CN110358509A - A method of improving ODS-W composite material heating conduction - Google Patents
A method of improving ODS-W composite material heating conduction Download PDFInfo
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- CN110358509A CN110358509A CN201910776161.2A CN201910776161A CN110358509A CN 110358509 A CN110358509 A CN 110358509A CN 201910776161 A CN201910776161 A CN 201910776161A CN 110358509 A CN110358509 A CN 110358509A
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Abstract
The invention discloses a kind of methods for improving ODS-W composite material heating conduction, are realized by way of adding surfactant triethanolamine.Compared with conventional wet chemical method, the present invention prepares W-Y in wet chemistry method2O3It joined surfactant triethanolamine in composite precursor powder process, not only reduce influence of the impurity element to experimental result, improve postorder and be sintered to obtain W-Y2O3The consistency of composite material, and Y2O3Be not distributed only over crystal boundary, in tungsten basal body there is also.Therefore the W-Y of addition triethanolamine preparation2O3The thermal diffusion coefficient of composite material improves 15-17%, and thermal conductivity improves 26-28%.
Description
Technical field
The present invention relates to a kind of preparation method of tungsten-based composite material, specifically a kind of raising ODS-W composite material
The method of heating conduction.
Background technique
In fusion stack operation, the radiation of a large amount of thermic load and high energy particle is born towards plasma material, is led
It causes material surface to produce serious damage, such as melts, crackle etc. reduces material property, and its use is greatly shortened
Service life, therefore the heating conduction towards plasma tungsten material is required very high.
Tungsten has many advantages, such as low-expansion coefficient, high heat conductance, high temperature creep-resisting, it is considered to be it is most promising towards it is equal from
Daughter material.But the brittleness problems of tungsten are also very important.By a series of research, find to add rare earth into tungsten basal body
Oxide such as Y2O3, can get the second phase enhancing tungsten material (ODS-W).When preparing ODS-W composite material, with wet chemistry method generation
For traditional mechanical alloying method not only it is possible to prevente effectively from the introducing of impurity, can also make grain size distribution uniform.But
It is larger that this method will lead to crystallite dimension.The thermal conductivity of material is reduced in addition, adding second in tungsten basal body and meeting.Therefore,
The present invention prepares W-Y in conventional wet chemical method2O3On the basis of composite precursor powder, it is added to surfactant triethanolamine,
On the one hand, W-Y is significantly reduced2O3Composite material crystallite dimension improves its consistency；On the other hand, Y2O3Not there is only
It in crystal boundary, and is distributed in inside tungsten basal body, and then improves W-Y2O3The heating conduction of composite material.
Summary of the invention
The present invention is intended to provide a kind of method for improving ODS-W composite material heating conduction.With preparation W-Y2O3Compound precursor
The conventional wet chemical method of body powder is compared, and surfactant triethanolamine is added in the present invention, significantly reduces W-Y2O3Composite material
Crystallite dimension, improve its consistency, and make Y2O3It is more uniform to be dispersed in tungsten basal body, to improve W-Y2O3It is compound
The heating conduction of material.
The method that the present invention improves ODS-W composite material heating conduction, is by adding in the preparation process of wet chemistry method
The mode of surfactant triethanolamine is added to realize.
Further, the addition quality of the surfactant is the 6-8% of ammonium metatungstate quality.
The method that the present invention improves ODS-W composite material heating conduction, includes the following steps:
Step 1: the preparation of presoma
By surfactant triethanolamine ((HOCH2CH2)3N, Aladdin, analyze it is pure), six nitric hydrate yttrium (Y
(NO3)3·6H2O, Aladdin, purity >=99.5%) and ammonium metatungstate (AMT, Aladdin, purity >=99.95%) respectively it is molten
Solution in deionized water, is poured into ammonium metatungstate solution after then mixing triethanolamine solution and six nitric hydrate yttrium solution,
Mixed solution is obtained after mixing evenly；By precipitating reagent oxalic acid (C2H2O4·2H2O is analyzed pure) it is added in mixed solution, it is put into oil
It is heated to 115-135 DEG C in bath and is stirred continuously until solution evaporating completely, obtains W-Y2O3Presoma；
In step 1, triethanolamine, six nitric hydrate yttriums, oxalic acid additive amount be respectively the 6-8% of ammonium metatungstate quality,
1.6%, 38.8%.
