CN104988342B - A kind of zircaloy melting and casting method - Google Patents
A kind of zircaloy melting and casting method Download PDFInfo
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- CN104988342B CN104988342B CN201510458819.7A CN201510458819A CN104988342B CN 104988342 B CN104988342 B CN 104988342B CN 201510458819 A CN201510458819 A CN 201510458819A CN 104988342 B CN104988342 B CN 104988342B
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- 229910001093 Zr alloy Inorganic materials 0.000 title claims abstract description 92
- 238000005266 casting Methods 0.000 title claims abstract description 73
- 230000008018 melting Effects 0.000 title claims abstract description 70
- 238000002844 melting Methods 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 54
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 37
- 239000000956 alloy Substances 0.000 claims abstract description 37
- 238000003723 Smelting Methods 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 238000005275 alloying Methods 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 25
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- 239000002002 slurry Substances 0.000 claims description 20
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 17
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 6
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 description 5
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- 229910052845 zircon Inorganic materials 0.000 description 3
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
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- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
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Landscapes
- Filtering Materials (AREA)
Abstract
A kind of zircaloy melting and casting method, comprise the following steps：Step one, melting once, the composition of sample analysis zircaloy ingot casting determine the alloying element for requiring supplementation with；Step 2, secondary smelting adjust alloying component, and stirring makes the component of zircaloy melt uniform；Step 3, purifies technological preparation, and the running channel that would be embedded with filter medium is preheating to 1,000 1200 DEG C；Ingot mould prepares, and ingot mould removing surface is clean, and no impurity and greasy dirt adhere to；Step 4, casting and purification, the zircaloy melt of melting is poured in running channel, and zircaloy melt is intercepted and adsorbed by filter medium by filter medium, the impurity in its alloy melt, and clean zircaloy melt is flowed in ingot mould, is cooled into ingot casting.This method is easy to operate, energy consumption is lower, clean-up effect is more preferable.
Description
Technical field
The present invention relates to zircaloy melting and casting method.
Background technology
At present, content of the zirconium in the earth's crust is very abundant, occupies the 20th by abundance, the improved corrosion performance of metal zirconium and high
The characteristic such as fusing point (1860 DEG C), be the new structure material of great application potential in Aero-Space and ship and nuclear power field
Material.Zirconium is close-packed hexagonal structure, referred to as a phases in room temperature, and its distinguishing feature is that room temperature tensile intensity is very low, less than 400MPa,
Requirement of the structural material to mechanical property cannot be met, therefore, in addition to being applied in nuclear industry, in other engineering fields very
Lack as structural material to apply, so far rarely found report, α-Zr occur allotropic transformation at 865 DEG C, are changed into body-centered
Cube β-Zr.As the range of application of Other Engineering material starts limitation occur, as zircaloy has its unique power
Learn and corrosion resistance, zircaloy initially enters the visual field of engineering field.The patent of Publication No. CN102260807A is by certainly
Consumption electric arc furnace method melting zircaloy, exist melting often, consume energy big defect.
The content of the invention
The technical problem to be solved in the present invention is to provide that a kind of easy to operate, energy consumption is lower, the more preferable zirconium of clean-up effect is closed
Golden melting and casting method.
In order to solve above-mentioned technical problem, the invention provides a kind of zircaloy melting and casting method, including following step
Suddenly：
The zircaloy of the identical trade mark is returned material and is put in the crucible of vacuum melting furnace by step one, melting once, vacuum
For 0.001-0.1Pa, abundant dried argon is then charged with, smelting temperature is 1000-1500 DEG C, and smelting time is 30-60
Minute, after zircaloy melts completely, pour in the filter plant for be embedded with filter medium and cast；After ingot casting cooling, open
Vacuum drying oven, takes out ingot formation, the exocuticle of alloy is disposed 1-2 millimeters, then the composition of sample analysis zircaloy ingot casting,
According to the requirement of alloy designations, calculating composition deviation, the alloying element for requiring supplementation with is determined；
Step 2, secondary smelting adjust alloying component, by the various alloying element simple substance of the alloying element deviation for making up or
Intermediate alloy, is together put into vacuum melting furnace with the zircaloy ingot casting of melting once, and vacuum is 0.001-0.1Pa, Ran Houchong
Enter abundant dried argon, 1000～1500 DEG C of smelting temperature, smelting time are 30～60 minutes, and stirring makes zircaloy melt
Component it is uniform；
Step 3, purifies technological preparation, and the running channel that would be embedded with filter medium is preheating to 1000-1200 DEG C；Ingot mould prepares,
By ingot mould removing surface totally, no impurity and greasy dirt attachment；
Step 4, casting and purification, the zircaloy melt of melting is poured in running channel, and zircaloy melt is situated between by filtering
Matter, the impurity in its alloy melt are intercepted and are adsorbed by filter medium, and clean zircaloy melt is flowed in ingot mould, are cooled down
Form ingot casting.
It is preferred that, the running channel and filter medium are constituted by contact material, and the contact material is by ceramics
Material and enhancing stabilizer composition, the ceramic powder is by MgO and ZrO26-12 in molar ratio:100 compositions, strengthen stabilizer by weight
Than the 0.5%-1% for ceramic powder, the enhancing stabilizer is cerium-rich rare earth to amount.
It is preferred that, the preparation method of the contact material is comprised the following steps：
Step 1, by ceramic powder and enhancing stabilizer mix homogeneously；
Step 2, wet ball grinding 20-24 hours, 80-100 DEG C of crushed after being dried；
Step 3, calcines 1.5-6 hours at 1400-1450 DEG C, and cooling is crushed；
Step 4, wet ball grinding 24-48 hours, crushed after being dried, screening at 80-100 DEG C.
