CN106378591A - Processing method for small-size and high-strength niobium-hafnium alloy bar - Google Patents
Processing method for small-size and high-strength niobium-hafnium alloy bar Download PDFInfo
- Publication number
- CN106378591A CN106378591A CN201611060587.0A CN201611060587A CN106378591A CN 106378591 A CN106378591 A CN 106378591A CN 201611060587 A CN201611060587 A CN 201611060587A CN 106378591 A CN106378591 A CN 106378591A
- Authority
- CN
- China
- Prior art keywords
- bar
- forging
- hafnium alloy
- small dimension
- niobium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Forging (AREA)
Abstract
The invention provides a processing method for a small-size and high-strength niobium-hafnium alloy bar. The processing method comprises the following steps that 1, a niobium-hafnium alloy ingot blank is sawn, and after being heated, the sawn niobium-hafnium alloy ingot blank is coated with an anti-oxidative protective lubricant; 2, the niobium-hafnium alloy ingot blank coated with the anti-oxidative protective lubricant is forged through upsetting and stretching to obtain a bar billet; 3, the bar billet is sequentially turned, ground and vacuum-annealed for the first time; 4, the vacuum-annealed bar billet is heated, the heated bar billet is coated with an anti-oxidative protective lubricant, and the bar billet coated with the anti-oxidative protective lubricant is formed through die forging to obtain a forging stock; 5, the forging stock is sequentially turned, ground and vacuum-annealed for the second time; 6, the vacuum-annealed forged stock is rolled with grooved rolls to obtain a small-size bar billet; and 7, the small-size bar billet is sequentially straightened, scalped, polished, pickled and annealed to obtain the small-size and high-strength niobium-hafnium alloy bar. The diameter of the section of the bar obtained according to the processing method is 8-20 mm, the room temperature tensile strength of the bar is up to above 465 MPa, the yield strength of the bar is up to above 350 MPa, the elongation of the bar is above 47%, and the grain structure of the bar is fine and uniform.
Description
Technical field
The invention belongs to niobium-base alloy processing technique field is and in particular to a kind of small dimension high intensity niobium hafnium alloy bar
Processing method.
Background technology
The nickel based super alloy that thermal structure part is commonly used, its maximum operation (service) temperature is 1100 DEG C, close to the fusing point of material itself,
The technical requirements of aerospace structure part far can not be met it is therefore necessary to find alternative materials.Refractory metal has height
Fusing point and low saturated vapor pressure, the high stress level under high temperature can be born so that it can be suitable for high-temperature field.Aviation
The structural member of space flight, loss of weight is always the key of research, the appearance of low-density niobium-base alloy, just solves need at that time
Ask.Niobium alloy because of its relatively low density, excellent intensity, good corrosion stability, low ductile-brittle transition temperature, and preferably
Room-temperature ductility, be a kind of promising high-temperature structural material.
In numerous niobium-base alloys, the niobium hafnium alloy C103 (Nb 10Hf 1Ti 0.7Zr) that the sixties in 20th century develops,
Because its excellent combination property is therefrom shown one's talent.Niobium hafnium alloy belongs to low strong series niobium alloy, and this alloy can processing stage
Height, easily welds, can be processed into variously-shaped, and such as high-performance rocket engine radiation Cooling Thrust Chamber and jet pipe extend segment structure
Part.Under niobium hafnium alloy hot environment, antioxygenic property is poor, must have safeguard procedures during use, adds the use after protective coating
Temperature, up to 1400～1500 DEG C, is preferred material during the current large-scale use in Nozzle of Liquid Rocket Motor position.With
The development need of aerospace flight technology, the serviceability of niobium alloy material, use environment etc. require more and more strictly, niobium alloy strengthening
Development direction mainly has two：One is to develop new alloy, and the niobium tungsten series alloy that such as western developed country is developed can be by material
Use temperature improve to 1650 DEG C；Two is to improve its preparation method and processing technology to existing alloy, improves the synthesis of material
Performance.
At present, niobium hafnium alloy mainly carries out the preparation of ingot casting by electronic torch melting and electric arc melting, after electric arc melting
Ingot casting crystal grain larger, typically die break is carried out by extrusion blooming.However, due to the restriction of extrusion equipment ability, causing
Selected extrusion ratio is generally less, and crystal grain can not be completely broken, therefore usually needs later stage forging or is pressed further by.
For the niobium hafnium alloy bar of big specification, conventional processing technology is directly to be obtained close to finished size by forging
Bar, find its tensile strength and yield strength up to 425MPa and 310MPa after detection.(a diameter of for small-sized bar
Φ 8mm～Φ 20mm), first method is to intermediate sizes specification, then finish forge or rotation by the bar stock warm and hot forging after extruding
Forge finished product；Second method is to finished size by extruding bar stock secondary extrusion.However, the little rule to the preparation of both technique
Find after the mechanics properties testing of lattice bar, the first technique obtains bar, mechanical property is poor, tensile strength and yield strength
It is only 415MPa and 304MPa respectively, even below only pass through the large scale rod bar that forging obtains；Although second bar mechanics
Performance has been lifted, and can reach 450MPa and 330MPa, but have a top layer and core set be woven with nearly two-stage grain size poor
Different, but also find the phenomenon of the front-end and back-end mechanical heterogeneity of bar.The bar power of the first technique of analysis shows
The main cause learning poor-performing is that its tissue crystal grain is larger, and Grain size distribution is uneven, is mainly manifested in the top layer of bar
Crystal grain is thinner, and core crystal grain is thicker, because its radial-deformation is inadequate the reason cause this result.Niobium hafnium alloy finish forge or
Person swages and belongs to the process of small deformation, high frequency time, and pass reduction is very low, and radial direction processing capacity is usually 1mm～2mm,
Lead to deform the top layer being concentrated mainly on bar, add that the forging permeability also showing as niobium hafnium alloy in actual production is also poor, rod
The crystal grain of material core only deforms, and has the characteristics that big crystal grain entails finished product, thus affecting its mechanical property.Additionally,
The tension that in finish forge or rotary swaging process, bar stock core is subject to persistently strengthens, and easily causes bar core crackle and occurs.Second
Although technique uses extrusion molding, larger yet with niobium hafnium alloy viscosity itself, and metal during the early stage extruding
Flowing is relatively slow, later stage metal flow quickly, often result in middle part metal and end metal mobility variant although being subject to
Three-dimensional stress, will also result in the difference of axial microstructure and mechanical property.If extrusion ratio is excessive, that is, bar stock diameter phase before and after extruding
Difference is very big, and the difference of radial-deformation also increases therewith.Relatively forge slightly higher, technique plus extruding production cost in industrial production
Cumbersome.
