CN105618768B - A kind of preparation method of high-compactness pure tungsten, pure molybdenum and its alloy material - Google Patents
A kind of preparation method of high-compactness pure tungsten, pure molybdenum and its alloy material Download PDFInfo
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- CN105618768B CN105618768B CN201511014392.8A CN201511014392A CN105618768B CN 105618768 B CN105618768 B CN 105618768B CN 201511014392 A CN201511014392 A CN 201511014392A CN 105618768 B CN105618768 B CN 105618768B
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The present invention proposes the preparation method of a kind of high-compactness pure tungsten, pure molybdenum and its alloy material.The key step of this method includes：Raw material powder is carried out break process, obtains broken powder by step 1；The broken powder that step 1 obtains is carried out forming processes, obtains material base by step 2；The material base that step 2 obtains is sintered by step 3, obtains the high-compactness pure tungsten, pure molybdenum and its alloy material.The high-compactness pure tungsten, pure molybdenum and its alloy material are consistency up to 98% or more.By improving the density of sintered state blank, the performances such as hardness, tensile strength, resistance to corrosion, machinability, the hot-working character of sintered state product can be effectively improved.This method is suitable for the powder metallurgy products such as pure tungsten, pure molybdenum, tungsten oxidation lanthanum alloy, tungsten oxidation cerium alloy, tungsten oxidation thorium alloy.
Description
Technical field
The present invention relates to a kind of technology preparing high density refractory metal more particularly to a kind of high-compactness pure tungsten,
The preparation method of pure molybdenum and its alloy material, belongs to field of powder metallurgy.
Background technology
Tungsten, molybdenum and its alloy, with its high-melting-point, high density, good thermal conductivity, low thermal coefficient of expansion, high temperature
The advantages such as non-deformability and preferable wearability, become the preferred material of the use occasions such as high temperature, intense radiation, in electricity
By extensive use in son, electric power, defence and military, the heating of kiln thermal field and structural member.
But the excellent properties of the above tungsten, molybdenum and its alloy material all have prodigious relationship with its consistency.Tungsten, molybdenum and
When 95% or more consistency of its alloy, if consistency reduces by 1%, thermal conductivity, conductivity can decline 10%, and hardness resists
The mechanical performance indexs such as tensile strength can be also remarkably decreased with the reduction of consistency.Currently, the tungsten of high-compactness, molybdenum and its alloy
Mainly by after powder metallurgy sintered, then the hot-working such as forged, rolled to improve its consistency.This traditional handicraft energy
So that material is reached 99% or more consistency, while also can greatly improve the mechanical property of material.But the disadvantage is that Zhi Nengsheng
Production shape is single, the smaller product of such as rodlike, plate or size.If it is required that production shape is complex or medium-sized three-dimensional ruler
Very little high-compactness product, then can not be obtained by deformation processing, or will produce great cost.
Invention content
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of high-compactness pure tungsten, pure molybdenum and its
The preparation method of alloy material.This method is by carrying out tungsten, molybdenum and its alloy powder after being crushed, with isostatic pressed of different shapes
Mold green compact, then be sintered, obtain the high-compactness sintered blank of required shape；This method can prepare big size, shape compared with
For complicated high density tungsten, molybdenum and its alloy material, and do not increase cost substantially, the densification of the tungsten, molybdenum and its alloy product
Degree is 98% or more.
To achieve the above object, the present invention uses following technical scheme：
The preparation method of a kind of high-compactness pure tungsten, pure molybdenum and its alloy material, includes the following steps：
Raw material powder is carried out break process, obtains broken powder by step 1；
The broken powder that step 1 obtains is carried out forming processes, obtains material base by step 2；
The material base that step 2 obtains is sintered by step 3, obtain the high-compactness pure tungsten, pure molybdenum and
Its alloy material.
The preparation method can effectively improve hardness, the tension of sintered state product by the density of raising sintered state blank
The performances such as intensity, resistance to corrosion, machinability, hot-working character.This method is suitable for pure tungsten, pure molybdenum, tungsten-lanthana
Alloy, tungsten-oxidation cerium alloy, tungsten-oxidation thorium alloy, molybdenum-oxidation lanthanum alloy, molybdenum-oxidation cerium alloy, molybdenum-oxidation thorium alloy etc.
