CN106636753B - A kind of Ni W Ca Al oxide-coated cathodes metal alkyl materials and its manufacture method - Google Patents
A kind of Ni W Ca Al oxide-coated cathodes metal alkyl materials and its manufacture method Download PDFInfo
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- CN106636753B CN106636753B CN201610928526.5A CN201610928526A CN106636753B CN 106636753 B CN106636753 B CN 106636753B CN 201610928526 A CN201610928526 A CN 201610928526A CN 106636753 B CN106636753 B CN 106636753B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
Abstract
The present invention is to introduce a kind of Ni W Ca Al oxide-coated cathodes metal alkyl materials and its manufacture method, is characterized in that：It is using tungsten, calcium, aluminium as main component, nickel is matrix alloy, the present invention be by vacuum induction melting furnace through high temperature melting, refining, the condensation crust step such as cast molding, reroll and the alloy finished product of respective thickness is made, for the present invention due to having the characteristics that dependable performance, service life are long, highest activationary temperature is low, it is 1898 hours that it, which tests specific average life span, and highest activationary temperature is 945 DEG C, emission current average value 16.5mA, tensile strength average value are 823N/mm2, performance number of the properties value than Ni W cathode substrate material be excellent.The present invention has good processing characteristics, can produce the Strip of different size, be widely used in electronic system, is the core material of the highly reliable super high frequency tube of manufacture and long-life kinescope.
Description
Technical field
The present invention relates to a kind of oxide-coated cathode Base Metal field, specifically a kind of Ni-W-Ca-Al oxide-coated cathodes
Metal alkyl materials and its manufacture method.
Background technology
Nickel tungsten is commonly used for the metal alkyl materials of heater-type oxide-coated cathode.General heater-type oxide-coated cathode, be
One layer of alkaline earth metal carbonate is coated on Base Metal, turns into a kind of good emitter after decomposition activation.Cathode material
Coating is usually to be made up of the carbonate of barium strontium calcium, organic solvent, plasticizer and binding agent.Under the operating temperature of negative electrode, base
Metal needs will have enough mechanical strengths, can excite element while good thermal stability to coating offer is provided, and evaporation is small,
And there is good vacuum performance and processing characteristics.
Existing metal alkyl materials are typically using nickel and nickel alloy etc., because mechanical strength is small, activator is few, activationary temperature
Height, chemical property are unstable, are to cause the service life of device short, reduce emission effciency, influence cathode life.
The content of the invention
The problem of present invention is directed to the above, there is provided a kind of Ni-W-Ca-Al oxide-coated cathodes metal alkyl materials and its manufacturer
Method, the present invention increase substantially the service life of oxidation negative electrode.
The purpose of the present invention is achieved by the following technical solution, and changes the weight hundred of the composition of Ni-W-Ca-Al alloys
Divide than composition and be：Ni is surplus, W:2.5 ~ 4.5%, Ca：0.1 ~ 0.19%, Al：0.1 ~ 0.2%, Cu≤0.02%, Si≤0.01%,
Mn≤0.02%, C≤0.05%, Mg≤0.03%, Fe≤0.03%, Zn≤0.003%, P+Pb+Sn+Bi+Sb+Cd+S≤0.002%.
The percentage of the preferable weight of Ni-W-Ca-Al alloys of the present invention forms：Ni is surplus, W:3.0~4.0%,Ca：
0.1 ~ 0.19%, Al：0.1 ~ 0.2%, Cu≤0.02%, Si≤0.01%, Mn≤0.02%, C≤0.05%, Mg≤0.03%, Fe≤
0.03%,Zn≤0.003%,P+Pb+Sn+Bi+Sb+Cd+S≤0.002%.
Present invention additionally comprises a kind of manufacture method of Ni-W-Ca-Al oxide-coated cathodes metal alkyl materials：It is characterized in that：
Its manufacture method is：It is raw material by electrolytic nickel, tungsten, calcium metal and metallic aluminium, the percentage by weight of each component on request is set
Weight calculation amount；Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking simultaneously vacuumizes, to true
Empty induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts, adjust
Power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C；
Chemical analysis is carried out to ingot casting, takes the ingot casting that chemical composition is qualified, the peeling of car light；The ingot casting that car light is removed the peel is carried out
Hot forging and hot rolling, hot forging temperature are 900 ~ 950 DEG C with hot-rolled temperature, and then cold rolling, rolling intermediate anneal temperature is 750 ~ 850
DEG C, solid solubility temperature is 810 ~ 840 DEG C, and Reduction by rolling is 35 ~ 39% before finished product, rolling pass working modulus 10 ~ 20% or so, two fire
Between general working rate control 40 ~ 44%.