It is preferred that, the preparation method of the filter medium is comprised the following steps：
Three-dimensional polyurethane foam sponge skeleton is immersed the NaOH solution that concentration is 10%～20% by step 1, pre-treatment
In, 2～4h is hydrolyzed at a temperature of 40～60 DEG C, is then rubbed repeatedly and is dried after presoma being rinsed with clear water, it is dry so as to clean
Net sponge；
Step 2, slurrying are progressively added on polyvinyl alcohol in water first, until the viscosity of polyethylene alcohol and water is 40-
50CPS and pH value are controlled at 40-50 DEG C, are stirred in 5-7, aqueous temperature, while add defoamer, by 200 mesh and
400 mesh contact materials are according to 3：1 weight ratio is poured in above-mentioned solution, is stirred, obtain slurry, 200 mesh contact materials and
The weight of 400 mesh contact materials accounts for the 75-85% of slurry weight；
Step 3, is coated with, and the three-dimensional polyurethane foam sponge skeleton that step 1 is obtained is immersed in the slurry that step 2 is obtained
In, fully discharge the gas in skeleton so as to which surface and inner homogeneous are coated with spreading mass, pull out；
Step 4, dries in the shade naturally and dries, and will be coated with being positioned at shady and cool ventilation of three-dimensional polyurethane foam sponge skeleton,
Carry out process of drying in the shade, 4-48 hours of drying in the shade make the semi-finished product to be dried of ceramic filter, by the filter medium after drying in the shade half into
Product are put in drying oven and are dried, and the programming rate of drying oven is 0.5-5 DEG C/min, is warmed up to 90-120 DEG C, and 1-2 is little for insulation
When, then furnace cooling, makes the semi-finished product to be sintered of filter medium；
Step 5, sintering, i.e., low-temperature space, more than 500 DEG C to 1200 DEG C～1570 DEG C of middle warm area below 500 DEG C and
Sinter in 1570 DEG C of high-temperature region, when sintering in low-temperature space, less than 200 DEG C programming rates are 2-5 DEG C/min, more than 200 DEG C
Be 1-3 DEG C/min to 400 DEG C of programming rates, 30 minutes are incubated when rising to 400 DEG C, are then warmed up to 500 with the speed of 3 DEG C/min
℃；When sintering in middle warm area, more than 500 DEG C to 1150 DEG C, speed is 4-5 DEG C/min；1150 DEG C to 1570 DEG C, this will in stage
Programming rate controls to be incubated 1 hour in 3-4 DEG C/min and at 1300 DEG C；When sintering in high-temperature region, 6-10 is incubated at 1570 DEG C
Hour, then furnace cooling, makes filter medium.
It is preferred that, in the step 2, the rotating speed for stirring polyethylene alcohol and water is 70～100 revs/min.
It is preferred that, in the step 2, the speed stirred after adding contact material is 80-150 rev/min.
It is preferred that, in the step 2, defoamer accounts for the 0.1%～1% of polyethylene alcohol and water gross weight.
It is preferred that, the preparation method for being embedded with the running channel of filter medium is comprised the following steps：
Step 1, making aluminum dipping form, make two aluminum dipping forms that are symmetrical, matching with the hollow part in running channel；
Step 2, casting, open aluminum dipping form, filter medium are put into aluminum dipping form position corresponding with filter cavity, after the aluminum dipping form that closes
Casting, makes wax be full of inside aluminum dipping form and filter medium；
Step 3, hanging sand, after wax solidification, open aluminum dipping form and take out the wax-pattern with filter medium, blow the filtration of wax melting mould and be situated between
The wax on surface at matter, until wax pattern surface exposes filter medium, is coated with contact material until desired thickness repeatedly in wax pattern surface
And dry in the shade 4～128 hours；
Step 4, wax melting, the product that step 3 is obtained is put in hot water, and wax melts disengaging in the process, the moon after pulling out
It is dry 8～24 hours；
Step 5, sintering, the product that sintering step 4 is obtained at 1050～1250 DEG C are simultaneously incubated 30min～2h, contact material
Material sinters shell into, in the embedded shell of filter medium, obtains the running channel with filter medium.
It is preferred that, in step 3, when wax pattern surface is coated with contact material, the contact material of 400 mesh is first coated with,
Then the contact material of 200 mesh is coated with the contact material of 400 mesh.
The melting of this zircaloy and casting method are had the advantage that compared with prior art：Step is simple, than consumable electric arc
Stove method reduces melting number of times, save energy consumption；Being mingled with for zircaloy is few, the content pole of the impurity element such as O, S, P, N, C
It is low, the structure of alloy is improved, the mechanical property of alloy is improved；Compared with foundry alloy, no significant difference reduces zirconium
The degradation of alloy is used, and is improve economic results in society, is realized the purpose of recycling.
Further, running channel and filter medium are made by contact material, and contact material adopts ZrO2As material of main part
To avoid reacting with zircaloy, in ZrO2Middle addition MgO and cerium-rich rare earth, are prepared by operations such as wet ball grinding, calcinings and are drawn,
The addition of MgO and cerium-rich rare earth and above-mentioned process are conducive to stable crystal form, obtain stable tetragonal structure ZrO2, it is to avoid it is pure
ZrO2Because of change in volume and heat effect caused by crystal conversion, so as to ensure its performance.In addition to zircaloy, this contact material and
Filter medium can be additionally used in purifying the activity metal or alloy lower than zirconium.
Further, preparation the method for filter medium used by the present invention is by the use of three-dimensional polyurethane foam sponge as bone
Frame, is coated with slurry in skeleton and obtains filter medium through drying and sintering procedure, by the three-dimensional for selecting different aperture density
Polyurethane foam sponge prepares the filter medium of different aperture density as skeleton, so as to intercept various sizes of impurity；Pass through
The programming rate of control sintering, completes stress relieving and avoids blind crack, with good normal temperature strength and elevated temperature strength, energy
Temperature change in purification process is adapted to enough, it is ensured that clean-up effect.
Further, running channel used by the present invention is made using above-mentioned contact material and purification medium, the preparation method of running channel
The characteristics of making full use of filter media surface to be covered with hole, is put into aluminum dipping form by making aluminum dipping form, by filter medium and casting is formed
Wax-pattern, simultaneously also running channel, wax melting are formed in filter media surface hanging sand in wax pattern surface and sinter shell into, filter medium here
During be embedded in running channel, so as to prepare integrally formed running channel, in the embedded running channel of filter medium, can guarantee that all zircaloys
Melt is intercepted by filter medium without dead angle, improves clean-up effect.
Description of the drawings
Sectional views of the Fig. 1 for filter plant.
Axonometric charts of the Fig. 2 for filter medium.
Fig. 3 is the front sectional view of many crucibles.
Specific embodiment
For effectively purification zircaloy, it is to avoid zircaloy melt is reacted with contact material, and the present invention can be kept away firstly the need of preparing
Exempt from the contact material with zircaloy reaction, this contact material mainly adopts zirconium oxide, and zirconium oxide can be prevented effectively from anti-with zircaloy
Should, but zirconium oxide has three kinds of crystal formations, and low temperature is monoclinic system, and high temperature is to be changed into cubic system under tetragonal crystal system, higher temperature,
Change in volume of the transformation between monoclinic crystal and tetragonal with 7%-9%, during heating, monoclinic crystal is changed into tetragonal, body
Product is shunk；During cooling, tetragonal is changed into monoclinic crystal, volumetric expansion, as crystal conversion causes bulk effect, so with pure
ZrO2It is difficult to manufacture stable finished product, it is necessary to carry out stable crystal form process.
Embodiment 1
The contact material of the present embodiment is made up of ceramic powder and enhancing stabilizer, and the ceramic powder is by MgO and ZrO2
In molar ratio 6:100 compositions, strengthen stabilizer by weight 0.5% for ceramic powder, and the enhancing stabilizer is preferably richness
Cerium mischmetal.The cation radius and Zr of MgO4+Close, they are in ZrO2In dissolubility it is very big, can and ZrO2Formation monocline,
Four directions and the substitutional solid solution of cube grade crystal formation.
