CN106591614B - A kind of manufacturing process of high life heat screen arc molybdenum plate - Google Patents
A kind of manufacturing process of high life heat screen arc molybdenum plate Download PDFInfo
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- CN106591614B CN106591614B CN201610991872.8A CN201610991872A CN106591614B CN 106591614 B CN106591614 B CN 106591614B CN 201610991872 A CN201610991872 A CN 201610991872A CN 106591614 B CN106591614 B CN 106591614B
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- 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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- 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
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- 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
- B22F3/18—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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22C32/0015—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 with only single oxides as main non-metallic constituents
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
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- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
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- 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
- B22F3/18—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
- B22F2003/185—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 by hot rolling, below sintering temperature
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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
- 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
A kind of manufacturing process of high life heat screen arc molybdenum plate, specifically include the preparation process of the powder A with rhenium blended nano aluminium oxide structure, the preparation process of nano lanthanum oxide, the preparation process of molybdenum plate, the step of preparing using molybdenum plate the step of molybdenum base and being pressed into target arc molybdenum plate using molybdenum base.One aspect of the present invention makes the outside diffusible oxydation reduced capability of molybdenum, improves the oxidation resistance of molybdenum, service life can improve more than 30% by the effect of complex element；On the other hand, powder metallurgy is rolled with machinery and be combined, the arc molybdenum plate relative density of preparation is higher, improves plasticity, avoids cracking；With uniform fine grain structure, physical property and mechanical property are improved.
Description
Technical field
The present invention relates to heat screen technical field, and in particular to a kind of manufacture work of high life heat screen arc molybdenum plate
Skill.
Background technology
LED and sapphire with smelting furnace in addition to molybdenum crucible is used, also using heat screen.Heat screen is the basis in heating furnace
The principle of reflected radiation heat and interlayer thermal resistance reaches heat-insulated and insulation, can reduce temperature by heat screen, average every layer every
Heat shielding can cool 5% or so.Particularly vacuum furnace, it is necessary to using heat screen, to prevent from polluting furnace atmosphere, prevent from blocking up
Fill in vacuum tube and vavuum pump.Wherein, heat screen is the screen cylinder combined by multilayer plate, up to 15 layers.It is required that sheet surface
Cleaning, bright, smooth, non-ripple and cut.
Heat screen can be divided into tungsten heat screen, molybdenum heat screen and steel heat screen three major types, heat screen and be used through long term high temperature,
Easily recrystallize, heat screen is become fragile, and then crack, reduce its service life.Therefore, tying again for heat screen how is made
Brilliant temperature improves, and is that production heat screen enterprise primarily solves the problems, such as.
The content of the invention
The purpose of the present invention is to improve a kind of manufacturing process of high life heat screen arc molybdenum plate, by improving molybdenum plate
Recrystallization temperature, reach the purpose in the life-span in life-span for the heat screen for improving molybdenum plate manufacture.
The used to achieve the above object technical scheme of the present invention is：A kind of system of high life heat screen arc molybdenum plate
Technique is made, is comprised the following steps：
Step 1: taking nano-aluminum hydroxide powder, 4h is calcined at 500 DEG C, alumina powder is made；Then weigh a certain amount of
Alumina powder, add volume ratio and be followed successively by 0.5：1：The hydrogen peroxide that concentrated nitric acid that 4 mass concentration is 65%, mass concentration are 30%
And deionized water, 30 ~ 50min is stood after stirring 4 ~ 8h, by the mixed solution of formation as in autoclave, at 120 ~ 200 DEG C
15 ~ 20h is heated, cooling, much filtrate is dried after filtering, obtains nano alumina powder, it is standby；Wherein, the quality of alumina powder
