Summary of the invention
Goal of the invention
Purpose of the present invention is exactly at the present situation of background technology and deficiency; adopt a kind of new smelting technique and alloyage process; in high temperature melting furnace; under vacuum state; under the protection of argon gas, the water cycle cooling is synthesized nickel aluminium vanadium ternary alloy by high-temperature aging, melting, the preparation of long period down; make the synthetic nickel aluminum vanadium alloy of preparation become possibility, with intensity, plasticity, toughness and the resistance to elevated temperatures that increases substantially alloy.
Technical scheme
Raw chemical material and subsidiary material that preparation is used are nickel, aluminium, vanadium, acetone, deionized water, argon gas, boron nitride, sand grains, and its consumption is as follows: with gram, milliliter, centimetre
3Be measure unit
Nickel: Ni 1220g ± 1g
Aluminium: Al 75g ± 1g
Vanadium: V 210g ± 1g
Acetone: CH
3COCH
3800ml ± 10ml
Deionized water: H
2O 2000ml ± 10ml
Argon gas: Ar 1000000cm
3± 1000cm
3
Boron nitride: BN 40g ± 1g
Sand grains: 5000g
The preparation method is as follows:
(1) selected raw chemical material
Required raw chemical material is carried out selected, and carries out control of purity:
Nickel: sheet material 99.99%
Aluminium: sheet material 99.98%
Vanadium: particle 99.99%
Acetone: liquid 99.95%
Deionized water: liquid 99.99%
Argon gas: gas 99.95%
Boron nitride: powder 99.5%
Sand grains: fineness 200 orders
(2) starting material preprocessing
1. nickel: sheet material cuts into 100 * 20 * 5mm bar shaped bulk
2. aluminium: sheet material cuts into 100 * 20 * 5mm bar shaped bulk
3. vanadium: pulverize, sieve, carry out repeatedly, particle diameter≤φ 6mm;
(3) clean vacuum smelting furnace
1. open the vacuum melting furnace top cover, with suction cleaner suction in-furnace dust dirt and objectionable impurities, time 5min;
2. scrub body of heater, bell inwall with deionized water 500ml, make its cleaning;
3. use acetone 200ml, scrub, clean fire door, bell mouth, make its cleaning;
4. dry body of heater, bell inwall, fire door, bell mouth, make vacuum melting furnace be in clean state;
(4) cleaning smelting pot
1. with metal slice cleaning smelting pot inside and outside wall scar and impurity;
2. with suction cleaner suction crucible inside and outside wall dust;
3. use acetone 200ml cleaning crucible inwall, make its cleaning;
4. dry crucible;
(5) clean casting mould, preheating, coating releasing agent
1. the alloy tool steel die that casting is used will be cleared up die cavity, rejects residue and objectionable impurities with metallic brush, shovel;
2. scrub mold cavity and outside with deionized water, make it clean, dry then;
3. dispose releasing agent: boron nitride 40g+ deionized water 100ml becomes liquid pasty state;
4. mold integral is put into drying baker and carry out preheating, 200 ℃ ± 5 ℃ of preheating temperatures, time 30min ± 2min;
5. apply releasing agent, in mold cavity, evenly brush releasing agent with metallic brush, releasing agent thickness 0.05mm dries standby;
(6) put alloy raw material
The blocky nickel 1220g ± 1g of bar shaped, aluminium 75g ± 1g are vertically put into crucible, and particulate state vanadium 210g ± 1g is filled in the space, closely knit layout;
(7) put casting die
Preheating and the casting die that applied the releasing agent boron nitride are placed the below, right side of smelting pot, be beneficial to the position of casting;
(8) connect tunger tube up and down
1. connect the argon gas pneumatic tube of upper of furnace body;
2. connect the argon gas bottom blowpipe of crucible bottom;
(9) smelting furnace extracting vacuum
1. the melting bell is covered on the body of heater, and sealing;
2. open mechanical sliding vane rotary pump, lobe pump, extract furnace air out, time 20min ± 2min;
3. open diffusion pump, extract vacuum in the stove, time 80min ± 2min makes vacuum tightness in the furnace chamber≤4 * 10
-3Pa;
(10) input protection gas-argon gas in stove
Open the upper of furnace body tunger tube, in furnace chamber, import argon gas, input speed 50000cm
3/ min, input time, 10min ± 1min made to be in the argon gas atmosphere in the furnace chamber;
After the argon gas input, the furnace chamber internal gas pressure continues to remain on 0.5 * 10
