niobium Composite Nozzle lower end；
Fig. 2 is upper end near net-shape mold wrapping structure schematic diagram；Wherein, 201- niobium alloy head, the upper end 202- core model,
Jacket, the upper end 204- jacket lid, the upper end 205- escape pipe outside the upper end 203-；
Fig. 3 is middle-end near net-shape mold wrapping structure schematic diagram；Wherein, the outer jacket of 301- middle-end, 302- middle-end core model,
303- middle-end jacket lid, 304- middle-end escape pipe；
Fig. 4 be lower end near net-shape mold wrapping structure schematic diagram, wherein 401- niobium alloy tail portion, the lower end 402- core model,
Jacket, the lower end 404- jacket lid, the lower end 405- escape pipe outside the lower end 403-.
Specific embodiment
A kind of segmented preparation method of rhenium niobium Composite Nozzle, the rhenium niobium Composite Nozzle includes head, straightway, receipts
Hold back section, throat, expansion segment and tail portion；Head be niobium alloy material, tail portion be niobium alloy material, straightway, converging portion, throat and
Expansion segment is rhenium material；Head is located at the top of straightway, and tail portion is located at the bottom of expansion segment, which is divided into
Three parts, respectively upper end, middle-end and lower end, upper end, lower end are rhenium niobium composite construction, and middle-end is rhenium substrate；Upper end is head
With a part of straightway, lower end is tail portion and a part of expansion segment；Middle-end include another part straightway, converging portion, throat and
Another part expansion segment；
Head is for welding, and tail portion is for welding；
The step of this method includes:
(a) high-purity rhenium powder is activated；
Select 100 mesh~325 mesh high-purity rhenium powder；First by rhenium powder purity greater than 99.99% hydrogen in 800 DEG C~
1050 DEG C of 0.5~4h of reduction treatment, then it is higher than 5 × 10 in vacuum degree-3Lower 900 DEG C~1200 DEG C 0.5~4h of heat treatment of Pa；
(b) upper end near net-shape mold jacket, middle-end near net-shape mold jacket and lower end near net-shape mold jacket are prepared；
Upper end near net-shape mold jacket includes jacket 203 outside upper end, upper end core model 202, upper end jacket lid 204 and niobium material
Head 201 has upper end escape pipe 205 on upper end jacket lid 204；
Middle-end near net-shape mold jacket includes middle-end outer jacket 301, middle-end core model 302, middle-end jacket lid 303, middle-end packet
Middle-end escape pipe 304 is had on upper shield 303；
Lower end near net-shape mold jacket includes jacket 403 outside lower end, lower end core model 402, lower end jacket lid 404 and niobium material
Tail portion 401 has lower end escape pipe 405 on lower end jacket lid 404；
The outer surface on niobium material head 201 have mechanical connecting structure, such as ratcheting groove structure, screw connection structure or
The connecting portion of pin pore structure, i.e. niobium material head 201 and straightway has mechanical connecting structure, for increasing niobium material head
The bonding strength in portion 201 and straightway；
The outer surface of niobium material tail portion 401 have mechanical connecting structure, such as ratcheting groove structure, screw connection structure or
The connecting portion of pin pore structure, i.e. niobium material tail portion 401 and expansion segment has mechanical connecting structure, for increasing niobium material tail
The bonding strength in portion 401 and expansion segment；
(c) upper end, middle-end and lower end are prepared；
Upper end the preparation method comprises the following steps:
(1) upper end core model 202 is mounted on to the bottom of jacket 203 outside upper end, then by 201 sets of niobium material head in upper end
On core model 202；
(2) high-purity rhenium powder for obtaining step (a) is packed full with jacket 203 and niobium material head 201, upper end core model outside upper end
In 202 cavitys formed, and jolt ramming；
(3) upper end jacket lid 204 is weldingly fixed on to the top of jacket 203 outside upper end, by upper end jacket lid 204
Upper end escape pipe 205 carries out degasification, and outgassing temperature is 750~900 DEG C, and the degasification time is 8~48h, vacuum when final encapsulation
Degree is less than 5 × 10-3Pa；
(4) the upper end near net-shape mold jacket for being packaged with high-purity rhenium powder for obtaining step (3) carries out hip treatment,
Jacket 203, upper end core model 202, upper end jacket lid 204 outside upper end are removed after hip treatment, obtain upper end blank；
Hip treatment temperature is 1250 DEG C~1400 DEG C, and the hip treatment time is 1~5h, hip treatment
Pressure >=110MPa；
(5) the upper end blank that step (4) obtains is machined by the size requirement of rhenium niobium Composite Nozzle, is obtained
End.
