CN107354339A - Dispersion intensifying platinum rhodium and platinum composite and preparation method thereof - Google Patents
Dispersion intensifying platinum rhodium and platinum composite and preparation method thereof Download PDFInfo
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- CN107354339A CN107354339A CN201710625159.6A CN201710625159A CN107354339A CN 107354339 A CN107354339 A CN 107354339A CN 201710625159 A CN201710625159 A CN 201710625159A CN 107354339 A CN107354339 A CN 107354339A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/04—Alloys based on a platinum group metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
- B22F2003/175—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging by hot forging, below sintering temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The invention belongs to technical field of metal material, and in particular to a kind of dispersion intensifying platinum rhodium and platinum composite and preparation method thereof.The technical problems to be solved by the invention are to provide the preparation method of a kind of dispersion intensifying platinum rhodium and platinum composite, comprise the following steps：Powder is made in dispersion intensifying platinum rhodium, platinum respectively, is laid in sintering mold, by sintering, annealing, hot pressing, sizing hot forging, unformed hot forging, surface treatment, the final obtained composite of rolling.The composite has weld, can carry out weld with alloy platinum material, platinum-rhodium alloy material, disperse alloy platinum material and disperse platinum rhodium material, while have the performance such as good elevated temperature strength, inoxidizability, anti-corrosion.
Description
Technical field
The invention belongs to technical field of metal material, and in particular to a kind of dispersion intensifying platinum rhodium and platinum composite and its system
Preparation Method.I.e. by the way that dispersion intensifying platinum rhodium and platinum are carried out compound to obtain a kind of new material.
Background technology
Platinum and platinum-rhodium alloy are widely used in glass industry.Dispersion-strengtherning alloy platinum material is using metal platinum as matrix, with gold
Belong to zirconium, yttrium, thorium, the new structural material that the oxide such as beryllium is dispersion-strengtherning phase, have good elevated temperature strength, inoxidizability with
And resistance to melting glass attack.However, dispersion intensifying platinum or dispersion intensifying platinum and the composite wood of platinum that existing method is prepared
The weld of material can not meet process requirements, so as to can not platinum dish one layer of disperse material of key component weld with to whole
Individual platinum product vessel structure is strengthened, or internally weld one layer of dispersion-strengtherning platinum material improves platinum dish
Corrosion resistance.
The content of the invention
It is difficult to forge platinum dish for existing dispersion-strengtherning alloy platinum material or the composite of dispersion intensifying platinum and platinum
The problem of connecing reinforcing, the invention provides a kind of dispersion intensifying platinum rhodium and platinum composite and preparation method thereof.It is prepared by this method
Obtained composite has weld, can be with alloy platinum material, platinum-rhodium alloy material, disperse alloy platinum material and disperse platinum rhodium material
Weld is carried out, while there is the performance such as good elevated temperature strength, inoxidizability, anti-corrosion.
First technical problem to be solved by this invention is to provide the system of a kind of dispersion intensifying platinum rhodium and platinum composite
Preparation Method.The preparation method comprises the following steps：
1st, dispersion intensifying platinum rhodium dust is prepared
1.1st, dispensing：0.01~0.06% disperse means by weight percentage, 1~30% rhodium, remaining be alloy platinum material carry out
Dispensing；
1.2nd, induction melting：Rhodium, alloy platinum material are subjected to melting in induction melting furnace, control smelting temperature for 1800~
2100 DEG C, frequency be 3~100KHz, and carry out degasification operation, be then cast into platinum rhodium ingot casting in the mould；
1.3 vacuum melting：By disperse means, platinum rhodium ingot casting vacuum ＜ 10Pa, 1800~2100 DEG C of temperature, frequency 8~
Abundant melting, obtains liquid alloy under the conditions of 100KHz；
1.4th, cast：By 1.3 gained liquid alloy cast moldings under an inert gas, cast temperature is 1800~2100
℃；
