CN106636709B - A kind of tungsten alloy sintering process using big flow gas - Google Patents
A kind of tungsten alloy sintering process using big flow gas Download PDFInfo
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- CN106636709B CN106636709B CN201610955213.9A CN201610955213A CN106636709B CN 106636709 B CN106636709 B CN 106636709B CN 201610955213 A CN201610955213 A CN 201610955213A CN 106636709 B CN106636709 B CN 106636709B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- C—CHEMISTRY; METALLURGY
- 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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- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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Abstract
The present invention relates to a kind of sintering methods of the tungsten alloy material using big flow gas.This method is primarily adapted for use in sintering process when producing tungsten alloy base in enormous quantities using indirectly heat sintering process, the process characteristic of the present invention is utilized in the method that big flow gas is passed through during sintering, it is truly realized the high-volume sintering of tungsten alloy base, single stove batch reaches more than 300kg, and sintered tungsten alloy base density is high, tissue and performance uniformity, it is sintered at low cost, follow-up calendering processing lumber recovery is high, significantly reduces production cost, improves production efficiency.
Description
It is on March 25th, 2013 applying date that the application, which is, and entitled " a kind of tungsten alloy using big flow gas is burnt
The divisional application of the Chinese patent application 201310096358.4 of knot technique ".
Technical field
The present invention relates to rare metal field of powder metallurgy, in particular it relates to which a kind of burnt using big flow gas
The method for tying tungsten alloy base.
Background technology
Tungsten alloy is due to having the characteristics that high-melting-point, high creep resistance energy, high elastic modulus, very high elevated temperature strength, extensively
It is general to be applied to the every field such as aerospace, military project, electronics, electric power, metallurgy, Medical Devices.Particularly, tungsten alloy is due to highly dense
Degree, high-melting-point and higher elevated temperature strength and hardness, make it be applied widely in military industry field.For example, in weapons work
In industry, tungsten alloy is used to make kinetic energy penetrator, plate armour and shell, grenade, tungsten alloy bullet, shrapnel head, guided missile aircraft
Balance marble, armor-piercing bullet measurement core, rocket accessory.In aerospace industry, tungsten alloy is used to make ion rocket
Ion ring, inlet sleeve, outlet sleeve, trunnion casing, blowing blade and the locating ring of solid propellant rocket, hot combustion gas reflection
Device and jet vane etc..In atomic energy industry, sheath material and high temperature resistant component etc. can be made.With the development of science and technology,
Increasingly strict requirement is proposed for tungsten alloy.
Most common alloy species refer to adulterate the bianry alloy of Si, Al, K, lanthanum, cerium, yttrium, zirconium, rhenium, thorium etc. in tungsten alloy
And their multicomponent alloy bar base, they are to make filament, argon arc welding, plasma welding, cutting, high temperature furnace component and height
The critical material of intensity gas discharge lamp part, thermocouple, these tungsten alloys are also used for military project purposes, such as make aircraft, tank
Shatter-proof filament, radar magnetron and for weld etc..
In the prior art, Si, Al, K, lanthanum, cerium, yttrium, zirconium, rhenium, the binary tungsten alloy of thorium and their polynary conjunction are adulterated
Gold bar has been produced and has been applied.Tungsten alloy base production technological process be mainly：Tungsten alloy powder → molding → sintering.Wherein, it burns
Knot is the critical process of tungsten alloy base production, which can be generally divided into evacuation (or sending hydrogen blown converter), heating, heat preservation, cooling
Four-stage.Strictly, heating and heat preservation therein are also referred to as sintered, however, the burning of the tungsten alloy base usually described in industry
Connection, sintering process or sintering process include this four-stage.
At present, the method for tungsten alloy sintering mainly has direct sintering and indirect sintering method.Direct sintering, that is, incipient fusion is burnt
Knot.Incipient fusion sintering process is suitble to small lot production for the smaller bar stock production of specification.In order to reduce cost, quality, someone are improved
Attempted indirect sintering method, i.e., it is but unsuccessful using Medium frequency induction sintering and electrical resistance sintering.Therefore, the prior art is still universal
Tungsten alloy is produced using incipient fusion sintering process.
The sintering temperature that Medium frequency induction is sintered and electrical resistance sintering uses is sintered less than incipient fusion, since heating rate is slow, temperature
Field is uniformly, it is possible to improve the tissue and performance of sintered article, of large quantities, lumber recovery is high, energy consumption is small, economic effect with producing
Therefore the advantages of benefit is high, is the direction of future development using Frequency Induction Heating method production tungsten alloy.Medium frequency induction sintering process exists
It has been well used in the production of molybdenum and molybdenum alloy, has also been applied in the production of pure tungsten.
Some producers have been attempted using intermediate frequency furnace sintered tungsten alloy preform, but are only passed through regular flow (i.e. less than 3m3/ hour
Flow) hydrogen.Although taking great effort, the stage of small lot sintering is remained in.At present, use is not seen
Intermediate frequency furnace is sintered the report of more than 100kg tungsten alloy bases.For example, the patent No. 95101208.8 discloses a kind of burning of tungalloy bar
Knot technique although the technique is attempted incipient fusion sintering process to be replaced to produce tungsten alloy base using Medium frequency induction sintering process, but still uses normal
Advise flow.Actually the patent technique discloses existing 17 years, and all tungsten alloy producers are still without a realization Median frequency sintering
To the replacement of incipient fusion sintering.Although many producers are all tested, all end in failure.The fact is that utilize the patent
When technique carries out the sintering of tungsten alloy intermediate frequency furnace, if routinely intermediate frequency furnace batch (300kg or so) shove charge, will lead to whole furnace charge
Tungsten alloy base density is too low after sintering, can not be subsequently processed further, and ultimately causes and all scraps.