The life-span of oxide-coated cathode has been significantly increased in the present invention.By substantial amounts of experiment, addition metal is finally taken
Ca, Al mode, Ca, Al are added in nickel tungsten, not only with high-temperature stability good possessed by nickel tungsten and
Earthquake-proof function, while Ca, Al can also provide appropriate reducing agent for alkali carbonate coating, improve the activity of negative electrode, so as to
The efficiency of negative electrode is improved, the life-span of oxidation negative electrode is greatly improved.
The present invention has the following advantages compared with oxide-coated cathode metal alkyl materials Ni-W alloys：
1st, the highest activationary temperature of material Ni-W-Ca-Al alloys of the present invention is 945 DEG C, the highest activation temperature of Ni-W alloys
Spend for 1030 DEG C.Material activation temperature of the present invention reduces 8.25% than Ni-W alloy, is improved the efficiency of negative electrode.
2nd, the average emitted of material Ni-W-Ca-Al alloys of the present invention is 16.5mA, and the average emitted of Ni-W alloys is
11.65mA, the average emitted of material of the present invention improve 41.63% than the average emitted of Ni-W alloy, improve the activity of negative electrode.
3rd, material Ni-W-Ca-Al alloys of the present invention aoxidize the metal alkyl materials of negative electrode the most, using average at 900 DEG C
Service life is 1898 hours, and Ni-W alloys are 1519 hours using average life at 900 DEG C, and maximum life span is reachable
1813 hours.The average life of material of the present invention improves 25% than the average life of Ni-W alloy, improves negative electrode
Life-span.
4th, the average value of the tensile strength of Ni-W-Ca-Al alloys of the invention is 823N/mm2, the tension of Ni-W alloys
Intensity is 717 N/mm2, the tensile strength than Ni-W alloy improves 14.8%, adds the intensity of cathode material.
The present invention carries out melting using vacuum induction melting furnace, ensure that the cleaning of melting environment, has purified the pure of product
Cleanliness, prevent objectionable impurities from influenceing the performance of material.
The manufacture method uses vacuum annealing process.Annealed using vacuum argon filling gas shielded, significantly protect band
Material surface quality.
The present invention will be described in further detail by example below, but following examples is only that the present invention is therein
Example, the rights protection scope that the present invention is limited is not represented, the scope of the present invention is with claims
It is defined.
Embodiment：
Embodiment 1
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.63 kilograms of nickel, tungsten
1.25 kilograms, 0.075 kilogram of calcium, 0.05 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.
Operation is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking is simultaneously vacuumized, given
Vacuum induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts,
Adjusting power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Each operation explanation：
1. raw material needs to select electrolytic nickel, tungsten rod, calcium metal, the aluminium ingot of high-quality；
2. conscientiously clearing up fire door and stove upper surface health before charging, avoid remaining the presence of other foreign matters.
3. the casting later stage, which casts at a slow speed, carries out feeding, reduce shrinkage cavity depth, to ensure inside ingot quality.
Constituent analysis：Ni surpluses, W:2.5 ~ 4.5%, Ca：0.1 ~ 0.19%, Al：0.1 ~ 0.2%, Cu≤0.02%, Si≤
0.01%,Mn≤0.02%,C≤0.05%,Mg≤0.03%,Fe≤0.03%,Zn≤0.003%,P+Pb+Sn+Bi+Sb+Cd+S≤
0.002%, analysis method is omited.
4. ingot bar specification is 40 × 120 × 500（mm）, thickness is 36 ~ 35 after surface is polished（mm）, it is intact with surface
Fall into and be defined.
5. ingot bar is heated to 900 ~ 950 DEG C, through first time hot rolling cogging to 15mm, after surface is repaired, through second of heat
7mm is rolled to, after surface is repaired, third time is carried out and is hot-rolled down to 3.5mm, cold rolling is carried out after surface treated.