1.5th, powder processed：Powder is made in material obtained by 1.4 cast moldings；
2nd, platinum powder end is prepared
2.1st, induction melting：Alloy platinum material is sensed under conditions of 3~100KHz of frequency, 1750~2000 DEG C of temperature
Melting, obtain liquid platinum；
2.2nd, cast：By 2.1 gained liquid platinum cast moldings, cast temperature is 1800~2100 DEG C；
2.3rd, powder processed：Powder is made in material obtained by 2.2 cast moldings；
3rd, dispersion intensifying platinum rhodium and platinum composite are prepared
3.1st, it is compound：By 1.5 and 2.3 gained powder overlapping tiles in sintering mould；
3.2nd, sinter：The powder that 3.1 are completed sinters at 1100~1500 DEG C；
3.3rd, anneal oxidation：3.2 gained materials are made annealing treatment at 1200~1450 DEG C；
3.4th, hot pressing：3.3 gained materials are suppressed under 600~1300 DEG C, 4~100MPa of pressure；
3.5th, sizing hot forging：3.4 gained materials are subjected to annealing 15~60 minutes at 1200~1450 DEG C, then
Forged on 200~400kg pneumatic hammers from upper and lower surfaces, 1200~1450 DEG C of initial forging temperature, final forging temperature 900~
1200 DEG C, forge 50~80% after being 3.4 hot pressing to thickness；
3.6th, unformed hot forging：3.5 gained materials are subjected to annealing 15~60 minutes at 1200~1450 DEG C, so
Forged afterwards on 200~400kg pneumatic hammers from six faces, 1200~1450 DEG C of initial forging temperature, final forging temperature 900~1200
DEG C, forge to less than 40% that thickness is 3.2 sintering gained substance thickness；
3.7th, it is surface-treated：The booty of 3.6 gained material surfaces, impurity are removed clean；
3.8th, roll：3.7 gained materials are rolled, in distance objective 0.3~0.8mm of thickness, 1200~
It is heat-treated 15~60 minutes at 1450 DEG C, after heat treatment terminates, then is rolled down to target thickness.
Specifically, in the preparation method step 1.1 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the disperse means are
At least one of zirconium, yttrium, calcium, lanthanum or titanium；Or the alloy that zirconium, yttrium, calcium, lanthanum or titanium are formed with platinum.
Preferably, in the preparation method step 1.1 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the alloy platinum material purity
For more than 99.9%.The alloy platinum material is sponge state, sheet material, sheet material or melted ingot.
Preferably, it is described in preparation method step 1.2,1.3 or 2.1 of above-mentioned dispersion intensifying platinum rhodium and platinum composite
Smelting time is 1~2 hour.
Preferably, in the preparation method step 1.4 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the inert gas is
Argon gas, pressure is in 0.02~0.08MPa.
Preferably, in the preparation method step 1.4 or 2.2 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the casting
It is shaped to be cast into bar-shaped, a diameter of 30~50mm.
Preferably, in the preparation method step 1.5 or 2.3 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the powder
Granularity be 500 μm of ＜.
Preferably, in the preparation method step 3.1 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the platinum powder accounts for platinum powder
With the 5~95% of dispersion intensifying platinum rhodium powder gross weight.
Preferably, in the preparation method step 3.1 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the sintering mould
For cuboid or other shapes mould.The sintering mould is made up of graphite or other materials not with platinum reaction.
Preferably, it is described to be sintered in vacuum in the preparation method step 3.2 of above-mentioned dispersion intensifying platinum rhodium and platinum composite
Carried out under degree ＜ 10Pa；Or carried out under inert gas shielding, protective gas pressure is 10~300Pa.The inert gas is
Argon gas.
Specifically, in the method and step 3.2 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the sintering time is 1~5
Hour.It is preferred that 3~4 hours.
Specifically, in the method and step 3.3 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the annealing time is
1~24 hour.It is preferred that 6~12 hours.
Specifically, in the method and step 3.4 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the press time is 1~2
Hour.
Preferably, in the preparation method step 3.8 of above-mentioned dispersion intensifying platinum rhodium and platinum composite, the distance objective is thick
Spend for 0.5mm.
Second technical problem to be solved by this invention is to provide by above-mentioned dispersion intensifying platinum rhodium and platinum composite
The dispersion intensifying platinum rhodium that preparation method is prepared and platinum composite.
