CN102901659A - Preparation method for metal alloy test rod - Google Patents
Preparation method for metal alloy test rod Download PDFInfo
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- CN102901659A CN102901659A CN2012103274004A CN201210327400A CN102901659A CN 102901659 A CN102901659 A CN 102901659A CN 2012103274004 A CN2012103274004 A CN 2012103274004A CN 201210327400 A CN201210327400 A CN 201210327400A CN 102901659 A CN102901659 A CN 102901659A
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Abstract
The present invention relates to the field of metal alloy test rod production, and provides a metal alloy test rod preparation method. According to the method, a vacuum suction casting device is adopted, wherein a vacuum chamber is filled with high purity argon to achieve pressure P1 of 0.02-0.06 MPa; when a button ingot surface layer is completely melted and a through hole on the bottom of an alloy ingot crucible is sealed through a liquid sealing manner, the vacuum chamber is continuously filled with high purity argon to increase pressure to P2, wherein pressure difference between the P2 and the P1 is 0.01-0.1 MPa; and pressure difference suction casting molding is adopted. The preparation method has the following characteristics that: high cleaning and high efficiency are provided; high uniformity and high accuracy of the components can be achieved; a size of the test rod can be phi 12 mm*120 mm; disadvantages of uniform component, difficult oxygen content control, long period or complex process, and the like of powder metallurgy, mold melting casting, extrusion molding, ingot processing and other test rod preparation methods are overcome; and strict requirements on the ideal alloy test rod by standard sample preparation, alloy design, performance testing, material feeding rod preparation and other processes can be met.
Description
Technical field
The present invention relates to the metal alloy coupon and make the field, be specifically the preparation high-purity, or the equal preparation method of even high-precision metal alloy coupon of alloying component height.
Background technology
High-purity, composition height be even high-precision alloy coupon preparation all, be the requisite sport technique segments in associated materials field such as chemical composition analysis, alloy designs, machining, powder metallurgy and hot investment casting, be mainly used in the technological processs such as the preparation of alloy standard specimen, performance test and feeding rod preparation.Usually these coupon preparation methods have following three kinds: 1. powder metallurgic method, and the general homogeneity of ingredients of the coupon of preparation and accurately higher, but the Control for Oxygen Content difficulty is larger, and process cycle is long; 2. hot investment casting, the good quantity of the coupon metallurgical quality of preparation is many, but oxygen content is higher, and composition is accurately even not and the cycle is long; 3. cut from the bulk foundry alloy, the coupon metallurgical quality of preparation is better, and quantity is more, but has macroscopical component segregation or segregation, and the composition deviation is arranged between coupon, is difficult to satisfy all even requirements for high precision of height.The more important thing is that these preparation methods production cycle is long and cost is high, the alloy that one-period generally can only satisfy 2-3 heterogeneity prepares demand, and composition is in a single day overproof, causes easily huge waste.If need to have between tens kinds or tens kinds heterogeneities of design preparation or composition the alloy coupon of micro fluctuation, these preparation methods will can't bear the heavy load.Therefore, the high effect cleaning novel preparation technology of developing a kind of ideal alloy coupon then is very necessary, will be with a wide range of applications.
Summary of the invention
For prior art above shortcomings part, the problem to be solved in the present invention is to provide a kind of preparation method of metal alloy coupon, and prepared coupon has high uniformity and high accuracy, has avoided the advantages such as segregation and loss.