The preparation method of the contact material is as follows：
Step 1, by ceramic powder and enhancing stabilizer mix homogeneously；
Step 2, wet ball grinding 20 hours are crushed after 80 DEG C of oven dryings；
Step 3, calcines 1.5 hours at 1400 DEG C, and cooling is crushed, and the contact material after so processing is uniform, and phase body
It is stable, due to carrying out solution treatment in advance, it is that follow-up sintering uniformly lays the foundation, the intensity of material is higher；
Step 4, wet ball grinding 24 hours are standby as contact material after drying at 80 DEG C, excessively 200 mesh and 400 mesh sieves, with
Just running channel and filter medium are prepared.
After obtaining above-mentioned contact material, you can the filtration for utilizing the contact material to prepare for intercepting impurity in zircaloy is situated between
Matter.Preparing the filter medium needs following material：Aggregate, 200 mesh and the above-mentioned contact material of 400 purposes；Binding agent, 24-88P
Polyvinyl alcohol, water, defoamer；Skeleton, three-dimensional polyurethane foam sponge.
The preparation method of the present embodiment filter medium is as follows：
Three-dimensional polyurethane foam sponge skeleton is immersed the NaOH solution that concentration is 10% mass ratio by step 1, pre-treatment
In, 2h is hydrolyzed at a temperature of 40 DEG C, is then rubbed repeatedly and is dried after being rinsed with clear water, so as to clean up sponge；
Step 2, slurrying are added on polyvinyl alcohol in water first, and the ratio of polyvinyl alcohol and water is 10:100 weight ratios,
Aqueous temperature is controlled at 35 DEG C, is stirred using shearing dispersion machine, is prevented polyvinyl alcohol from reuniting in water or being attached on appearance
On wall, dissolution velocity is affected, but the speed for stirring can not be too fast, rotating speed is at 150 revs/min, while adding froth breaking
Agent (accounts for the 0.1% of polyethylene alcohol and water weight), and substantial amounts of foam otherwise occurs, the quality of the solution that impact makes will
200 mesh contact materials and 400 mesh contact materials are according to 3：1 weight ratio is poured in above-mentioned solution, is carried out using shearing dispersion machine
Stirring, 80 revs/min of the speed of stirring, the weight for obtaining slurry, 200 mesh contact materials and 400 mesh contact materials account for slurry weight
The 75% of amount；
Step 3, is coated with, and the three-dimensional polyurethane foam sponge skeleton that step 1 is obtained is immersed in the slurry that step 2 is obtained
In, fully discharge the gas in skeleton so as to which surface and inner homogeneous are coated with spreading mass, pull out；
Step 4, is dried, and will be coated with being positioned at shady and cool ventilation of three-dimensional polyurethane foam sponge skeleton, carries out place of drying in the shade
Reason, dries in the shade 4 hours so that framework material size is substantially stabilized, makes the semi-finished product to be dried of ceramic filter, after drying in the shade
Filter medium semi-finished product are put in drying oven is dried, and the programming rate of drying oven is 0.5 DEG C/min, is warmed up to 90 DEG C, is protected
Temperature 1 hour, then furnace cooling, fully to remove the volatizable material in slurry, completes the stress relieving of framework material, makes
The semi-finished product to be sintered of ceramic filter medium；
Step 5, sintering, i.e., low-temperature space (less than 500 DEG C), middle warm area (more than 500 DEG C to 1200 DEG C～1570 DEG C) and
Sinter in the temperature range of high-temperature region (1570 DEG C), when sintering in low-temperature space, less than 200 DEG C programming rates are 2 DEG C/min,
More than 200 DEG C to 400 DEG C programming rates are 1 DEG C/min, are incubated 30 minutes, then with the speed liter of 3 DEG C/min when rising to 400 DEG C
Temperature in sample powder accumulation body forms fine crack caused by preventing binding agent evaporation rate too fast and reduces examination to 500 DEG C
The intensity and surface matter of sample
Amount, or even cause waste product；When sintering in middle warm area, more than 500 DEG C to 1150 DEG C, speed is 4 DEG C/min, is heated up
Speed can be with quicker；1150 DEG C to 1570 DEG C, zirconium oxide starts transformation phase transformation of the generation by the opposite Tetragonal of oblique side or Emission in Cubic
The variable density for causing is up to 13%, and certain region of stress concentration even micro-crack, this stage are necessarily formed in sintered body
Speed controlling be will heat up in 3 DEG C/min and 1 hour is incubated at 1300 DEG C, can make phase transformation uniformly and discharge certain transformation stress,
Excessive micro-crack is avoided to be formed to greatest extent；When sintering in high-temperature region, 6 hours are incubated at 1570 DEG C, are best in order to reach
Normal temperature strength and elevated temperature strength, in this stage, zirconium oxide can make zirconic stable phasor due to the solid solution effect of stabilizer
Reach certain degree, while be released the stress produced due to great number of grains phase transformation, then furnace cooling, make as
Filter medium 102 shown in Fig. 2.
Three-dimensional polyurethane foam sponge in sintering process because high temperature disappear, so as to the original in three-dimensional polyurethane foam sponge
There is position to form corresponding hole, and then the hole needed for obtaining, select the three-dimensional polyurethane foam sea of difference PPI (void density)
Silk floss prepares the filter medium of difference PPI (such as 10-110PPI) by carrying out above-mentioned preparation process.
The sectional view of the filter plant 10 using gravity head is illustrated in figure 1, the filter plant 10 includes being integrally formed
Running channel 101, multiple filter mediums 102 being embedded in running channel 101 and the ingot mould 103 being connected with 101 outlet at bottom of running channel,
Preferably, the running channel 101 is cylindrical, and 101 bottom of running channel has 104,3 PPI of filter cavity of radially protruding
The different adaptations of filter medium 102 are placed in the filter cavity 104, and the PPI of this 3 filter mediums 102 is along melt liquid flow path direction
(i.e. from top to bottom) raises successively, to intercept the impurity that volume is gradually reduced successively.The quantity and PPI of filter medium 102 can
It is arranged as required to, is not limited to the present embodiment.