The inventive method powder processed after raw material platinum is refined by special process, and by dispersion-strengtherning alloy platinum material powder,
The dispersion intensifying platinum rhodium being prepared after both are compound by specific processing step and condition and platinum composite have can be with
Platinum, platinum-rhodium alloy, dispersion intensifying platinum and dispersion intensifying platinum rhodium material carry out the performance of reliable hot forging；Also there is dispersion-strengtherning simultaneously
The intensity of alloy platinum material, toughness, resistance to Poisoning, low volatility.Gained composite products of the invention can pass through hot forging mode pair
The key component of platinum dish is strengthened, and the vessel particularly made to disperse material are strengthened, and it is non-key to play saving
The usage amount of part platinum.One block of 0.3mm thickness forging welding material of forging welding, can extend this part of platinum channel on 1mm thickness platinum channels
Life-span 50~100%.
Brief description of the drawings
Used rectangular mould 1. bottom plate X1 2. side plate X4 when Fig. 1 is sintered
Fig. 2 composite inner institutional frameworks；Top is the institutional framework of alloy platinum material, and bottom is dispersion-strengtherning alloy platinum material
Institutional framework, both are combined together under microstate
Embodiment
Because existing dispersion intensifying platinum rhodium material has good elevated temperature strength, inoxidizability and resistance to melting glass attack
Property, in order to improve the performance of vessel, it is desirable in the one layer of dispersion-strengthened material in the surface of vessel or key position weld, but
Existing dispersion-strengthened material or its composite do not have weld, can not be with vessel weld.
In order that dispersion intensifying platinum rhodium material has weld, the present inventor has found by lot of experiments, can be strong to disperse
Change platinum rhodium material to be modified, it is compound with alloy platinum material to be passed to special technique, so as to be prepared with weld
Composite.
Specifically, the preparation method of dispersion intensifying platinum rhodium and platinum composite, comprises the following steps：
1st, dispersion intensifying platinum rhodium dust is prepared
1.1st, dispensing：0.01~0.06% disperse means by weight percentage, 1~30% rhodium, remaining be alloy platinum material carry out
Dispensing；
1.2nd, induction melting：Rhodium, alloy platinum material are subjected to melting in induction melting furnace, control smelting temperature for 1800~
2100 DEG C, frequency be 3~100KHz, and carry out degasification operation, be then cast into platinum rhodium ingot casting in the mould；
1.3 vacuum melting：By disperse means, platinum rhodium ingot casting vacuum ＜ 10Pa, 1800~2100 DEG C of temperature, frequency 8~
Abundant melting, obtains liquid alloy under the conditions of 100KHz；
1.4th, cast：By 1.3 gained liquid alloy cast moldings under an inert gas, cast temperature is 1800~2100
℃；
1.5th, powder processed：Powder is made in material obtained by 1.4 cast moldings；
2nd, platinum powder end is prepared
2.1st, induction melting：Alloy platinum material is sensed under conditions of 3~100KHz of frequency, 1750~2000 DEG C of temperature
Melting, obtain liquid platinum；
2.2nd, cast：By 2.1 gained liquid platinum cast moldings, cast temperature is 1800~2100 DEG C；
2.3rd, powder processed：Powder is made in material obtained by 2.2 cast moldings；
3rd, dispersion intensifying platinum rhodium and platinum composite are prepared
3.1st, it is compound：1.5 and 2.3 gained powder are laid in sintering mould, one of which is laid on mould, separately
One kind is laid on former；
3.2nd, sinter：The powder that 3.1 are completed sinters at 1100~1500 DEG C；
3.3rd, anneal oxidation：3.2 gained materials are made annealing treatment at 1200~1450 DEG C；
3.4th, hot pressing：3.3 gained materials are suppressed under 600~1300 DEG C, 4~100MPa of pressure；
3.5th, sizing hot forging：3.4 gained materials are subjected to annealing 15~60 minutes at 1200~1450 DEG C, then
Forged on 200~400kg pneumatic hammers from upper and lower surfaces, 1200~1450 DEG C of initial forging temperature, final forging temperature 900~
1200 DEG C, forge 50~80% after being 3.4 hot pressing to thickness；
3.6th, unformed hot forging：3.5 gained materials are subjected to annealing 15~60 minutes at 1200~1450 DEG C, so
Forged afterwards on 200~400kg pneumatic hammers from six faces, 1200~1450 DEG C of initial forging temperature, final forging temperature 900~1200
DEG C, forge to less than 40% that thickness is 3.2 sintering gained substance thickness；
3.7th, it is surface-treated：The booty of 3.6 gained material surfaces, impurity are removed clean；
3.8th, roll：3.7 gained materials are rolled, in distance objective 0.3~0.8mm of thickness, 1200~
It is heat-treated 15~60 minutes at 1450 DEG C, after heat treatment terminates, then is rolled down to target thickness.