Since small lot sintering cannot embody the cost advantage of intermediate frequency furnace, the sintering of tungsten alloy base at present is still that incipient fusion is burnt
Knot occupies dominant position.Intermediate frequency furnace or resistance-heated furnace substitution vertical sintering furnace sintering pure tungsten base already largely should in actual production
With, and economize on electricity, solar term effect are clearly.But intermediate frequency furnace or resistance-heated furnace substitution vertical sintering furnace sintered tungsten alloy preform are but
Be not indiscriminately imitate pure tungsten base sintering process it is so simple.In fact, the sintering process that many producers have attempted to indiscriminately imitate pure tungsten base comes
Sintered tungsten alloy preform, but all end in failure.
As it can be seen that this field is for a long time there is the demand for high-volume sintered tungsten alloy preform, however do not propose have yet
The technical solution of effect thirsts for solution but yet unresolved issue for a long time to solve this.
Invention content
Exist the purpose of the present invention is to solve the problems, such as tungsten alloy base when indirect sintering produces.
For purposes of brevity, Doped Tungsten, example will be known as doped with one or more tungsten alloys in Si, Al and K
Such as, the tungsten alloy containing cerium is known as cerium tungsten, the tungsten alloy containing lanthanum is known as lanthanum tungsten.It should be appreciated that the tungsten alloy containing zirconium
Zirconium tungsten is can be described as, and so on.
For the purpose of the application, defining the accumulative gas consumption of name is：From shove charge to coming out of the stove, add up what is be passed through by air inlet
Gas flow.Also defining practical accumulative gas consumption is：From the gas flow of shove charge actual consumption to during coming out of the stove.
" regular flow " of gas used herein refers to≤3m3The flow of/hour.Naturally, unconventional flow is then
Refer to>3m3The flow of/hour.
Described " room temperature " refers to common environment temperature, such as 0-40 DEG C, such as 10-30 DEG C, particularly 20- herein
25℃。
Gas used herein be selected from hydrogen, nitrogen, argon gas, neon, argon gas and its mixture, have protection and/
Or reduction.Hydrogen more than 50% is included for the preferred gas of the application, preferably greater than 60% hydrogen is more preferably big
In 70% hydrogen, more preferably greater than 80% hydrogen, more preferably greater than 90% hydrogen, more preferably greater than 95% hydrogen,
More preferably it is made of substantially hydrogen.
In general, before sintering, tungsten alloy powder is shaped to strip or rodlike or analogous shape blank material form.In this Shen
Please in, " tungsten alloy base ", " tungalloy bar ", " tungsten alloy billet ", " sintered blank ", " tungsten alloy blank material " and " tungsten alloy web "
It can be used interchangeably.
The object of the present invention is to provide a kind of sintering process of new tungsten alloy, and solving cannot in intermediate frequency furnace or resistance furnace
Carry out the technical barrier of high-volume sintering.
Thus, provide a kind of method for carrying out tungsten alloy sintering, which is characterized in that tungsten alloy base is fitted into it in sintering furnace
Afterwards, this method includes：
From room temperature to 2300 DEG C or 2500 DEG C, preferably from 1200 DEG C -2300 DEG C, preferably 1400 DEG C -1800 DEG C of temperature
In range heating process, in more than 70% time, during being preferably somebody's turn to do in more than 80% time, during being more preferably somebody's turn to do
In more than 90% time, during being more preferably somebody's turn to do in more than 95% time, during being more preferably somebody's turn to do in 100% time,
Flow is passed through in sintering furnace as 10-200m3/ hour, preferably 20-80m3/ hour, more preferably 30-60m3/ hour
Gas,
Wherein described gas is selected from hydrogen, nitrogen, argon gas, neon, helium and its mixture.
In a preferred embodiment, which further includes after the cessation of the heating, and increase gas flow is for example
Increase to 20-200m3/ hour, preferably 30-80m3/ hour, more preferably 40-60m3/ hour, until coming out of the stove.
In a further preferred embodiment, which includes being fitted into sintering furnace later to going out from tungsten alloy base
In all processes of stokehold, flow is passed through in sintering furnace as 10-200m3/ hour, preferably 20-80m3/ hour, more preferably
For 30-60m3The gas of/hour.
It is that impurity is generated and waved in particular in 1400-1800 DEG C of temperature range since tungsten alloy is at 1200-2300 DEG C
The stage for sending out most, it will therefore be appreciated that it is critically important to the impurities removal of tungsten alloy that unconventional flow gas is used in this stage.
When actually controlling, in order to facilitate the operation, the temperature range for being passed through unconventional flow gas can also be extended to highest
Temperature terminates (such as 2300 DEG C, such as 2500 DEG C), can also extend to cooling and terminate, can also shorten so cold
But the time, and then shorten the production cycle.As long as should be understood that gas flow control in required range, operating
In, a certain value of the gas flow rate constant in required range can be controlled, gas flow can also be controlled required
In the range of change.
In sintering process, the method gradually to heat up can also be used, such as is warming up to 1200 DEG C and keeps the temperature 1 hour, then
It is warming up to 1500 DEG C and keeps the temperature 1 hour, be then warming up to 1800 DEG C and keep the temperature 1 hour again, and so on.Other of this sort modes
It is well known in the present art and the present invention may be used, all without departing from the scope of the present invention.
The maximum temperature reached in sintering process can be any temperature in 2300 DEG C -2500 DEG C, such as 2350
DEG C, 2400 DEG C.However, it can still be adjusted on this basis.To the present invention sintering process in maximum temperature without
Any restrictions.
In a preferred embodiment of this aspect, gas includes the hydrogen more than 50% (by volume), preferably greatly
In 60% hydrogen, more preferably greater than 70% hydrogen, more preferably greater than 80% hydrogen, more preferably greater than 90% hydrogen,
More preferably greater than 95% hydrogen, is more preferably made of hydrogen substantially.
In a preferred embodiment of this aspect, tungsten alloy base is binary and polynary tungsten alloy base, such as Doped Tungsten
Alloy preform, the tungsten alloy base containing cerium, the tungsten alloy base containing zirconium, the tungsten alloy base containing yttrium, contain the tungsten alloy base containing lanthanum
Have the tungsten alloy base of thorium, the tungsten alloy base containing rhenium and containing selected from cerium, lanthanum, yttrium, four kinds of elements of zirconium any two, three kinds
Or four kinds of tungsten alloy base.