Present embodiments provide a kind of method for running channel 101 being prepared using above-mentioned contact material and filter medium 102, made
Filter medium 102 is embedded in running channel 101, is comprised the following steps：
Step 1, make aluminum dipping form, make two it is symmetrical, close after the aluminum dipping form that matches with the hollow part in running channel 101；
Step 2, casting, open aluminum dipping form, filter medium 102 are put into aluminum dipping form and 104 corresponding position of filter cavity, are closed
Casting after wax-pattern, makes wax be full of inside wax-pattern and filter medium 102；
Step 3, hanging sand shell, after wax solidification, open aluminum dipping form and take out the wax-pattern with filter medium 102, to avoid
The wax on 102 surface of filter medium is too thick, contact material cannot be close to filter medium 102, electricity consumption blowing when being coated with contact material
Wax-pattern, until wax pattern surface exposes filter medium 102, is immersed binding agent (for essence by the wax on surface at wax melting mould filter medium 102
The step of preparation method of close casting conventional binding agent, alternatively filter medium 2 slurries for obtaining) after be coated with 400 on its surface
Purpose contact material dries in the shade 12 hours as surface layer, immerses in binding agent and in facing surface and is coated with the contact material of 200 mesh
(surface thickness is about 1mm), dry in the shade 12 hours, in immersion binding agent and in facing surface, refractory material is coated with (such as mullite, oxygen
Change aluminium powder, magnesia powder, zircon powder etc.), dry in the shade 12 hours, repeat to immerse binding agent, be coated with refractory material and dry in the shade
12 hours the step of, acquisition, are embedded with filter medium 102 and the housing with contact material as surface layer (thickness is about 10mm).Due to shell
, only with about 1mm thickness contact materials as surface layer, while meeting performance need, remainder is using lower resistance to of cost for body
Fiery material is so as to cost-effective；
Step 4, wax melting, the product that step 3 is obtained is put in hot water, and wax melts and departs from, and dries in the shade 8 little after pulling housing out
When；
Step 5, sintering, the capsid product that sintering step 4 is obtained at 1050 DEG C are simultaneously incubated 30min, contact material housing
Sinter shell into, and filter medium is embedded in shell, so as to obtain the running channel 101 with filter medium 102.
Table one shows the pouring experiment result of running channel 101 obtained in the present embodiment, and 5 stoves only have filtration Jie of a stove
Matter 102 is washed away, and shows that the running channel 101 and filter medium 102 of the present embodiment acquisition have good thermal shock resistance.
Table one:Pouring experiment effect
Melting and casting can be carried out to zircaloy using filter plant 10, the process is comprised the following steps：
The zircaloy of the identical trade mark is returned material and is put in the crucible of vacuum melting furnace by step one, melting once, vacuum
For 0.001Pa, abundant dried argon is then charged with, smelting temperature is 1000 DEG C, and smelting time is 30 minutes, and zircaloy is complete
After full thawing, pour in the filter plant for be embedded with filter medium and cast；After ingot casting cooling, vacuum drying oven is opened, take out casting
The exocuticle of alloy is disposed 1 millimeter by ingot cogging, then the composition of sample analysis zircaloy ingot casting, according to alloy designations
Require, calculating composition deviation, determine the alloying element for requiring supplementation with.As the composition of alloy is failed to understand, need in melting once
Confirm the main component of alloy, to be adjusted when secondary smelting, alloying component is prevented because returning material
Source manages not good, and composition tolerances occurs.
Step 2, secondary smelting adjust alloying component, by the various alloying element simple substance of the alloying element deviation for making up or
Intermediate alloy, is together put into vacuum melting furnace with the zircaloy ingot casting of melting once, and vacuum is 0.001Pa, is then charged with filling
Divide dried argon, 1000 DEG C of smelting temperature, smelting time is 30 minutes, is stirred by electromagnetic induction so that zircaloy melts
The component of body is uniform.
Step 3, purifies technological preparation, and the running channel that would be embedded with filter medium is preheating to 1000 DEG C；Ingot mould prepares, will casting
Ingot mould (being metal or ceramic material) removing surface is clean, and no impurity and greasy dirt adhere to.
Step 4, casting and purification, the zircaloy melt of melting is poured in running channel, and zircaloy melt is situated between by filtering
Matter, the impurity in its alloy melt are intercepted and are adsorbed by filter medium, and clean zircaloy melt is flowed in ingot mould, are cooled down
Form ingot casting.
Jing is tested, and contact material prepared by the method for the present embodiment can be prevented effectively from and zircaloy reaction, so as to avoid drawing
Enter impurity, also do not affected by change in volume caused by crystal conversion and heat effect, so as to ensure its performance.Through this enforcement
Example method obtained in filter medium 102 without blind crack, with good thermal shock resistance.Can be by mistake by the method for the present embodiment
Filter medium 102 is embedded in running channel 101, and filter medium 102 can guarantee that all zircaloy melts without dead angle ground quilt in being embedded in running channel
Filter medium 102 is intercepted, and improves clean-up effect.The method that melting and casting are carried out to zircaloy using filter plant 10 compares consumable
Electric arc furnace method reduces melting number of times, save energy consumption；Being mingled with for zircaloy be few, and the impurity element such as O, S, P, N, C contains
Amount is extremely low, improves the structure of alloy, improves the mechanical property of alloy；The degradation for reducing zircaloy is used, and is improve
Economic results in society, realize the purpose of recycling.
Embodiment 2
The contact material of the present embodiment is made up of ceramic powder and enhancing stabilizer, and the ceramic powder is by MgO and ZrO2
In molar ratio 8.5:100 compositions, strengthen stabilizer by weight 0.8% for ceramic powder, and the enhancing stabilizer is preferably
Cerium-rich rare earth.
The preparation method of the contact material is as follows：
Step 1, by ceramic powder and enhancing stabilizer mix homogeneously；
Step 2, wet ball grinding 22 hours are crushed after 90 DEG C of oven dryings；
Step 3, calcines 2 hours at 1425 DEG C, and cooling is crushed, and the contact material after so processing is uniform, and Xiang Tiwen
It is fixed, due to carrying out solution treatment in advance, it is that follow-up sintering uniformly lays the foundation, the intensity of material is higher；
Step 4, wet ball grinding 36 hours are standby as contact material after drying at 90 DEG C, excessively 200 mesh and 400 mesh sieves, with
Just running channel and filter medium are prepared.
After obtaining above-mentioned contact material, you can the filtration for utilizing the contact material to prepare for intercepting impurity in zircaloy is situated between
Matter.Preparing the filter medium needs following material：Aggregate, 200 mesh and the above-mentioned contact material of 400 purposes；Binding agent, 24-88P
Polyvinyl alcohol, water, defoamer；Skeleton, three-dimensional polyurethane foam sponge.