In the inventive method 1.1, the disperse means are at least one of zirconium, yttrium, calcium, lanthanum or titanium；Or zirconium, yttrium, calcium,
The alloy that lanthanum or titanium are formed with platinum.
In the inventive method 1.1, the alloy platinum material purity is more than 99.9%.The alloy platinum material is sponge state, sheet material, plate
Material or melted ingot.
In the inventive method 1.2,1.3 or 2.1, the smelting time is 1~2 hour.
In the inventive method 1.4, the inert gas is argon gas, and pressure is 0.02~0.08MPa.
In the inventive method 1.4 or 2.2, the cast molding is to be cast into bar-shaped, a diameter of 30~50mm.
In the inventive method 1.5 or 2.3, the granularity of the powder is 500 μm of ＜.
In the inventive method 3.1, the sintering mould is cuboid or other shapes mould.The sintering mould by
Graphite or other materials not with platinum reaction are made.
In the inventive method 3.2, described be sintered under vacuum ＜ 10Pa is carried out；Or carried out under inert gas shielding,
Protective gas pressure is 10~300Pa.The inert gas is argon gas.
In the inventive method 3.8, the distance objective thickness is 0.5mm.
In the inventive method 1.5 or 2.3, the powder processed carries out powder processed using conventional method, and different process has different ginsengs
Number, powder processed can use various ways, and the key of powder is granule size in the inventive method, it is only necessary to ensures the grain of powder
Degree is below 500 μm, but granularity is the smaller the better.
In the inventive method step 2, powder processed need to be refined again to alloy platinum material, the properties of product that otherwise powder processed obtains can not
Meet follow-up requirement.
In the inventive method 3.1, general control platinum powder accounts for the 5~95% of gross weight.The more composite elongation percentage of platinum powder
It is better, but elevated temperature strength, inoxidizability, corrosion resistance can reduce；Dispersion intensifying platinum is then opposite.So can be according to composite wood
Expect the addition of requirement both reasonable designs within the above range of performance.Platinum powder and dispersion-strengtherning platinum powder can be 1 ︰ 1,
95 ︰ 5 can be up to.
It is different according to the different filling thickness of mould in the inventive method 3.1, general filling tiling thickness is 80~
200mm, finished ingot thickness are generally 10~40mm.
In the inventive method 3.2, sintering time is not particularly limited, and when sintering time is long, then can be lost time and energy consumption,
Properties of product are influenceed without special.In order to take into account performance and energy consumption, it is 1~5 hour to control sintering time.It is preferred that 3~4 hours.
In the inventive method 3.3, annealing time is not particularly limited, and when annealing time is long, then can be lost time and energy consumption,
Properties of product are influenceed without special.In order to take into account performance and energy consumption, the annealing time is 1~24 hour.It is preferred that 6~12
Hour.
In the inventive method 3.4, the press time is 1~2 hour.
In the inventive method step 3,3.1 is simply simply overlapping by two kinds of powder tilings；3.2 are made by way of sintering
It is bonded together, thickness change unobvious；3.3 change interior tissue by annealing, thickness change unobvious；3.4
Make its top and bottom more fine and close with respect to previous step by hot pressing mode, but it is fine and close not enough, and now thickness change is larger；3.5
Make it more fine and close in upper and lower surfaces by way of hot forging of shaping, other faces are fine and close compared with previous step, now due to 3.4 hot pressing
It is to carry out hot pressing from upper and lower surfaces, then upper and lower surfaces are relatively more fine and close, if 3.5 are all forged from six faces respectively
Beat, then properties of product can be caused bad, so need to be forged from upper and lower surfaces, while being forged from upper and lower surfaces
Other faces can be promoted fine and close compared with previous step；3.6 to be forged by the method for unformed hot forging from six faces to thickness be 3.2 to burn
When tying less than the 40% of gained substance thickness, density of material has met to require；3.7 bring one into because abovementioned steps are likely to result in
A little impurity, so as to go the removal of impurity；Density is rolled down to required size by 3.8 up to desired material, and operation of rolling product is close
Degree is substantially unchanged, and in order to ensure quality, being rolled down to 0.3~0.8mm of distance objective thickness also needs to be heat-treated, and then rerolls
Make target thickness.By above-mentioned steps, so as to obtain the composite with weld, other performances can be entered according to demand
Row regulation.