In a preferred embodiment of this aspect, sintering furnace is the intermediate frequency furnace or use using Frequency Induction Heating
The resistance furnace of resistance heating.
In general, the batch of intermediate frequency furnace or resistance furnace is 300kg tungsten alloy bases or so.However, according to intermediate frequency furnace or resistance
The specific design and configuration of stove, can also be packed into the even more tungsten alloy bases of 50-500kg, such as be packed into 100-400kg,
Such as 310kg is packed into, it is packed into 300kg.According to actual needs or even the intermediate frequency furnace or resistance furnace of bigger batch.Thus, to this
The batch of invention is not limited.
In a preferred embodiment of this aspect, each tungsten alloy base is kept not contact with each other.For example, make in sintering
Each tungsten alloy base is kept not contact with each other with baffle assembly, sintering effect can be further enhanced.
In a preferred embodiment of this aspect, recycling is carried out to the gas discharged from exhaust outlet, so as to
Gas utilization efficiency is improved, it is cost-effective.
General theory is not bound by, applicant thinks that Chinese 95101208.8 patents cannot realize high-volume in intermediate frequency furnace
The main reason for (for example, about 300Kg) is sintered is：The patent technique only recognizes that gas such as hydrogen rises as protective gas
Isolation air prevents the effect of tungsten alloy high-temperature oxydation, but do not recognize, does not also mention the size pair of gas flow at all
The key and decisive influence of sintering process, and other do the tungsten alloy producer attempted and also do not recognize this point at all.
It is not bound by general theory, applicant thinks that the present invention can be successfully the reason is that, big flow in the present invention
Gas also acts as other effects in addition to above-mentioned effect.For example, tungsten alloy base is discharged in sintering process impurity element (such as
Oxide) it discharges out of the furnace quickly, so as to which the atmosphere in sintering furnace be made to be purified in time；Again since a large amount of gases follow in stove
Ring plays heat transfer effect so that the temperature for being sintered material is more uniform, so as to improve the density and close of tungsten alloy sintering
Uniformity is spent, sintered density is up to 18.5g/cm3More than, it is even less that the sintering period can shorten to original half；Meanwhile it holds
Being passed through for gas of continuous big flow further enhances protective effect.
Applicant recognizes through a large number of experiments, sintering of the atmosphere around each tungsten alloy base to this tungsten alloy base
Quality plays the role of key and decisive influence.
In process practice, since pure tungsten does not adulterate, purity is inherently high, and the impurity discharged in sintering is few, gas
Flow is small to nor affect on sintering quality, so can make the sintering success of pure tungsten small gas (such as hydrogen) flow.Phase
Than under, tungsten alloy contains alloy additive, has a large amount of impurity to discharge in sintering, batch is bigger, the impurity level of discharge
Bigger, sintering atmosphere more deteriorates, from room temperature to 2500 DEG C, particularly at 1200-2300 DEG C, more particularly in 1400-1800
DEG C temperature range is that impurity is generated and volatilized most stages, the gas that unconventional flow is passed in this stage be it is critically important,
The a large amount of impurity generated in sintering process can be taken away in time, fully ensure that sintering quality.In most of the time at this stage, example
Being passed through unconventional flow gas such as more than 70%, more than 80%, more than 90%, in more than 95% time can obtain satisfactorily
Effect.Most preferably, it is passed through unconventional flow gas always in this stage.However, understanding indiscriminately imitates sintering pure tungsten less than this point
Technique carry out sintered tungsten alloy preform and can only just fail.
If it is appreciated that being passed through the gas of unconventional flow in entire sintering process, it undoubtedly can also make tungsten alloy
The sintering of base succeeds；It if being passed through the gas of unconventional flow in cooling procedure, can also increase cooling velocity, improve life
Efficiency is produced, and flow is bigger, cooling effect is better.
The sintering of tungalloy bar incipient fusion is the technique for accounting for empery status at present.Due in being sintered in incipient fusion one one into
Row sintering, sintering atmosphere is very good, so not having any problems.Certainly, shortcoming is in high volume to be sintered.
However, in Frequency Induction Heating sintering or during electrical resistance sintering, many tungsten alloy bases are put together sintering, atmosphere is non-
It is often severe.At this moment, only it can just ensure intermediate frequency furnace or resistance-heated furnace to tungsten alloy base using unconventional big flow gas
Successful sintering.
During using this method application Median frequency sintering and electrical resistance sintering tungsten alloy, single stove batch can reach more than 300kg,
Sintered tungsten alloy com-pact density is high, such as density reaches 18.5g/cm3More than, tissue and performance uniformity, lumber recovery
Height is greatly shortened the production cycle (it is even shorter to shorten to pervious 50%), is really sintered instead of incipient fusion, realizes use
Intermediate frequency furnace or resistance furnace carry out the mass production of tungsten alloy.
Description of the drawings
Fig. 1 is heating and the keeping temprature curve of embodiment 10.
Specific embodiment
For the purpose this specification, the amount of all expression compositions, reaction condition etc. in the specification and in the claims
Number in all cases it is understood that be modified by term " about ", unless otherwise specified.Correspondingly, the following specification
It is approximation with the numerical parameter provided in the appended claims, the desirable property that can be attempted according to the present invention
And change, unless the contrary indication.At least, and application of the doctrine of equivalents on right is not intended to limit, each
Numerical parameter at least should round up technology and explain according to the digit of the effective digital reported and according to common.
The mode for illustrating and not to limit provides following embodiment.Only for illustrative purposes only, in following embodiment
In, the gas used is made of substantially hydrogen.
Embodiment
1 cerium tungsten alloy item of embodiment
By cerium tungsten alloy powder through isostatic cool pressing compression moulding, cerium tungsten alloy item, this method technique known for industry are obtained.