Ratio with the volume of concentrated nitric acid is 0.3g：1mL；
Step 2: according to 0.15：1 mass ratio, nano alumina powder made from step 1 and rhenium powder are taken successively, will aoxidize
Deionized water is added in aluminium powder, 5 ~ 10min is disperseed under Ultrasonic Conditions, then adds rhenium powder, continues scattered 5 ~ 10min, system
Suspension is obtained, much filtrate is simultaneously calcined 5 by 2 ~ 3h of heating water bath, filtering at 500 ~ 600 DEG C under the conditions of 60 ~ 80 DEG C by suspension
~ 8h, the powder A with rhenium blended nano aluminium oxide structure is made, it is standby；
Step 3: according to 1：1.2：1.8 ~ 2.0 volume ratio, the lanthanum acetate solution, dense that concentration is 0.4mol/L is taken successively
The hydrogenperoxide steam generator for being 1.0mol/L for 3.0mol/L potassium hydroxide solution and concentration is spent, by potassium hydroxide solution and peroxide
Change hydrogen solution to be added portionwise in lanthanum acetate solution, be then transferred in autoclave, pressurize, pressure limit 0.05 ~
0.50Mpa, 20 ~ 55min is incubated at 70 ~ 80 DEG C, then natural cooling 2.5h, filtered, elution, dried at 105 ~ 110 DEG C
Produce Nano-lanthanum hydroxide crystal；According to 1g：2 ~ 10mL ratio, after taking Nano-lanthanum hydroxide crystal and deionized water mixing,
10 ~ 40min of ultrasonic disperse, 4 ~ 8h is stood, filter, dried at 105 ~ 130 DEG C, grinding, after crossing 12500 mesh sieves, in 650 ~ 750
It is calcined at DEG C, soaking time is 0.5 ~ 2h, and nano lanthanum oxide is made, standby；
Step 4: according to 1：0.2~0.5：0.1~0.3：0.5 ~ 0.7 weight ratio, takes molybdenum powder, hafnium powder, step 2 system successively
Nano lanthanum oxide made from the powder A and step 3 obtained, molybdenum powder, hafnium powder, powder A and nano lanthanum oxide are mixed
30min obtains mixed powder, and mixed powder is carried out into 10 ~ 30min of cold isostatic compaction in the case where pressure is 100 ~ 300MPa, obtains base
Body, after sintering 0.5 ~ 1.0h at 300 ~ 400 DEG C, heat is carried out under the conditions of 100 ~ 200MPa, 1200 ~ 1450 DEG C, nitrogen atmosphere
0.5 ~ 2.0h of isostatic pressing, being made has certain thickness molybdenum plate, standby；
Step 5: after molybdenum plate pickling, will be placed in the horizontal chamber furnace (oven) that temperature is 1750 ~ 1900 DEG C after 1 ~ 3h of heating, will
After molybdenum plate carries out hot rolling three times along its length, after molybdenum plate alkali cleaning, 0.5 ~ 1h is incubated at 820 ~ 900 DEG C, after cooling,
At 300 ~ 500 DEG C the hot rolling that thickness deformation amount is 10% is carried out along molybdenum plate length direction；Then it is incubated 0.5 at 820 ~ 900 DEG C again
~ 1h, after cooling, cold rolling three times is carried out along molybdenum plate width, molybdenum base is made, it is standby；
Step 6: between obtained molybdenum base is placed in into the disk roller of veneer reeling machine, molybdenum base is suppressed into camber, and by the molybdenum of compacting
Base and the default model consistent with target arc molybdenum plate radian are contrasted, until molybdenum base is pressed into target arc molybdenum plate.
Further, the method that molybdenum plate is carried out to hot rolling three times along its length in step 5 is：By molybdenum plate 1250 ~
The single hot-roll that thickness deformation amount is 30 ~ 33% is carried out in 1350 DEG C of temperature range；Continue along molybdenum plate length direction, 1150 ~
The secondary hot rolling that the thickness deformation amount after single hot-roll is 10 ~ 20% is carried out in 1200 DEG C of temperature range；Continue along molybdenum plate length
Direction, the hot rolling three times that the thickness deformation amount after secondary hot rolling is 10 ~ 20% is carried out in 1050 ~ 1100 DEG C of temperature ranges.Its
In, first rolling is not more than 20r/min, and roll rotational speed is not more than 60r/min during rolling afterwards, and nip pressure is not more than 60T.
Further, the method that molybdenum plate is carried out to cold rolling three times in the width direction in step 5 is：Molybdenum plate is subjected to thickness
Deflection is 1 ~ 2% once cold rolling；Continue along molybdenum plate width, it is 1 ~ 2% to carry out the thickness deformation amount after once cold rolling
Secondary cold-rolling；Continue along molybdenum plate width, carry out the cold rolling three times that the thickness deformation amount after secondary cold-rolling is 1 ~ 2%.
In step 5, lower a time is carried out again after molybdenum plate is melted down into 3 ~ 10min of insulation after every time rolling in the operation of rolling
Rolling.
Pickling in step 5 uses volume ratio as 1：3：3 HF, H2SO4And HNO3Mix acid liquor.
Veneer reeling machine used in the present invention is three rolls plate bending machine of the prior art, including a upper roll wheel and two lower rolls
Wheel, the molybdenum base being wrapped are placed between upper roll wheel and lower roll wheel.