Embodiment 1
The ratio in the present embodiment being both platinum powder and dispersion intensifying platinum rhodium powder is 1 ︰ 1, in actual production, both ratios
95 ︰ 5 can be up to according to demand.
1st, dispensing：Dispersion intensifying platinum rhodium powder：Disperse means 0.06%, rhodium 10%, surplus are platinum of the purity more than 99.9%
Ingot；Platinum powder：Platinum ingot casting of the purity more than 99.9%；
2nd, induction melting：Platinum ingot and rhodium are placed in induction melting furnace and carry out melting, temperature is 2000 DEG C, and frequency is
30KHz, smelting time is 2 hours, and carries out degasification operation, is cast into platinum rhodium ingot casting in the mould；Platinum ingot casting is passed through into sensing
Smelting furnace carries out melting, and frequency can be selected in 30KHz, and for smelting temperature at 2000 DEG C, smelting time obtained the liquid of platinum at 2 hours
Metal；
3rd, vacuum melting：Disperse means, platinum rhodium ingot casting are put into vacuum melting furnace and carry out melting in vacuum melting furnace, vacuum
5Pa is spent, temperature is 1900 DEG C, and the time is 2 hours, obtains being sufficiently mixed uniform liquid alloy；
4th, it is cast into bar：The platinum liquid metal and 3 obtained liquid alloys that 2 are obtained are cast to ready casting respectively
Club-shaped material is cast in mould, for bar diameter between 30mm, cast temperature is 1900 DEG C；
5th, powder processed：By the dispersion intensifying platinum rhodium bar of 4 cast moldings, by powder manufacturing apparatus, dispersion intensifying platinum rhodium is prepared into
Powder, 500 μm of powder size are stand-by；Platinum rod is then also passed through into powder manufacturing apparatus, be prepared into platinum powder end, 500 μm of powder size,
It is stand-by；
6th, powder stacks：The powder that 5 are obtained is piled up in the in-mold molding of sintering according to 1 ︰ 1 ratio；First will
6kg platinum powders are all deposited in cuboid mould inside, with grafter that surface is floating after all completing, then that 6kg disperses is strong
Change platinum rhodium powder and be deposited in cuboid mould inside again, wait after being stuffed entirely with, the thickness of whole cuboid is 130mm, stand-by；
7th, sinter：6 ready powder moulding mixtures are sintered in sintering furnace, vacuum 5Pa, sintering temperature 1400
DEG C, the time is 5 hours；
8th, anneal oxidation is handled：The product that 7 are obtained is made annealing treatment at a temperature of 1450 DEG C, and processing time is 12
Between hour；
9th, hot pressing：The product that 8 are obtained, is positioned in hot press, and temperature at 600 DEG C, pressed in 100MPa by pressure
System, the press time was at 2 hours；
10th, sizing hot forging：The product that 9 are obtained carries out annealing 60 minutes at 1450 DEG C, then 400kg air again
Forged, can only be forged from upper and lower surfaces on hammer, 1450 DEG C of initial forging temperature forges number 2 times, final forging temperature 1100
DEG C, forge 2 times, then 3 times the step for repetition, until the fine and close simultaneously ingot shape of product；
11st, unformed hot forging：The product that will be obtained after 10 hot forgings, carries out annealing 45 minutes at 1450 DEG C, then
Forged again on 2400kg pneumatic hammers, now need to forge six faces of spindle, make it all fine and close in all directions；Begin to forge
1450 DEG C of temperature, forges number 2 times, 1100 DEG C of final forging temperature, forges 2 times.The step for repeating, make the thickness of spindle (up and down
Distance between face) for sintering after 40%；
12nd, it is surface-treated：The upper and lower surface of the product obtained by mechanical means such as milling, plane, mills by 11 is handled, will
The removals such as booty, impurity on two sides are clean；
13rd, roll：The product that 12 are obtained is rolled on milling train, when being rolled down to 1.0mm, it is necessary to carry out 1400
DEG C heat treatment, heat treatment time be 60 minutes, after the completion of heat treatment, then be rolled down to the thickness 0.5mm of target plate.