The preparation method of the present embodiment filter medium is as follows：
Three-dimensional polyurethane foam sponge skeleton is immersed the NaOH solution that concentration is 15% mass ratio by step 1, pre-treatment
In, 3h is hydrolyzed at a temperature of 40-60 DEG C, is then rubbed repeatedly and is dried after being rinsed with clear water, so as to clean up sponge；
Step 2, slurrying are added on polyvinyl alcohol in water first, and polyvinyl alcohol (powder) is 11 with the ratio of water:100
Weight ratio, aqueous temperature control at 40 DEG C, using shearing dispersion machine be stirred, rotating speed at 150 revs/min, together
When add defoamer (accounting for the 0.1% of polyethylene alcohol and water weight), by 200 mesh contact materials and 400 mesh contact materials according to 3：1
Weight ratio pour in above-mentioned solution, using shearing dispersion machine be stirred, 100 revs/min of the speed of stirring, obtain slurry,
The weight of 200 mesh contact materials and 400 mesh contact materials accounts for the 80% of slurry weight；
Step 3, is coated with, and the three-dimensional polyurethane foam sponge skeleton that step 1 is obtained is immersed in the slurry that step 2 is obtained
In, fully discharge the gas in skeleton so as to which surface and inner homogeneous are coated with spreading mass, pull out；
Step 4, is dried, and will be coated with being positioned at shady and cool ventilation of three-dimensional polyurethane foam sponge skeleton, carries out place of drying in the shade
Reason, dries in the shade 36 hours, makes the semi-finished product to be dried of ceramic filter, and the filter medium semi-finished product after drying in the shade are put into drying oven
Inside dried, the programming rate of drying oven is 2 DEG C/min, is warmed up to 110 DEG C, is incubated 2 hours, and then furnace cooling, makes
The semi-finished product to be sintered of ceramic filter medium；
Step 5, sintering, i.e., low-temperature space (less than 500 DEG C), middle warm area (more than 500 DEG C to 1200 DEG C～1570 DEG C) and
Sinter in the temperature range of high-temperature region (1570 DEG C), when sintering in low-temperature space, less than 200 DEG C programming rates are 3 DEG C/min,
More than 200 DEG C to 400 DEG C programming rates are 2 DEG C/min, are incubated 30 minutes, then with the speed liter of 3 DEG C/min when rising to 400 DEG C
Temperature is to 500 DEG C；When sintering in middle warm area, more than 500 DEG C to 1150 DEG C, speed is 4 DEG C/min；1150 DEG C to 1570 DEG C, this
Stage will heat up speed controlling in 3 DEG C/min and be incubated 1 hour at 1300 DEG C；When sintering in high-temperature region, 8 are incubated at 1570 DEG C
Hour, then furnace cooling, makes filter medium 102 as shown in Figure 2.
The filter plant 10 of the present embodiment is identical with 1 structure of embodiment, repeats no more.Present embodiments provide a kind of utilization
The method that above-mentioned contact material and filter medium 102 prepare running channel 101, makes filter medium 102 be embedded in running channel 101, including with
Lower step：
Step 1, make aluminum dipping form, make two it is symmetrical, close after the aluminum dipping form that matches with the hollow part in running channel 101；
Step 2, casting, open aluminum dipping form, filter medium 102 are put into aluminum dipping form and 104 corresponding position of filter cavity, are closed
Casting after wax-pattern, makes wax be full of inside wax-pattern and filter medium 102, and casting speed is unsuitable too fast, in order to avoid 102 quilt of filter medium
Wash away；
Step 3, hanging sand shell, after wax solidification, open aluminum dipping form and take out the wax-pattern with filter medium 102, to avoid
The wax on 102 surface of filter medium is too thick, contact material cannot be close to filter medium 102, electricity consumption blowing when being coated with contact material
Wax-pattern, until wax pattern surface exposes filter medium 102, is immersed binding agent (for essence by the wax on surface at wax melting mould filter medium 102
The step of preparation method of close casting conventional binding agent, alternatively filter medium 2 slurries for obtaining) after be coated with 400 on its surface
Purpose contact material after drying in the shade 48 hours, is immersed in binding agent and in facing surface and is coated with the contact material of 200 mesh as surface layer
(surface thickness is about 1mm), dry in the shade 48 hours, in immersion binding agent and in facing surface, refractory material is coated with (such as mullite, oxygen
Change aluminium powder, magnesia powder, zircon powder etc.), dry in the shade 48 hours, repeat to immerse binding agent, be coated with refractory material and dry in the shade
48 hours the step of, acquisition, are embedded with filter medium 102 and the housing with contact material as surface layer (thickness is about 10mm).Due to shell
, only with about 1mm thickness contact materials as surface layer, while meeting performance need, remainder is using lower resistance to of cost for body
Fiery material is so as to cost-effective；
Step 4, wax melting, the product that step 3 is obtained is put in hot water, and wax melts disengaging in the process, the moon after pulling out
It is dry 16 hours；
Step 5, sintering, the product that sintering step 4 is obtained at 1050 DEG C are simultaneously incubated 2h, and contact material sinters shell into,
So as to by filter medium embedded shell, obtain the running channel 101 with filter medium 102.
Table two shows the pouring experiment result of running channel 101 obtained in the present embodiment, compared with Example 1, the present embodiment
The filter medium 102 of 5 stoves do not washed away, show that running channel 101 that the present embodiment obtains and filter medium 102 have excellent
Good thermal shock resistance.
Table two:Pouring experiment effect
| Batch | Heat (batch) number 1 | Heat (batch) number 2 | Heat (batch) number 3 | Heat (batch) number 4 | Heat (batch) number 5 |
| Effect | Well | Well | Well | Well | Well |
| Remarks |
Melting and casting can be carried out to zircaloy using filter plant 10, the process is comprised the following steps：
The zircaloy of the identical trade mark is returned material and is put in the crucible of vacuum melting furnace by step one, melting once, vacuum
For 0.001Pa, abundant dried argon is then charged with, smelting temperature is 1450 DEG C, and smelting time is 40 minutes, and zircaloy is complete
After full thawing, pour in the filter plant for be embedded with filter medium and cast；After ingot casting cooling, vacuum drying oven is opened, take out casting
The exocuticle of alloy is disposed 1 millimeter by ingot cogging, then the composition of sample analysis zircaloy ingot casting, according to alloy designations
Require, calculating composition deviation, determine the alloying element for requiring supplementation with.As the composition of alloy is failed to understand, need in melting once
Confirm the main component of alloy, to be adjusted when secondary smelting, alloying component is prevented because returning material
Source manages not good, and composition tolerances occurs.
Step 2, secondary smelting adjust alloying component, by the various alloying element simple substance of the alloying element deviation for making up or
Intermediate alloy, is together put into vacuum melting furnace with the zircaloy ingot casting of melting once, and vacuum is 0.001Pa, is then charged with filling
Divide dried argon, 1450 DEG C of smelting temperature, smelting time is 30 minutes, is stirred by electromagnetic induction so that zircaloy melts
The component of body is uniform.
Step 3, purifies technological preparation, and the running channel that would be embedded with filter medium is preheating to 1150 DEG C；Ingot mould prepares, will casting
Ingot mould (being metal or ceramic material) removing surface is clean, and no impurity and greasy dirt adhere to.