Beneficial effect：1st, the lanthana of nano particle size is made using Nano-lanthanum hydroxide roasting by the present invention, is formed after sintering
Lanthana be in single nanoparticle dispersity, show the property of nano-scale particle, may be considered after the addition still
In single_phase system, dispersivity is good in diffusion process, nanometer with reference to mutually can be moved on other crystal grain, make diffusion layer have compared with
High toughness, the defects of avoiding alloy fragility big；Meanwhile the rare earth element for having very big affinity to oxygen passes through oxide grain boundary
The trend of the surface migration higher to oxidation activity, during travel motion, larger active rare-earth ion convergent collection is inclined
Analysis has blocked oxygen to the passage of molybdenum depths diffusible oxydation, has changed molybdenum oxidation mechanism, make molybdenum to external diffusion at oxide grain boundary
Oxidability weakens, and improves the oxidation resistance of molybdenum, and service life can improve more than 30%.
2nd, lanthanum and the impurity O being gathered on crystal boundary generate small lanthana, play a part of purifying crystal boundary, and prevent crystalline substance
The migration on boundary, reduce serious segregation of the oxygen in grain boundaries, strengthen crystal boundary adhesion, improve the brittleness at room temperature of blank；Can
To improve the tensile strength and yield strength of rolling molybdenum product simultaneously on the premise of plasticity is hardly reduced；It is significantly increased
The fracture toughness of molybdenum materials, by the fracture toughness of material brings up to more than 3 ~ 4 times of pure Mo.The compound molybdenum filament of rare earth, rhenium
Show excellent high annealing intensity, and with the higher elongation percentage of the molybdenum filament more metal-doped than the single of same content, more preferable
Mouldability and processability.
3rd, isostatic cool pressing and high temperature insostatic pressing (HIP) are combined and prepare molybdenum plate by the present invention, are then rolled, by powder metallurgy with
Machinery, which rolls, to be combined, and the arc molybdenum plate relative density of preparation is higher, is improved plasticity, is avoided cracking；With uniform thin
Grain structure, improve physical property and mechanical property.
4th, alkali cleaning in step 5,300 ~ 500 DEG C of rolling after annealing, can reduce resistance of deformation, reinforcing fibre tissue, increase
Add timber intensity and extensibility, annealing can eliminate residual stress and processing caused by deformation and harden, and improve the plasticity of base substrate.
The present invention improves the recrystallization temperature of obtained arc molybdenum plate, can improve 300 ~ 600 DEG C, improves plasticity, improves heat screen
Machinability.
Embodiment
The high life heat screen of the present invention is made with the manufacturing process of arc molybdenum plate with reference to specific embodiment further
Illustrate so that those skilled in the art can be better understood from the present invention and can be practiced, but illustrated embodiment not as
Limitation of the invention.
Isostatic cool pressing and high temperature insostatic pressing (HIP) are combined by the present invention prepares molybdenum plate, is then rolled, by powder metallurgy and machine
Tool, which rolls to be combined, prepares arc molybdenum plate, and specific embodiment is as follows：
Embodiment 1
A kind of high life heat screen manufacturing process of arc molybdenum plate, comprises the following steps：
Step 1: taking nano-aluminum hydroxide powder, 4h is calcined at 500 DEG C, alumina powder is made；Then weigh a certain amount of
Alumina powder, add volume ratio and be followed successively by 0.5：1：The hydrogen peroxide that concentrated nitric acid that 4 mass concentration is 65%, mass concentration are 30%
And deionized water, 45min is stood after stirring 8h, it is cold by the mixed solution of formation as in autoclave, heating 20h at 160 DEG C
But, much filtrate is dried after filtering, obtains nano alumina powder, it is standby；Wherein, the quality of alumina powder and the volume of concentrated nitric acid
Ratio be 0.3g：1mL；
Step 2: according to 0.15：1 mass ratio, nano alumina powder made from step 1 and rhenium powder are taken successively, will aoxidize
Deionized water is added in aluminium powder, 10min is disperseed under Ultrasonic Conditions, then adds rhenium powder, continues scattered 5min, is made and suspends
Liquid, by suspension, much filtrate is simultaneously calcined 7h at 550 DEG C, is made and is mixed with rhenium by heating water bath 2h, filtering under the conditions of 80 DEG C
The powder A of miscellaneous nano oxidized constructed of aluminium, it is standby；