The finished product that the present embodiment is obtained samples, and sampling specification is as follows：Long 100mm, wide 10mm, thick 0.5mm, and in temperature
For 1400 DEG C when do strength test.Under equal stress, the high temperature elongation percentage of compound type dispersion-strengtheplatinum-rhodium platinum-rhodium be it is common more
Strengthen platinum rhodium 3 times are dissipated, are 1 times of common platinum rhodium, high temperature service life is 2.5 times of common platinum.And composite of the present invention has
Good weld performance, forging welding can be carried out with dispersion-strengtherning platinum-rhodium alloy, in vessel prepared by dispersion intensifying platinum rhodium thick 1.0mm
Bending part carries out forging welding, can extend 3 months life-spans herein.
Embodiment 2
The ratio in the present embodiment being both platinum powder and dispersion intensifying platinum rhodium powder is 1 ︰ 4, in actual production, both ratios
95 ︰ 5 can be up to according to demand.
1st, dispensing：Dispersion intensifying platinum rhodium powder：Disperse means 0.03%, rhodium 10%, surplus are platinum of the purity more than 99.9%
Ingot；Platinum powder：Platinum ingot casting of the purity more than 99.9%；
2nd, induction melting：Platinum ingot and rhodium are placed in induction melting furnace and carry out melting, temperature is 1950 DEG C, and frequency is
60KHz, smelting time is 1 hour, and carries out degasification operation, is cast into platinum rhodium ingot casting in the mould.Platinum ingot casting is passed through into sensing
Smelting furnace carries out melting, and frequency can be selected in 30KHz, and for smelting temperature at 1950 DEG C, smelting time obtained the liquid of platinum at 1 hour
Metal；
3rd, vacuum melting：Disperse means, platinum rhodium ingot casting are put into vacuum melting furnace and carry out melting in vacuum melting furnace, vacuum
5Pa is spent, temperature is 1950 DEG C, and the time is 2 hours, obtains being sufficiently mixed uniform liquid alloy；
4th, it is cast into bar：The platinum liquid metal and 3 obtained liquid alloys that 2 are obtained are cast to ready casting respectively
Club-shaped material is cast in mould, for bar diameter between 30mm, cast temperature is 1900 DEG C；
5th, powder processed：By the dispersion intensifying platinum rhodium bar of 4 cast moldings, by powder manufacturing apparatus, dispersion intensifying platinum rhodium is prepared into
Powder, 300 μm of powder size are stand-by.Platinum rod is then also passed through into powder manufacturing apparatus, be prepared into platinum powder end, 300 μm of powder size,
It is stand-by；
6th, powder stacks：The powder that 5 are obtained is according to 1：4 ratio is piled up in the in-mold molding of sintering.First will
2kg platinum powders are all deposited in cuboid mould inside, with grafter that surface is floating after band all completes, then that 8kg disperses is strong
Change platinum rhodium powder and be deposited in cuboid mould inside again, after band is stuffed entirely with, the thickness of whole cuboid is 110mm, stand-by；
7th, sinter：6 ready powder moulding mixtures are sintered in sintering furnace, vacuum 5Pa, sintering temperature 1200
DEG C, the time is 4 hours；
8th, anneal oxidation is handled：The product that 7 are obtained is made annealing treatment at a temperature of 1450 DEG C, and processing time is 24
Between hour；
9th, hot pressing：The product that 8 are obtained, is positioned in hot press, and temperature at 800 DEG C, suppressed in 60MPa by pressure,
Press time was at 1 hour；
10th, sizing hot forging：The product that 9 are obtained carries out annealing 30 minutes at 1450 DEG C, then 300kg air again
Forged, can only be forged from upper and lower surfaces on hammer, 1450 DEG C of initial forging temperature forges number 1 time, final forging temperature 1000
DEG C, forge 1 time, then 3 times the step for repetition, until the fine and close simultaneously ingot shape of product；
11st, unformed hot forging：The product that will be obtained after 10 hot forgings, 30 points of annealing is carried out at 1200~1450 DEG C
Clock, is then forged on 300kg pneumatic hammers again, is now needed to forge six faces of spindle, it is all caused in all directions