Powder metallurgy product.
In above-mentioned preparation method, raw material powder described in step 1 is pure tungsten powder, pure molybdenum as a preferred implementation manner,
Powder, tungsten alloy powder or molybdenum alloy powder；The tungsten alloy powder can be tungsten-oxidation lanthanum alloy, tungsten-oxidation cerium alloy or tungsten-oxidation
Thorium alloy, the molybdenum alloy powder can be molybdenum-oxidation lanthanum alloy, molybdenum-oxidation cerium alloy or molybdenum-oxidation thorium alloy.Tungsten alloy powder
It is commercial product with molybdenum alloy powder or proportioning is prepared using this field conventional method as requested, such as atomization or machinery
Mixing method.
In above-mentioned preparation method, the average particle size of raw material powder described in step 1 is 1.5 as a preferred implementation manner,
~10 μm (such as 2 μm, 3 μm, 5 μm, 7 μm, 9 μm, 9.5 μm).
In above-mentioned preparation method, break process described in step 1 is broken using air-flow as a preferred implementation manner,
Broken machine is crushed.Using air-flow breaking method, on the one hand energy continuous production, yield are high, at low cost, on the other hand can reduce original
Feed powder agglomeration improves green compact compactness.
In above-mentioned preparation method, broken as a preferred implementation manner, using the air-flow crusher in step 1
When broken, feed rate be 0.5~2.0kg/min (such as 0.6kg/min, 0.8kg/min, 1 kg/min, 1.2kg/min,
1.4kg/min, 1.6kg/min, 1.8kg/min, 1.9kg/min), stream pressure be 0.2~1.2MPa (such as 0.3MPa,
0.4MPa, 0.5MPa, 0.6MPa, 0.7MPa, 0.8MPa, 0.9MPa, 1MPa, 1.1MPa), grader rotating speed is 10~120Hz
(such as 15Hz, 20Hz, 30Hz, 40Hz, 50Hz, 60Hz, 70Hz, 80Hz, 90Hz, 105Hz, 115Hz), air source are air, nitrogen
At least one of gas, argon gas.
In above-mentioned preparation method, forming processes described in step 2 are using cold etc. quiet as a preferred implementation manner,
The technique of pressure carries out forming processes.
In above-mentioned preparation method, as a preferred implementation manner, the pressure of isostatic cool pressing described in step 2 be 120~
240MPa (such as 125MPa, 130MPa, 145MPa, 160MPa, 175MPa, 200MPa, 220MPa, 230MPa, 235MPa),
Dwell time be 15-25min (such as 16min, 17min, 19min, 21min, 23min, 24min), pressure release speed be 2~
8MPa/min (such as 2.5MPa/min, 3MPa/min, 4MPa/min, 5MPa/min, 6MPa/min, 7MPa/min,
7.5MPa/min)。
In above-mentioned preparation method, sintering processes described in step 3 are in non-oxide gas as a preferred implementation manner,
It is carried out under atmosphere or under vacuum；It is highly preferred that the nonoxidizing atmosphere is at least one of nitrogen atmosphere, nitrogen atmosphere and argon atmospher.
Further, sintering processes described in step 3 are when carrying out in a hydrogen atmosphere, and hydrogen flowing quantity is 10~20m3/ h (such as 11m3/
h、112m3/h、13m3/h、14m3/h、 15m3/h、16m3/h、17m3/h、18m3/h、19m3/h)。
In above-mentioned preparation method, sintering processes described in step 3 are to use intermediate frequency sense as a preferred implementation manner,
Heating furnace is answered to be sintered.
In above-mentioned preparation method, the sintering temperature of sintering processes described in step 3 is as a preferred implementation manner,
1700~2400 DEG C (such as 1720 DEG C, 1750 DEG C, 1800 DEG C, 1900 DEG C, 2000 DEG C, 2100 DEG C, 2200 DEG C, 2300 DEG C,
2350 DEG C), soaking time be 0.5~10h (such as 0.8h, 1.2h, 1.6h, 2.4h, 3h, 4h, 5h, 6h, 7h, 8h, 9h,
9.5h)。
High-compactness crucible can be prepared using the above method, such as：Relative density be 98% or more (95.2%,
95.5%, 95.8%, 96.5%, 97.5%, 98.2%, 98.5%), outer diameter be 135-150mm (such as 136mm, 137mm,
139mm, 142mm, 146mm, 148mm, 149mm), highly for 110-140mm (such as 112mm, 115mm, 118mm, 122mm,
126mm, 130mm, 134mm, 136mm, 138mm), wall thickness is 5-15mm (6mm, 8mm, 10mm, 12mm, 14mm).