Content of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, provides a kind of small dimension high-strength
The processing method of degree niobium hafnium alloy bar.The small-sized bar being obtained using the method processing, surface quality is good, and dimensional tolerance is easy
Control, mechanical property excellent and uniform, room temperature tensile intensity up to more than 465MPa, yield strength up to more than 350MPa,
Elongation percentage reaches more than 47%.
For solving above-mentioned technical problem, the technical solution used in the present invention is：A kind of small dimension high intensity niobium hafnium alloy rod
The processing method of material is it is characterised in that the method comprises the following steps：
After step one, the niobium hafnium alloy ingot blank sawing being circle by cross sectional shape, put into heating in chamber type electric resistance furnace
To 100 DEG C～160 DEG C, then niobium hafnium alloy extruding surface of ingot blank after the heating uniformly coats antioxidant defense lubricant；
Step 2, surface in step one is coated with antioxidant defense lubricant niobium hafnium alloy extruding ingot blank in temperature be
Carry out upsetting pull forging, obtaining cross sectional shape is circular bar stock under conditions of 1250 DEG C～1300 DEG C；
Step 3, bar stock described in step 2 is carried out successively with turning, reconditioning and the first vacuum annealing are processed；
Step 4, the bar stock after processing through the first vacuum annealing in step 3 is put into and is heated to 100 in chamber type electric resistance furnace
DEG C～160 DEG C, then bar stock surface after the heating uniformly coat antioxidant defense lubricant, afterwards surface is coated with antioxygen
The bar stock changing protecting lubricant carries out die-forging forming under conditions of temperature is 1150 DEG C～1250 DEG C, and obtaining cross sectional shape is circle
The forging stock of shape；
Step 5, forging stock described in step 4 is carried out successively with turning, reconditioning and the second vacuum annealing are processed；
Step 6, the bar being 900 DEG C～1000 DEG C in temperature by the forging stock after processing through the second vacuum annealing in step 5
Carry out groove rolling, obtaining cross sectional shape is circular small dimension bar stock under part；The diameter of section of described small dimension bar stock is
8.5mm～20.5mm；
Step 7, small dimension bar stock described in step 6 is carried out successively align, strips off the skin, polishes, pickling and finished products
Process, obtaining cross sectional shape is circular small dimension high intensity niobium hafnium alloy bar, the diameter of section of this bar be 8mm～
20mm, tensile strength under 25 DEG C of room temperature conditions for this bar is more than 465MPa, and yield strength is more than 350MPa, elongation percentage
For more than 47%.
A kind of processing method of above-mentioned small dimension high intensity niobium hafnium alloy bar is it is characterised in that described in step one
The diameter of section of niobium hafnium alloy ingot blank is 100mm～110mm.
A kind of processing method of above-mentioned small dimension high intensity niobium hafnium alloy bar is it is characterised in that described in step 2
The forging mode that upsetting pull forging is pulled out using three upsettings three, wherein three times jumping-up forgings all make the height of ingot blank reduce 40%～50%,
Three times pulling forging in, front pull out twice to ingot blank original length, pull out for the third time to ingot blank diameter of section be 70mm～
80mm, the general working rate of described upsetting pull forging is 36.0%～51.2%.
A kind of processing method of above-mentioned small dimension high intensity niobium hafnium alloy bar is it is characterised in that described in step 3
First vacuum annealing process temperature be 1150 DEG C～1200 DEG C, described first vacuum annealing process time be 60min～
90min.
A kind of processing method of above-mentioned small dimension high intensity niobium hafnium alloy bar is it is characterised in that described in step 2
The diameter of section of bar stock is 70mm～80mm, and the diameter of section of forging stock described in step 4 is 35mm～45mm.
A kind of processing method of above-mentioned small dimension high intensity niobium hafnium alloy bar is it is characterised in that described in step 4
Die-forging forming adopts the forging mode of the axial pulling of multi-pass, the single pass radial direction drafts of described die-forging forming be 5mm～
6mm, the general working rate of described die-forging forming is 64.9%～71.9%.
A kind of processing method of above-mentioned small dimension high intensity niobium hafnium alloy bar is it is characterised in that described in step 5
Second vacuum annealing process temperature be 1050 DEG C～1100 DEG C, described second vacuum annealing process time be 60min～
90min.
A kind of processing method of above-mentioned small dimension high intensity niobium hafnium alloy bar is it is characterised in that described in step 6
Groove rolling adopts ellipse-circular hole rolling system, during groove rolling the elongation percentage of each passes be 1.30～
1.69, the general working rate of described groove rolling is 75.0%～95.0%.
A kind of processing method of above-mentioned small dimension high intensity niobium hafnium alloy bar is it is characterised in that described in step 7
The pickle that pickling is adopted is nitrate acid and hydrofluoric acid mixed acid, and described nitrate acid and hydrofluoric acid mixed acid by water, mass concentration is
68% red fuming nitric acid (RFNA) and hydrofluoric acid that mass concentration is 50% mix form by volume at 6: 3: 1.
A kind of processing method of above-mentioned small dimension high intensity niobium hafnium alloy bar is it is characterised in that described in step 7
The temperature that finished products are processed is 950 DEG C～1000 DEG C, and the time that described finished products are processed is 60min～90min.