Step 3: according to 1：1.2：1.8 volume ratio, takes the lanthanum acetate solution, concentration that concentration is 0.4mol/L to be successively
3.0mol/L potassium hydroxide solution and concentration is 1.0mol/L hydrogenperoxide steam generator, by potassium hydroxide solution and hydrogen peroxide
Solution by portions is added in lanthanum acetate solution, is then transferred in autoclave, pressurization, pressure limit 0.5Mpa, at 80 DEG C
35min is incubated, then natural cooling 2.5h, filtered, elute much filtrate, much filtrate is dried at 105 DEG C and produces a nanometer hydroxide
Lanthanum crystal；According to 1g：2mL ratio, after taking Nano-lanthanum hydroxide crystal and deionized water mixing, ultrasonic disperse 40min, stand
8h, filter, dried at 125 DEG C, grinding, after crossing 12500 mesh sieves, be calcined at 700 DEG C, soaking time 2h, nanometer is made
Lanthana, it is standby；
Step 4: according to 1：0.2：0.3：0.5 weight ratio, take successively molybdenum powder, hafnium powder, powder A made from step 2 with
And nano lanthanum oxide made from step 3, molybdenum powder, hafnium powder, powder A and nano lanthanum oxide are subjected to mixing 30min and obtain mixed powder
Body, mixed powder is subjected to cold isostatic compaction 20min in the case where pressure is 220MPa, base substrate is obtained, 1h is sintered at 300 DEG C
Afterwards, hip moulding 2h is carried out under the conditions of 200MPa, 1250 DEG C, nitrogen atmosphere, being made has certain thickness molybdenum plate, standby
With；
Step 5: after molybdenum plate pickling, will be placed in the horizontal chamber furnace (oven) that temperature is 1750 DEG C after heating 3h, molybdenum plate edge is long
After degree direction carries out hot rolling three times, after molybdenum plate alkali cleaning, 1h is incubated at 820 DEG C, after cooling, along molybdenum plate length at 330 DEG C
Direction carries out the hot rolling that thickness deformation amount is 10%；Then 1h is incubated at 820 DEG C again, after cooling, is carried out along molybdenum plate width
Cold rolling three times, molybdenum base is made, it is standby；Wherein, the method that molybdenum plate carries out hot rolling three times along its length is：By molybdenum plate at 1250 DEG C
Temperature range in carry out the single hot-roll that thickness deformation amount is 30%；Continue along molybdenum plate length direction, 1150 DEG C of humidity province
The secondary hot rolling that thickness deformation amount after interior progress single hot-roll is 10%；Continue along molybdenum plate length direction, in 1050 DEG C of temperature
The hot rolling three times that the thickness deformation amount spent in section after carrying out secondary hot rolling is 10%, wherein, first rolling is not more than 20r/min,
Roll rotational speed is not more than 60r/min during rolling afterwards, and nip pressure is not more than 60T.
The method that molybdenum plate carries out cold rolling three times in the width direction is：By molybdenum plate carry out thickness deformation amount be 1% it is once cold
Roll；Continue along molybdenum plate width, carry out the secondary cold-rolling that the thickness deformation amount after once cold rolling is 2%；Continue along molybdenum plate width
Direction, carry out the cold rolling three times that the thickness deformation amount after secondary cold-rolling is 2%.
Step 6: between obtained molybdenum base is placed in into the disk roller of veneer reeling machine, molybdenum base is suppressed into camber, and by the molybdenum of compacting
Base and the default model consistent with target arc molybdenum plate radian are contrasted, until molybdenum base is pressed into target arc molybdenum plate.
In step 5, carried out down again together after molybdenum plate is melted down into 3 ~ 10min of insulation after every time rolling in the operation of rolling
Secondary rolling.Pickling uses volume ratio as 1：3：3 HF, H2SO4And HNO3Mix acid liquor；Alkali cleaning use mass concentration for 10 ~
15% sodium hydroxide solution, the temperature of alkali cleaning is 80 ~ 100 DEG C, and the time of alkali cleaning is 20 ~ 60s.
The lanthana that the present invention adds, the recrystallization temperature of molybdenum can be made to improve to 300 ~ 500 DEG C, using adding for the present invention
Work technique, it can improve the plasticity of molybdenum plate, improve the machinability of heat screen.The hot-rolled temperature of step 4 of the present invention is maintained at
1300~1350℃；Step 5 hot-rolled temperature is maintained at 800 ~ 1200 DEG C, and the passage of a fire 2 ~ 3, single pass deformation amount controlling exists
In 25%；It can be heat-treated according to the soft or hard degree of sheet material；Cold rolling single deformation amount controlling is in 20%.
