CN101444791A - Hot-rolled heating technology of large single-index heavy molybdenum plate - Google Patents

Hot-rolled heating technology of large single-index heavy molybdenum plate Download PDF

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Publication number
CN101444791A
CN101444791A CNA2007101897156A CN200710189715A CN101444791A CN 101444791 A CN101444791 A CN 101444791A CN A2007101897156 A CNA2007101897156 A CN A2007101897156A CN 200710189715 A CN200710189715 A CN 200710189715A CN 101444791 A CN101444791 A CN 101444791A
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sintering
heating
molybdenum plate
hot
pricked
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CNA2007101897156A
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刘劲波
吴维治
毕琳
赵宏宇
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China Nonferrous Metals Processing Technology Co Ltd
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China Nonferrous Metals Processing Technology Co Ltd
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Abstract

The invention relates to a hot-rolled heating technology of a large single-index heavy molybdenum plate in the rare metal plastic working and manufacturing field. The technology consists of blending, pressing, sintering, heating and hot rolling and comprises the following steps: filling a required powder material containing alloy ingredients in a large blender for the blending, filling the blended powder material in a plastic sleeve with a support frame and sealing the mouth of the plastic sleeve; pressing the plastic sleeve and the support frame into a plate billet in a large isostatic pressing machine; sintering the plate billet to obtain a hot rolled billet, pre-sintering the hot rolled billet and then sintering at a high temperature in a large sintering furnace, sequentially heating the billet in an induction heating furnace protected by oxygen consumption gas, a radiation heating furnace with a feeding device and a discharge device and a roller hearth type heating furnace protected by oxygen consumption gas, and hot rolling by an automatic control four-high reversible hot rolling mill and an automatic control two-high four-high reversible hot rolling mill which are provided with special hydraulic thickness. The hot-rolled heating technology can effectively solve the problem of difficulty in manufacturing large-scale large single-index heavy molybdenum plates, has the advantages of low cost, low energy consumption and environmental protection, and is mainly used in rolling mill equipment of large single-index heavy molybdenum, tungsten and titanium plates.