It is close.1450 DEG C of initial forging temperature, forges number 2 times, 900 DEG C of final forging temperature, forges 2 times.The step for repeating, make the thickness of spindle
(distance between top and bottom) is 30% after sintering；
12nd, it is surface-treated：The upper and lower surface of the product obtained by mechanical means such as milling, plane, mills by 11 is handled, will
The removals such as booty, impurity on two sides are clean；
13rd, roll：The product that 12 are obtained rolled on milling train be rolled down to 0.8mm when, it is necessary to carry out 1400 DEG C
Heat treatment, heat treatment time be 60 minutes, after the completion of heat treatment, then be rolled down to the thickness 0.3mm of target plate.
The finished product that the present embodiment is obtained samples, and sampling specification is as follows：Long 100mm, wide 10mm, thick 0.3mm, and in temperature
For 1400 DEG C when do strength test.Under equal stress, the high temperature elongation percentage of compound type dispersion-strengtheplatinum-rhodium platinum-rhodium be it is common more
Strengthen platinum rhodium 1.5 times are dissipated, are 0.8 times of common platinum rhodium, high temperature service life is 4 times of common platinum-rhodium alloy.And the present invention is compound
Material has good weld performance.Forging welding can be carried out with dispersion-strengtherning platinum-rhodium alloy, in the thick dispersion intensifying platinum rhodium systems of 1.0mm
Standby vessel bending part carries out forging welding, can extend 5 months life-spans herein.
Claims (10)
1. the preparation method of dispersion intensifying platinum rhodium and platinum composite, it is characterised in that：Comprise the following steps：
Step 1, prepare dispersion intensifying platinum rhodium dust
1.1st, dispensing：0.01~0.06% disperse means by weight percentage, 1~30% rhodium, remaining be alloy platinum material carry out dispensing；
1.2nd, induction melting：Rhodium, alloy platinum material are subjected to melting in induction melting furnace, it is 1800~2100 to control smelting temperature
DEG C, frequency be 3~100KHz, and carry out degasification operation, be then cast into platinum rhodium ingot casting in the mould；
1.3 vacuum melting：By disperse means, platinum rhodium ingot casting vacuum ＜ 10Pa, 1800~2100 DEG C of temperature, frequency 8~
Abundant melting, obtains liquid alloy under the conditions of 100KHz；
1.4th, cast：By 1.3 gained liquid alloy cast moldings under an inert gas, cast temperature is 1800~2100 DEG C；
1.5th, powder processed：Powder is made in material obtained by 1.4 cast moldings；
Step 2, prepare platinum powder end
2.1st, induction melting：Alloy platinum material is carried out into sensing under conditions of 3~100KHz of frequency, 1750~2000 DEG C of temperature to melt
Refining, obtains liquid platinum；
2.2nd, cast：By 2.1 gained liquid platinum cast moldings, cast temperature is 1800~2100 DEG C；
2.3rd, powder processed：Powder is made in material obtained by 2.2 cast moldings；
Step 3, prepare dispersion intensifying platinum rhodium and platinum composite
3.1st, it is compound：By 1.5 and 2.3 gained powder overlapping tiles in sintering mould；
3.2nd, sinter：The powder that 3.1 are completed sinters at 1100~1500 DEG C；
3.3rd, anneal oxidation：3.2 gained materials are made annealing treatment at 1200~1450 DEG C；
3.4th, hot pressing：3.3 gained materials are suppressed under 600~1300 DEG C, 4~100MPa of pressure；
3.5th, sizing hot forging：3.4 gained materials are subjected to annealing 15~60 minutes at 1200~1450 DEG C, Ran Hou
Forged on 200~400kg pneumatic hammers from upper and lower surfaces, 1200~1450 DEG C of initial forging temperature, final forging temperature 900~1200
DEG C, forge 50~80% after being 3.4 hot pressing to thickness；
3.6th, unformed hot forging：3.5 gained materials are subjected to annealing 15~60 minutes at 1200~1450 DEG C, Ran Hou
Forged on 200~400kg pneumatic hammers from six faces, 1200~1450 DEG C of initial forging temperature, 900~1200 DEG C of final forging temperature,
Forge to less than 40% that thickness is 3.2 sintering gained substance thickness；
3.7th, it is surface-treated：The booty of 3.6 gained material surfaces, impurity are removed clean；
3.8th, roll：3.7 gained materials are rolled, in distance objective 0.3~0.8mm of thickness, at 1200~1450 DEG C
Lower heat treatment 15~60 minutes, after heat treatment terminates, then is rolled down to target thickness.