Embodiment 2
A kind of high life heat screen manufacturing process of arc molybdenum plate, comprises the following steps：Step 1: take a nanometer hydroxide
Aluminium powder, 4h is calcined at 500 DEG C, alumina powder is made；Then a certain amount of alumina powder is weighed, volume ratio is added and is followed successively by
0.5：1：The hydrogen peroxide and deionized water that concentrated nitric acid that 4 mass concentration is 65%, mass concentration are 30%, stand after stirring 4h
30min, by the mixed solution of formation as 16h in autoclave, is heated at 120 DEG C, cool down, dry much filtrate after filtering,
Nano alumina powder is obtained, it is standby；Wherein, the ratio of the quality of alumina powder and the volume of concentrated nitric acid is 0.3g：1mL；
Step 2: according to 0.15：1 mass ratio, nano alumina powder made from step 1 and rhenium powder are taken successively, will aoxidize
Deionized water is added in aluminium powder, 7min is disperseed under Ultrasonic Conditions, then adds rhenium powder, continues scattered 6min, is made and suspends
Liquid, by suspension, much filtrate is simultaneously calcined 8h at 500 DEG C, is made and is mixed with rhenium by heating water bath 3h, filtering under the conditions of 60 DEG C
The powder A of miscellaneous nano oxidized constructed of aluminium, it is standby；
Step 3: according to 1：1.2：2.0 volume ratio, takes the lanthanum acetate solution, concentration that concentration is 0.4mol/L to be successively
3.0mol/L potassium hydroxide solution and concentration is 1.0mol/L hydrogenperoxide steam generator, by potassium hydroxide solution and hydrogen peroxide
Solution by portions is added in lanthanum acetate solution, is then transferred in autoclave, pressurization, pressure limit 0.05Mpa, at 70 DEG C
55min is incubated, then natural cooling 2.5h, filtered, elution, the drying Nano-lanthanum hydroxide crystal at 108 DEG C；According to
1g：7mL ratio, after taking Nano-lanthanum hydroxide crystal and deionized water mixing, ultrasonic disperse 10min, 4h is stood, filtered, in
Dry at 105 DEG C, grinding, after crossing 12500 mesh sieves, be calcined at 750 DEG C, soaking time 1.8h, nano lanthanum oxide is made, it is standby
With；
Step 4: according to 1：0.5：0.1：0.7 weight ratio, take successively molybdenum powder, hafnium powder, powder A made from step 2 with
And nano lanthanum oxide made from step 3, molybdenum powder, hafnium powder, powder A and nano lanthanum oxide are subjected to mixing 30min and obtain mixed powder
Body, mixed powder is subjected to cold isostatic compaction 10min in the case where pressure is 300MPa, base substrate is obtained, 0.8h is sintered at 400 DEG C
Afterwards, hip moulding 1.5h is carried out under the conditions of 130MPa, 1350 DEG C, nitrogen atmosphere, being made has certain thickness molybdenum plate,
It is standby；
Step 5: after molybdenum plate pickling, it will be placed in the horizontal chamber furnace (oven) that temperature is 1850 DEG C after heating 1.8h, by molybdenum plate edge
After length direction carries out hot rolling three times, after molybdenum plate alkali cleaning, 0.6h is incubated at 900 DEG C, after cooling, along molybdenum plate at 500 DEG C
Length direction carries out the hot rolling that thickness deformation amount is 10%；Then 0.6h is incubated at 850 DEG C again, after cooling, along molybdenum plate width side
To cold rolling three times is carried out, molybdenum base is made, it is standby；Wherein, the method that molybdenum plate carries out hot rolling three times along its length is：Molybdenum plate is existed
The single hot-roll that thickness deformation amount is 33% is carried out in 1350 DEG C of temperature range；Continue along molybdenum plate length direction, at 1160 DEG C
The secondary hot rolling that the thickness deformation amount after single hot-roll is 12% is carried out in temperature range；Continue along molybdenum plate length direction, 1100
DEG C temperature range in carry out the hot rolling three times that the thickness deformation amount after secondary hot rolling is 20%；Wherein, first rolling is not more than
20r/min, roll rotational speed is not more than 60r/min during rolling afterwards, and nip pressure is not more than 60T.
The method that molybdenum plate carries out cold rolling three times in the width direction is：By molybdenum plate carry out thickness deformation amount be 2% it is once cold
Roll；Continue along molybdenum plate width, carry out the secondary cold-rolling that the thickness deformation amount after once cold rolling is 1%；Continue along molybdenum plate width
Direction, carry out the cold rolling three times that the thickness deformation amount after secondary cold-rolling is 1%.
Step 6: between obtained molybdenum base is placed in into the disk roller of veneer reeling machine, molybdenum base is suppressed into camber, and by the molybdenum of compacting
Base and the default model consistent with target arc molybdenum plate radian are contrasted, until molybdenum base is pressed into target arc molybdenum plate.