Description

Hot-rolled heating technology of large single-index heavy molybdenum plate
Technical field
The present invention relates to the rare metal pressure processing and make the field, mainly be meant hot-rolled heating technology of large single-index heavy molybdenum plate.
Background technology
Molybdenum belongs to refractory metal, have fusing point height, deformation temperature height, temperature drop is fast, resistance of deformation is big and descend with temperature sharply raise, mould-crisp transition temperature constantly descends with the increase of distortion degree and characteristics such as at high temperature easily air-breathing, easy oxidation.
Molybdenum plate band and deep processed product thereof are widely used in industrial departments such as space flight, chemical industry, metallurgy.Its deep processed product comprises: electronics sputtering target, controllable silicon electronic products such as molybdenum disk.Molybdenum and molybdenum alloy belong to rare refractory metal, and it is very high that hot processing temperature requires, and the producer that therefore has abundant processing experience in the world seldom.Generally can produce thickness in the world below 1.5mm, width specifications more than 600mm and thickness can reach the sheet material of 500mm in the above width specifications of 2mm, more than the length of two kinds of sheet materials all in the scope of 2000mm.Therefore so also just can not satisfy in the world demand far away to large piece weight molybdenum.
The technology that China's domestic production molybdenum plate band is commonly used is the molybdenum powder mixed material at present; on forcing press, be pressed into slab; put into the hydrogen shield sintering furnace then and carry out sintering; molybdenum plate base behind the sintering carries out hot rolling after sending into and being heated to 1350~1500 ℃ in the hydrogen shield molybdenum filament heating furnace, and every twice are melted down heating once.Put it into 500~600 ℃ 95%NaHO+5%KNO after hot rolling is intact again 4Soda boiling 1.5~3 minutes to be to remove surface scale in the solution tank, takes out rapidly then to put into cold water and wash---and alkali is quick-fried; Put into 90%HCl+10H again 2NO 4Carry out pickling in the solution, be white molybdenum plate after the taking-up drying.---cold rolling---annealing that warm-rolling is carried out to molybdenum plate afterwards again in dry back is up to reaching finished product thickness.Adopt this traditional handicraft mainly to have following problem:
(1) the molybdenum billet that exists in the process of the compacting of large-scale molybdenum billet and sintering is because of causing the unequal of density through dress powder, compacting and sintering;
The infeasibility of the molybdenum billet heating that (2) in heating process, exists and the inhomogeneities of temperature;
(3) the instantaneous cooling of molybdenum is fast, yield strength height at high temperature, and with temperature reduce a little its intensity level increase fast, plasticity sharply descends and produce influence the molybdenum plate quality;
(4) cost height and serious environment pollution;
Summary of the invention
In order to improve the shortcoming that prior art exists, the invention provides a kind of hot-rolled heating technology, produce required molybdenum plate thereby this technology can not only solve the problem of above-mentioned existence, and at the bottom of the cost, environmental protection.
The technical solution adopted for the present invention to solve the technical problems is:
Adopt batch mixing and---suppress---sintering---heating---hot rolling technology;
With the alloy ingredient powder material of the needs batch mixing in the large-scale batch mixer of packing into, pack into mixed powder in the garment bag that has bracing frame and the plastic cement running-on is sealed; In macrotype isostatic pressing machine, garment bag and bracing frame are pressed into slab; Sintering goes out hot rolling blank in the large scale sintering stove, carries out presintering in stove earlier, after carry out high temperature sintering; Select for use induction heater, radiation furnace, three kinds of different type of furnaces of roller hearth type heating furnace to heat in regular turn; Adopt four rollers and two, four-roller type special hydraulic thickness to control the reversible hot milling roll hot rolling automatically.
Described induction heater adopts the oxygen consumption gas shield.
The gas of the oxygen consumption gas shield of described induction heater is hydrogen.
Described radiation furnace has brings drawing mechanism into.
The described drawing mechanism of bringing into adopts the hydraulic way transmission.
The transmission of described employing hydraulic way is to adopt crotch formula structure.
The described drawing mechanism of bringing into adopts the mechanical system transmission.
The described drawing mechanism of bringing into adopts the pneumatic mode transmission.
Adopt the protection of combustion type oxygen consumption at the bottom of the roller of described roller hearth type heating furnace.
The gas that described roller hearth type heating furnace oxygen consumption gas shield is adopted is hydrogen.
The invention has the beneficial effects as follows that (1) has solved the molybdenum billet that exists because of cause the unequal problem of density through dress powder, compacting and sintering in the compacting of large-scale molybdenum billet and sintering process.
(2) realize feasibility and the temperature homogeneity that big specification rolled piece heats, satisfied the demand of the big molybdenum plate base of hot rolling temperature.
(3) solved because the instantaneous cooling of molybdenum is fast, the high-temperature yield strength height, and with temperature reduce a little intensity level increase fast, plasticity sharply descends and the problem that influences the molybdenum plate quality that produces, hot rolling is carried out smoothly, and reduced investment, instant effect reach a tractor serves several purposes, have improved utilization rate of equipment and installations.
(4) reduced cost and reduced environmental pollution.
Description of drawings
Fig. 1 is big molybdenum plate workshop technology plane;