Then, cerium tungsten alloy item is divided into three batches.
First cerium tungsten alloy treaty 310kg is put into the intermediate frequency furnace for be connected with recyclegas and is sintered.The intermediate frequency furnace
Equipped with gas purification circulation recycling system.From room temperature to being first passed through regular flow (3m before 1200 DEG C3/ hour)
Hydrogen, increase gas flow after being warming up to 1200 DEG C to 42m3/ hour opens gas purification cycle as described herein again
Using system, until being warming up to 2300 DEG C, after keeping the temperature 2 hours at this temperature, stop heating, increase is passed through gas flow extremely
56m3The hydrogen cooling down of/hour stops hydrogen before coming out of the stove when about 100 DEG C and is passed through, it is sharp again to stop gas purification cycle
Use system.
After coming out of the stove, detect finished product tungalloy bar density >=18.5g/cm3, through the processing such as subsequently swaging or rolling,
It was found that processing performance is good.
Comparative example 1a cerium tungsten alloy items
The second batch cerium tungsten alloy treaty 300kg obtained in embodiment 1 is also placed in the intermediate frequency furnace for be connected with gas and is carried out
Sintering, the intermediate frequency furnace are not equipped with gas purification circulation recycling system.Start latter lead directly into regular flow in heating
(3m3/ hour) gas, stop heating after keeping the temperature 4 hours at 2300 DEG C, cooling down, until about 100 DEG C of whens come out of the stove before stop
Only hydrogen is passed through.After coming out of the stove, detection finished product tungalloy bar density≤17g/cm3, subsequently the processing such as swaged or rolled
When crack, all scrap.
Comparative example 1b cerium tungsten alloy items
The third obtained from embodiment 1 batch cerium tungsten alloy item takes out one (about 1.2kg), is carried out using vertical sinter furnace
Sintering, the technique are known for industry.3m is passed through in sintering process always3The hydrogen of/hour, until cooling terminates.After coming out of the stove, inspection
Survey finished product tungalloy bar density about 18.1g/cm3, the processing such as subsequently swaged or rolled, it is found that processing performance is good.
Embodiment 1 and the more details of comparative example 1a and 1b are referring to the following table 1.
1 embodiment of table, 1 all technical compares
2 yttrium tungalloy bar of embodiment
By yttrium tungsten alloy powder through isostatic pressed into tungsten alloy billet, this method is the known technique of industry.Then, still yttrium
Tungalloy bar is divided into three batches.
First yttrium tungsten alloy treaty 300kg is put into intermediate frequency furnace and is sintered, which is not equipped with gas
Decontamination cycle reutilization system.It is 42m to start latter straight-through inbound traffics in heating3The hydrogen of/hour then proceedes to be warming up to burning
2300 DEG C of junction temperature, after keeping the temperature 2 hours, break heating electricity, is still passed through flow as 42m3The hydrogen cooling down of/hour, until
Stop hydrogen before coming out of the stove at about 100 DEG C to be passed through.After coming out of the stove, detection finished product tungalloy bar density >=18.5g/cm3, through subsequently revolving
Forging or rolling find that processing performance is good.
Comparative example 2a yttrium tungalloy bars
The second batch yttrium tungsten alloy treaty 300kg obtained in embodiment 2 is also placed in the intermediate frequency furnace for be connected with gas and is carried out
Sintering, the intermediate frequency furnace are not equipped with gas purification circulation recycling system.Start latter lead directly into 3m in heating3/ hour
Gas, stops heating after keeping the temperature 4 hours after reaching 2300 DEG C, cooling down stops hydrogen before coming out of the stove when about 100 DEG C and leads to
Enter.After coming out of the stove, detection finished product tungalloy bar density≤17g/cm3, subsequently crack when being swaged or being rolled when processing,
All scrap.
Comparative example 2b yttrium tungalloy bars
Take out one (about 1.2kg) in the third prepared from embodiment 2 batch yttrium tungalloy bar, using vertical sinter furnace into
Row sintering, the technique are known for industry.3m is passed through in sintering process always3The hydrogen of/hour, until cooling terminates.After sintering,
Detect finished product tungalloy bar density about 18g/cm3, the processing such as subsequently swaged or rolled, it is found that processing performance is good.
3 zirconium tungalloy bar of embodiment
Then zirconium tungalloy bar is still divided into three batches by zirconium tungsten alloy powder through isostatic pressed into tungsten alloy billet.
Then, first zirconium tungsten alloy treaty 320kg is put into intermediate frequency furnace and be sintered, which is not equipped with
Gas purification circulation recycling system.3m is first passed through when heating up and starting3The gas of/hour increases gas after being warming up to 1200 DEG C
Body flow is to 10m3/ hour then proceedes to be warming up to 2300 DEG C, after keeping the temperature 2 hours at this temperature, stops heating, still logical
Enter 10m3The hydrogen flowing quantity cooling down of/hour stops hydrogen before coming out of the stove when about 100 DEG C and is passed through.
After coming out of the stove, detection finished product tungalloy bar density >=18.5g/cm3, through the processing such as subsequently swaging or rolling, find
Processing performance is good.
Comparative example 3a zirconium tungalloy bars
The second batch zirconium tungalloy bar obtained in embodiment 3 is also placed in the intermediate frequency furnace with gas and is sintered, it should
Intermediate frequency furnace is not equipped with gas purification circulation recycling system.Start latter lead directly into 3m in heating3The gas of/hour,
Stop heating after keeping the temperature 4 hours at 2300 DEG C, cooling down stops hydrogen before coming out of the stove when about 100 DEG C and is passed through.
After coming out of the stove, detection finished product tungalloy bar density≤17g/cm3, subsequently opened when being swaged or being rolled when processing
It splits, all scraps.