Middle-end the preparation method comprises the following steps:
(1) middle-end core model 302 is mounted on to the bottom of jacket 301 outside middle-end；
(2) high-purity rhenium powder for obtaining step (a) is packed full with the cavity that the outer jacket 301 of middle-end is formed with middle-end core model 302
In, and jolt ramming；
(3) middle-end jacket lid 303 is weldingly fixed on to the top of jacket 301 outside middle-end, by middle-end jacket lid 303
Middle-end escape pipe 304 carries out degasification, and outgassing temperature is 750~900 DEG C, and the degasification time is 8~48h, vacuum when final encapsulation
Degree is less than 5 × 10-3Pa；
(4) the middle-end near net-shape mold jacket for being packaged with high-purity rhenium powder for obtaining step (3) carries out hip treatment,
After hip treatment using the outer jacket 301 of method removal middle-end of machining or chemistry milling, middle-end core model 302, in
Jacket lid 303 is held, the pure rhenium blank of middle-end is obtained；
Hip treatment temperature is 1250 DEG C~1400 DEG C, and the hip treatment time is 1~5h, hip treatment
Pressure >=110MPa；
(5) the middle-end rhenium blank that step (4) obtains is subjected to high-temperature heat treatment again, is then carried out at high temperature hot isostatic pressing again
Reason, high-temperature heat treatment atmosphere are in vacuum or hydrogen atmosphere, at 1800 DEG C~2600 DEG C of high-temperature heat treatment temperature, high-temperature heat treatment
0.5~6h of time, 1600 DEG C~2000 DEG C of high temperature hip treatment temperature, 1~4h of high temperature hip treatment time, high temperature
Hip treatment pressure is 130MPa~200MPa；
(6) step (5) treated the pure rhenium blank of middle-end is machined out by the size requirement of rhenium niobium Composite Nozzle, is obtained
To middle-end；
Lower end the preparation method comprises the following steps:
(1) lower end core model 402 is mounted on to the bottom of jacket 403 outside lower end, then by 401 sets of niobium material tail portion in lower end
On core model 402；
(2) high-purity rhenium powder for obtaining step (a) is packed full with jacket 403 and niobium material tail portion 401, lower end core model outside lower end
In 402 cavitys formed, and jolt ramming；
(3) lower end jacket lid 404 is weldingly fixed on to the top of jacket 403 outside lower end, under leading on lower end jacket lid 404
It brings out tracheae 405 and carries out degasification, outgassing temperature is 750~900 DEG C, and the degasification time is 8~48h, vacuum degree when final encapsulation
Less than 5 × 10-3Pa；
(4) the lower end near net-shape mold jacket for being packaged with high-purity rhenium powder for obtaining step (3) carries out hip treatment,
Jacket 403, lower end core model 402, lower end jacket lid 404 outside lower end are removed after hip treatment, obtain lower end blank；
Hip treatment temperature is 1250 DEG C~1400 DEG C, and the hip treatment time is 1~5h, hip treatment
Pressure >=110MPa；
(5) the lower end blank that step (4) obtains is machined by the size requirement of rhenium niobium Composite Nozzle, is obtained down
End.
(d) upper end that step (c) obtains is all made of electron-bombardment welding with middle-end, lower end and middle-end or Laser Welding connects
It connects, speed of welding is 0.5~3m/min, obtains rhenium niobium Composite Nozzle.