1-1 induction heater among the figure, the 1-2 radiation furnace, the 1-3 roller hearth type heating furnace, 1-4 two or four rollers heat/warm-rolling machine, the 1-5 surface is the Shot Blasting unit continuously, the 1-6 coiling machine.
Fig. 2 is the induction heater structural representation;
Fig. 3 is radiation furnace and brings the drawing mechanism structural representation into;
No. 1.2 stove 2. blanks 3. fire doors 4. forks support 5. hydraulic cylinders, 6. forks, 7. V shape framves among the figure
Fig. 4 is the roller hearth type heating furnace structural representation;
Fig. 5 is the structural representation that radiation furnace prepares to lift blank;
Fig. 6 is that radiation furnace is finished the structural representation that lifts the blank process;
Fig. 7 is that radiation furnace is finished the structure structural representation that lifts blank;
The specific embodiment
Technological process of the present invention is as follows:
Batch mixing---compacting---sintering---heating---hot rolling.
Batch mixing is that the alloying component powder that needs are various is packed into and carried out batch mixing in the large-scale batch mixer, and mixed powder packed into has in the garment bag of bracing frame, and the plastic cement running-on is sealed;
Compacting is finished in macrotype isostatic pressing machine.Garment bag is put into macrotype isostatic pressing machine together with bracing frame be pressed into slab;
Sintering is that sintering goes out hot rolling blank in the large scale sintering stove, carries out presintering in stove earlier, after carry out high temperature sintering;
For the cogging of satisfying bulk molybdenum base and hot rolling requirement to temperature, select for use No. 1, No. 2 with No. 3 three kinds of online heating of the different type of furnaces to satisfy the required temperature of hot rolling work.
The molybdenum plate sintered blank is heated to 1400~1500 ℃ from normal temperature, if adopt traditional molybdenum filament hydrogen furnace, then heat time heating time long, hydrogen and electric energy are also wasteful.No. 1 stove has been selected induction heater for use, adopt hydrogen as protective gas in the stove, can fast the sintering billet be heated to 1350~1500 ± 10 ℃ from normal temperature within 20 minutes, the ingot blank that will evenly heat by automatic charging device is shifted the hot-rolling mill roller-way onto then, enters the hot-rolling mill cogging; When rolling 2~5 passages on hot-rolling mill, temperature has dropped to 1150~1200 ℃, and rolled piece plasticity significantly reduces, and must heat once more, can continue rolling.
No. 2 stove adopts the gas mode of heating to heat, and in minutes can bring up to the rolled piece temperature about 1350 ℃ from primary finishing temperature.Rolled piece can commutate going into the stokehold, thereby can carry out that thereby twice heating make material each to being heated evenly; Gas heating stove can utilize the imperfect combustion of gases such as Gao Qing, natural gas, high heating value gas to prevent the oxidation of molybdenum base.Because heat time heating time is shorter, the oxidation of molybdenum base is few, thereby has alleviated bad compound polluted metal surface; We have adopted fork truck formula mechanism the turnover stove mechanism of No. 2 stoves: at the roller-way of the hot rolling V shape frame of putting on the shelf, can select 3~9 forks for use according to the charge length of final heating, fork is fixed on the crotch of roller-way transmission mechanism, when rolling each crotch actual be backplate between roller-way, fork is vertical bar formula structure, each fork can be under the hydraulic cylinder behind the crotch drives level of synchronization turnover burner hearth, blank carried away on the roller-way that burner hearth is sent on the plane or blank taken out in the burner hearth and put on the roller-way.Can lift blank is high when making input and output material, the following of every fork all has a fork that has small-sized assembly pulley to support, and can be promoted to support by hydraulic cylinder the crotch balance is lifted.
No. 2 stove practical operations are as follows: during hot rolling, behind the rolled piece temperature drop, the control of employing computer program, rolled piece is run to roll segments directly over the crotch, stop workpiece motion s, the hydraulic cylinder of fork below will be pitched between roller-way by the mechanism that has the assembly pulley stand and lift, and fork supports rolled piece, leave the height that roller-way is elevated to eminence furnace bottom bearing platform 30 to 50mm simultaneously; Oven door opening, the band material crotch that the hydraulic cylinder behind the crotch will rise by the support of fork downslide wheels, is sent material into burner hearth along assembly pulley; Hydraulic cylinder under the assembly pulley stand descends 50 to 80mm, and material steadily is placed on the heating bearing platform of furnace bottom, withdraws from burner hearth rapidly, closes fire door.Because fork is placed between the roller roller, and is the same with other roller-way backplates, play preventing that rolled piece from boring the effect under the roller-way end to end down.More than operation is because whole computer program is controlled, and whole process time is very short, has guaranteed the temperature homogeneity and the low energy consumption of burner hearth and has reduced the scaling loss that is heated rolled piece.
After heating hot rolling several times repeatedly through No. 2 stoves, calculate according to the deflection of rolled piece and can enter the warm-rolling stage, we select for use hot rolling roller-way rear end to add roller hearth type heating furnace as No. 3 stoves.
No. 3 stoves heating rolled piece temperature is 600~1250 ± 10 ℃, and furnace bottom is the water-cooled roller-way, and burner is arranged up and down with the heating rolled piece.The every rolling twice of rolled piece can heat once in No. 3 stoves during warm-rolling, have guaranteed rolling temperature and have reduced resistance of deformation; The temperature drop of employing gas nozzle heating minimizing rolled piece under the mill table.Lower limit temperature is mainly used in the sheet material leveling, to improve the sheet material glacing flatness.