The present invention adopts following technical scheme: a kind of preparation method of metal alloy coupon, it adopts suction pouring equipment, utilizing draught head to inhale casts to mould molding, described suction pouring equipment comprises upper vacuum chamber setting up and down and lower vacuum chamber, upper vacuum chamber top is provided with arc gum, the bottom is provided with a plurality of station copper crucibles upper vacuum chamber and the sealing of lower vacuum chamber is separated, and passes through the water circulation water-cooled around the copper crucible; Wringing fit is inlaid with the alloy pig crucible in station copper crucible therein, and through hole is left in the bottom, and upper vacuum chamber and lower vacuum chamber are connected; Concrete preparation process is:
1) according to mass ratio and the scaling loss compensation rule of alloy constituent element, adopt high pure raw material to be made into 10-100g alloy bag;
2) the alloy bag is placed described copper crucible, pass into high-purity argon gas after vacuumizing, carry out receiving after the starting the arc melting arc and solidify and make the button ingot;
3) the button ingot is inserted in the alloy pig crucible, the metal die of coupon is placed below the lower vacuum chamber crucible, closing apparatus, and be evacuated to 5 * 10
-3More than the Pa, be filled with high-purity argon gas P 1 to 0.02-0.06MPa;
4) open recirculated water and arc gum and carry out the argon arc melting, when button ingot top layer melt fully and the through hole of fluid-tight alloy pig crucible bottom after, continue upwards to be filled with high-purity argon gas in the vacuum chamber and make pressure rise to P2;
5) continue to increase the monitor system of arc gum, the scull fusing of button ingot bottom punctured, under the effect of pressure reduction △ P up and down rapidly die casting in the inner chamber of coupon mould.
Further, being evacuated to vacuum tightness step 2) is 5 * 10
-3More than the Pa, passing into high-purity argon gas to pressure is 0.02-0.06MPa again, repeats starting the arc melting and receive arc to solidify 3-10 time.
Further, described through-hole aperture size is Φ 1mm-Φ 10mm(diameter).
Further, the pressure reduction △ P between P2 and the P1 is 0.01-0.1MPa.
Further, keeping the water temperature of recirculated water in the step 4) is 18-30 ℃.
Further, step 2) arc gum carries out the low current starting the arc in, and the size of electric current is 20-50A; Raise the melting electric current gradually to 200-500A.
Further, step 4) in the step 5) in the melting curent change scope of arc gum be 50-500A.
Further, the monitor system that continues to increase arc gum in the step 5) makes electric current be increased to gradually 200-500A.
Further, it is auxiliary to carry out electromagnetic agitation step 2) in the fusion process.
Further, the tungsten that described alloy pig crucible employing conductive performance is high and thermal capacitance is large or niobium alloy are as material.
The present invention has following advantage and beneficial effect:
1. the alloy coupon of the present invention preparation, the pollution source＜0.01wt.% such as O and C, the above principal element error of 10wt% can≤0.2wt%; The element error of 1～10wt% can≤0.1wt%; The following micro-error of 1wt% can≤minimum effective accuracy; Coupon full-size can reach Ф 12mm * 120mm(diameter * length).
2. have the mosaic texture of indirect water-cooling owing to this system, thereby avoided the pollution of crucible and nozzle, make preparation process have Cleaning ability; Simultaneously, the button ingot solidifies in metal die rapidly when the short and liquation of fusing time fills type again, and coupon has kept high uniformity and the high accuracy of button ingot composition, has avoided segregation and loss; In addition, preparation process is once to inhale type casting moulding, and this device systems can be prepared 4 heterogeneity alloy coupons from melting to inhaling casting in the 8h, have high efficiency.
3. molten alloy becomes the button ingot to adopt the low current starting the arc and gradually rising means of electric current is that the size of electric current is 20-50A step 2 of the present invention); Raise the melting electric current gradually to 200-500A, in this parameter area, effectively controlled raw material and splashed.
4. alloy wraps in the auxiliary lower upset melting of electromagnetic agitation 3-10 time; Thereby can obtain better high-purity, high uniformity and high-precision desirable button ingot.
5. selected pressure reduction and the through-hole aperture of the present invention guaranteed the rapid stamp of solution, so that coupon has kept high uniformity and the high accuracy of button ingot composition, avoided segregation and loss.
The invention solves the technical deficiencies such as uneven components, Control for Oxygen Content difficulty, cycle length or complex procedures that the coupon preparation methods such as powder metallurgy, investment cast, extrusion modling and ingot casting processing exist; Can satisfy the techniques such as standard specimen preparation, alloy designs, performance test and feeding rod preparation to the strict demand of ideal alloy coupon.