In the step (b), the material of upper end core model 202 is pure niobium or niobium alloy (such as niobium hafnium alloy or the conjunction of niobium tungsten
Gold)；
The material of middle-end core model 302 is pure niobium or niobium alloy (such as niobium hafnium alloy or niobium tungsten alloy)；
The material of lower end core model 402 is pure niobium or niobium alloy (such as niobium hafnium alloy or niobium tungsten alloy)；
The material of jacket 203 is steel, titanium, tantalum or niobium material outside upper end；
The material of upper end jacket lid 204 is steel, titanium, tantalum or niobium material；
The material of the outer jacket 301 of middle-end is steel, titanium, tantalum or niobium material；
The material of middle-end jacket lid 303 is steel, titanium, tantalum or niobium material；
The material of jacket 403 is steel, titanium, tantalum or niobium material outside lower end；
The material of lower end jacket lid 404 is steel, titanium, tantalum or niobium material；
The assembling of jacket 203 and upper end jacket lid 204 uses argon arc welding, electric welding or gas welding outside upper end；
The outer jacket 301 of middle-end and the assembling of middle-end jacket lid 303 use argon arc welding, electric welding or gas welding；
Assembling argon arc welding, electric welding or the gas welding of jacket 403 and lower end jacket lid 404 outside lower end.
Present invention will be further explained below with reference to the attached drawings and examples.
Embodiment 1
It is to manufacture a kind of overall sizeFor rhenium niobium Composite Nozzle (such as Fig. 1), illustrate the present invention
The specific embodiment of method.
(a) activation processing of rhenium powder
Select the high-purity rhenium powder of 100 mesh；First by the 1000 DEG C of reduction treatments in hydrogen of the purity greater than 99.99% of rhenium powder
2 hours；It is higher than 5 × 10 in vacuum again-3Lower 1000 DEG C of Pa are heat-treated 1 hour；
(b) jacket design and assembling
According to pre-prepared rhenium niobium Composite Nozzle (such as Fig. 1) shape of product, size, the compound spray of rhenium niobium is separately designed and processed
Upper end near net-shape mold jacket, middle-end near net-shape mold jacket and the lower end near net-shape mold jacket of pipe, upper end near net-shape mold
The structure of jacket, middle-end near net-shape mold jacket and lower end near net-shape mold jacket is respectively as shown in Fig. 2,3 and 4；
(c) dress powder and degasification encapsulate
High-purity rhenium powder obtained by step (a) is loaded into upper end near net-shape mold jacket in step (b), middle-end near net respectively
In shape mold jacket, lower end near net-shape mold jacket, after filling jolt ramming, covers jacket lid and be welded and fixed；Band is covered by jacket
Some escape pipes, to being wrapped in 750 DEG C of progress degasification, degasification 10 hours, vacuum degree was higher than 5 × 10 when final encapsulation-3Pa。
(d) Low Temperature Thermal hydrostatic pressing
By step (c) near net-shape mold jacket in upper end obtained, middle-end near net-shape mold jacket, lower end near net-shape mold
Jacket removes jacket, upper end core model and upper end jacket lid outside upper end respectively at 1250 DEG C, hot isostatic pressing 2 hours, pressure 120MPa
Afterwards, upper end blank is obtained；Outside removal lower end after jacket, lower end core model and lower end jacket lid, lower end blank is obtained；
(e) on jet pipe, middle-end processing
By step (d) upper end blank obtained and lower end blank, pass through machining by the size requirement of jet pipe
Obtain the compound top and bottom of rhenium niobium of jet pipe；
(f) middle-end jacket removes
By the middle-end near net-shape mold jacket after step (d) hip treatment, institute is removed using the method for machining
There are the outer jacket of middle-end, middle-end core model and middle-end jacket lid, obtains pure rhenium blank i.e. middle-end blank；
(g) middle-end blank high-temperature heat treatment and hip treatment；
By step (f) pure rhenium blank obtained, in vacuum atmosphere, at 1800 DEG C of temperature, it is heat-treated 3 hours；Again will
Rhenium blank obtained is at 1600 DEG C, hot isostatic pressing 2h, pressure 130MPa.
(h) middle-end is machined
It by step (g) pure rhenium blank obtained, requires to be finished according to the outer dimension of rhenium jet pipe, obtain
End.
(i) upper, middle and lower end welding forming
Middle-end obtained in the upper end, lower end of rhenium niobium Composite Nozzle obtained in step (e) and step (h) is passed through
Vacuum electron beam welding connection, speed of welding 0.6m/min are final to obtain required complete rhenium niobium Composite Nozzle.