Hot rolling can adopt two kinds of types: when the billet that is 150 kilograms to 700 kilograms, be that product width is at 650 to 1650 millimeters width products, hot rolling billet thickness is when 70~160 millimeters sintering blank, and milling train can adopt two, the four-roller type hydraulic thickness is controlled reversible hot milling roll automatically; Product width is less than 650 millimeters, and billet weight is at 170 to 200 kilograms, and milling train selects for use the four-roller type hydraulic thickness to control reversible hot milling roll automatically.
The hot rolling start rolling temperature is 1400~1500 ℃, and after the several passages of process are rolling, the rolled piece temperature will be reduced to 1150~1200 ℃.The 50MPa of its resistance of deformation during also by open rolling increases to 220MPa, and the maximum elongation coefficient also drops to 7~8% from 60%.When billet is 150 kilograms to 700 kilograms, because the rolling roughing first passage deformation extent of molybdenum requires and should surpass 25%, preferably reach 30%, in order to prevent rolled piece splitting when rolling, two rolling systems are just adopted in roughing, and enough nip angles are arranged in the time of so just can guaranteeing the first passage heavy reduction, increase drafts, heat and the multi-pass hot rolling for 1~5 time through No. 1 stove 1 passage and No. 2 stoves, rolled piece can roll to 8~50 millimeters thick;
Heat in No. 3 stoves during the rolled piece warm-rolling, mill roll becomes four-high mill.Thereby milling train adopts thinner working roll to reduce total draught pressure when rolling in order to the contact arc length that reduces rolled piece and roll, makes excessive that mill data need not select, the manufacture difficulty of minimizing milling train.The every rolling twice of rolled piece can heat once in No. 3 stoves, have guaranteed rolling temperature and rolling quality; Adopt the gas nozzle local heat to reduce the temperature drop of rolled piece under the mill table and on the roll, reduced roll be full of cracks and rolled piece oxidation rate.
The special formula hydraulic thickness of four rollers is controlled weight that reversible hot milling roll is mainly used in 50~100 millimeters thickness automatically at 170 to 200 kilograms sintering molybdenum billet hot rolling cogging.This moment, the drafts mainly due to first passage reached 25~30 millimeters, and under the situation that guarantees nip angle, roll-force and template, less size just can be selected in the working roll footpath, as 550 millimeters, thereby reduced the complexity that milling train is designed.
The working roll of above-mentioned two kinds of milling trains is when warm-rolling, because molybdenum reduction resistance of deformation increase along with temperature under 600~1200 ℃ is very fast.When work roll diameter is big,, roll-force is significantly increased, cause warm-rolling to carry out to rolling being difficult to that can batch 1.5 millimeters of ideal thickness as press because of roll elastic flattening produces easily with 550 millimeters rolling rolled pieces below 4 millimeters of working roll.
In order to guarantee to roll minimum rolled thickness, we improve rolling mill structure: to be subjected to the contact-making surface of stress metal be the product of rolled piece width and contact arc length to roll when rolling, and contact arc length equals the square root of drafts and working roll radius product, so adopting the scheme that reduces the working roll roller diameter is to reach the ideal scheme that continues to be rolled down to than minimal thickness, it can make flattens the arc length degree when rolling and is reduced, and required draught pressure obviously reduces.
Moment of torsion was very big when the heavy molybdenum plate band of big base was used the hot-rolling mill cogging, therefore the rolling mill universal nodal axisn is also very big, make at one and cause the working roll diameter of axle and cardan axis seriously not to match, make the roll transmission be difficult to realize by the working roll that changes into than minor diameter on the milling train of working roll transmission.
We have adopted the top working roll diameter constant for this reason, only bottom working roll is changed into passive pony roll footpath working roll, as 250~300 millimeter (having strengthened the stroke of roll roll line Adjustment System simultaneously), rolled piece thickness when having significantly reduced roller pressing, reduced draught pressure, warm-rolling to 1.5 millimeter is achieved.Consider the trend of the direction perk that the oriented roller of rolled piece footpath is little, we have adopted special roller-way design to guarantee not perk of rolled piece.
More than two kinds of milling trains all have functions such as hydraulic bending roll, guaranteed that the template of rolled piece is straight.
Hot rolling or warm-rolling enter surface treating machine after the goods specification.We have carried out a large amount of tests to the molybdenum plate surface treatment, though adopting blasting treatment can remove oxide skin, but sandblast needs tinning not to be suitable for serialization production, a large amount of oxide skin powder is difficult to separate from sand, cause metal loss, the speed that sandblasts is uncontrollable, and the product heating alters a great deal with thickness is different with sclerosis.We have selected speed change Shot Blasting technology for use at this, because ball blast speed can change arbitrarily, the gait of march of material also can change with the need, thereby has guaranteed products surface quality.Also guarantee ball blast by return with filtration system circulation in, the oxide skin dust is separated from ball smoothly, has improved workman's working condition and has reclaimed rare metal.
Metal after the surface treatment batches rolling as what made-up belt was used behind machine, be sent to annealing furnace annealing rolled by cold rolling machine altogether; Laggard No. 3 stoves of the processing that surface requirements is high are heated to 400~600 ℃, use the duo mill leveling.
This technology not only is suitable for and large common-substance molybdenum plate, also is applicable to big substance tungsten, titanium plate.