Comparative example 3b zirconium tungalloy bars
The third prepared from embodiment 3 batch zirconium tungalloy bar is taken out one (about 1.2kg) and is carried out using vertical sinter furnace
Sintering, the technique are known for industry.3m is passed through in sintering process always3The hydrogen of/hour, until cooling terminates.It is examined after sintering
Survey finished product tungalloy bar density about 18g/cm3, the processing such as subsequently swaged or rolled, it is found that processing performance is good.
4 lanthanum tungalloy bar of embodiment
By lanthanum tungsten alloy powder through isostatic pressed into tungsten alloy billet, then this method technique known for industry closes lanthanum tungsten
Gold bar is divided into three batches.
First lanthanum tungsten alloy treaty 300kg is put into be passed through in intermediate frequency furnace and is sintered, which is not equipped with
Gas purification circulation recycling system.3m is first passed through after heating starts3The gas of/hour increases gas after being warming up to 1200 DEG C
Body flow is to 200m3/ hour then proceedes to be warming up to 2300 DEG C, after keeping the temperature 2 hours at such a temperature, stops heating, still protects
It holds and is passed through flow as 200m3The hydrogen cooling down of/hour stops hydrogen before coming out of the stove when about 100 DEG C and is passed through.
After coming out of the stove, detection finished product tungalloy bar density >=18.5g/cm3, through the processing such as subsequently swaging or rolling, find
Processing performance is good.
Comparative example 4a lanthanum tungalloy bars
The second batch lanthanum tungsten alloy treaty 300kg obtained in embodiment 2 is also placed in the intermediate frequency furnace with gas and is carried out
Sintering, the intermediate frequency furnace are not equipped with gas purification circulation recycling system.Start latter lead directly into 3m in heating3/ hour
Gas, stops heating after keeping the temperature 4 hours at 2300 DEG C, cooling down stops hydrogen before coming out of the stove when about 100 DEG C and is passed through.
Detection sintering rod density≤17g/cm3, subsequently crack when being swaged or being rolled when processing, all scrap.
Comparative example 4b lanthanum tungalloy bars
The third prepared from embodiment 4 batch lanthanum tungalloy bar is taken out one (about 1.2kg) and is carried out using vertical sinter furnace
Sintering, the technique are known for industry.3m is passed through in sintering process always3The hydrogen of/hour, until cooling terminates.It is examined after sintering
Survey finished product tungalloy bar density about 17.9g/cm3, the processing such as subsequently swaged or rolled, it is found that processing performance is good.
Embodiment 5 adulterates tungalloy bar
The tungsten alloy powder of Si, Al and K will be mixed, be doping tungsten rod through isostatic pressing, then also doping tungsten alloy
Item is divided into three batches.
First is put into intermediate frequency furnace and is sintered, which is not equipped with gas purification cycling and reutilization system
System.3m is first passed through after heating starts3The gas of/hour increases gas flow to 42m after being warming up to 1000 DEG C3/ hour, then
2300 DEG C are continuously heating to, after keeping the temperature 2 hours at a temperature of, stops heating, increase hydrogen flowing quantity is 56m3/ hour to drop as early as possible
Temperature cooling stops hydrogen before coming out of the stove when about 100 DEG C and is passed through.
After coming out of the stove, detection finished product tungalloy bar density >=18.5g/cm3, through the processing such as subsequently swaging or rolling, find
Processing performance is good.
Comparative example 5a adulterates tungalloy bar
By the second batch obtained in embodiment 5 doping tungalloy bar about 300kg be also placed in the intermediate frequency furnace with gas into
Row sintering, the intermediate frequency furnace are not equipped with gas purification circulation recycling system.Start latter lead directly into 3m in heating3/ hour
Gas, stop heating after keeping the temperature 4 hours at 2300 DEG C, cooling down, until about 100 DEG C of whens come out of the stove before stop hydrogen and lead to
Enter.
After coming out of the stove, detection finished product tungalloy bar density≤17g/cm3, subsequently opened when being swaged or being rolled when processing
It splits, all scraps.
Comparative example 5b adulterates tungalloy bar
The third prepared in embodiment 5 batch doping tungalloy bar (one, about 1.2kg) is burnt using vertical sinter furnace
Knot, the technique are known for industry.3m is passed through in sintering process always3The hydrogen of/hour, until cooling terminates.It is detected after sintering
Finished product tungalloy bar density about 18g/cm3, product is qualified after the processing such as subsequently being swaged or being rolled.
6 thorium tungalloy bar of embodiment
By thorium tungsten alloy powder through isostatic pressed into tungsten alloy billet, then this method technique known for industry closes thorium tungsten
Gold bar is divided into three batches.
First thorium tungsten alloy treaty 300kg is put into be passed through in intermediate frequency furnace and is sintered, which is not equipped with
Gas purification circulation recycling system.3m is first passed through when heating up and starting3The gas of/hour increases gas after being warming up to 1200 DEG C
Body flow is to 30m3/ hour then proceedes to be warming up to 2300 DEG C, after the temperature 2 hours, stops heating, is passed through flow
For 40m3The hydrogen cooling down of/hour stops hydrogen before coming out of the stove when about 100 DEG C and is passed through.
After coming out of the stove, detect finished product tungalloy bar density >=18.5g/cm3, through the processing such as subsequently swaging or rolling, hair
Existing processing performance is good.
Comparative example 6a thorium tungalloy bars
The second batch thorium tungsten alloy treaty 300kg obtained in embodiment 5 is also placed in the intermediate frequency furnace for be connected with gas and is carried out
Sintering, the intermediate frequency furnace are not equipped with gas purification circulation recycling system.It is passed through 3m always in whole process3/ hour
Gas, stops heating after keeping the temperature 4 hours at 2300 DEG C, cooling down stops hydrogen before coming out of the stove when about 100 DEG C and is passed through.
Detection sintering rod density≤17g/cm3, subsequently crack when being swaged or being rolled when processing, all scrap.