Step 2: reduction
By gained W-Y2O3Presoma grinding is placed in tube furnace, is restored in a hydrogen atmosphere.In reduction process, first
In 555-655 DEG C heat preservation 50-70 minutes, then in 745-845 DEG C heat preservation 115-135 minutes, obtain W-Y2O3Composite powder.
Step 3: the preparation of block
The W-Y that step 2 is obtained2O3Composite powder is fitted into the graphite jig that diameter is 20mm, then graphite jig is put into
In discharge plasma sintering furnace, come into full contact with pressure head with mold；Sintering furnace chamber is vacuumized when sintering procedure does not start, when
Furnace chamber pressure is less than 10Pa, and sintering procedure starting keeps the temperature 5-7 minutes when being warming up to 790-840 DEG C first, then raises temperature to
1620-1670 DEG C heat preservation 30-60 seconds.In sintering process, heating rate is 100 DEG C/min, and sintering procedure terminates rear mold with furnace
It is cooled to room temperature to get W-Y is arrived2O3Composite material, consistency 97-99%.
In sintering process, the pressure that 790-840 DEG C of front mold is born is no more than 15MPa, and pressure is no more than later
51MPa。
The beneficial effects of the present invention are embodied in:
Compared with conventional wet chemical method, the present invention prepares W-Y in wet chemistry method2O3It is added in composite precursor powder process
Surfactant triethanolamine, not only reduces influence of the impurity element to experimental result, improves postorder and be sintered to obtain W-
Y2O3The consistency of composite material, and Y2O3Be not distributed only over crystal boundary, in tungsten basal body there is also.Therefore addition triethanolamine
The W-Y of preparation2O3The thermal diffusion coefficient of composite material improves 15-17%, and thermal conductivity improves 26-28%.
Detailed description of the invention
Fig. 1 is W-Y2O3The FE-SEM of composite material.As can be seen from the figure composite material crystallite dimension is 1-2 μm；Y2O3
It is distributed in crystal boundary, and crystallite dimension about 100nm.
Fig. 2 is W-Y2O3The TEM (a-b) and High-Resolution Map (c) of composite material.It can be seen that Y2O3In the presence of in tungsten basal body,
Crystallite dimension about 20nm.
Fig. 3 (a) and (b) are W-Y respectively2O3Composite material thermal diffusion coefficient and thermal conductivity and temperature relation figure.With conventional wet
Chemical method is compared, the W-Y of addition triethanolamine preparation2O3The thermal diffusion coefficient of composite material improves 17%, and thermal conductivity improves
28%.
Specific embodiment
Embodiment 1:
The method that ODS-W composite material heating conduction is improved in the present embodiment, includes the following steps:
Step 1: the preparation of presoma
By surfactant triethanolamine ((HOCH2CH2)3N, Aladdin, analyze it is pure), six nitric hydrate yttrium (Y
(NO3)3·6H2O, Aladdin, purity >=99.5%) and ammonium metatungstate (AMT, Aladdin, purity >=99.95%) respectively it is molten
Solution obtains a certain amount of solution in deionized water, pours into inclined tungsten after then mixing the solution of triethanolamine and six nitric hydrate yttriums
In acid ammonium solution, it is uniformly mixing to obtain mixed solution；By precipitating reagent oxalic acid (C2H2O4·2H2O is analyzed pure) mixed solution is added
In, it is put into oil bath pan and is heated to 115 DEG C and is stirred continuously until solution evaporating completely, obtains W-Y2O3Presoma.
Step 2: reduction
By gained W-Y2O3Presoma grinding is placed in tube furnace, is restored in a hydrogen atmosphere.In reduction process, 555 DEG C
Heat preservation 70 minutes, 745 DEG C keep the temperature 115 minutes, obtain W-Y2O3Composite granule.
The additive amount of triethanolamine, six nitric hydrate yttriums and oxalic acid is respectively the 6%, 1.6% of ammonium metatungstate quality,
38.8%.