Embodiment 2
It is to manufacture a kind of overall sizeFor rhenium niobium Composite Nozzle (such as Fig. 1), illustrate the present invention
The specific embodiment of method.
(a) activation processing of rhenium powder
Select the high-purity rhenium powder of -100 mesh；First by the 900 DEG C of reduction treatments in hydrogen of the purity greater than 99.99% of rhenium powder
2.5 hour；It is higher than 5 × 10 in vacuum again-3Lower 1000 DEG C of Pa are heat-treated 1 hour；.
(b) jacket design and assembling
According to pre-prepared rhenium niobium Composite Nozzle (such as Fig. 1) shape of product, size, the compound spray of rhenium niobium is separately designed and processed
Pipe upper, middle and lower end near net-shape mold jacket and niobium alloy component；Upper, middle and lower mold packet needed for rhenium niobium Composite Nozzle (such as Fig. 1)
Nested structure and niobium alloy component are respectively as shown in Fig. 2,3 and 4；
(c) dress powder and degasification encapsulate
High-purity rhenium powder obtained by step (a) is loaded into step (b) in assembled upper, middle and lower terminal mould jacket, is filled
After jolt ramming, covers jacket lid and be welded and fixed；The escape pipe having is covered by jacket, to being wrapped in 800 DEG C of progress degasification, degasification
8 hours, vacuum degree was higher than 5 × 10 when final encapsulation-3Pa。
(d) Low Temperature Thermal hydrostatic pressing
Step (c) upper, middle and lower end obtained is wrapped in 1250 DEG C, hot isostatic pressing 3 hours, pressure 130MPa.
(e) on jet pipe, middle-end processing
By on step (d) rhenium jet pipe obtained, middle-end, jet pipe is obtained by machining by the size requirement of jet pipe
The compound top and bottom of rhenium niobium；
(f) middle-end jacket removes
By the middle-end rhenium jet pipe of step (d) hip treatment, all sheath materials are removed using the method for machining,
Obtain pure rhenium blank.
(g) heat treatment of middle-end superhigh temperature and hot isostatic pressing
By step (f) pure rhenium blank obtained, in vacuum atmosphere, at 2000 DEG C of temperature, it is heat-treated 2 hours；Again will
Rhenium blank obtained is at 1700 DEG C, hot isostatic pressing 2h, pressure 130MPa.
(h) middle-end is machined
By step (g) pure rhenium blank obtained, require to be finished according to the outer dimension of rhenium jet pipe.
(i) upper, middle and lower end welding forming
Jet pipe middle-end obtained in the upper and lower end of rhenium niobium Composite Nozzle obtained in step (e) and step (h) is logical
Vacuum electron beam welding connection is crossed, speed of welding 1.2m/min is final to obtain required complete rhenium niobium Composite Nozzle.
The rhenium niobium Composite Nozzle prepared by approach described above, then welded with titanium alloy ejector filler and niobium alloy extended segment
The body portion formed afterwards can meet the test run requirement of 2000 DEG C of the product.
The above, optimal specific embodiment only of the invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
The content that description in the present invention is not described in detail belongs to the well-known technique of professional and technical personnel in the field.
Claims (10)
1. a kind of segmented preparation method of rhenium niobium Composite Nozzle, it is characterised in that: the rhenium niobium Composite Nozzle include head,
Straightway, converging portion, throat, expansion segment and tail portion；Head is niobium alloy material, and tail portion is niobium alloy material, straightway, convergence
Section, throat and expansion segment are rhenium material；Head is located at the top of straightway, and tail portion is located at the bottom of expansion segment, which is answered
It closes jet pipe and is divided into three parts, respectively upper end, middle-end and lower end, upper end, lower end are rhenium niobium composite construction, and middle-end is rhenium substrate；
Upper end is head and a part of straightway, and lower end is tail portion and a part of expansion segment；Middle-end includes another part straightway, convergence
Section, throat and another part expansion segment；
Head is for welding, and tail portion is for welding；
The step of this method includes:
(a) high-purity rhenium powder is activated；
(b) upper end near net-shape mold jacket, middle-end near net-shape mold jacket and lower end near net-shape mold jacket are prepared；
(c) upper end near net-shape mold jacket, middle-end near net-shape mold jacket and the lower end near net-shape mold of step (b) preparation are utilized
Jacket prepares upper end, middle-end and lower end；
(d) upper end that step (c) obtains is all made of electron-bombardment welding with middle-end, lower end and middle-end or Laser Welding is connect, obtained
To rhenium niobium Composite Nozzle.