6. vacuum annealing temperature is 750-850 DEG C between pony-roughing pass, soaking time is 2.5-3 hours, between twice annealing
For general working rate between 40-44%, rolling pass working modulus is 10-20% or so, and finished product working modulus is controlled in 35-39%, is processed into
Finished product.
Embodiment 2
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.38 kilograms of nickel, tungsten
1.5 kilograms, 0.05 kilogram of calcium, 0.075 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.
Operation is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking is simultaneously vacuumized, given
Vacuum induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts,
Adjusting power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 3
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.33 kilograms of nickel, tungsten
1.5 kilograms, 0.075 kilogram of calcium, 0.1 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.Behaviour
Make as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking simultaneously vacuumizes, to true
Empty induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts, adjust
Power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 4
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.41 kilograms of nickel, tungsten
1.5 kilograms, 0.095 kilogram of calcium, 0 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.Operation
It is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking simultaneously vacuumizes, to vacuum
Induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts, Power Regulation
Rate 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 5
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.45 kilograms of nickel, tungsten
1.5 kilograms, 0 kilogram of calcium, 0.05 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.Operation
It is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking simultaneously vacuumizes, to vacuum
Induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts, Power Regulation
Rate 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 6
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.13 kilograms of nickel, tungsten
1.75 kilograms, 0.05 kilogram of calcium, 0.075 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.
Operation is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking is simultaneously vacuumized, given
Vacuum induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts,
Adjusting power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 7
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.13 kilograms of nickel, tungsten
1.75 kilograms, 0.075 kilogram of calcium, 0.05 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.
Operation is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking is simultaneously vacuumized, given
Vacuum induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts,
Adjusting power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 8
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.10 kilograms of nickel, tungsten
1.75 kilograms, 0.075 kilogram of calcium, 0.075 kilogram of aluminium（Load model ZG0.050 25 kilograms of vaccum sensitive stoves step by step
In）.Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking simultaneously vacuumizes, to vacuum
Induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts, Power Regulation
Rate 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 9
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.08 kilograms of nickel, tungsten
1.75 kilograms, 0.075 kilogram of calcium, 0.1 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.
Operation is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking is simultaneously vacuumized, given
Vacuum induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts,
Adjusting power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 10
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.08 kilograms of nickel, tungsten
1.75 kilograms, 0.095 kilogram of calcium, 0.075 kilogram of aluminium（Load model ZG0.050 25 kilograms of vaccum sensitive stoves step by step
In）.Operation is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking is simultaneously taken out true
Sky, start fusing metal to vacuum induction melting furnace power transmission, fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3mm/Hg
During post, adjusting power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, fill
Ar2To 400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, it is powered to be cast into ingot casting, cast temperature is 1550 ~
1650℃.The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 11
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 48.88 kilograms of nickel, tungsten 2
Kilogram, 0.05 kilogram of calcium, 0.075 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.Operation
It is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking simultaneously vacuumizes, to vacuum
Induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts, Power Regulation
Rate 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 12
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 47.85 kilograms of nickel, tungsten 2
Kilogram, 0.075 kilogram of calcium, 0.075 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.Behaviour
Make as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking simultaneously vacuumizes, to true
Empty induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts, adjust
Power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 13
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 47.81 kilograms of nickel, tungsten 2
Kilogram, 0.095 kilogram of calcium, 0.1 kilogram of aluminium（It is fitted into step by step in model ZG0.050 25 kilograms of vaccum sensitive stoves）.Operation
It is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking simultaneously vacuumizes, to vacuum
Induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts, Power Regulation
Rate 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely
400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C.
The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
Embodiment 14
（1）Using nickel, tungsten, calcium, aluminium as raw material alloyage material, each component designing quality is respectively 47.60 kilograms of nickel, tungsten
2.25 kilograms, 0.075 kilogram of calcium, 0.075 kilogram of aluminium（Load model ZG0.050 25 kilograms of vaccum sensitive stoves step by step
In）.Operation is as follows：Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking is simultaneously taken out true
Sky, start fusing metal to vacuum induction melting furnace power transmission, fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3mm/Hg
During post, adjusting power 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, fill
Ar2To 400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, it is powered to be cast into ingot casting, cast temperature is 1550 ~
1650℃.The module of the aftershaping of cooling 20 minutes separates with mould, takes chemical composition analysis.