Claims (9)

1. big single molybdenum plate heat is pricked heating process, the i.e. technology of forming by batch mixing, compacting, sintering, heating, hot rolling, it is characterized in that:, pack into mixed powder in the garment bag that has bracing frame and the plastic cement running-on is sealed the alloy ingredient powder material of the needs batch mixing in the large-scale batch mixer of packing into; In macrotype isostatic pressing machine, garment bag and bracing frame are pressed into slab; Sintering goes out hot rolling blank in the large scale sintering stove, carries out presintering in stove earlier, after carry out high temperature sintering; Select for use the induction heater of oxygen consumption gas shield, the radiation furnace of bringing drawing mechanism into, three kinds of different type of furnaces of oxygen consumption gas shield roller hearth type heating furnace to heat in regular turn; Adopt four rollers and two, four-roller type special hydraulic thickness to control the reversible hot milling roll hot rolling automatically.
2. big single molybdenum plate heat according to claim 1 is pricked heating process, and it is characterized in that: the gas of described induction heater oxygen consumption gas shield is hydrogen.
3. big single molybdenum plate heat according to claim 1 is pricked heating process, and it is characterized in that: the described drawing mechanism of bringing into adopts the hydraulic way transmission.
4. big single molybdenum plate heat according to claim 3 is pricked heating process, and it is characterized in that: what described hydraulic way transmission was adopted is crotch formula structure.
5. big single molybdenum plate heat according to claim 4 is pricked heating process, it is characterized in that: described crotch formula structure is meant by the lever of three to nine jaws and the motion of driving jaw to be formed.
6. big single molybdenum plate heat according to claim 1 is pricked heating process, and it is characterized in that: the described drawing mechanism of bringing into adopts the mechanical system transmission.
7. big single molybdenum plate heat according to claim 1 is pricked heating process, and it is characterized in that: the described drawing mechanism of bringing into adopts the pneumatic mode transmission.
8. big single molybdenum plate heat according to claim 1 is pricked heating process, and it is characterized in that: the gas of described roller hearth type heating furnace oxygen consumption gas shield is hydrogen.
9. big single molybdenum plate heat according to claim 1 is pricked heating process, and it is characterized in that: it is speed change Shot Blasting technology that anhydrous physical method is adopted in surface treatment, and adopts accurate self-circulation environmental-friendly system.
CNA2007101897156A 2007-10-10 2007-10-10 Hot-rolled heating technology of large single-index heavy molybdenum plate Pending CN101444791A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102615282A (en) * 2012-03-27 2012-08-01 苏州先端稀有金属有限公司 Processing method for manufacturing wide molybdenum sheet
CN105220095A (en) * 2014-06-13 2016-01-06 北京矿冶研究总院 Preparation method of large single-heavy molybdenum plate
CN109092925A (en) * 2018-10-10 2018-12-28 安徽艾普智能装备有限公司 A kind of forming method of plate
CN110306180A (en) * 2019-08-07 2019-10-08 杨唯加 For improving the hot rolling technology of tungsten molybdenum bar surface hardness
CN114589305A (en) * 2022-04-22 2022-06-07 西安瑞福莱钨钼有限公司 Method for manufacturing molybdenum alloy for fast neutron reactor

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102615282A (en) * 2012-03-27 2012-08-01 苏州先端稀有金属有限公司 Processing method for manufacturing wide molybdenum sheet
CN105220095A (en) * 2014-06-13 2016-01-06 北京矿冶研究总院 Preparation method of large single-heavy molybdenum plate
CN109092925A (en) * 2018-10-10 2018-12-28 安徽艾普智能装备有限公司 A kind of forming method of plate
CN110306180A (en) * 2019-08-07 2019-10-08 杨唯加 For improving the hot rolling technology of tungsten molybdenum bar surface hardness
CN114589305A (en) * 2022-04-22 2022-06-07 西安瑞福莱钨钼有限公司 Method for manufacturing molybdenum alloy for fast neutron reactor
CN114589305B (en) * 2022-04-22 2024-02-13 西安瑞福莱钨钼有限公司 Method for manufacturing molybdenum alloy for fast neutron reactor

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