5Pa;
(11) the water cycle cooling body of unlatching smelting furnace outside carries out the body of heater cooling;
(12) melting, casting nickel aluminum vanadium alloy
1. open the smelting pot well heater, make the interior temperature of smelting pot begin to heat up by 20 ℃ ± 3 ℃, 30 ℃/min of heat-up rate is warming up to 1900 ℃ ± 5 ℃, heating-up time 60min ± 2min;
2. after the fusing of nickel aluminium vanadium raw materials, open the defeated argon pipe of crucible bottom, be blown into argon gas, be blown into speed 5000cm
3/ min, and form argon stream, promote alloying element nickel+aluminium in the crucible+vanadium liquation and form stirring stream, continue to be blown into argon gas time 10min ± 1min, make alloying element mix fusion evenly;
3. alloying element will carry out alloying reaction in the Argon fusion process, and reaction formula is as follows:
In the formula:
Ni
3AlV: nickel aluminum vanadium alloy;
4. after the alloy liquation melting in the crucible, adjust power, make it cooling, when reducing to 1500 ℃ ± 5 ℃, 10min ± 1min is left standstill in constant temperature, insulation under this temperature;
5. in the melting furnace chamber, in argon gas atmosphere, the crucible that fills the nickel aluminum vanadium alloy liquation is aimed at the casting die of bottom right sidepiece, the alloy liquation is poured into dies cavity, water and stop after full;
6. the closing crucible well heater cuts out bottom Argon pipe, and in argon gas atmosphere, under vacuum state, the mould after the casting cools to 300 ℃ ± 5 ℃ with the furnace, time 60min ± 1min;
(13) cooling of coming out of the stove
1. close top argon-filled tube, vacuum diffusion pump, open the melting bell, take out casting die;
The casting die that 2. ingot casting will be housed places the exsiccant fine sand, is cooled to 20 ℃ ± 3 ℃ in physical environment;
(14) demoulding is got ingot and is cleared up finishing
1. take out ingot casting, with brush, shovel, emery cloth cleaning ingot casting scar;
2. use lathe finish turning ingot casting cylindrical and end face, become nickel aluminum vanadium alloy product φ 60 * 60mm;
3. with 400,600 grit papers polishing alloy product surface, making surfaceness is Ra0.16-0.32 μ m;
(15) high-temperature aging is handled
The nickel aluminum vanadium alloy product of finishing is carried out the high-temperature aging processing;
1. the nickel aluminum vanadium alloy product with φ 60 * 60mm places on the work stage of high-temperature aging stove;
2. close the high-temperature aging stove, make its sealing;
Open vacuum pump, extract the timeliness furnace air, vacuum tightness is 1 * 10
-3Pa;
3. connect tunger tube, input argon gas, input speed 3000cm
3/ min ± 100cm
3/ min makes the interior pressure of stove continue to remain on 1 * 10
-1Pa;
4. open high-temperature aging stove well heater, temperature is warming up to 750 ℃ ± 3 ℃, 25 ℃/min of heat-up rate, heating-up time 30min by 20 ℃ ± 3 ℃;
5. when temperature rises to 750 ℃ ± 3 ℃, stop to heat up, in this temperature constant temperature, insulation, in argon gas atmosphere, under vacuum state, timeliness 1100h ± 1h is the nickel aluminum vanadium alloy finished product after the timeliness;
(16) naturally cooling
The nickel aluminum vanadium alloy finished product that high-temperature aging is handled places clean physical environment to be cooled to 20 ℃ ± 3 ℃;
(17) detect, analyze, chemically examine
The nickel aluminum vanadium alloy finished product that high-temperature aging is handled detects, chemically examines, analyzes, and detects its composition, color and luster, mechanical and physical performance;
1. carry out chemical composition analysis with spectrograph:
Nickel: aluminium: vanadium=75.12: 9.86: 15.02;
2. carry out metallographic structure crystal grain state analysis with transmission electron microscope;
3. carry out the mechanical property analysis with universal testing machine:
Hardness: HV590
Tensile strength: 1102MPa
Yield strength: 910MPa
Impelling strength: 30J/cm
2
Extensibility: 18%
(18) storage package
The nickel aluminum vanadium alloy finished product of preparation to be packed with soft material, place clean environment, waterproof, protection against the tide, anti-oxidation, anti-acid and alkali corrosion, 20 ℃ ± 3 ℃ of storing temps, relative humidity≤20%.