In step 5, lower a time is carried out again after molybdenum plate is melted down into 3 ~ 10min of insulation after every time rolling in the operation of rolling
Rolling；Pickling uses volume ratio as 1：3：3 HF, H2SO4And HNO3Mix acid liquor.
Embodiment 3
A kind of high life heat screen manufacturing process of arc molybdenum plate, comprises the following steps：Step 1: take a nanometer hydroxide
Aluminium powder, 4h is calcined at 500 DEG C, alumina powder is made；Then a certain amount of alumina powder is weighed, volume ratio is added and is followed successively by
0.5：1：The hydrogen peroxide and deionized water that concentrated nitric acid that 4 mass concentration is 65%, mass concentration are 30%, stand after stirring 6.5h
50min, by the mixed solution of formation as 15h in autoclave, is heated at 200 DEG C, cool down, dry much filtrate after filtering,
Nano alumina powder is obtained, it is standby；Wherein, the ratio of the quality of alumina powder and the volume of concentrated nitric acid is 0.3g：1mL；
Step 2: according to 0.15：1 mass ratio, nano alumina powder made from step 1 and rhenium powder are taken successively, will aoxidize
Deionized water is added in aluminium powder, 5min is disperseed under Ultrasonic Conditions, then adds rhenium powder, continues scattered 10min, is made and suspends
Liquid, by suspension, much filtrate is simultaneously calcined 6h by heating water bath 2.5h, filtering at 600 DEG C under the conditions of 65 DEG C, and being made has rhenium
The powder A of dopen Nano aluminium oxide structure, it is standby；
Step 3: according to 1：1.2：1.9 volume ratio, takes the lanthanum acetate solution, concentration that concentration is 0.4mol/L to be successively
3.0mol/L potassium hydroxide solution and concentration is 1.0mol/L hydrogenperoxide steam generator, by potassium hydroxide solution and hydrogen peroxide
Solution by portions is added in lanthanum acetate solution, is then transferred in autoclave, pressurization, pressure limit 0.3Mpa, at 77 DEG C
20min is incubated, then natural cooling 2.5h, filtered, elution, the drying Nano-lanthanum hydroxide crystal at 110 DEG C；According to
1g：10mL ratio, after taking Nano-lanthanum hydroxide crystal and deionized water mixing, ultrasonic disperse 33min, 6.5h is stood, filtered,
Dry at 130 DEG C, grinding, after crossing 12500 mesh sieves, be calcined at 650 DEG C, soaking time 0.5h, nano lanthanum oxide is made,
It is standby；
Step 4: according to 1：0.4：0.2：0.6 weight ratio, take successively molybdenum powder, hafnium powder, powder A made from step 2 with
And nano lanthanum oxide made from step 3, molybdenum powder, hafnium powder, powder A and nano lanthanum oxide are subjected to mixing 30min and obtain mixed powder
Body, mixed powder is subjected to cold isostatic compaction 30min in the case where pressure is 100MPa, base substrate is obtained, 0.5h is sintered at 350 DEG C
Afterwards, hip moulding 0.5h is carried out under the conditions of 100MPa, 1450 DEG C, nitrogen atmosphere, being made has certain thickness molybdenum plate,
It is standby；
Step 5: after molybdenum plate pickling, will be placed in the horizontal chamber furnace (oven) that temperature is 1900 DEG C after heating 1h, molybdenum plate edge is long
After degree direction carries out hot rolling three times, after molybdenum plate alkali cleaning, 0.8h is incubated at 860 DEG C, after cooling, is grown at 300 DEG C along molybdenum plate
Spend direction and carry out the hot rolling that thickness deformation amount is 10%；Then 0.5h is incubated at 900 DEG C again, after cooling, along molybdenum plate width
Cold rolling three times is carried out, molybdenum base is made, it is standby；Wherein, the method that molybdenum plate carries out hot rolling three times along its length is：Molybdenum plate is existed
The single hot-roll that thickness deformation amount is 31% is carried out in 1260 DEG C of temperature range；Continue along molybdenum plate length direction, at 1200 DEG C
The secondary hot rolling that the thickness deformation amount after single hot-roll is 20% is carried out in temperature range；Continue along molybdenum plate length direction, 1060
DEG C temperature range in carry out the hot rolling three times that the thickness deformation amount after secondary hot rolling is 13%, first rolling is not more than 20r/
Min, roll rotational speed is not more than 60r/min during rolling afterwards, and nip pressure is not more than 60T, reduces roll pair to greatest extent
The tension of base substrate.