2. a kind of segmented preparation method of rhenium niobium Composite Nozzle according to claim 1, it is characterised in that: the step
Suddenly in (a), method that high-purity rhenium powder is activated are as follows:
Select 100 mesh~325 mesh high-purity rhenium powder；First by rhenium powder 800 DEG C~1050 in hydrogen of the purity greater than 99.99%
DEG C 0.5~4h of reduction treatment, then it is higher than 5 × 10 in vacuum degree-3Lower 900 DEG C~1200 DEG C 0.5~4h of heat treatment of Pa.
3. a kind of segmented preparation method of rhenium niobium Composite Nozzle according to claim 1, it is characterised in that: the step
Suddenly in (b), upper end near net-shape mold jacket includes jacket outside upper end, upper end core model, upper end jacket lid and niobium material head, upper end
Jacket is covered with upper end escape pipe；
Middle-end near net-shape mold jacket includes middle-end outer jacket, middle-end core model, middle-end jacket lid, and middle-end jacket is covered with middle-end
Escape pipe；
Lower end near net-shape mold jacket includes jacket outside lower end, lower end core model, lower end jacket lid and niobium material tail portion, lower end jacket
It covers with lower end escape pipe.
4. a kind of segmented preparation method of rhenium niobium Composite Nozzle according to claim 3, it is characterised in that: niobium material head
The outer surface in portion has mechanical connecting structure, and the outer surface of niobium material tail portion has mechanical connecting structure.
5. a kind of segmented preparation method of rhenium niobium Composite Nozzle according to claim 4, it is characterised in that: connection structure
For ratcheting groove structure, screw connection structure or pin pore structure.
6. a kind of segmented preparation method of rhenium niobium Composite Nozzle according to claim 1, it is characterised in that: the step
Suddenly in (b), the material of upper end core model is pure niobium or niobium alloy；
The material of middle-end core model is pure niobium or niobium alloy；
The material of lower end core model is pure niobium or niobium alloy；
The material of jacket is steel, titanium, tantalum or niobium material outside upper end；
The material of upper end jacket lid is steel, titanium, tantalum or niobium material；
The material of the outer jacket of middle-end is steel, titanium, tantalum or niobium material；
The material of middle-end jacket lid is steel, titanium, tantalum or niobium material；
The material of jacket is steel, titanium, tantalum or niobium material outside lower end；
The material of lower end jacket lid is steel, titanium, tantalum or niobium material；
The assembling of jacket and upper end jacket lid uses argon arc welding, electric welding or gas welding outside upper end；
The assembling of the outer jacket of middle-end and middle-end jacket lid uses argon arc welding, electric welding or gas welding；
Assembling argon arc welding, electric welding or the gas welding of jacket and lower end jacket lid outside lower end.
7. a kind of segmented preparation method of rhenium niobium Composite Nozzle according to claim 3, it is characterised in that: the step
Suddenly in (c), the method for upper end near net-shape mold jacket preparation upper end is utilized are as follows:
(1) upper end core model is mounted on to the bottom of jacket outside upper end, then covers on niobium material head on the core model of upper end；
(2) high-purity rhenium powder for obtaining step (a) is packed full with the cavity that jacket and niobium material head, upper end core model are formed outside upper end
In, and jolt ramming；
(3) upper end jacket lid is weldingly fixed on to the top of jacket outside upper end, the upper end escape pipe covered by upper end jacket into
Row degasification, outgassing temperature are 750~900 DEG C, and the degasification time is 8~48h, and vacuum degree when final encapsulation is less than 5 × 10- 3Pa；
(4) the upper end near net-shape mold jacket for being packaged with high-purity rhenium powder for obtaining step (3) carries out hip treatment, heat etc.