The present invention compared with prior art has advantages below：
1st, because the high-temperature oxidation resistance of niobium hafnium alloy is poor, after extruding surface of ingot blank coating antioxidant defense lubricant, no
Oxidational losses when alloy only can be made to forge at high temperature reduces, and also can play heat loss effect when reducing forging.Forging
Tri- jumping-ups of Shi Caiyong, and Upsetting is larger, fibr tissue can will be caused fully broken by extruding, jumping-up in ingot blank
Make center hardly possible deformed grains to edge flowing so that repeatedly grow after bar stock radial direction microstructure homogenization.
2nd, the first stage annealing after upsetting pull forging not only can eliminate processing hardening, it is also possible that the material of following process
The probability that the defects such as crackle, folding in material reduces, and improves yield rate.Second forging adopts the die-forging forming of heavy reduction,
So that plastic deformation is transferred to bar stock core, reach the effect of die break.Compare the middle bar stock prepared by extrusion process,
Through the bar stock forged twice, the grain size difference of top layer and core is much smaller so that following process is more easy to reach radially tissue
Homogenization.
3rd, in order to avoid finish forge or the insufficient problem of the deformation causing of swaging, or the performance that extruding causes is uneven
Problem, the present invention prepares small-sized bar using groove rolling technique, and its pass reduction is much larger than finish forge or technique of swaging,
And improving general working rate to more than 75%, the plastic deformation of rolling can be deep into bar stock core, can obtain close after annealing
Uniform fine grained texture is so that mechanical property has been lifted, and the ellipse-circular hole system used can both can guarantee that rolling
High efficiency, and preferable Surface of Rod Bar can be obtained.
In sum, the small-sized bar being obtained using the inventive method processing, surface quality is good, and dimensional tolerance is easily-controllable
System, good mechanical performance, the tensile strength under the conditions of room temperature (25 DEG C) up to more than 465MPa, yield strength up to 350MPa with
On, elongation percentage reaches more than 47%.
With reference to embodiment, the present invention is described in further detail.
Specific embodiment
Embodiment 1
It is raw material for Φ 100mm niobium hafnium alloy ingot blank that the present embodiment adopts specification, and preparation specification is that Φ 8mm small dimension is high-strength
Degree niobium hafnium alloy bar, the processing method of the present embodiment small dimension high intensity niobium hafnium alloy bar comprises the following steps：
Step one, cross sectional shape is circular, diameter of section be the niobium hafnium alloy ingot blank sawing of 100mm, sawing is long
Degree is not more than 250mm, is then placed in chamber type electric resistance furnace being heated to 150 DEG C, afterwards niobium hafnium alloy extruding ingot blank after the heating
Surface uniformly coats antioxidant defense lubricant, and the concrete coating of the present embodiment is Ti-1200 antioxidant defense lubricant, coating
Thickness is 0.2mm；
Step 2, surface in step one is coated with antioxidant defense lubricant niobium hafnium alloy extruding ingot blank in intermediate frequency sense
Answer stove heat to 1260 DEG C, then ingot blank is extruded to the niobium hafnium alloy being heated to 1260 DEG C and carry out upsetting pull forging, obtain section shape
Shape is circular bar stock；The diameter of section of described bar stock is 70mm；The forging mode that described upsetting pull forging is pulled out using three upsettings three, its
In three jumping-ups all make ingot blank highly reduce 46%, front pull out twice to original length, third time pulling makes diameter reach Φ
70mm, the general working rate of forging is 51%；Final forging temperature must be more than 900 DEG C, otherwise carries out melting down heating；
Step 3, turning, reconditioning are carried out successively to bar stock described in step 2, lacked with removing superficial oxidation skin and forging
Fall into such as folding, crackle etc., then carry out the first vacuum annealing process, the temperature that described first vacuum annealing is processed is 1200 DEG C,
The time that described first vacuum annealing is processed is 60min；Obtain the bar stock of a diameter of Φ 66mm；
Step 4, the bar stock after processing through the first vacuum annealing in step 3 is put into and is heated to 150 in chamber type electric resistance furnace
DEG C, then bar stock surface after the heating uniformly coats antioxidant defense lubricant, and concrete coating is Ti-1200 antioxygen chemoprevention
Shield lubricant, coating thickness is 0.2mm, and the bar stock that surface is coated with antioxidant defense lubricant afterwards is 1160 DEG C in temperature
Under conditions of carry out die-forging forming, obtaining cross sectional shape is circular forging stock, and the diameter of section of described forging stock is 35mm；Described mould
It is swaged into the forging mode using axially pulling for the shape, the single pass radial direction drafts wherein in forging process is not more than 6mm, fall mould rule
Lattice are followed successively by：Φ 60mm, Φ 55mm, Φ 50mm, Φ 45mm, Φ 40mm, Φ 35mm, forging general working rate is 71.9%.Finish-forging
Temperature must be more than 900 DEG C, otherwise carries out melting down heating；
Step 5, turning, reconditioning are carried out successively to forging stock described in step 4, lacked with removing superficial oxidation skin and forging
Fall into such as folding, crackle, then carry out the second vacuum annealing process；The temperature that described second vacuum annealing is processed is 1080 DEG C, institute
The time stating the second vacuum annealing process is 60min；Obtain the forging stock of a diameter of Φ 31mm；
Step 6, by step 5 through second vacuum annealing process after forging stock temperature be 960 DEG C under conditions of carry out
Groove rolling, obtaining cross sectional shape is circular small dimension bar stock；The diameter of section of described small dimension bar stock is 8.5mm；Described
Groove rolling uses 6 to ellipse-circular hole system, the passage lengthening coefficient of each pair pass is respectively 1.64,1.60,
1.57th, 1.54,1.49,1.41, rolling general working rate is 92.5%；
Step 7, small dimension bar stock described in step 6 is carried out successively align, strips off the skin, polishes, pickling, until surface
The defects such as the ears or side handles of a utensil, misrun and oxidation thoroughly remove, and finally carry out finished products process, and obtaining cross sectional shape is circular small dimension
High intensity niobium hafnium alloy bar, the diameter of section of this bar is 8mm；The pickle adopting during described pickling is nitrate acid and hydrofluoric acid
Mixed acid, the red fuming nitric acid (RFNA) that described nitrate acid and hydrofluoric acid mixed acid is 68% by water, mass concentration and the hydrogen fluorine that mass concentration is 50%
Acid mixes forms by volume at 6: 3: 1；The temperature that described finished products are processed is 950 DEG C, and described finished products are processed
Time is 60min.