The high-compactness crucible prepared using the above method, material use pure tungsten, pure molybdenum, tungsten alloy or molybdenum alloy；It is described
Tungsten alloy is preferably tungsten-oxidation lanthanum alloy, tungsten-oxidation cerium alloy or tungsten-oxidation thorium alloy, and the molybdenum alloy is preferably molybdenum-oxygen
Change lanthanum alloy, molybdenum-oxidation cerium alloy or molybdenum-oxidation thorium alloy.
Compared with prior art, the beneficial effects of the invention are as follows：
1) can be sintered out the refractory metals sintered articles such as the tungsten, molybdenum and its alloy of high-compactness, consistency 98% with
On.
2) without increasing excessive processing step, reduce cost to the greatest extent.
3) by changing the shape of isostatic tooling, special-shaped product of different shapes can be produced, traditional handicraft is compensated for
The single disadvantage of shape of product.
4) it is suitable for batch production.
Description of the drawings
Fig. 1 is the sectional structure and overlooking structure diagram that the embodiment of the present invention 1 requires obtained product, wherein (a) is
The sectional structure of product；(b) be product plan structure.
Fig. 2 is the sectional structure and overlooking structure diagram that the embodiment of the present invention 2 requires obtained product, wherein (a) is
The sectional structure of product；(b) be product plan structure.
Fig. 3 is the sectional structure and overlooking structure diagram that the embodiment of the present invention 3 requires obtained product, wherein (a) is
The sectional structure of product；(b) be product plan structure.
Fig. 4 is the metallographic structure photo of high-compactness pure tungsten crucible prepared by the embodiment of the present invention 1.
Fig. 5 is the metallographic structure photo of the pure molybdenum crucible of high-compactness prepared by the embodiment of the present invention 2.
Specific implementation mode
In order to make the content of the present invention more clearly understood, it below according to specific embodiments of the present invention and combines
Attached drawing, the present invention is described in further detail.
The various raw materials used in following embodiment are commercial product.
Embodiment 1
The present embodiment prepares the pure tungsten crucible that a kind of relative density is 98.5%, the appearance and size of tungsten crucible be Φ 138 ×
140, wall thickness 5mm, as shown in Figure 1, being as follows：
(1) tungsten powder (average particle size is 2.5 μm) is crushed, feed rate 1.0kg/min with air-flow crusher,
Stream pressure is 0.8MPa, and grader rotating speed is 60Hz, and the average particle size of tungsten powder is 2.3 μm after being crushed.
(2) broken tungsten powder is fitted into progress isostatic cool pressing processing in cold isostatic mould, to obtain material base；It is cold etc.
The pressure of static pressure is 240MPa, and dwell time 20min, pressure release speed is 4MPa/min.
(3) material base obtained in (2) is sintered with Medium Frequency Induction Heating Furnace；Sintering carries out under a hydrogen atmosphere, hydrogen flowing quantity
For 15m3/ hour, sintering temperature are 2300 DEG C, soaking time 4h, finally obtain high-compactness pure tungsten crucible.
The relative density for 10 high-compactness pure tungsten crucibles that the present embodiment method obtains is measured using hydrostatic weighing method,
Relative density is 98.5%, actual density 19.05g/cm3.Fig. 4 is high-compactness pure tungsten crucible manufactured in the present embodiment
Metallographic structure photo, as can be seen from the figure crystal grain is uniform, and crystal grain hole is less and smaller, has confirmed higher consistency.
Embodiment 2
The present embodiment prepares the pure molybdenum crucible that a kind of relative density is 99%, the appearance and size of molybdenum crucible be Φ 145 ×
110, wall thickness 10mm, as shown in Fig. 2, being as follows：
(1) it by molybdenum powder (average particle size is 3.5 μm), is crushed with air-flow crusher, feed rate 0.5kg/min,
Stream pressure is 1.2MPa, and grader rotating speed is 30Hz, and the average particle size of molybdenum powder is 3.3 μm after being crushed.