Comparative example 6b thorium tungalloy bars
The third prepared from embodiment 6 batch thorium tungalloy bar is taken out one (about 1.2kg) and is carried out using vertical sinter furnace
Sintering, the technique are known for industry.3m is passed through in sintering process always3The hydrogen of/hour, until cooling terminates.It is examined after sintering
Survey sintering rod density about 18g/cm3, the processing such as subsequently swaged or rolled, it is found that processing performance is good.
7 tungsten-rhenium alloy item of embodiment
By tungsten-rhenium alloy powder through isostatic pressed into tungsten alloy billet, then this method technique known for industry closes rhenium tungsten
Gold bar is divided into three batches.
First tungsten-rhenium alloy treaty 300kg is put into be passed through in intermediate frequency furnace and is sintered, which is not equipped with
Gas purification circulation recycling system.3m is first passed through when heating up and starting3The gas of/hour increases gas after being warming up to 1200 DEG C
Body flow is to 45m3/ hour then proceedes to be warming up to 2300 DEG C, after the temperature 2 hours, stops heating, is passed through flow
For 60m3The hydrogen cooling down of/hour stops hydrogen before coming out of the stove when about 100 DEG C and is passed through.
After coming out of the stove, detection finished product tungalloy bar density >=18.5g/cm3, through the processing such as subsequently swaging or rolling, find
Processing performance is good.
Comparative example 7a tungsten-rhenium alloy items
The second batch tungsten-rhenium alloy treaty 290kg obtained in embodiment 7 is also placed in the intermediate frequency furnace with gas and is carried out
Sintering, the intermediate frequency furnace are not equipped with gas purification circulation recycling system.Start latter lead directly into 3m in heating3/ hour
Gas, stops heating after keeping the temperature 4 hours at 2300 DEG C, cooling down stops hydrogen before coming out of the stove when about 100 DEG C and is passed through.
After coming out of the stove, detection finished product tungalloy bar density≤17g/cm3, subsequently opened when being swaged or being rolled when processing
It splits, all scraps.
Comparative example 7b tungsten-rhenium alloy items
The third prepared from embodiment 7 batch tungsten-rhenium alloy item is taken out one (about 1.2kg) and is carried out using vertical sinter furnace
Sintering, the technique are known for industry.Heating starts latter lead directly into 3m3The hydrogen of/hour, until cooling terminates.
After coming out of the stove, the density about 18g/cm of finished product tungalloy bar is detected3, the processing such as subsequently swaged or rolled, found
Processing performance is good.
8 cerium tungsten alloy item of embodiment
By cerium tungsten alloy powder through isostatic pressed into tungsten alloy billet, this method is the known technique of industry.Then, still cerium
Tungalloy bar is divided into three batches.
First cerium tungsten alloy treaty 300kg is put into intermediate frequency furnace and is sintered, which is not equipped with gas
Decontamination cycle reutilization system.It is 60m to start latter straight-through inbound traffics in heating3The hydrogen of/hour and the mixed gas of nitrogen,
The volume ratio of wherein hydrogen and nitrogen is about 1:1.It then proceedes to be warming up to 2300 DEG C of sintering temperature, after keeping the temperature 2 hours, heating of breaking
Electricity is still passed through flow as 60m3The hydrogen of/hour and the mixed gas cooling down of nitrogen, before coming out of the stove when about 100 DEG C
Stop being passed through for mixed gas.After coming out of the stove, detection finished product tungalloy bar density >=18.5g/cm3, through subsequently swaging or rolling,
It was found that processing performance is good.
Comparative example 8a cerium tungsten alloy items
The second batch cerium tungsten alloy treaty 300kg obtained in embodiment 8 is also placed in the intermediate frequency furnace for being connected with mixed gas
It is sintered, which is not equipped with gas purification circulation recycling system.Start latter lead directly into 3m in heating3/ small
When hydrogen and nitrogen mixed gas, wherein the volume ratio of hydrogen and nitrogen be 1:1, keep the temperature 4 hours after reaching 2300 DEG C
Stop heating afterwards, cooling down stops being passed through for mixed gas before coming out of the stove when about 100 DEG C.After coming out of the stove, finished product tungsten is detected
Alloy rod density≤17g/cm3, subsequently crack when being swaged or being rolled when processing, all scrap.
Comparative example 8b cerium tungsten alloy items
Take out one (about 1.2kg) in the third prepared from embodiment 8 batch cerium tungsten alloy item, using vertical sinter furnace into
Row sintering, the technique are known for industry.3m is passed through in sintering process always3The hydrogen of/hour and the mixed gas of nitrogen, until
Cooling terminates.After sintering, finished product tungalloy bar density about 18g/cm is detected3, the processing such as subsequently swaged or rolled, find plus
Work is functional.
9 yttrium tungalloy bar of embodiment
By yttrium tungsten alloy powder through isostatic pressed into tungsten alloy billet, this method is the known technique of industry.Then, still yttrium
Tungalloy bar is divided into three batches.
First yttrium tungsten alloy treaty 300kg is put into intermediate frequency furnace and is sintered, which is not equipped with gas
Decontamination cycle reutilization system.It is 50m to start latter straight-through inbound traffics in heating3The argon gas of/hour then proceedes to be warming up to burning
2300 DEG C of junction temperature, after keeping the temperature 2 hours, break heating electricity, is still passed through flow as 50m3The argon gas cooling down of/hour, until
Stop argon gas before coming out of the stove at about 100 DEG C to be passed through.After coming out of the stove, detection finished product tungalloy bar density >=18.5g/cm3, through subsequently revolving
Forging or rolling find that processing performance is good.
Comparative example 9a yttrium tungalloy bars
The second batch yttrium tungsten alloy treaty 300kg obtained in embodiment 9 is also placed in the intermediate frequency furnace for be connected with argon gas and is carried out
Sintering, the intermediate frequency furnace are not equipped with gas purification circulation recycling system.Start latter lead directly into 3m in heating3/ hour
Argon gas, stops heating after keeping the temperature 4 hours after reaching 2300 DEG C, cooling down stops argon gas before coming out of the stove when about 100 DEG C and leads to
Enter.After coming out of the stove, detection finished product tungalloy bar density≤17g/cm3, subsequently crack when being swaged or being rolled when processing,
All scrap.