The mechanical property of the niobium hafnium alloy bar being obtained using the present embodiment processing is as shown in table 1.
The mechanical property of table 1 embodiment 1 niobium hafnium alloy bar
Understand in conjunction with table 1：The surface quality of the niobium hafnium alloy bar of a diameter of 8mm manufactured in the present embodiment is good, and size is public
Difference easy to control, mechanical property excellent, its room temperature (25 DEG C) tensile strength, yield strength and elongation percentage are superior to conventional method system
Standby small-sized bar.
Embodiment 2
It is raw material for Φ 105mm niobium hafnium alloy ingot blank that the present embodiment adopts specification, and preparation specification is that Φ 12mm small dimension is high
Intensity niobium hafnium alloy bar, the processing method of the present embodiment small dimension high intensity niobium hafnium alloy bar comprises the following steps：
Step one, cross sectional shape is circular, diameter of section be the niobium hafnium alloy ingot blank sawing of 105mm, sawing is long
Degree is not more than 250mm, is then placed in chamber type electric resistance furnace being heated to 150 DEG C, afterwards niobium hafnium alloy extruding ingot blank after the heating
Surface uniformly coats antioxidant defense lubricant, and the concrete coating of the present embodiment is Ti-1200 antioxidant defense lubricant, coating
Thickness is 0.2mm；
Step 2, surface in step one is coated with antioxidant defense lubricant niobium hafnium alloy extruding ingot blank in intermediate frequency sense
Answer stove heat to 1280 DEG C, then ingot blank is extruded to the niobium hafnium alloy being heated to 1280 DEG C and carry out upsetting pull forging, obtain section shape
Shape is circular bar stock；The diameter of section of described bar stock is 75mm；The forging mode that described upsetting pull forging is pulled out using three upsettings three, its
In three jumping-ups all make ingot blank highly reduce 44%, front pull out twice to original length, third time pulling makes diameter reach Φ
75mm, the general working rate of forging is 49%；Final forging temperature must be more than 900 DEG C, otherwise carries out melting down heating；
Step 3, turning, reconditioning are carried out successively to bar stock described in step 2, lacked with removing superficial oxidation skin and forging
Fall into such as folding, crackle etc., then carry out the first vacuum annealing process, the temperature that described first vacuum annealing is processed is 1180 DEG C,
The time that described first vacuum annealing is processed is 60min；Obtain the bar stock of a diameter of Φ 71mm；
Step 4, the bar stock after processing through the first vacuum annealing in step 3 is put into and is heated to 150 in chamber type electric resistance furnace
DEG C, then bar stock surface after the heating uniformly coats antioxidant defense lubricant, and concrete coating is Ti-1200 antioxygen chemoprevention
Shield lubricant, coating thickness is 0.2mm, and the bar stock that surface is coated with antioxidant defense lubricant afterwards is 1180 DEG C in temperature
Under conditions of carry out die-forging forming, obtaining cross sectional shape is circular forging stock, and the diameter of section of described forging stock is 40mm；Described mould
Be swaged into the forging mode using axially pulling for the shape, the single pass radial direction drafts in forging process is not more than 6mm, fall mould specification according to
Secondary it is：Φ 65mm, Φ 60mm, Φ 55mm, Φ 50mm, Φ 45mm, Φ 40mm, forging general working rate is 68.3%, final forging temperature
900 DEG C must be more than, otherwise carry out melting down heating；
Step 5, turning, reconditioning are carried out successively to forging stock described in step 4, lacked with removing superficial oxidation skin and forging
Fall into such as folding, crackle, then carry out the second vacuum annealing process；The temperature that described second vacuum annealing is processed is 1070 DEG C, institute
The time stating the second vacuum annealing process is 60min；Obtain the forging stock of a diameter of Φ 36mm；
Step 6, by step 5 through second vacuum annealing process after forging stock temperature be 960 DEG C under conditions of carry out
Groove rolling, obtaining cross sectional shape is circular small dimension bar stock；The diameter of section of described small dimension bar stock is 12.5mm；Described
Groove rolling uses 5 to ellipse-circular hole system, the passage lengthening coefficient of each pair pass is respectively 1.65,1.61,
1.54th, 1.47,1.38, rolling general working rate is 87.9%；
Step 7, small dimension bar stock described in step 6 is carried out successively align, strips off the skin, polishes, pickling, until surface
The defects such as the ears or side handles of a utensil, misrun and oxidation thoroughly remove, and finally carry out finished products process, and obtaining cross sectional shape is circular small dimension
High intensity niobium hafnium alloy bar, the diameter of section of this bar is 12mm；The pickle adopting during described pickling is nitrate acid and hydrofluoric acid
Mixed acid, the red fuming nitric acid (RFNA) that described nitrate acid and hydrofluoric acid mixed acid is 68% by water, mass concentration and the hydrogen fluorine that mass concentration is 50%
Acid mixes forms by volume at 6: 3: 1；The temperature that described finished products are processed is 960 DEG C, and described finished products are processed
Time is 60min.
The mechanical property of the niobium hafnium alloy bar being obtained using the present embodiment processing is as shown in table 2.
The mechanical property of table 2 embodiment 2 niobium hafnium alloy bar
Understand in conjunction with table 2：The surface quality of the niobium hafnium alloy bar of a diameter of 12mm manufactured in the present embodiment is good, and size is public
Difference easy to control, mechanical property excellent, its room temperature (25 DEG C) tensile strength, yield strength and elongation percentage are superior to conventional method system
Standby small-sized bar.