Step 3: the preparation of block
By the W-Y after reduction2O3Composite powder is fitted into the graphite jig that diameter is 20mm, then graphite jig is put into
In electric plasma agglomeration furnace, come into full contact with pressure head with mold.Sintering furnace chamber is vacuumized when sintering procedure does not start, works as furnace
Cavity pressure is less than 10Pa, sintering procedure starting.5 minutes are kept the temperature when mold temperature rises to 790 DEG C, is warming up to 1620 DEG C of heat preservations 30
Second.In sintering process, heating rate is 100 DEG C/min, and sintering procedure terminates rear mold and cools to room temperature with the furnace to get W- is arrived
Y2O3Composite material, consistency 97%, thermal diffusion coefficient improve 15%, and thermal conductivity improves 26%.
In sintering process, the pressure that 790 DEG C of front mold is born is no more than 15MPa, and pressure is no more than 51MPa later.
Embodiment 2:
The method that ODS-W composite material heating conduction is improved in the present embodiment, includes the following steps:
Step 1: the preparation of presoma
By surfactant triethanolamine ((HOCH2CH2)3N, Aladdin, analyze it is pure), six nitric hydrate yttrium (Y
(NO3)3·6H2O, Aladdin, purity >=99.5%) and ammonium metatungstate (AMT, Aladdin, purity >=99.95%) respectively it is molten
Solution obtains a certain amount of solution in deionized water, pours into inclined tungsten after then mixing the solution of triethanolamine and six nitric hydrate yttriums
In acid ammonium solution, it is uniformly mixing to obtain mixed solution；By precipitating reagent oxalic acid (C2H2O4·2H2O is analyzed pure) mixed solution is added
In, it is put into oil bath pan and is heated to 125 DEG C and is stirred continuously until solution evaporating completely, obtains W-Y2O3Presoma.
Step 2: reduction
By gained W-Y2O3Presoma grinding is placed in tube furnace, is restored in a hydrogen atmosphere.In reduction process, 605 DEG C
Heat preservation 60 minutes, 795 DEG C keep the temperature 125 minutes, obtain W-Y2O3Composite granule.
The additive amount of triethanolamine, six nitric hydrate yttriums and oxalic acid is respectively the 7%, 1.6% of ammonium metatungstate quality,
38.8%.
Step 3: the preparation of block
By the W-Y after reduction2O3Composite powder is fitted into the graphite jig that diameter is 20mm, then graphite jig is put into
In electric plasma agglomeration furnace, come into full contact with pressure head with mold.Sintering furnace chamber is vacuumized when sintering procedure does not start, works as furnace
Cavity pressure is less than 10Pa, sintering procedure starting.6 minutes are kept the temperature when mold temperature rises to 820 DEG C, is warming up to 1640 DEG C of heat preservations 45
Second.In sintering process, heating rate is 100 DEG C/min, and sintering procedure terminates rear mold and cools to room temperature with the furnace to get W- is arrived
Y2O3Composite material, consistency 98%, thermal diffusion coefficient improve 16%, and thermal conductivity improves 27%.
In sintering process, the pressure that 820 DEG C of front mold is born is no more than 15MPa, and pressure is no more than 51MPa later.
Embodiment 3:
The method that ODS-W composite material heating conduction is improved in the present embodiment, includes the following steps:
Step 1: the preparation of presoma
By surfactant triethanolamine ((HOCH2CH2)3N, Aladdin, analyze it is pure), six nitric hydrate yttrium (Y
(NO3)3·6H2O, Aladdin, purity >=99.5%) and ammonium metatungstate (AMT, Aladdin, purity >=99.95%) respectively it is molten
Solution obtains a certain amount of solution in deionized water, pours into inclined tungsten after then mixing the solution of triethanolamine and six nitric hydrate yttriums
In acid ammonium solution, it is uniformly mixing to obtain mixed solution；By precipitating reagent oxalic acid (C2H2O4·2H2O is analyzed pure) mixed solution is added
In, it is put into oil bath pan and is heated to 135 DEG C and is stirred continuously until solution evaporating completely, obtains W-Y2O3Presoma.
Step 2: reduction
By gained W-Y2O3Presoma grinding is placed in tube furnace, is restored in a hydrogen atmosphere.In reduction process, 655 DEG C
Heat preservation 50 minutes, 845 DEG C keep the temperature 135 minutes, obtain W-Y2O3Composite granule.