(2) broken molybdenum powder is fitted into progress isostatic cool pressing processing in cold isostatic mould, to obtain material base；It is cold etc.
The pressure of static pressure is 220MPa, and dwell time 20min, pressure release speed is 3.5MPa/min.
(3) material base obtained in (2) is sintered with Medium Frequency Induction Heating Furnace；Sintering carries out under a hydrogen atmosphere, hydrogen flowing quantity
For 12m3/ hour, sintering temperature are 2000 DEG C, soaking time 5h, finally obtain the pure molybdenum crucible of high-compactness.
The relative density for 10 pure molybdenum crucibles of high-compactness that the present embodiment method obtains is measured using hydrostatic weighing method,
Relative density is 99%.Fig. 5 is the metallographic structure photo of the pure molybdenum crucible of high-compactness manufactured in the present embodiment, can be with from figure
Find out that crystal grain is uniform, crystal grain hole is less and smaller, has confirmed higher consistency.
Embodiment 3
The present embodiment prepares a kind of tungsten-lanthana alloy crucible that relative density is 99%, and the appearance and size of crucible is Φ
145 × 110, wall thickness 15mm, as shown in figure 3, being as follows：
(1) by tungsten-lanthana powder, (average particle size is 2.3 μm, and the mass percent of lanthana is 1%, mixed using batch mixer
Close), it is crushed with air-flow crusher, feed rate 0.8kg/min, stream pressure 0.6MPa, grader rotating speed
For 20Hz, the average particle size of alloyed powder is 2.0 μm after being crushed.
(2) broken alloyed powder is fitted into progress isostatic cool pressing processing in cold isostatic mould, to obtain material base；It is cold
The pressure of isostatic pressed is 240MPa, and dwell time 20min, pressure release speed is 2MPa/min.
(3) material base obtained in (2) is sintered with Medium Frequency Induction Heating Furnace；Sintering carries out under a hydrogen atmosphere, hydrogen flowing quantity
For 15m3/ hour, sintering temperature are 2330 DEG C, soaking time 10h, finally obtain high-compactness tungsten-lanthana alloy crucible.
The phase for 10 high-compactness tungsten-lanthana alloy crucibles that the present embodiment method obtains is measured using hydrostatic weighing method
To density, relative density 99%.The metallographic structure figure of high-compactness tungsten-lanthana alloy crucible manufactured in the present embodiment is aobvious
Show that crystal grain is uniform, crystal grain hole is less and smaller, has confirmed higher consistency.
Embodiment 4
The present embodiment prepares a kind of molybdenum-lanthana alloy crucible that relative density is 98.5%, the appearance and size of molybdenum crucible
It is as follows for Φ 145 × 110, wall thickness 15mm：
(1) by molybdenum-lanthana powder, (average particle size is 3.3 μm, and the mass percent of lanthana is 1%, mixed using batch mixer
Close), it is crushed with air-flow crusher, feed rate 0.8kg/min, stream pressure 0.6MPa, grader rotating speed
For 20Hz, the average particle size of alloyed powder is 3.0 μm after being crushed.
(2) broken alloyed powder is fitted into progress isostatic cool pressing processing in cold isostatic mould, to obtain material base；It is cold
The pressure of isostatic pressed is 240MPa, and dwell time 20min, pressure release speed is 2MPa/min.
(3) material base obtained in (2) is sintered with Medium Frequency Induction Heating Furnace；Sintering carries out under a hydrogen atmosphere, hydrogen flowing quantity
For 15m3/ hour, sintering temperature are 2330 DEG C, soaking time 10h, finally obtain high-compactness molybdenum-lanthana alloy crucible.