Embodiment 3
It is raw material for Φ 110mm niobium hafnium alloy ingot blank that the present embodiment adopts specification, and preparation specification is that Φ 18mm small dimension is high
Intensity niobium hafnium alloy bar, the processing method of the present embodiment small dimension high intensity niobium hafnium alloy bar comprises the following steps：
Step one, cross sectional shape is circular, diameter of section be the niobium hafnium alloy ingot blank sawing of 110mm, sawing is long
Degree is not more than 250mm, is then placed in chamber type electric resistance furnace being heated to 150 DEG C, afterwards niobium hafnium alloy extruding ingot blank after the heating
Surface uniformly coats antioxidant defense lubricant, and the concrete coating of the present embodiment is Ti-1200 antioxidant defense lubricant, coating
Thickness is 0.2mm；
Step 2, surface in step one is coated with antioxidant defense lubricant niobium hafnium alloy extruding ingot blank in intermediate frequency sense
Answer stove heat to 1290 DEG C, then ingot blank is extruded to the niobium hafnium alloy being heated to 1290 DEG C and carry out upsetting pull forging, obtain section shape
Shape is circular bar stock；The diameter of section of described bar stock is 80mm；The forging mode that described upsetting pull forging is pulled out using three upsettings three, its
In three jumping-ups all make ingot blank highly reduce 42%, front pull out twice to original length, third time pulling makes diameter reach Φ
80mm, the general working rate of forging is 47.1%；Final forging temperature must be more than 900 DEG C, otherwise carries out melting down heating；
Step 3, turning, reconditioning are carried out successively to bar stock described in step 2, lacked with removing superficial oxidation skin and forging
Fall into such as folding, crackle etc., then carry out the first vacuum annealing process, the temperature that described first vacuum annealing is processed is 1160 DEG C,
The time that described first vacuum annealing is processed is 60min；Obtain the bar stock of a diameter of 76mm；
Step 4, the bar stock after processing through the first vacuum annealing in step 3 is put into and is heated to 150 in chamber type electric resistance furnace
DEG C, then bar stock surface after the heating uniformly coats antioxidant defense lubricant, and concrete coating is Ti-1200 antioxygen chemoprevention
Shield lubricant, coating thickness is 0.2mm, and the bar stock that surface is coated with antioxidant defense lubricant afterwards is 1160 DEG C in temperature
Under conditions of carry out die-forging forming, obtaining cross sectional shape is circular forging stock, and the diameter of section of described forging stock is 45mm；Described mould
Be swaged into the forging mode using axially pulling for the shape, the single pass radial direction drafts in forging process is not more than 6mm, fall mould specification according to
Secondary it is：Φ 70mm, Φ 65mm, Φ 60mm, Φ 55mm, Φ 50mm, Φ 45mm, forging general working rate is 64.9%.Final forging temperature
900 DEG C must be more than, otherwise carry out melting down heating；
Step 5, turning, reconditioning are carried out successively to forging stock described in step 4, lacked with removing superficial oxidation skin and forging
Fall into such as folding, crackle, then carry out the second vacuum annealing process；The temperature that described second vacuum annealing is processed is 1060 DEG C, institute
The time stating the second vacuum annealing process is 60min；Obtain the forging stock of a diameter of Φ 41mm；
Step 6, by step 5 through second vacuum annealing process after forging stock temperature be 960 DEG C under conditions of carry out
Groove rolling, obtaining cross sectional shape is circular small dimension bar stock；The diameter of section 18.5mm of described small dimension bar stock；Described hole
Type rolling uses 4 to ellipse-circular hole system, the passage lengthening coefficient of each pair pass is respectively 1.69,1.58,1.42,
1.30, rolling general working rate is 79.6%；
Step 7, small dimension bar stock described in step 6 is carried out successively align, strips off the skin, polishes, pickling, until surface
The defects such as the ears or side handles of a utensil, misrun and oxidation thoroughly remove, and finally carry out finished products process, and obtaining cross sectional shape is circular small dimension
High intensity niobium hafnium alloy bar, the diameter of section of this bar is 18mm；The pickle adopting during described pickling is nitrate acid and hydrofluoric acid
Mixed acid, the red fuming nitric acid (RFNA) that described nitrate acid and hydrofluoric acid mixed acid is 68% by water, mass concentration and the hydrogen fluorine that mass concentration is 50%
Acid mixes forms by volume at 6: 3: 1；The temperature that described finished products are processed is 970 DEG C, and described finished products are processed
Time is 60min.
The mechanical property of the niobium hafnium alloy bar being obtained using the present embodiment processing is as shown in table 3.
The mechanical property of table 3 embodiment 3 niobium hafnium alloy bar
Understand in conjunction with table 3：The surface quality of the niobium hafnium alloy bar of a diameter of 18mm manufactured in the present embodiment is good, and size is public
Difference easy to control, mechanical property excellent, its room temperature (25 DEG C) tensile strength, yield strength and elongation percentage are superior to conventional method system
Standby small-sized bar.