Description of drawings
Fig. 1 is suction pouring device structure synoptic diagram of the present invention;
Fig. 2 is the Ti-44.5Al-3Nb-0.6Si alloy button ingot of the inventive method embodiment 1 preparation;
Fig. 3 is the metal alloy coupon that the inventive method embodiment 1 preparation is of a size of Ф 9mm * 100mm.
Sequence number among the figure, vacuum chamber on 1,2 times vacuum chambers, 3 copper crucibles, 4 alloy cast crucibles, 5 through holes, 6 metal dies, 7 water circulations, 8 button ingots, 9 arc gums, 10 is the alloy bag.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in detail:
As shown in Figure 1, be suction pouring device structure synoptic diagram of the present invention, this equipment comprises upper vacuum chamber 1 setting up and down and lower vacuum chamber 2, being provided with a plurality of station copper crucibles 3 in the upper vacuum chamber separates upper vacuum chamber 1 and lower vacuum chamber 2 sealings, pass through water circulation 7 water-cooleds around the copper crucible 3, wringing fit is inlaid with alloy pig crucible 4 in some station copper crucibles therein, and the upper end is provided with arc gum 9; Through hole 5 is left in alloy pig crucible 4 bottoms, and through hole 5 is connected upper vacuum chamber 1 and lower vacuum chamber 2, and such mosaic texture makes water circulation 7 involutory ingot crucibles 4 form the indirect water-cooling effect; During use, will treat that button ingot 8 puts into alloy pig crucible 4, and adopt arc gum 9 to carry out the argon arc melting until finish the casting process of inhaling.
Embodiment 1Ti-44.5Al-3Nb-0.6Si(at.%) preparation of alloy coupon
According to Ti-44.5Al-3Nb-0.6Si(at.%) massfraction (Ti:62.29wt.% of alloy constituent element, Al:30.21wt.%, Nb:7.01wt.%, Si:0.42wt.%) and scaling loss compensation rule (Ti and Nb do not add compensation, Al and Si all add 0.4%), employing high pure raw material by a certain percentage (Ti:Al:Nb:Si=1:0.49:0.11:0.013) is made into 10-100g alloy bag 10, and it is inserted in the copper crucible 3, is evacuated to vacuum tightness and reaches 5 * 10
-3More than the Pa, pass into again the high-purity argon gas that pressure is 0.05MPa; Under visual condition, carry out the low current starting the arc, and the melting electric current that raises gradually, avoid raw material to splash, wherein the size of low current is 20A; Raise the melting electric current gradually to 200A.Under electromagnetic agitation is assisted that the fusing of alloy bag is evenly thorough, and the receipts arc is frozen into the button ingot; With its upset melting, repeat this process 6 times afterwards, thus the high-purity of obtaining, high uniformity and high-precision button ingot, alloy button ingot as shown in Figure 2.The button ingot surface is smooth evenly as seen from the figure.
The button ingot is inserted in the alloy pig crucible, the metal die 6 of coupon is placed on below the crucible, close vacuum chamber 1 and lower vacuum chamber 2, and be evacuated to 5 * 10
-3More than the Pa, be filled with subsequently high-purity argon gas P
1To 0.06MPa; Open recirculated water and arc gum and carry out the argon arc melting, the electric current of arc gum is 70A, and circulating water temperature is 30 ℃, when button ingot top layer melt fully and the through hole of fluid-tight alloy pig crucible bottom after, continue in vacuum chamber, to be filled with an amount of high-purity argon gas and make pressure rise to P
2To 0.08MPa, form pressure reduction △ P at vacuum chamber 1 and metal die 5 inner chambers; Afterwards, the monitor system that continues to increase arc gum to the electric current of arc gum increases to 400A gradually, after a few minutes, the heat for the treatment of arc gum punctures the scull fusing of button ingot bottom, liquid under the effect of pressure reduction △ P up and down rapidly die casting in the inner chamber of coupon metal die 6, be frozen into rapidly the alloy coupon, the through-hole aperture size is Φ 8mm in the present embodiment.As shown in Figure 3, the coupon smooth surface, evenly.After testing, alloy button ingot in this alloy coupon, the pollution source＜0.01wt.% such as O and C, Ti and Al principal element error≤0.2wt%; Nb element error≤0.1wt%, details such as table 1.The prepared Ф 9mm * 100mm that is of a size of.