Step 4, casting and purification, the zircaloy melt of melting is poured in running channel, and zircaloy melt is situated between by filtering
Matter, the impurity in its alloy melt are intercepted and are adsorbed by filter medium, and clean zircaloy melt is flowed in ingot mould, are cooled down
Form ingot casting.
Jing is tested, and contact material prepared by the method for the present embodiment can be prevented effectively from and zircaloy reaction, so as to avoid drawing
Enter impurity, also do not affected by change in volume caused by crystal conversion and heat effect, so as to ensure its performance.Through this enforcement
Example method obtained in filter medium 102 without blind crack, with good thermal shock resistance.Can be by mistake by the method for the present embodiment
Filter medium 102 is embedded in running channel 101, and filter medium 102 can guarantee that all zircaloy melts without dead angle ground quilt in being embedded in running channel
Filter medium 102 is intercepted, and improves clean-up effect.The method that melting and casting are carried out to zircaloy using filter plant 10 compares consumable
Electric arc furnace method reduces melting number of times, save energy consumption；Being mingled with for zircaloy be few, and the impurity element such as O, S, P, N, C contains
Amount is extremely low, improves the structure of alloy, improves the mechanical property of alloy；The degradation for reducing zircaloy is used, and is improve
Economic results in society, realize the purpose of recycling.
Embodiment 3
The contact material of the present embodiment is made up of ceramic powder and enhancing stabilizer, and the ceramic powder is by MgO and ZrO2
In molar ratio 12:100 compositions, strengthen stabilizer by weight 1% for ceramic powder, and the enhancing stabilizer is preferably rich cerium
Rare earth.
The preparation method of the contact material is as follows：
Step 1, by ceramic powder and enhancing stabilizer mix homogeneously；
Step 2, wet ball grinding 24 hours are crushed after 100 DEG C of oven dryings；
Step 3, calcines 2.5 hours at 1450 DEG C, and cooling is crushed, and the contact material after so processing is uniform, and phase body
It is stable, due to carrying out solution treatment in advance, it is that follow-up sintering uniformly lays the foundation, the intensity of material is higher；
Step 4, wet ball grinding 48 hours are standby as contact material after drying at 100 DEG C, excessively 200 mesh and 400 mesh sieves,
To prepare running channel and filter medium.
After obtaining above-mentioned contact material, you can the filtration for utilizing the contact material to prepare for intercepting impurity in zircaloy is situated between
Matter.Preparing the filter medium needs following material：Aggregate, 200 mesh and the above-mentioned contact material of 400 purposes；Binding agent, 24-88P
Polyvinyl alcohol, water, defoamer；Skeleton, three-dimensional polyurethane foam sponge.
The preparation method of the present embodiment filter medium is as follows：
Three-dimensional polyurethane foam sponge skeleton is immersed the NaOH solution that concentration is 20% mass ratio by step 1, pre-treatment
In, 4h is hydrolyzed at a temperature of 40-60 DEG C, is then rubbed repeatedly and is dried after being rinsed with clear water, so as to clean up sponge；
Step 2, slurrying are added on polyvinyl alcohol in water first, and polyvinyl alcohol (powder) is 10 with the ratio of water:100
Weight ratio, aqueous temperature control at 45 DEG C, using shearing dispersion machine be stirred, rotating speed at 100 revs/min, while
Defoamer (accounting for the 1% of polyethylene alcohol and water weight) is added, by 200 mesh contact materials and 400 mesh contact materials according to 3：1 weight
Amount is stirred using shearing dispersion machine than pouring in above-mentioned solution, and 150 revs/min of the speed of stirring obtains slurry, 200 mesh
The weight of contact material and 400 mesh contact materials accounts for the 85% of slurry weight；
Step 3, is coated with, and the three-dimensional polyurethane foam sponge skeleton that step 1 is obtained is immersed in the slurry that step 2 is obtained
In, fully discharge the gas in skeleton so as to which surface and inner homogeneous are coated with spreading mass, pull out；
Step 4, is dried, and will be coated with being positioned at shady and cool ventilation of three-dimensional polyurethane foam sponge skeleton, carries out place of drying in the shade
Reason, dries in the shade 48 hours, makes the semi-finished product to be dried of ceramic filter, and the filter medium semi-finished product after drying in the shade are put into drying oven
Inside dried, the programming rate of drying oven is 5 DEG C/min, is warmed up to 120 DEG C, is incubated 2 hours, and then furnace cooling, makes
The semi-finished product to be sintered of ceramic filter medium；
Step 5, sintering, i.e., low-temperature space (less than 500 DEG C), middle warm area (more than 500 DEG C to 1200 DEG C～1570 DEG C) and
Sinter in the temperature range of high-temperature region (1570 DEG C), when sintering in low-temperature space, less than 200 DEG C programming rates are 5 DEG C/min,
More than 200 DEG C to 400 DEG C programming rates are 3 DEG C/min, are incubated 30 minutes, then with the speed liter of 3 DEG C/min when rising to 400 DEG C
Temperature is to 500 DEG C；When sintering in middle warm area, more than 500 DEG C to 1150 DEG C, speed is 5 DEG C/min；1150 DEG C to 1570 DEG C, this
Stage will heat up speed controlling in 4 DEG C/min and be incubated 1 hour at 1300 DEG C；When sintering in high-temperature region, it is incubated at 1570 DEG C
10 hours, then furnace cooling, made filter medium 102 as shown in Figure 2.
The filter plant 10 of the present embodiment is identical with 1 structure of embodiment, repeats no more.Present embodiments provide a kind of utilization
The method that above-mentioned contact material and filter medium 102 prepare running channel 101, makes filter medium 102 be embedded in running channel 101, including with
Lower step：
Step 1, make aluminum dipping form, make two it is symmetrical, close after the aluminum dipping form that matches with the hollow part in running channel 101；
Step 2, casting, open aluminum dipping form, filter medium 102 are put into aluminum dipping form and 104 corresponding position of filter cavity, are closed
Casting after wax-pattern, makes wax be full of inside wax-pattern and filter medium 102, and casting speed is unsuitable too fast, in order to avoid 102 quilt of filter medium
Wash away；
Step 3, hanging sand shell, after wax solidification, open aluminum dipping form and take out the wax-pattern with filter medium 102, to avoid
The wax on 102 surface of filter medium is too thick, contact material cannot be close to filter medium 102, electricity consumption blowing when being coated with contact material
Wax-pattern, until wax pattern surface exposes filter medium 102, is immersed binding agent (for essence by the wax on surface at wax melting mould filter medium 102
The step of preparation method of close casting conventional binding agent, alternatively filter medium 2 slurries for obtaining) after be coated with 400 on its surface
Purpose contact material after drying in the shade 128 hours, is immersed in binding agent and in facing surface and is coated with the contact material of 200 mesh as surface layer
Material (surface thickness is about 1mm), dries in the shade 128 hours, is coated with refractory material (as do not come in immersion binding agent and in facing surface
Stone, alumina powder, magnesia powder, zircon powder etc.), dry in the shade 128 hours, repeat to immerse binding agent, be coated with refractory material
The step of with drying in the shade 128 hours, acquisition is embedded with filter medium 102 and the housing with contact material as surface layer, and (thickness is about
10mm).Due to housing only with about 1mm thickness contact materials as surface layer, while meeting performance need, remainder is adopted
The lower refractory material of cost is so as to cost-effective；
Step 4, wax melting, the product that step 3 is obtained is put in hot water, and wax melts disengaging in the process, the moon after pulling out
It is dry 24 hours；
Step 5, sintering, the product that sintering step 4 is obtained at 1050 DEG C are simultaneously incubated 2h, and contact material sinters shell into,
So as to by filter medium embedded shell, obtain the running channel 101 with filter medium 102.