The additive amount of triethanolamine, six nitric hydrate yttriums and oxalic acid is respectively the 8%, 1.6% of ammonium metatungstate quality,
38.8%.
Step 3: the preparation of block
By the W-Y after reduction2O3Composite powder is fitted into the graphite jig that diameter is 20mm, then graphite jig is put into
In electric plasma agglomeration furnace, come into full contact with pressure head with mold.Sintering furnace chamber is vacuumized when sintering procedure does not start, works as furnace
Cavity pressure is less than 10Pa, sintering procedure starting.7 minutes are kept the temperature when mold temperature rises to 840 DEG C, is warming up to 1670 DEG C of heat preservations 60
Second.In sintering process, heating rate is 100 DEG C/min, and sintering procedure terminates rear mold and cools to room temperature with the furnace to get W- is arrived
Y2O3Composite material, consistency 99%, thermal diffusion coefficient improve 17%, and thermal conductivity improves 28%.
In sintering process, the pressure that 840 DEG C of front mold is born is no more than 15MPa, and pressure is no more than 51MPa later.
Claims (7)
1. a kind of method for improving ODS-W composite material heating conduction, it is characterised in that:
It is the addition surfactant triethanolamine in wet chemistry method preparation process.
2. according to the method described in claim 1, it is characterized by:
The addition quality of the surfactant is the 6-8% of ammonium metatungstate quality.
3. method according to claim 1 or 2, it is characterised in that include the following steps:
Step 1: the preparation of presoma
Surfactant triethanolamine, six nitric hydrate yttriums and ammonium metatungstate are dissolved in deionized water respectively, then by three
It is poured into ammonium metatungstate solution after ethanolamine solutions and the mixing of six nitric hydrate yttrium solution, obtains mixed solution after mixing evenly；
Precipitating reagent oxalic acid is added in mixed solution, be heated to 115-135 DEG C and is stirred continuously until solution evaporating completely, obtains W-
Y2O3Presoma；
Step 2: reduction
By gained W-Y2O3Presoma grinding is placed in tube furnace, is restored in a hydrogen atmosphere, and W-Y is obtained2O3Composite powder；
Step 3: the preparation of block
The W-Y that step 2 is obtained2O3Composite powder is fitted into the graphite jig that diameter is 20mm, then graphite jig is put into electric discharge
In plasma agglomeration furnace, come into full contact with pressure head with mold；Sintering furnace chamber is vacuumized when sintering procedure does not start, works as furnace chamber
Pressure is less than 10Pa, and sintering procedure starting keeps the temperature 5-7 minutes when being warming up to 790-840 DEG C first, then raises temperature to 1620-
1670 DEG C heat preservation 30-60 seconds.
4. according to the method described in claim 3, it is characterized by:
In step 1, triethanolamine, six nitric hydrate yttriums, oxalic acid additive amount be respectively the 6-8% of ammonium metatungstate quality,
1.6%, 38.8%.
5. according to the method described in claim 3, it is characterized by:
In step 2, it is described reduction be first in 555-655 DEG C heat preservation 50-70 minutes, then in 745-845 DEG C of heat preservation 115-135
Minute, obtain W-Y2O3Composite powder.
6. according to the method described in claim 3, it is characterized by:
In step 3 sintering process, heating rate be 100 DEG C/min, sintering procedure terminate rear mold cool to the furnace room temperature to get
To W-Y2O3Composite material, consistency 97-99%.
7. according to the method described in claim 3, it is characterized by:
In step 3 sintering process, the pressure for being warming up to 790-840 DEG C of front mold receiving is no more than 15MPa, and subsequent pressure does not surpass
Cross 51MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112030026A (en) * | 2020-08-31 | 2020-12-04 | 合肥工业大学 | Preparation method of high-hardness and high-density composite rare earth oxide doped tungsten-based composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112030026A (en) * | 2020-08-31 | 2020-12-04 | 合肥工业大学 | Preparation method of high-hardness and high-density composite rare earth oxide doped tungsten-based composite material |
| CN112030026B (en) * | 2020-08-31 | 2021-10-15 | 合肥工业大学 | Preparation method of high-hardness and high-density composite rare earth oxide doped tungsten-based composite material |
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Application publication date: 20191022 |