Embodiment 4
It is raw material for Φ 100mm niobium hafnium alloy ingot blank that the present embodiment adopts specification, and preparation specification is that Φ 20mm small dimension is high
Intensity niobium hafnium alloy bar, the processing method of the present embodiment small dimension high intensity niobium hafnium alloy bar comprises the following steps：
Step one, cross sectional shape is circular, diameter of section be the niobium hafnium alloy ingot blank sawing of 100mm, sawing is long
Degree is not more than 250mm, is then placed in chamber type electric resistance furnace being heated to 100 DEG C, afterwards niobium hafnium alloy extruding ingot blank after the heating
Surface uniformly coats antioxidant defense lubricant, and the concrete coating of the present embodiment is Ti-1200 antioxidant defense lubricant, coating
Thickness is 0.2mm；
Step 2, surface in step one is coated with antioxidant defense lubricant niobium hafnium alloy extruding ingot blank in intermediate frequency sense
Answer stove heat to 1300 DEG C, then ingot blank is extruded to the niobium hafnium alloy being heated to 1300 DEG C and carry out upsetting pull forging, obtain section shape
Shape is circular bar stock；The diameter of section of described bar stock is 80mm；The forging mode that described upsetting pull forging is pulled out using three upsettings three, its
In three jumping-ups all make ingot blank highly reduce 40%, front pull out twice to original length, third time pulling makes diameter reach Φ
80mm, the general working rate of forging is 36.0%；Final forging temperature must be more than 900 DEG C, otherwise carries out melting down heating；
Step 3, turning, reconditioning are carried out successively to bar stock described in step 2, lacked with removing superficial oxidation skin and forging
Fall into such as folding, crackle etc., then carry out the first vacuum annealing process, the temperature that described first vacuum annealing is processed is 1200 DEG C,
The time that described first vacuum annealing is processed is 90min；Obtain the bar stock of a diameter of 76mm；
Step 4, the bar stock after processing through the first vacuum annealing in step 3 is put into and is heated to 100 in chamber type electric resistance furnace
DEG C, then bar stock surface after the heating uniformly coats antioxidant defense lubricant, and concrete coating is Ti-1200 antioxygen chemoprevention
Shield lubricant, coating thickness is 0.2mm, and the bar stock that surface is coated with antioxidant defense lubricant afterwards is 1250 DEG C in temperature
Under conditions of carry out die-forging forming, obtaining cross sectional shape is circular forging stock, and the diameter of section of described forging stock is 45mm；Described mould
Be swaged into the forging mode using axially pulling for the shape, the single pass radial direction drafts in forging process is not more than 6mm, fall mould specification according to
Secondary it is：Φ 70mm, Φ 65mm, Φ 60mm, Φ 55mm, Φ 50mm, Φ 45mm, forging general working rate is 64.9%.Final forging temperature
900 DEG C must be more than, otherwise carry out melting down heating；
Step 5, turning, reconditioning are carried out successively to forging stock described in step 4, lacked with removing superficial oxidation skin and forging
Fall into such as folding, crackle, then carry out the second vacuum annealing process；The temperature that described second vacuum annealing is processed is 1050 DEG C, institute
The time stating the second vacuum annealing process is 90min；Obtain the forging stock of a diameter of 41mm；
Step 6, by step 5 through second vacuum annealing process after forging stock temperature be 1000 DEG C under conditions of carry out
Groove rolling, obtaining cross sectional shape is circular small dimension bar stock；The diameter of section of described small dimension bar stock is 20.5mm；Described
Groove rolling uses 3 to ellipse-circular hole system, the passage lengthening coefficient of each pair pass is respectively 1.69,1.62,
1.46, the general working rate of rolling is 75.0%；
Step 7, small dimension bar stock described in step 6 is carried out successively align, strips off the skin, polishes, pickling, until surface
The defects such as the ears or side handles of a utensil, misrun and oxidation thoroughly remove, and finally carry out finished products process, and obtaining cross sectional shape is circular small dimension
High intensity niobium hafnium alloy bar, the diameter of section of this bar is 20mm；The pickle adopting during described pickling is nitrate acid and hydrofluoric acid
Mixed acid, the red fuming nitric acid (RFNA) that described nitrate acid and hydrofluoric acid mixed acid is 68% by water, mass concentration and the hydrogen fluorine that mass concentration is 50%
Acid mixes forms by volume at 6: 3: 1；；The temperature that described finished products are processed is 1000 DEG C, and described finished products are processed
Time be 90min.
The mechanical property of the niobium hafnium alloy bar being obtained using the present embodiment processing is as shown in table 4.
The mechanical property of table 4 embodiment 4 niobium hafnium alloy bar
Understand in conjunction with table 4：The surface quality of the niobium hafnium alloy bar of a diameter of 20mm manufactured in the present embodiment is good, and size is public
Difference easy to control, mechanical property excellent, its room temperature (25 DEG C) tensile strength, yield strength and elongation percentage are superior to conventional method system
Standby small-sized bar.
The above, be only presently preferred embodiments of the present invention, not the present invention imposed any restrictions.Every according to invention skill
Any simple modification, change and equivalence changes that art is substantially made to above example, all still fall within technical solution of the present invention
Protection domain in.
Claims (10)
1. a kind of processing method of small dimension high intensity niobium hafnium alloy bar is it is characterised in that the method comprises the following steps：
After step one, the niobium hafnium alloy ingot blank sawing being circle by cross sectional shape, put into and in chamber type electric resistance furnace, be heated to 100
DEG C～160 DEG C, then after the heating niobium hafnium alloy extruding surface of ingot blank uniformly coat antioxidant defense lubricant；
Step 2, surface in step one is coated with antioxidant defense lubricant niobium hafnium alloy extruding ingot blank temperature be 1250
DEG C～1300 DEG C under conditions of carry out upsetting pull forging, obtaining cross sectional shape is circular bar stock；
Step 3, bar stock described in step 2 is carried out successively with turning, reconditioning and the first vacuum annealing are processed；
Step 4, by step 3 through first vacuum annealing process after bar stock put into be heated in chamber type electric resistance furnace 100 DEG C～
160 DEG C, then bar stock surface after the heating uniformly coat antioxidant defense lubricant, afterwards surface is coated with antioxygen chemoprevention
The bar stock of shield lubricant carries out die-forging forming under conditions of temperature is 1150 DEG C～1250 DEG C, and it is circular for obtaining cross sectional shape
Forging stock；
Step 5, forging stock described in step 4 is carried out successively with turning, reconditioning and the second vacuum annealing are processed；
Step 6, by step 5 through second vacuum annealing process after forging stock temperature be 900 DEG C～1000 DEG C under conditions of
Carry out groove rolling, obtaining cross sectional shape is circular small dimension bar stock；The diameter of section of described small dimension bar stock be 8.5mm～
20.5mm；
Step 7, small dimension bar stock described in step 6 is carried out successively align, strips off the skin, polishes, pickling and finished products are processed,
Obtaining cross sectional shape is circular small dimension high intensity niobium hafnium alloy bar, and the diameter of section of this bar is 8mm～20mm, this rod
Tensile strength under 25 DEG C of room temperature conditions for the material be more than 465MPa, yield strength be more than 350MPa, elongation percentage be 47% with
On.