Table three shows the pouring experiment result of running channel 101 obtained in the present embodiment, and 5 stoves only have filtration Jie of a stove
Matter 102 is washed away, and shows that the running channel 101 and filter medium 102 of the present embodiment acquisition have good thermal shock resistance.
Table three:Pouring experiment effect
Melting and casting can be carried out to zircaloy using filter plant 10, the process is comprised the following steps：
The zircaloy of the identical trade mark is returned material and is put in the crucible of vacuum melting furnace by step one, melting once, vacuum
For 0.1Pa, abundant dried argon is then charged with, smelting temperature is 1500 DEG C, and smelting time is 60 minutes, and zircaloy is complete
After thawing, pour in the filter plant for be embedded with filter medium and cast；After ingot casting cooling, vacuum drying oven is opened, take out ingot casting
The exocuticle of alloy is disposed 2 millimeters by cogging, then the composition of sample analysis zircaloy ingot casting, wanting according to alloy designations
Ask, calculating composition deviation, determine the alloying element for requiring supplementation with.As the composition of alloy is failed to understand, need true in melting once
Recognize the main component of alloy, to be adjusted when secondary smelting, alloying component is prevented because returning coming for material
Source manages not good, and composition tolerances occurs.
Step 2, secondary smelting adjust alloying component, by the various alloying element simple substance of the alloying element deviation for making up or
Intermediate alloy, is together put into vacuum melting furnace with the zircaloy ingot casting of melting once, and vacuum is 0.1Pa, is then charged with fully
Dried argon, 1500 DEG C of smelting temperature, smelting time are 60 minutes, are stirred by electromagnetic induction so that zircaloy melt
Component it is uniform.
Step 3, purifies technological preparation, and the running channel that would be embedded with filter medium is preheating to 1200 DEG C；Ingot mould prepares, will casting
Ingot mould (being metal or ceramic material) removing surface is clean, and no impurity and greasy dirt adhere to.
Step 4, casting and purification, the zircaloy melt of melting is poured in running channel, and zircaloy melt is situated between by filtering
Matter, the impurity in its alloy melt are intercepted and are adsorbed by filter medium, and clean zircaloy melt is flowed in ingot mould, are cooled down
Form ingot casting.
Jing is tested, and contact material prepared by the method for the present embodiment can be prevented effectively from and zircaloy reaction, so as to avoid drawing
Enter impurity, also do not affected by change in volume caused by crystal conversion and heat effect, so as to ensure its performance.Through this enforcement
Example method obtained in filter medium 102 without blind crack, with preferable thermal shock resistance.Can be by mistake by the method for the present embodiment
Filter medium 102 is embedded in running channel 101, and filter medium 102 can guarantee that all zircaloy melts without dead angle ground quilt in being embedded in running channel
Filter medium 102 is intercepted, and improves clean-up effect.
The method that melting and casting are carried out to zircaloy using filter plant 10 reduces melting than consumable electroarc furnace method
Number of times, save energy consumption；Being mingled with for zircaloy is few, and the content of the impurity element such as O, S, P, N, C is extremely low, improves the gold of alloy
Phase structure, improves the mechanical property of alloy；The degradation for reducing zircaloy is used, and is improve economic results in society, is realized and follow
The purpose that ring is used.
In above-mentioned each embodiment, one the step of zircaloy melting and casting method in used crucible, the present invention
A kind of many crucibles are additionally provided, the front sectional view of many crucibles is illustrated in figure 3, including for containing melt and can avoid
The inner crucible 1 of contaminated melt, the outer crucible 3 for supporting inner crucible 1 and fire resisting packed layer 2, the inner crucible 1
Volume is slightly less than outer crucible 3 and is placed in outer crucible 3, and fire resisting packed layer 2 is padded in 1 outer wall of inner crucible and outer crucible 3
Between inwall.
Outer crucible 3 acts primarily as spacing and protection inner crucible 1 effect, prevents the melt leakage in inner crucible 1, by
In outer crucible 3 not with melt contacts, which can be by cast iron, cast steel, graphite, MgO, Al2O3、SiO2Or the combination of above-mentioned substance
Constitute, so as to reduces cost.
The inner crucible 1 and melt contacts, undertake the effect for containing melt, preferably by the contact material structure of above-mentioned preparation
Into reacting with melt contacts so as to be prevented effectively from.Compared with prior art, as inner crucible 1 has outer crucible 3
Support and protect, therefore its thickness is so thick without the need for picture prior art, reduce thickness and advantageously reduce difficulty of processing and cost, adopt
This structure has very big meaning to reduces cost, the zirconic application of popularization.2 positioning inner crucibles 1, chi of the fire resisting packed layer
Very little expansion buffer and the effect for preventing inner crucible 1 from misplacing, preferably by the deformable fire resisting such as resistance to Pyroxylin, glass fibre, rock wool
The combination of material or above-mentioned substance is constituted, it is to avoid 1 outer wall of inner crucible is received with 3 inwall directly contact of outer crucible, inner crucible 1
Thermal expansion is buffered.