2. the preparation method of dispersion intensifying platinum rhodium according to claim 1 and platinum composite, it is characterised in that：Step
In 1.1, the disperse means are at least one of zirconium, yttrium, calcium, lanthanum or titanium；Or the conjunction that zirconium, yttrium, calcium, lanthanum or titanium are formed with platinum
Gold.
3. the preparation method of dispersion intensifying platinum rhodium according to claim 1 and platinum composite, it is characterised in that：Step
1.2nd, in 1.3 or 2.1, the smelting time is 1~2 hour.
4. the preparation method of dispersion intensifying platinum rhodium according to claim 1 and platinum composite, it is characterised in that：Step
In 1.5 or 2.3, the granularity of the powder is 500 μm of ＜.
5. the preparation method of dispersion intensifying platinum rhodium according to claim 1 and platinum composite, it is characterised in that：Step
In 3.1, the platinum powder accounts for the 5~95% of platinum powder and dispersion intensifying platinum rhodium powder gross weight.
6. the preparation method of dispersion intensifying platinum rhodium according to claim 1 and platinum composite, it is characterised in that：Step
In 3.2, described be sintered under vacuum ＜ 10Pa is carried out；Or carried out under inert gas shielding, protective gas pressure be 10~
300Pa。
7. the preparation method of dispersion intensifying platinum rhodium according to claim 1 and platinum composite, it is characterised in that：Step
In 3.2, the sintering time is 1~5 hour；It is preferred that 3~4 hours.
8. the preparation method of dispersion intensifying platinum rhodium according to claim 1 and platinum composite, it is characterised in that：Step
In 3.3, the annealing time is 1~24 hour；It is preferred that 6~12 hours.
9. the preparation method of dispersion intensifying platinum rhodium according to claim 1 and platinum composite, it is characterised in that：Step
In 3.4, the press time is 1~2 hour.
10. it is prepared more by the preparation method of any one of the claim 1~9 dispersion intensifying platinum rhodium and platinum composite
Dissipate and strengthen platinum rhodium and platinum composite.
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| CN110004317A (en) * | 2019-05-08 | 2019-07-12 | 昆明贵金属研究所 | A kind of oxide strengthens the electric arc melting preparation method of platinum rhodium based composites |
| CN110926637A (en) * | 2019-11-07 | 2020-03-27 | 无锡英特派金属制品有限公司 | Preparation method of industrial anti-attenuation platinum and platinum-rhodium thermocouple |
| CN110983095A (en) * | 2019-12-25 | 2020-04-10 | 无锡英特派金属制品有限公司 | Method for compounding dispersion-strengthened platinum rhodium and common platinum rhodium |
| CN111530963A (en) * | 2020-04-29 | 2020-08-14 | 成都光明派特贵金属有限公司 | Manufacturing method of glass liquid stirring rod main shaft |
| CN113073224A (en) * | 2021-03-19 | 2021-07-06 | 泓武科技材料(苏州)有限公司 | Preparation method of platinum group metal dispersion strengthening material |
| CN116005017A (en) * | 2021-10-22 | 2023-04-25 | 张保强 | Method for controlling and recycling smelting loss of platinum-based alloy dispersion strengthening material |
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