2. a kind of processing method of small dimension high intensity niobium hafnium alloy bar according to claim 1 is it is characterised in that walk
The diameter of section of niobium hafnium alloy ingot blank described in rapid is 100mm～110mm.
3. a kind of processing method of small dimension high intensity niobium hafnium alloy bar according to claim 1 is it is characterised in that walk
The forging mode that the forging of upsetting pull described in rapid two is pulled out using three upsettings three, wherein three times jumping-up forgings all make the height of ingot blank reduce
40%～50%, three times pulling forging in, front pull out twice to ingot blank original length, pull out for the third time to the diameter of section of ingot blank
For 70mm～80mm, the general working rate of described upsetting pull forging is 36.0%～51.2%.
4. a kind of processing method of small dimension high intensity niobium hafnium alloy bar according to claim 1 is it is characterised in that walk
Described in rapid three first vacuum annealing process temperature be 1150 DEG C～1200 DEG C, described first vacuum annealing process time be
60min～90min.
5. a kind of processing method of small dimension high intensity niobium hafnium alloy bar according to claim 1 is it is characterised in that walk
The diameter of section of bar stock described in rapid two is 70mm～80mm, and the diameter of section of forging stock described in step 4 is 35mm～45mm.
6. a kind of processing method of small dimension high intensity niobium hafnium alloy bar according to claim 1 is it is characterised in that walk
Die-forging forming described in rapid four adopts the forging mode that multi-pass axially pulls out, the single pass radial direction drafts of described die-forging forming
For 5mm～6mm, the general working rate of described die-forging forming is 64.9%～71.9%.
7. a kind of processing method of small dimension high intensity niobium hafnium alloy bar according to claim 1 is it is characterised in that walk
Described in rapid five second vacuum annealing process temperature be 1050 DEG C～1100 DEG C, described second vacuum annealing process time be
60min～90min.
8. a kind of processing method of small dimension high intensity niobium hafnium alloy bar according to claim 1 is it is characterised in that walk
Groove rolling described in rapid six adopts ellipse-circular hole rolling system, and during groove rolling, the elongation percentage of each passes is equal
For 1.30～1.69, the general working rate of described groove rolling is 75.0%～95.0%.
9. a kind of processing method of small dimension high intensity niobium hafnium alloy bar according to claim 1 is it is characterised in that walk
The pickle that described in rapid seven, pickling is adopted is nitrate acid and hydrofluoric acid mixed acid, and described nitrate acid and hydrofluoric acid mixed acid is by water, matter
Amount concentration be 68% red fuming nitric acid (RFNA) and hydrofluoric acid that mass concentration is 50% mix form at 6: 3: 1 by volume.
10. a kind of small dimension high intensity niobium hafnium alloy bar according to claim 1 processing method it is characterised in that
The temperature that finished products described in step 7 are processed is 950 DEG C～1000 DEG C, the time that described finished products are processed be 60min～
90min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611060587.0A CN106378591A (en) | 2016-11-28 | 2016-11-28 | Processing method for small-size and high-strength niobium-hafnium alloy bar |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611060587.0A CN106378591A (en) | 2016-11-28 | 2016-11-28 | Processing method for small-size and high-strength niobium-hafnium alloy bar |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106378591A true CN106378591A (en) | 2017-02-08 |
Family
ID=57959256
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611060587.0A Pending CN106378591A (en) | 2016-11-28 | 2016-11-28 | Processing method for small-size and high-strength niobium-hafnium alloy bar |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106378591A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108097737A (en) * | 2017-12-09 | 2018-06-01 | 西安诺博尔稀贵金属材料有限公司 | The preparation method of neutron-absorbing component metal hafnium tubing in a kind of heap |
| CN109675956A (en) * | 2018-12-28 | 2019-04-26 | 宁夏东方钽业股份有限公司 | A kind of preparation method of small dimension Niobium Superconducting stick |
| CN110722014A (en) * | 2019-10-21 | 2020-01-24 | 青岛理工大学 | Preparation method and application of Nb ingot blank and Nb rod |
| CN111097797A (en) * | 2018-10-29 | 2020-05-05 | 山东钢铁股份有限公司 | Bright material manufacturing system and method for alloy steel bar |
| CN111941001A (en) * | 2019-12-30 | 2020-11-17 | 宁夏东方超导科技有限公司 | Manufacturing method of large-grain radio-frequency superconducting niobium cavity |
| CN113718110A (en) * | 2021-08-11 | 2021-11-30 | 九江有色金属冶炼有限公司 | Preparation method of high-quality niobium plate for controlling plate structure by accumulated energy |
| CN114273584A (en) * | 2021-12-27 | 2022-04-05 | 无锡派克新材料科技股份有限公司 | Forging-modifying method for 1200 KG-grade high-temperature oxidation-resistant alloy |
| CN115647733A (en) * | 2022-10-11 | 2023-01-31 | 中国核动力研究设计院 | Hafnium standard substance and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10280080A (en) * | 1997-04-03 | 1998-10-20 | Tohnichi Mfg Co Ltd | Aluminum alloy tool and its production |
| CN103397289A (en) * | 2013-08-11 | 2013-11-20 | 西北有色金属研究院 | Preparation method of TC4ELI titanium alloy bar |
| CN103861982A (en) * | 2012-12-18 | 2014-06-18 | 宁夏东方钽业股份有限公司 | Forging method of Nb (Niobium) rotary target cast ingot |