The method that molybdenum plate carries out cold rolling three times in the width direction is：By molybdenum plate carry out thickness deformation amount be 1.5% it is once cold
Roll；Continue along molybdenum plate width, carry out the secondary cold-rolling that the thickness deformation amount after once cold rolling is 1.5%；Continue wide along molybdenum plate
Direction is spent, carries out the cold rolling three times that the thickness deformation amount after secondary cold-rolling is 1.5%.
Step 6: between obtained molybdenum base is placed in into the disk roller of veneer reeling machine, molybdenum base is suppressed into camber, and by the molybdenum of compacting
Base and the default model consistent with target arc molybdenum plate radian are contrasted, until molybdenum base is pressed into target arc molybdenum plate.
In step 5, lower a time is carried out again after molybdenum plate is melted down into 3 ~ 10min of insulation after every time rolling in the operation of rolling
Rolling；Pickling therein uses volume ratio as 1：3：3 HF, H2SO4And HNO3Mix acid liquor.
In the present invention, molybdenum plate amounts to seven rollings with width along its length, avoids because rolling is insufficient to allow change
Shape expands to molybdenum plate centre, the problem of in turn resulting in the defects of molybdenum plate end is cracked, and larger deflection makes molybdenum plate
Internal metallic element has reached the category of metallic bond gravitation, improves intercrystalline adhesion.Through length direction and width
Exist after the rolling of different directions, in molybdenum plate interlaced fibrous elongate grains and, arrangement it is compact, hole is few, intercrystalline
Contact surface combines closely.Meanwhile crisscross rolling, vertically and horizontally organize mutually overlap joint to interlock, crystal grain arrangement is more uniformly distributed,
Can be effectively prevented from it is each to discontinuity when produce defect, moreover, tandem rolling crackle trend with roll to synchronism it is small,
And extensions path effective length is grown, and retardation has been further expanded to crackle.
Electron microscopic observation discovery is scanned to powder A produced by the present invention, rhenium is adhered to the surface of nano alumina particles,
Solve the problems, such as that nano particle is easily reunited, powder A is added to nano particle size truly in molybdenum powder, give full play to
The advantage of nano particle.The addition of aluminum oxide, in the case of a high temperature, gas phase hydrous oxide can be prevented in molybdenum particle surface
Deposition, and then suppress growing up for molybdenum particle, play a part of refinement.
Contain (Mo, Hf) in the molybdenum product of the present inventionxOyParticle, the intensity and consistency of molybdenum product are improved, moreover, hafnium
Tiny, disperse high-melting-point carbide particle is generated with carbon reaction, dispersion-strengthened action is played at high temperature, improves alloy strength
And plasticity.
Claims (6)
1. a kind of manufacturing process of high life heat screen arc molybdenum plate, it is characterised in that comprise the following steps：
Step 1: taking nano-aluminum hydroxide powder, 4h is calcined at 500 DEG C, alumina powder is made；Then a certain amount of oxidation is weighed
Aluminium powder, add volume ratio and be followed successively by 0.5：1：The hydrogen peroxide and go that concentrated nitric acid that 4 mass concentration is 65%, mass concentration are 30%
Ionized water, 30 ~ 50min is stood after stirring 4 ~ 8h, by the mixed solution of formation as in autoclave, is heated at 120 ~ 200 DEG C
15 ~ 20h, cooling, much filtrate is dried, obtain nano alumina powder after filtering, standby；Wherein, the quality of alumina powder with it is dense
The ratio of the volume of nitric acid is 0.3g：1mL；
Step 2: according to 0.15：1 mass ratio, nano alumina powder made from step 1 and rhenium powder are taken successively, by alumina powder
Middle addition deionized water, 5 ~ 10min is disperseed under Ultrasonic Conditions, then add rhenium powder, continue scattered 5 ~ 10min, be made outstanding
Supernatant liquid, by suspension, much filtrate is simultaneously calcined 5 ~ 8h by 2 ~ 3h of heating water bath, filtering at 500 ~ 600 DEG C under the conditions of 60 ~ 80 DEG C,
The powder A with rhenium blended nano aluminium oxide structure is made, it is standby；
Step 3: according to 1：1.2：1.8 ~ 2.0 volume ratio, takes the lanthanum acetate solution, concentration that concentration is 0.4mol/L to be successively
3.0mol/L potassium hydroxide solution and concentration is 1.0mol/L hydrogenperoxide steam generator, by potassium hydroxide solution and hydrogen peroxide