The chemical analysis results of table 1Ti-44.5Al-3Nb-0.6Si coupon different parts
The result shows: the central constituent element content of each several part is even in the coupon.Near calculated value.
Be with the difference of embodiment 1, the alloy bag inserted in the copper crucible 3 of equipment among the present invention, be evacuated to vacuum tightness and reach 8 * 10
-3More than the Pa, pass into again the high-purity argon gas that pressure is 0.06MPa; Under visual condition, carry out the low current starting the arc, and the melting electric current that raises gradually, avoid raw material to splash, wherein the size of low current is 30A; Raise the melting electric current gradually to 500A.Under electromagnetic agitation is assisted that the fusing of alloy bag is evenly thorough, and the receipts arc is frozen into the button ingot; With its upset melting, repeat this process 10 times afterwards, thus the high-purity of obtaining, high uniformity and high-precision button ingot, and the visible button ingot surface of result is smooth evenly.
The button ingot is inserted in the alloy pig crucible, the metal die of coupon is placed on below the crucible, close vacuum chamber 1 and lower vacuum chamber 2, and be evacuated to 9 * 10
-3More than the Pa, be filled with subsequently high-purity argon gas P
1To 0.04MPa; Open recirculated water and arc gum and carry out the argon arc melting, the electric current of arc gum is 100A, circulating water temperature is 18 ℃, when button ingot top layer melt fully and the through hole of fluid-tight alloy pig crucible bottom after, continue in vacuum chamber, to be filled with an amount of high-purity argon gas and make pressure rise to P
2To 0.09MPa, form pressure reduction △ P at vacuum chamber 1 and metal die 5 inner chambers; Afterwards, the monitor system that continues to increase arc gum to the electric current of arc gum increases to 500A gradually, after a few minutes, the heat for the treatment of arc gum punctures the scull fusing of button ingot bottom, liquid under the effect of pressure reduction △ P up and down rapidly die casting in the inner chamber of coupon metal die 6, be frozen into rapidly the alloy coupon, the through-hole aperture size is Φ 5mm in the present embodiment.The result shows, the coupon smooth surface, evenly.After testing, alloy button ingot in this alloy coupon, the pollution source＜0.01wt.% such as O and C, Ti and Al principal element error≤0.2wt%; Nb element error≤0.1wt%.
Claims (8)
1. the preparation method of a metal alloy coupon, it is characterized in that, adopt suction pouring equipment, utilizing draught head to inhale casts to mould molding, described suction pouring equipment comprises upper vacuum chamber setting up and down and lower vacuum chamber, upper vacuum chamber top is provided with arc gum, and the bottom is provided with a plurality of station copper crucibles upper vacuum chamber and the sealing of lower vacuum chamber are separated, and passes through the water circulation water-cooled around the copper crucible; Wringing fit is inlaid with the alloy pig crucible in station copper crucible therein, and through hole is left in the bottom, and upper vacuum chamber and lower vacuum chamber are connected; Concrete preparation process is:
1) according to mass ratio and the scaling loss compensation rule of alloy constituent element, adopt high pure raw material to be made into 10-100g alloy bag;
2) the alloy bag is placed described copper crucible, pass into high-purity argon gas after vacuumizing, arc gum carries out receiving after the starting the arc melting arc and solidifies and make the button ingot;
3) the button ingot is inserted in the alloy pig crucible, the metal die of coupon is placed below the lower vacuum chamber crucible, closing apparatus, and be evacuated to 5 * 10
-3More than the Pa, be filled with high-purity argon gas P1 to 0.02-0.06MPa;
4) open recirculated water and arc gum and carry out the argon arc melting, when button ingot top layer melt fully and the through hole of fluid-tight alloy pig crucible bottom after, continue upwards to be filled with high-purity argon gas in the vacuum chamber and make pressure rise to P2, the pressure reduction △ P between P2 and the P1 is 0.01-0.1MPa;
5) continue to increase the monitor system of arc gum, the scull fusing of button ingot bottom punctured, under the effect of pressure reduction △ P up and down rapidly die casting in the inner chamber of coupon mould.