（2）After taking the qualified ingot bar of chemical composition to carry out surface grinding process, carry out hot forging and hot rolling, warm and hot forging temperature with
Hot-rolled temperature is 900 ~ 950 DEG C, rolls 750 ~ 850 DEG C of intermediate anneal temperature, and 810 ~ 840 DEG C of solid solubility temperature is total between twice annealing
Working modulus control is 40 ~ 44%, rolling pass working modulus 10% ~ 20% or so, and rolling pass working modulus is 35 ~ 39% before finished product, most
Finish to gauge makes specification as band thick 0.2mm.
The band of each taking-up same size is taken from examples detailed above, by using the experimental method test material such as depression curve
Activationary temperature, the life-span, average emitted level etc., as a result such as table 1.Each result is carried out from table to contrast nickel tungsten calloy
The preferred scope of composition be：The percentage by weight of nickel-base alloy composition forms：Ni surpluses, W:3.0~4.0%,Ca：0.1~
0.19%, Al：0.1 ~ 0.2%, other impurities composition will be controlled in certain limit：Cu≤0.02%,Si≤0.01%,Mn≤0.02%,
C≤0.05%,Mg≤0.03%,Fe≤0.03%,Zn≤0.003%,P+Pb+Sn+Bi+Sb+Cd+S≤0.002%.
Each example uses identical experimental condition, is tested, as a result such as table 1.
Table 1
Claims (2)
- A kind of 1. manufacture method of Ni-W-Ca-Al oxide-coated cathodes metal alkyl materials：It is characterized in that：By electrolytic nickel, metal Tungsten, calcium metal and metallic aluminium are raw material, and the percentage by weight of each component is as follows：Ni is surplus, W：2.50 ~ 4.5%, Ca：0.1~ 0.19%, Al：0.1 ~ 0.2%, other impurities composition will be controlled in certain limit：Cu≤0.02%, Si≤0.01%, Mn≤0.02%, C≤0.05%, Mg≤0.03%, Fe≤0.03%, Zn≤0.003%, P+Pb+Sn+Bi+Sb+Cd+S≤0.002%；Electrolytic nickel, tungsten rod and aluminium block are loaded in alumina crucible, calcium metal loads feeder, and banking simultaneously vacuumizes, to vacuum Induction melting furnace power transmission starts fusing metal, and fusing power is 50 ~ 60KW；Treat that vacuum reaches 5 × 10-3During mm/Hg posts, Power Regulation Rate 30-40KW, after refining 20 ~ 30 minutes, have a power failure and condense to molten metal surface crust；Again after power transmission fusing, Ar is filled2Extremely 400mmHg posts, add calcium metal, turndown 2-4 times, treat the 60-90 seconds, powered to be cast into ingot casting, cast temperature is 1550 ~ 1650 DEG C； Chemical analysis is carried out to ingot casting, takes the ingot casting that chemical composition is qualified, the peeling of car light；The ingot casting that car light is removed the peel carries out hot forging and heat Roll, hot forging temperature is 900 ~ 950 DEG C with hot-rolled temperature, then cold rolling, and rolling intermediate anneal temperature is 750 ~ 850 DEG C, solid solution temperature Spend for 810 ~ 840 DEG C, Reduction by rolling is 35 ~ 39% before finished product, rolling pass working modulus 10 ~ 20%, total between twice annealing Working modulus is controlled 40 ~ 44%.
- 2. the manufacture method of Ni-W-Ca-Al oxide-coated cathodes metal alkyl materials according to claim 1：It is characterized in that： The percentage by weight of the Ni-W-Ca-Al oxide-coated cathode metal alkyl materials compositions forms：Ni is surplus, W:3.0~4.0%, Ca：0.1 ~ 0.19%, Al：0.1 ~ 0.2%, other impurities composition will be controlled in certain limit：Cu≤0.02%,Si≤0.01%,Mn ≤0.02%,C≤0.05%,Mg≤0.03%,Fe≤0.03%,Zn≤0.003%,P+Pb+Sn+Bi+Sb+Cd+S≤0.002%。
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