Solution by portions is added in lanthanum acetate solution, is then transferred in autoclave, pressurization, 0.05 ~ 0.50Mpa of pressure limit,
20 ~ 55min is incubated at 70 ~ 80 DEG C, then natural cooling 2.5h, filtered, elution, the drying nanometer hydrogen at 105 ~ 110 DEG C
Lanthana crystal；According to 1g：2 ~ 10mL ratio, after taking Nano-lanthanum hydroxide crystal and deionized water mixing, ultrasonic disperse 10 ~
40min, 4 ~ 8h is stood, filter, dried at 105 ~ 130 DEG C, grinding, after crossing 12500 mesh sieves, be calcined at 650 ~ 750 DEG C, protected
The warm time is 0.5 ~ 2h, and nano lanthanum oxide is made, standby；
Step 4: according to 1：0.2~0.5：0.1~0.3：0.5 ~ 0.7 weight ratio, molybdenum powder, hafnium powder is taken successively, made from step 2
Nano lanthanum oxide made from powder A and step 3, mixing 30min is carried out by molybdenum powder, hafnium powder, powder A and nano lanthanum oxide
Mixed powder is obtained, mixed powder is subjected to 10 ~ 30min of cold isostatic compaction in the case where pressure is 100 ~ 300MPa, obtains base substrate,
After sintering 0.5 ~ 1.0h at 300 ~ 400 DEG C, high temperature insostatic pressing (HIP) is carried out under the conditions of 100 ~ 200MPa, 1200 ~ 1450 DEG C, nitrogen atmosphere
0.5 ~ 2.0h is molded, being made has certain thickness molybdenum plate, standby；
Step 5: after molybdenum plate pickling, it will be placed in the horizontal chamber furnace (oven) that temperature is 1750 ~ 1900 DEG C after 1 ~ 3h of heating, by molybdenum plate
After carrying out hot rolling three times along its length, after molybdenum plate alkali cleaning, 0.5 ~ 1h is incubated at 820 ~ 900 DEG C, after cooling, 300 ~
At 500 DEG C the hot rolling that thickness deformation amount is 10% is carried out along molybdenum plate length direction；Then 0.5 ~ 1h is incubated at 820 ~ 900 DEG C again,
After cooling, cold rolling three times is carried out along molybdenum plate width, molybdenum base is made, it is standby；
Step 6: between obtained molybdenum base is placed in into the disk roller of veneer reeling machine, molybdenum base is suppressed into camber, and by the molybdenum base of compacting and
The default model consistent with target arc molybdenum plate radian is contrasted, until molybdenum base is pressed into target arc molybdenum plate.
A kind of 2. manufacturing process of high life heat screen arc molybdenum plate according to claim 1, it is characterised in that：Step
The method that molybdenum plate is carried out to hot rolling three times along its length in five is：Molybdenum plate is carried out in 1250 ~ 1350 DEG C of temperature range
Thickness deformation amount is 30 ~ 33% single hot-roll；Continue, along molybdenum plate length direction, to carry out in 1150 ~ 1200 DEG C of temperature ranges
The secondary hot rolling that thickness deformation amount after single hot-roll is 10 ~ 20%；Continue along molybdenum plate length direction, in 1050 ~ 1100 DEG C of temperature
The hot rolling three times that the thickness deformation amount spent in section after carrying out secondary hot rolling is 10 ~ 20%.
A kind of 3. manufacturing process of high life heat screen arc molybdenum plate according to claim 2, it is characterised in that：For the first time
Roll rotational speed is not more than 20r/min during rolling, and roll rotational speed is not more than 60r/min during rolling afterwards, and nip pressure is not more than
60T。
A kind of 4. manufacturing process of high life heat screen arc molybdenum plate according to claim 1, it is characterised in that：Step
The method that molybdenum plate is carried out to cold rolling three times in the width direction in five is：By molybdenum plate carry out thickness deformation amount be 1 ~ 2% it is once cold
Roll；Continue along molybdenum plate width, carry out the secondary cold-rolling that the thickness deformation amount after once cold rolling is 1 ~ 2%；Continue wide along molybdenum plate
Direction is spent, carries out the cold rolling three times that the thickness deformation amount after secondary cold-rolling is 1 ~ 2%.
A kind of 5. manufacturing process of high life heat screen arc molybdenum plate according to claim 1, it is characterised in that：Step
In five, molybdenum plate is melted down to the rolling for carrying out lower a time after 3 ~ 10min of insulation again in the operation of rolling after every time rolling.
A kind of 6. manufacturing process of high life heat screen arc molybdenum plate according to claim 1, it is characterised in that：Step
Pickling in five uses volume ratio as 1：3：3 HF, H2SO4And HNO3Mix acid liquor.
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