The rounded closed jar of described vacuum melting furnace shape, the mid-way is provided with smelting pot 14 in body of heater 7, smelting pot 14 outsides by ruhmkorff coil 15 around, crucible 14 bottoms connect argon blowing hole 19, argon blowing hole 19 connects Argon pipe 20, Argon valve 21, argon bottle 24, crucible 14 lower right side are provided with casting die 16, casting die top is provided with pouring gate 17, body of heater 7 tops are bell 11, the mid-way is provided with feeder 8 on the bell 11, thermoscope 9, and go deep into crucible 14 internal upper parts, bell 11 upper right quarters are provided with viewing window 10, pore 18, bell 11 upper left quarters are provided with argon gas mouth 29, and connect tunger tube 22, argon gas valve 23, argon bottle 24, the middle and upper part of body of heater 7 by water cycle prolong 12 around, the left side central portion of body of heater 7 is provided with dust removal filter 6, in the furnace chamber 28 that body of heater 7 and bell 11 sealing backs form is argon gas 25, is nickel aluminum vanadium alloy liquation 26 in the crucible 14, is nickel aluminum vanadium alloy ingot 27 in the casting die 16.
The chemical ingredients ratio of described nickel aluminum vanadium alloy product is: nickel: aluminium: vanadium=75.12: 9.86: 15.02.
The smelting temperature of described nickel aluminum vanadium alloy is 1900 ℃ ± 5 ℃; smelting time is 10min ± 1min; constant temperature, insulation, dwell temperature are 1500 ℃ ± 5 ℃; time of repose is 10min ± 1min; blow at vacuum state, argon shield, argon gas, finish under the water cycle cooling, vacuum tightness continues to remain on 0.5 * 10
5Pa.
The aging temp of described nickel aluminum vanadium alloy is 750 ℃ ± 3 ℃, and aging time is 1100h ± 1h, carries out under vacuum state, argon shield, and vacuum tightness continues to remain on 1 * 10
-1Pa.
Beneficial effect
The present invention compares with background technology; has tangible advance; make the preparation nickel aluminum vanadium alloy become possibility; it is the deficiency at the alumel mechanical property; on the basis of alumel, add the metallic element vanadium; be prepared into novel nickel aluminium vanadium high temperature alloy; in preparation process, adopt accurate proportioning raw materials, selected raw chemical material; precut is pulverized; the cleaning smelting furnace; smelting pot; casting die, extracting vacuum, input argon gas; Argon stirs; the water cycle cooling, high melt, casting; make the nickel aluminum vanadium alloy ingot; cooling back finishing ingot casting surface is then at high temperature; vacuum; under the argon shield, carry out the long period ageing treatment; finally make the nickel aluminum vanadium alloy product; its smelting temperature is 1900 ℃, 750 ℃ of aging temps, aging time 1100h; the nickel aluminum vanadium alloy product stable mechanical property of preparation; its hardness can reach HV590, and tensile strength can reach 1102MPa, and yield strength can reach 910MPa; extensibility can improve 50%; impelling strength can improve 43%, and high temperature resistant fusing point can reach 1394 ℃, this preparation method; technology is reasonable; be the method that ideal prepares nickel aluminum vanadium alloy, this preparation method also can be used for the preparation of similar high temperature alloy.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing
Shown in Figure 1, be preparation technology's schema, each preparation parameter is wanted strict control, operation according to the order of sequence.
Preparing required raw chemical material and subsidiary material is to determine by the amount ratio that sets in advance, with gram, milliliter, centimetre
3Be measure unit, when carrying out industrialization and produce, can kilogram, rise, rice
3Be measure unit, and carry out corresponding calculating.
Prepare required smelting furnace, smelting pot, casting die and want strictness to clear up, clean, the melting nickel aluminum vanadium alloy is carried out under clean state, prevent the impurity intervention, in order to avoid influence the mechanical property of the chemical reaction and the product of alloy.
Want strict seal between smelting furnace body of heater and the bell, unaffected to guarantee the vacuum tightness in the furnace chamber.
The melting nickel aluminum vanadium alloy carries out under vacuum state, so the vacuum tightness in the furnace chamber is crucial, vacuumizing available two steps finishes, extract air in the furnace chamber out with sliding vane rotary pump, lobe pump earlier, time is 20min ± 2min, and then vacuumize with diffusion pump, make that vacuum tightness reaches in the furnace chamber≤4 * 10
-3Pa, and keep.