2. according to the preparation method of metal alloy coupon claimed in claim 1, it is characterized in that step 2) in to be evacuated to vacuum tightness be 5 * 10
-3More than the Pa, passing into high-purity argon gas to pressure is 0.02-0.06 MPa again, repeats starting the arc melting and receive arc to solidify 3-10 time.
3. according to the preparation method of metal alloy coupon claimed in claim 1, it is characterized in that described through-hole aperture size is Φ 1mm-Φ 10mm.
4. according to the preparation method of metal alloy coupon claimed in claim 1, it is characterized in that keeping the water temperature of recirculated water in the step 4) is 18-30 ℃.
5. according to the preparation method of metal alloy coupon claimed in claim 1, it is characterized in that step 2) in arc gum carry out the low current starting the arc, the size of electric current is 20-50A; Raise the melting electric current gradually to 200-500A.
6. according to the preparation method of metal alloy coupon claimed in claim 1, it is characterized in that, step 4) in the step 5) in the melting curent change scope of arc gum be 50-500A.
7. according to the preparation method of claim 1 or 2 described metal alloy coupons, it is characterized in that step 2) in to carry out electromagnetic agitation in the fusion process auxiliary.
8. according to the preparation method of metal alloy coupon claimed in claim 1, it is characterized in that the tungsten that described alloy pig crucible employing conductive performance is high and thermal capacitance is large or niobium alloy are as material.
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| CN201210327400.4A CN102901659B (en) | 2012-09-06 | 2012-09-06 | Preparation method for metal alloy test rod |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104073661A (en) * | 2014-06-27 | 2014-10-01 | 梁永忠 | Preparation method of zinc alloy applied to pressure casting |
| CN104894413A (en) * | 2015-04-16 | 2015-09-09 | 新疆大学 | Copper and copper alloy temperature control-pressure regulation smelting method |
| CN105290328A (en) * | 2015-11-10 | 2016-02-03 | 沈阳黎明航空发动机(集团)有限责任公司 | Method for reducing microporosity during casting of high-temperature alloy test bar |
| CN105331828A (en) * | 2015-11-09 | 2016-02-17 | 云南钛业股份有限公司 | Metallurgy fastener furnace copper crucible and smelting method thereof |
| CN110864947A (en) * | 2019-11-15 | 2020-03-06 | 江苏隆达超合金航材有限公司 | Preparation method of sample for rapidly determining chemical components in alloy slag |
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| CN102534272A (en) * | 2010-12-15 | 2012-07-04 | 李庆新 | Processing method for high vacuum smelting of cobalt base molybdenum magnesium alloy |
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Patent Citations (6)
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| JPH02295669A (en) * | 1989-05-09 | 1990-12-06 | Kobe Steel Ltd | Suction casting method |
| JPH0740032A (en) * | 1993-07-28 | 1995-02-10 | Toyota Motor Corp | Metal mold casting method and its device |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104073661A (en) * | 2014-06-27 | 2014-10-01 | 梁永忠 | Preparation method of zinc alloy applied to pressure casting |
| CN104894413A (en) * | 2015-04-16 | 2015-09-09 | 新疆大学 | Copper and copper alloy temperature control-pressure regulation smelting method |
| CN105331828A (en) * | 2015-11-09 | 2016-02-17 | 云南钛业股份有限公司 | Metallurgy fastener furnace copper crucible and smelting method thereof |
| CN105290328A (en) * | 2015-11-10 | 2016-02-03 | 沈阳黎明航空发动机(集团)有限责任公司 | Method for reducing microporosity during casting of high-temperature alloy test bar |
| CN105290328B (en) * | 2015-11-10 | 2017-06-13 | 沈阳黎明航空发动机(集团)有限责任公司 | A kind of method for reducing microporosity in cast superalloy coupon |
| CN110864947A (en) * | 2019-11-15 | 2020-03-06 | 江苏隆达超合金航材有限公司 | Preparation method of sample for rapidly determining chemical components in alloy slag |
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