Static pressure after treatment removes jacket, upper end core model, upper end jacket lid outside upper end, obtains upper end blank；
Hip treatment temperature is 1250 DEG C~1400 DEG C, and the hip treatment time is 1~5h, hip treatment pressure
≥110MPa；
(5) the upper end blank that step (4) obtains is machined by the size requirement of rhenium niobium Composite Nozzle, obtains upper end.
8. a kind of segmented preparation method of rhenium niobium Composite Nozzle according to claim 3, it is characterised in that: the step
Suddenly in (c), the method for middle-end near net-shape mold jacket preparation middle-end is utilized are as follows:
(1) middle-end core model is mounted on to the bottom of jacket outside middle-end；
(2) high-purity rhenium powder for obtaining step (a) is packed full in the cavity that the outer jacket of middle-end and middle-end core model are formed, and jolt ramming；
(3) middle-end jacket lid is weldingly fixed on to the top of jacket outside middle-end, the middle-end escape pipe covered by middle-end jacket into
Row degasification, outgassing temperature are 750~900 DEG C, and the degasification time is 8~48h, and vacuum degree when final encapsulation is less than 5 × 10-3Pa；
(4) the middle-end near net-shape mold jacket for being packaged with high-purity rhenium powder for obtaining step (3) carries out hip treatment, heat etc.
Static pressure after treatment is obtained using method removal middle-end outer jacket, middle-end core model, the middle-end jacket lid of machining or chemistry milling
To the pure rhenium blank of middle-end；
Hip treatment temperature is 1250 DEG C~1400 DEG C, and the hip treatment time is 1~5h, hip treatment pressure
≥110MPa；
(5) the middle-end rhenium blank that step (4) obtains is subjected to high-temperature heat treatment again, then carries out high temperature hip treatment again,
High-temperature heat treatment atmosphere is in vacuum or hydrogen atmosphere, at 1800 DEG C~2600 DEG C of high-temperature heat treatment temperature, when high-temperature heat treatment
Between 0.5~6h, 1600 DEG C~2000 DEG C of high temperature hip treatment temperature, high temperature hip treatment time 1~4h, Gao Wenre
Isostatic pressing pressure is 130MPa~200MPa；
(6) step (5) treated the pure rhenium blank of middle-end is machined out by the size requirement of rhenium niobium Composite Nozzle, is obtained
End.
9. a kind of segmented preparation method of rhenium niobium Composite Nozzle according to claim 1, it is characterised in that: the step
Suddenly in (c), the method for lower end near net-shape mold jacket preparation lower end is utilized are as follows:
(1) lower end core model is mounted on to the bottom of jacket outside lower end, then covers niobium material tail portion on the core model of lower end；
(2) high-purity rhenium powder for obtaining step (a) is packed full with the cavity that jacket and niobium material tail portion, lower end core model are formed outside lower end
In, and jolt ramming；
(3) lower end jacket lid is weldingly fixed on to the top of jacket outside lower end, the lower end escape pipe that logical lower end jacket covers carries out
Degasification, outgassing temperature are 750~900 DEG C, and the degasification time is 8~48h, and vacuum degree when final encapsulation is less than 5 × 10-3Pa；
(4) the lower end near net-shape mold jacket for being packaged with high-purity rhenium powder for obtaining step (3) carries out hip treatment, heat etc.
Static pressure after treatment removes jacket, lower end core model, lower end jacket lid outside lower end, obtains lower end blank；
Hip treatment temperature is 1250 DEG C~1400 DEG C, and the hip treatment time is 1~5h, hip treatment pressure
≥110MPa；
(5) the lower end blank that step (4) obtains is machined by the size requirement of rhenium niobium Composite Nozzle, obtains lower end.
10. a kind of segmented preparation method of rhenium niobium Composite Nozzle according to claim 1, it is characterised in that: described
In step (d), speed of welding is 0.5~3m/min.
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| CN114433842A (en) * | 2022-03-03 | 2022-05-06 | 宁波江丰热等静压技术有限公司 | Sheath for hot isostatic pressing |
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