The melting of nickel aluminum vanadium alloy be under the whole process protection of inert protective gas-argon gas, blowing under the stirring of argon gas finish; the input of argon gas is crucial; argon gas atmosphere is finished by the tunger tube input in the furnace chamber, to guarantee having enough argon gas to blow the liquation vibration, it is mixed.
In argon filling, Argon process, make the furnace chamber internal gas pressure remain on 0.5 * 10 all the time
5Pa, and open the argon gas production well, make to press in the furnace chamber to keep balance, be beneficial to safety.
The water cycle cooling of melting body of heater is crucial, in order to guarantee body of heater melting under continuous high temperature, continue to carry out the water cycle cooling of body of heater, to increase the security of body of heater.
The casting of nickel aluminum vanadium alloy is finished in the melting furnace chamber, after the melting of alloy liquation, the crucible inner melt be aimed at the casting die pouring gate, water full till, make it become ingot, cool to 300 ℃ ± 5 ℃ with the furnace, the back of coming out of the stove is imbedded in the exsiccant fine sand together with ingot casting, naturally cools to 20 ℃ ± 3 ℃ in air, take out ingot casting then, after the cleaning,, become the nickel aluminum vanadium alloy product of φ 60 * 60mm through surface-conditioning, finish turning.
Nickel aluminum vanadium alloy product after surperficial finish turning, polishing will carry out high-temperature aging in aging oven; will be under vacuum state, under the argon shield; continue timeliness 1100h ± 1h; after the long period timeliness; finally make the nickel aluminum vanadium alloy finished product, carry out composition, mechanical property detection then, analyze, contrast.
Shown in Figure 2, be vacuum melting furnace one-piece construction figure, sliding vane rotary pump 1 connects lobe pump 3 through magnetic valve 2, lobe pump 3 connects diffusion pump 5 through pneumavalve 4, and diffusion pump 5 connects body of heater 7 through dust removal filter 6, and body of heater 7 tops are bell 11, bell 11 tops are provided with viewing window 10, feeder 8, thermoscope 9, production well 18, the right part of body of heater 7 is provided with electric control box 13 and is connected by lead, and the rear portion of body of heater 7 is provided with argon bottle 24, and is connected by tunger tube.
Shown in Figure 3, be smelting furnace melting state graph, body of heater 7 is wanted strict clean seal with bell 14, and with vacuum tightness in the holding chamber, pore 18 is pores from inside to outside, when the argon gas amount is excessive in the chamber, can discharge a small amount of argon gas this moment, so that pressure equilibrium in the chamber, thermoscope 9 can be measured the crucible for smelting temperature at any time, viewing window 10 can be observed crucible for smelting and blow situation and handle the casting situation, and water cycle cooling tube 12 uninterruptedly carries out in fusion process.
Figure 4 shows that smelting temperature and time coordinate graph of a relation, among the figure as can be known: ordinate zou is a temperature value, and X-coordinate is a time value, temperature begins to heat up by 20 ℃, be the A point, heat-up rate is 30 ℃/min, when temperature rises to 1900 ℃ ± 5 ℃, it is the B point, at this temperature constant temperature, be incubated, leave standstill, alloy reaction, i.e. B-C section, be cooled to 1500 ℃ then, be the D point, and constant temperature, be incubated, leave standstill, the uniform alloy composition, it is the D-E section, cooling then, cooling is reduced to 300 ℃ by the E point, be the F point, take out mould and ingot casting in this temperature.
Shown in Figure 5, be high-temperature aging temperature and product yield strength coordinate graph of a relation, ordinate zou is yield strength MPa, X-coordinate is a temperature ℃, among the figure as can be known: nickel aluminum vanadium alloy is when 750 ℃ ± 3 ℃ of aging temps, and its mechanical property yield strength is best, i.e. the H point, G, J, K, M point effect are relatively poor, so aging temp is chosen as 750 ℃ ± 3 ℃.
Shown in Figure 6, be that the nickel aluminum vanadium alloy square section amplifies 1000 times of metallurgical structure figure, among the figure as can be known: metallographic structure compactness is good, and the disperse of crystal grain precipitated phase distributes, and is more even, is irregular alignment, and alloying is outstanding, ruler units 10 μ m.
Shown in Figure 7, be nickel aluminum vanadium alloy and alumel mechanical property contrast table, in the table as can be known: the mechanical property of nickel aluminum vanadium alloy is better than alumel, its hardness can reach HV590, yield strength can reach 910MPa, tensile strength can reach 1102MPa, and extensibility can improve 50%, and impelling strength can improve 43%.