| CN104492849A (en) * | 2014-11-29 | 2015-04-08 | 西安诺博尔稀贵金属材料有限公司 | Preparation method of Hafnium square rod for nuclear reactor |
| CN105436232A (en) * | 2015-12-08 | 2016-03-30 | 西安诺博尔稀贵金属材料有限公司 | High-quantity hafnium rod manufacturing method |
-
2016
- 2016-11-28 CN CN201611060587.0A patent/CN106378591A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10280080A (en) * | 1997-04-03 | 1998-10-20 | Tohnichi Mfg Co Ltd | Aluminum alloy tool and its production |
| CN103861982A (en) * | 2012-12-18 | 2014-06-18 | 宁夏东方钽业股份有限公司 | Forging method of Nb (Niobium) rotary target cast ingot |
| CN103397289A (en) * | 2013-08-11 | 2013-11-20 | 西北有色金属研究院 | Preparation method of TC4ELI titanium alloy bar |
| CN104492849A (en) * | 2014-11-29 | 2015-04-08 | 西安诺博尔稀贵金属材料有限公司 | Preparation method of Hafnium square rod for nuclear reactor |
| CN105436232A (en) * | 2015-12-08 | 2016-03-30 | 西安诺博尔稀贵金属材料有限公司 | High-quantity hafnium rod manufacturing method |
Non-Patent Citations (3)
| Title |
|---|
| 康永林等: "《轧制工程学》", 30 September 2014, 北京冶金工业出版社 * |
| 杨晓维等: "航天用NbHf10-1合金锭挤压工艺研究", 《稀有金属与硬质合金》 * |
| 沈莲等: "《机械工程材料与设计选材》", 30 April 1996, 西安交通大学出版社 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108097737A (en) * | 2017-12-09 | 2018-06-01 | 西安诺博尔稀贵金属材料有限公司 | The preparation method of neutron-absorbing component metal hafnium tubing in a kind of heap |
| CN108097737B (en) * | 2017-12-09 | 2019-08-27 | 西安诺博尔稀贵金属材料有限公司 | The preparation method of neutron-absorbing component metal hafnium tubing in a kind of heap |
| CN111097797A (en) * | 2018-10-29 | 2020-05-05 | 山东钢铁股份有限公司 | Bright material manufacturing system and method for alloy steel bar |
| CN111097797B (en) * | 2018-10-29 | 2021-07-02 | 山东钢铁股份有限公司 | Bright material manufacturing system and method for alloy steel bar |
| CN109675956A (en) * | 2018-12-28 | 2019-04-26 | 宁夏东方钽业股份有限公司 | A kind of preparation method of small dimension Niobium Superconducting stick |
| CN110722014A (en) * | 2019-10-21 | 2020-01-24 | 青岛理工大学 | Preparation method and application of Nb ingot blank and Nb rod |
| CN111941001A (en) * | 2019-12-30 | 2020-11-17 | 宁夏东方超导科技有限公司 | Manufacturing method of large-grain radio-frequency superconducting niobium cavity |
| CN111941001B (en) * | 2019-12-30 | 2023-05-23 | 宁夏东方超导科技有限公司 | Manufacturing method of large-grain radio frequency superconducting niobium cavity |
| CN113718110A (en) * | 2021-08-11 | 2021-11-30 | 九江有色金属冶炼有限公司 | Preparation method of high-quality niobium plate for controlling plate structure by accumulated energy |
| CN114273584A (en) * | 2021-12-27 | 2022-04-05 | 无锡派克新材料科技股份有限公司 | Forging-modifying method for 1200 KG-grade high-temperature oxidation-resistant alloy |
| CN114273584B (en) * | 2021-12-27 | 2024-04-05 | 无锡派克新材料科技股份有限公司 | Forging method for 1200 KG-grade high-temperature antioxidant alloy |
| CN115647733A (en) * | 2022-10-11 | 2023-01-31 | 中国核动力研究设计院 | Hafnium standard substance and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106378591A (en) | Processing method for small-size and high-strength niobium-hafnium alloy bar | |
| CN1816641B (en) | Processing of titanium-aluminum-vanadium alloys and products made thereby | |
| CN106955893B (en) | A kind of processing method of superplastic forming SP700 titanium-alloy thin-plates | |
| CN111360074B (en) | Preparation method of heterogeneous lamellar structure medium/high-entropy alloy foil | |
| CN103846305A (en) | Preparation machining method of large-diameter pipe material and special-shaped pipe fitting | |
| CN102397889B (en) | Process for preparing GH4145 alloy pipes | |
| CN106391747B (en) | The method that nuclear fuel High-purity Niobium silk is prepared using general industry with niobium bar as raw material | |
| CN109457198A (en) | A kind of aluminum alloy materials and preparation method thereof of the anti-corrosion low stress of superhigh intensity | |
| CN110170543A (en) | A kind of titanium alloy seamless pipe short route processing method | |
| CN105441713A (en) | A titanium alloy seamless tube and a manufacturing method thereof | |
| CN110205572B (en) | Preparation method of two-phase Ti-Al-Zr-Mo-V titanium alloy forged rod | |
| CN107649628A (en) | A kind of processing method of ZK61 high-strength magnesium alloys forging | |
| CN112337972A (en) | Method for preparing high-performance magnesium alloy through secondary deformation | |
| CN107916359A (en) | A kind of preparation method of the medium managese steel with favorable forming property | |
| CN112662973B (en) | Method for manufacturing zirconium alloy pressure pipe of fuel channel of nuclear reactor | |
| RU2635650C1 (en) | Method of thermomechanical processing of high-alloyed pseudo- (titanium alloys alloyed by rare and rare-earth metals | |
| CN116921491A (en) | Preparation method of high-strength titanium alloy pipe | |
| RU2110600C1 (en) | Method for producing articles from zirconium alloys | |
| KR20220023763A (en) | Manufacturing method of zirconium alloy pipe | |
| CN114082783B (en) | Preparation method of single-pass large-reduction magnesium alloy plate | |
| CN110935826A (en) | Forming method of fine-grain weak-texture copper alloy conical shell | |
| CN116673422A (en) | Forging method of TC4 titanium alloy large-size forged bar | |
| RU2697309C1 (en) | Method of making wire from high-strength titanium-based alloys | |
| CN117531862A (en) | Preparation method for eliminating coarse-grain ring of Al-Zn-Mg-Cu aluminum alloy hexagonal rod material | |
| AU2004239246B2 (en) | Processing of titanium-aluminum-vanadium alloys and products made thereby |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170208 |
|
| RJ01 | Rejection of invention patent application after publication |