Claims (9)
1. a kind of zircaloy melting and casting method, it is characterised in that comprise the following steps：
The zircaloy of the identical trade mark is returned material and is put in the crucible of vacuum melting furnace by step one, melting once, and vacuum is
0.001-0.1Pa, is then charged with abundant dried argon, and smelting temperature is 1000-1500 DEG C, and smelting time is 30-60 point
Clock, after zircaloy melts completely, pours in the filter plant for be embedded with filter medium and is cast；After ingot casting cooling, open true
Empty stove, takes out ingot formation, the exocuticle of alloy is disposed 1-2 millimeters, and then the composition of sample analysis zircaloy ingot casting, presses
According to the requirement of alloy designations, calculating composition deviation, the alloying element for requiring supplementation with is determined；
Step 2, secondary smelting adjust alloying component, by the various alloying element simple substance of the alloying element deviation for making up or centre
Alloy, is together put into vacuum melting furnace with the zircaloy ingot casting of melting once, and vacuum is 0.001-0.1Pa, is then charged with filling
Divide dried argon, 1000～1500 DEG C of smelting temperature, smelting time is 30～60 minutes, and stirring makes the group of zircaloy melt
Divide uniform；
Step 3, purifies technological preparation, and the running channel that would be embedded with filter medium is preheating to 1000-1200 DEG C；Ingot mould prepares, will casting
Ingot mould removing surface is clean, and no impurity and greasy dirt adhere to；
Step 4, casting and purification, the zircaloy melt of melting is poured in running channel, and zircaloy melt passes through filter medium, its
Impurity in alloy melt is intercepted and is adsorbed by filter medium, and clean zircaloy melt is flowed in ingot mould, is cooled into
Ingot casting.
2. zircaloy melting according to claim 1 and casting method, it is characterised in that：The running channel and filter medium are equal
It is made up of contact material, the contact material is made up of ceramic powder and enhancing stabilizer, and the ceramic powder is by MgO and ZrO2
6-12 in molar ratio:100 compositions, strengthen stabilizer by weight the 0.5%-1% for ceramic powder, and the enhancing stabilizer is
Cerium-rich rare earth.
3. zircaloy melting according to claim 2 and casting method, it is characterised in that：The preparation side of the contact material
Method is comprised the following steps：
Step 1, by ceramic powder and enhancing stabilizer mix homogeneously；
Step 2, wet ball grinding 20-24 hours, 80-100 DEG C of crushed after being dried；
Step 3, calcines 1.5-6 hours at 1400-1450 DEG C, and cooling is crushed；
Step 4, wet ball grinding 24-48 hours, crushed after being dried, screening at 80-100 DEG C.
4. zircaloy melting according to claim 3 and casting method, it is characterised in that：The preparation side of the filter medium
Method is comprised the following steps：
Step 1, pre-treatment, in being 10%～20% NaOH solution by three-dimensional polyurethane foam sponge skeleton immersion concentration,
2～4h is hydrolyzed at a temperature of 40～60 DEG C, is then rubbed repeatedly and is dried after presoma being rinsed with clear water, so as to clean up sea
It is continuous；
Step 2, slurrying are progressively added on polyvinyl alcohol in water first, until the viscosity of polyethylene alcohol and water is 40-50CPS
And pH value, in 5-7, aqueous temperature is controlled at 40-50 DEG C, is stirred, while defoamer is added, by 200 mesh and 400 mesh
Contact material is according to 3：1 weight ratio is poured in above-mentioned solution, is stirred, and obtains slurry, 200 mesh contact materials and 400 mesh
The weight of contact material accounts for the 75-85% of slurry weight；
Step 3, is coated with, and the three-dimensional polyurethane foam sponge skeleton that step 1 is obtained is immersed in the slurry that step 2 is obtained, and is filled
Divide the gas discharged in skeleton so as to which surface and inner homogeneous are coated with spreading mass, pull out；
Step 4, dries in the shade naturally and dries, and will be coated with being positioned at shady and cool ventilation of three-dimensional polyurethane foam sponge skeleton, carries out
Dry in the shade process, 4-48 hours of drying in the shade make the semi-finished product to be dried of ceramic filter, and the filter medium semi-finished product after drying in the shade are put
Enter in drying oven and dried, the programming rate of drying oven is 0.5-5 DEG C/min, is warmed up to 90-120 DEG C, is incubated 1-2 hours,
Then furnace cooling, makes the semi-finished product to be sintered of filter medium；
Step 5, sintering, i.e., the low-temperature space, more than 500 DEG C to 1200 DEG C～1570 DEG C of middle warm area and 1570 below 500 DEG C
DEG C high-temperature region in sinter, when sintering in low-temperature space, less than 200 DEG C programming rates are 2-5 DEG C/min, more than 200 DEG C to 400
DEG C programming rate is 1-3 DEG C/min, is incubated 30 minutes, is then warmed up to 500 DEG C with the speed of 3 DEG C/min when rising to 400 DEG C；
When sintering in middle warm area, more than 500 DEG C to 1150 DEG C, speed is 4-5 DEG C/min；1150 DEG C to 1570 DEG C, this stage will heat up
Speed controlling is incubated 1 hour in 3-4 DEG C/min and at 1300 DEG C；When sintering in high-temperature region, 6-10 hours are incubated at 1570 DEG C,
Then furnace cooling, makes filter medium.
5. zircaloy melting according to claim 4 and casting method, it is characterised in that：In the step 2, poly- second is stirred
The rotating speed of alkene alcohol and water is 70～100 revs/min.
6. zircaloy melting according to claim 4 and casting method, it is characterised in that：In the step 2, contact is added
The speed stirred after material is 80-150 rev/min.
7. zircaloy melting according to claim 4 and casting method, it is characterised in that：In the step 2, defoamer is accounted for
The 0.1%～1% of polyethylene alcohol and water gross weight.
8. zircaloy melting according to claim 4 and casting method, it is characterised in that：It is embedded with the described of filter medium to pour
The preparation method in road is comprised the following steps：
Step 1, making aluminum dipping form, make two aluminum dipping forms that are symmetrical, matching with the hollow part in running channel；
Step 2, casting, open aluminum dipping form, filter medium are put into aluminum dipping form position corresponding with filter cavity, note after the aluminum dipping form that closes
Wax, makes wax be full of inside aluminum dipping form and filter medium；
Step 3, hanging sand, after wax solidification, open aluminum dipping form and take out the wax-pattern with filter medium, blow at wax melting mould filter medium
The wax on surface, until wax pattern surface exposes filter medium, is coated with contact material until desired thickness the moon repeatedly in wax pattern surface
It is dry 4～128 hours；
Step 4, wax melting, the product that step 3 is obtained is put in hot water, and wax melts disengaging in the process, dry in the shade 8 after pulling out～
24 hours；
Step 5, sintering, the product that sintering step 4 is obtained at 1050～1250 DEG C are simultaneously incubated 30min～2h, and contact material burns
Form shell, in the embedded shell of filter medium, obtain the running channel with filter medium.
9. zircaloy melting according to claim 8 and casting method, it is characterised in that：In step 3, apply in wax pattern surface
When hanging contact material, the contact material of 400 mesh is first coated with, the contact material of 200 mesh is then coated with the contact material of 400 mesh
Material.
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| CN102260807B (en) * | 2011-06-15 | 2013-07-03 | 燕山大学 | Zirconium alloy and preparation method thereof |
| CN103317114B (en) * | 2013-07-01 | 2015-08-05 | 沈阳铸造研究所 | A kind of metal mold casting method for zircaloy |
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