The 10 high-compactness molybdenum-lanthana alloy crucibles obtained using the present embodiment method are measured using hydrostatic weighing method
Relative density, relative density 98.5%.The metallographic group of high-compactness tungsten-lanthana alloy crucible manufactured in the present embodiment
It knits figure and shows that crystal grain is uniform, crystal grain hole is less and smaller, has confirmed higher consistency.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (6)
1. the preparation method of a kind of high-compactness pure tungsten, pure molybdenum and its alloy material, which is characterized in that include the following steps：
Raw material powder is carried out break process by step 1, obtains broken powder, and the raw material powder is pure tungsten powder, pure molybdenum powder, tungsten
The average particle size of alloyed powder or molybdenum alloy powder, the raw material powder is 2.3~3.5 μm, and the break process is broken using air-flow
Machine is crushed, and when carrying out broken using the air-flow crusher, feed rate is 0.5~1.0kg/min, and stream pressure is
0.6~1.2MPa, classification unit frequency are 20~60Hz, and air source is at least one of air, nitrogen, argon gas；
The broken powder that step 1 obtains is carried out forming processes, obtains material base, the forming processes are by step 2
Forming processes are carried out using the technique of isostatic cool pressing, the pressure of the isostatic cool pressing is 220~240MPa, dwell time 19-
21min, pressure release speed are 2~4MPa/min；
The material base that step 2 obtains is sintered by step 3, obtains the high-compactness pure tungsten, pure molybdenum and its conjunction
The sintering temperature of golden material, the sintering processes is 2000~2350 DEG C, and soaking time is 4~9.5h, and the high-compactness is pure
The consistency of tungsten, pure molybdenum and its alloy material is 98.5% or more.
2. preparation method according to claim 1, which is characterized in that the tungsten alloy powder is tungsten-oxidation lanthanum alloy, tungsten-oxygen
It is molybdenum-oxidation lanthanum alloy, molybdenum-oxidation cerium alloy or molybdenum-thorium oxide to change cerium alloy or tungsten-oxidation thorium alloy, the molybdenum alloy powder
Alloy.
3. preparation method according to claim 1, which is characterized in that sintering processes described in step 3 are in nonoxidizing atmosphere
It is carried out under lower or vacuum.
4. preparation method according to claim 3, which is characterized in that the nonoxidizing atmosphere is nitrogen atmosphere, nitrogen atmosphere and argon
At least one of atmosphere.
5. preparation method according to claim 4, which is characterized in that sintering processes described in step 3 in a hydrogen atmosphere into
When row, hydrogen flowing quantity is 10~20m3/h。
6. preparation method according to claim 1, which is characterized in that the sintering processes be using Medium Frequency Induction Heating Furnace into
Row sintering.
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| CN106513684B (en) * | 2016-11-10 | 2019-04-05 | 洛阳科威钨钼有限公司 | A kind of production method of tungsten-molybdenum alloy rotary target material |
| CN107190195A (en) * | 2017-05-04 | 2017-09-22 | 鹤山市沃得钨钼实业有限公司 | A kind of W-REO alloys crucible and its manufacture method |
| AT15903U1 (en) * | 2017-09-29 | 2018-08-15 | Plansee Se | Molybdenum sintered part |
| CN107931358B (en) * | 2017-12-21 | 2019-06-25 | 金堆城钼业光明（山东）股份有限公司 | A kind of preparation method of molybdenum tungsten lanthanum alloy silk |
| CN108465817B (en) * | 2018-03-15 | 2020-05-12 | 北京矿冶科技集团有限公司 | Preparation method of high-density pure tungsten product with uniform structure |
| CN108772558A (en) * | 2018-06-15 | 2018-11-09 | 赣州有色冶金研究所 | A kind of compound tungsten crucible of multielement rare earth and its preparation method and application |
| CN109894472B (en) * | 2019-03-14 | 2021-01-01 | 安泰天龙钨钼科技有限公司 | Rolling method of molybdenum plate for spinning molybdenum crucible with large length-diameter ratio |
| CN113492211B (en) * | 2020-04-08 | 2023-11-14 | 安泰科技股份有限公司 | Preparation method of high-uniformity granularity-controllable metal powder |
| CN112176236A (en) * | 2020-10-19 | 2021-01-05 | 北京工业大学 | La2O3W-Mo-doped alloy material and preparation method thereof |
| CN112792308B (en) * | 2020-12-25 | 2022-07-26 | 有研工程技术研究院有限公司 | Roller for continuous induction type rapid quenching furnace and manufacturing method thereof |
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| CN1739894A (en) * | 2005-09-15 | 2006-03-01 | 自贡硬质合金有限责任公司 | Airflow crushing stepped tungsten carbide powder producing process |
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