Comparative example 9b yttrium tungalloy bars
Take out one (about 1.2kg) in the third prepared from embodiment 9 batch yttrium tungalloy bar, using vertical sinter furnace into
Row sintering, the technique are known for industry.3m is passed through in sintering process always3The argon gas of/hour, until cooling terminates.After sintering,
Detect finished product tungalloy bar density about 18.1g/cm3, the processing such as subsequently swaged or rolled, it is found that processing performance is good.
10 tungsten-rhenium alloy item of embodiment
By tungsten-rhenium alloy powder through isostatic pressed into tungsten alloy billet, this method is the known technique of industry.Then, still rhenium
Tungalloy bar is divided into three batches.
First tungsten-rhenium alloy treaty 300kg is put into intermediate frequency furnace and is sintered, which is not equipped with gas
Decontamination cycle reutilization system.Using ladder-elevating temperature heat preserving mode sintered tungsten alloy preform, specially such as the following table 2 and shown in FIG. 1
Heating and keeping temperature rule：
Heating and keeping temperature rule in 2 embodiment 10 of table
It is 3m to start latter straight-through inbound traffics in heating3The hydrogen of/hour, until temperature reaches 1000 DEG C, in the temperature
It is 40m to change gas flow during heat preservation3/ hour, the gas flow being passed through thereafter are always maintained at 40m3/ hour, until 2300 DEG C
Maximum temperature, it is 3m at this moment to change gas flow3/ hour, after keeping the temperature 2 hours, break heating electricity.2300 DEG C are risen to from room temperature altogether
Meter takes 13 hours, wherein the time for being passed through big flow gas is 10 hours；The time for being passed through conventional gas flow is small for 3
When, (i.e. 1 hour) is specially risen in 1000 DEG C of heating process from room temperature and (i.e. 2 is small in insulating process at 2300 DEG C
When).After cooling is come out of the stove, detection finished product tungalloy bar density >=18.5g/cm3, through subsequently swaging or rolling, find processability
It can be good.
Comparative example 10a tungsten-rhenium alloy items
The second batch tungsten-rhenium alloy treaty 300kg obtained in embodiment 10 is also placed in the intermediate frequency furnace for be connected with hydrogen and is carried out
Sintering, the intermediate frequency furnace are not equipped with gas purification circulation recycling system.Start latter lead directly into 3m in heating3/ hour
Hydrogen, stops heating after keeping the temperature 4 hours after reaching 2300 DEG C, cooling down stops hydrogen before coming out of the stove when about 100 DEG C and leads to
Enter.After coming out of the stove, detection finished product tungalloy bar density≤17g/cm3, subsequently crack when being swaged or being rolled when processing,
All scrap.
Comparative example 10b tungsten-rhenium alloy items
One (about 1.2kg) is taken out in the third prepared from embodiment 10 batch tungsten-rhenium alloy item, using vertical sinter furnace
It is sintered, the technique is known for industry.3m is passed through in sintering process always3The hydrogen of/hour, until cooling terminates.Sintering
Afterwards, detection finished product tungalloy bar density about 18.1g/cm3, the processing such as subsequently swaged or rolled, it is found that processing performance is good.
It should be appreciated that those skilled in the art can make the present invention various adjustment with modification without departing from the present invention's
Range.
Claims (35)
1. a kind of sintering method of tungsten alloy base, which is characterized in that after tungsten alloy base is fitted into sintering furnace, this method packet
It includes：
Within time of the temperature from room temperature to during 2300 DEG C more than 70%, flow is passed through as 10-200m3The gas of/hour
Body,
Wherein described gas is selected from hydrogen, nitrogen, argon gas, neon, helium and its mixture.
2. a kind of sintering method of tungsten alloy base, which is characterized in that after tungsten alloy base is fitted into sintering furnace, this method packet
It includes：
Within time of the temperature from room temperature to during 2500 DEG C more than 70%, it is passed through flow 10-200m3The gas of/hour
Body, wherein the gas is selected from hydrogen, nitrogen, argon gas, neon, helium and its mixture.
3. a kind of sintering method of tungsten alloy base, which is characterized in that after tungsten alloy base is fitted into sintering furnace, this method packet
It includes：
It is warming up in the time of 2300 DEG C of more than 70% processes from 1200 DEG C in temperature, is passed through flow 10-200m3The gas of/hour
Body, wherein the gas is selected from hydrogen, nitrogen, argon gas, neon, helium and its mixture.
4. a kind of sintering method of tungsten alloy base, which is characterized in that after tungsten alloy base is fitted into sintering furnace, this method packet
It includes：
It is warming up in the time of 1800 DEG C of more than 70% processes from 1200 DEG C in temperature, is passed through flow 10-200m3The gas of/hour
Body, wherein the gas is selected from hydrogen, nitrogen, argon gas, neon, helium and its mixture.
5. a kind of sintering method of tungsten alloy base, which is characterized in that after tungsten alloy base is fitted into sintering furnace, this method packet
It includes：
It is warming up in temperature from 1400 DEG C during 1800 DEG C in more than 70% time, is passed through flow 10-200m3The gas of/hour
Body, wherein the gas is selected from hydrogen, nitrogen, argon gas, neon, helium and its mixture.
6. any one of them sintering method of claim 1-5, wherein being passed through within more than the 80% of temperature-rise period time
Flow 10-200m3The gas of/hour.
7. any one of them sintering method of claim 1-5, wherein being passed through within more than the 90% of temperature-rise period time
Flow 10-200m3The gas of/hour.
8. any one of them sintering method of claim 1-5, wherein being passed through flow within the 95% of temperature-rise period time
10-200m3The gas of/hour.
9. any one of them sintering method of claim 1-5, wherein being passed through flow within the 100% of temperature-rise period time
10-200m3The gas of/hour.
10. any one of them sintering method of claim 1-5, wherein being passed through flow as 20-80m3The gas of/hour.
11. any one of them sintering method of claim 1-5, wherein being passed through flow as 30-60m3The gas of/hour.
12. any one of them sintering method of claim 1-5 further includes after the cessation of the heating, increases gas flow, until
It comes out of the stove.
13. any one of them sintering method of claim 1-5 further includes after the cessation of the heating, increase gas flow to 20-
200m3/ hour, until coming out of the stove.
14. any one of them sintering method of claim 1-5 further includes after the cessation of the heating, increase gas flow to 30-
80m3/ hour, until coming out of the stove.
15. any one of them sintering method of claim 1-5 further includes after the cessation of the heating, increase gas flow to 40-
60m3/ hour, until coming out of the stove.
16. any one of them sintering method of claim 1-5, including after being fitted into sintering furnace from tungsten alloy base to coming out of the stove
In preceding all processes, flow is passed through in sintering furnace as 10-200m3The gas of/hour.
17. any one of them sintering method of claim 1-5, including after being fitted into sintering furnace from tungsten alloy base to coming out of the stove
In preceding all processes, flow is passed through in sintering furnace as 20-80m3The gas of/hour.
18. any one of them sintering method of claim 1-5, including after being fitted into sintering furnace from tungsten alloy base to coming out of the stove
In preceding all processes, flow is passed through in sintering furnace as 30-60m3The gas of/hour.
19. the sintering method described in any one of claim 1-5, wherein the gas includes the hydrogen more than 50%, with body
Product percentages.
20. the sintering method described in any one of claim 1-5, wherein the gas includes the hydrogen more than 60%, with body
Product percentages.
21. the sintering method described in any one of claim 1-5, wherein the gas includes the hydrogen more than 70%, with body
Product percentages.
22. the sintering method described in any one of claim 1-5, wherein the gas includes the hydrogen more than 80%, with body
Product percentages.
23. the sintering method described in any one of claim 1-5, wherein the gas includes the hydrogen more than 90%, with body
Product percentages.
24. the sintering method described in any one of claim 1-5, wherein the gas includes the hydrogen more than 95%, with body
Product percentages.
25. the sintering method described in any one of claim 1-5, wherein the gas is made of hydrogen.
26. the sintering method described in any one of claim 1-5, wherein tungsten alloy base are binary and polynary tungsten alloy base.
27. the sintering method described in claim 26, wherein binary and polynary tungsten alloy base are doped with selected from Si, Al and K
In one or more Doped Tungsten alloy preform.
28. the sintering method described in claim 26, wherein binary and polynary tungsten alloy base be selected from the tungsten alloy base containing cerium,
Tungsten alloy base containing lanthanum, the tungsten alloy base containing yttrium, the tungsten alloy base containing thorium, contains rhenium at the tungsten alloy base containing zirconium
Tungsten alloy base and containing selected from cerium, lanthanum, yttrium, four kinds of elements of zirconium any two, the tungsten alloy bases of three kinds or four kinds.
29. the sintering method described in any one of claim 1-5 and 27-28, sintering furnace therein is adds using Medium frequency induction
The intermediate frequency furnace of heat or the resistance furnace using resistance heating.
30. the sintering method described in any one of claim 1-5 and 27-28 wherein in sintering process, makes each tungsten alloy
Base does not contact with each other.
31. the sintering method described in any one of claim 1-5 and 27-28, wherein in sintering process, by using partition board
Component makes each tungsten alloy base not contact with each other.
32. the sintering method described in any one of claim 1-5 and 27-28, wherein carrying out recycling to gas.
33. the sintering method described in any one of claim 1-5 and 27-28, wherein passing through gas purification cycling and reutilization system
System carries out recycling to gas.
34. the sintering method described in any one of claim 1-5 and 27-28 gradually heats up wherein being used in sintering process
Method.
35. the sintering method described in any one of claim 1-5 and 27-28, wherein controlling gas flow in sintering process
Change in required range.
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| CN201310095987.5A Active CN103657354B (en) | 2012-08-31 | 2013-03-25 | Circulation recycling system and technique are reclaimed in gas purification for tungsten alloy sintering furnace |
| CN2013201368098U Expired - Fee Related CN203244899U (en) | 2012-08-31 | 2013-03-25 | Gas recovery, purification and recycling system of tungsten alloy sintering furnace |
| CN201610955213.9A Active CN106636709B (en) | 2012-08-31 | 2013-03-25 | A kind of tungsten alloy sintering process using big flow gas |
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| CN105149580B (en) * | 2015-08-21 | 2017-05-03 | 北京矿冶研究总院 | Support for sintering tungsten bars of intermediate frequency furnace |
| CN105244301B (en) * | 2015-10-14 | 2018-06-19 | 上海华力微电子有限公司 | The device and method that a kind of AL etching machine bench heat recycles |
| CN106424703B (en) * | 2016-09-22 | 2018-08-28 | 东睦新材料集团股份有限公司 | A kind of preparation method of compressor piston |
| CN106906396A (en) * | 2017-03-06 | 2017-06-30 | 威海多晶钨钼科技有限公司 | A kind of uniform fine grain Tungsten Bar and preparation method thereof |
| CN107008912A (en) * | 2017-04-28 | 2017-08-04 | 江苏威拉里新材料科技有限公司 | A kind of gas purge system for smelting furnace |
| CN114657431B (en) * | 2022-02-18 | 2023-01-17 | 安泰天龙钨钼科技有限公司 | Energetic tungsten alloy material and preparation method thereof |
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| CN106636709A (en) | 2017-05-10 |
| CN103657354B (en) | 2016-09-07 |
| CN103667756B (en) | 2016-12-28 |
| CN103667756A (en) | 2014-03-26 |
| CN203244899U (en) | 2013-10-23 |
| CN203501764U (en) | 2014-03-26 |
| CN103657354A (en) | 2014-03-26 |
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