CN107716917B - A kind of method that gas carburization method reaction in-situ prepares W/WC composite powder - Google Patents
A kind of method that gas carburization method reaction in-situ prepares W/WC composite powder Download PDFInfo
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- CN107716917B CN107716917B CN201710853077.7A CN201710853077A CN107716917B CN 107716917 B CN107716917 B CN 107716917B CN 201710853077 A CN201710853077 A CN 201710853077A CN 107716917 B CN107716917 B CN 107716917B
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- noah
- ark
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- powder
- phenolic resin
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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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
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
Abstract
The invention discloses a kind of method that gas carburization method reaction in-situ prepares W/WC composite powder, specifically: tungsten powder and phenolic resin are weighed, and is laid in Noah's ark respectively；Noah's ark is placed in atmosphere furnace, under Ar atmosphere protection, heating, heating, heat preservation are cooled to room temperature to get W/WC composite powder is arrived.Using W/WC composite powder made from the method for the present invention, on the one hand the high-temperature behavior of tungsten-bast alloy can be improved in the WC nano particle of W particle surface for Dispersed precipitate, on the other hand play pinning effect to alloy strength.Therefore, W/WC composite powder prepares tungsten-bast alloy as starting powder, and the high-temperature behavior of alloy can be improved, while avoiding the problem of easily reuniting when directly adding WC nano particle.
Description
Technical field
The invention belongs to composite powder preparation technical fields, and in particular to a kind of gas carburization method reaction in-situ preparation W/WC
The method of composite powder.
Background technique
Tungsten-bast alloy is widely used in height and presses off because it is with performances such as tungsten high-melting-point, high rigidity, low thermal expansion coefficients
It closes with high temperature resistant components such as electrical contact, the larynx lining of various guided missiles, jet vane, nose cones, it is therefore desirable to which it is with good high temperatures
Energy.But any metal can all soften at high temperature, 17% when compression strength is only room temperature at 900 DEG C such as tungsten-copper alloy is left
It is right.Ceramic particle is suitable when mechanical property at high temperature is with room temperature as a kind of reinforced phase, thus introduces ceramic particle and increase
It is mutually the optimal selection for improving tungsten-bast alloy high-temperature behavior by force.In conjunction with there is good interface in order to be uniformly distributed, with matrix
Ceramic particle enhance tungsten-bast alloy, need to also be improved from source powder.WC not only has at room temperature as a kind of ceramic phase
There is higher hardness, and when hardness is with room temperature at high temperature is suitable, the one kind that can be used as hard material and high temperature material adds
Add agent.Existing research person is introduced directly into WC as a kind of additional particle in tungsten-bast alloy, has certain journey to the performance of alloy
The improvement of degree, and with the refinement of WC particle, performance is more excellent.But WC is inevitably sent out in preparation process as a kind of additional particle
Raw agglomeration, the performance for influencing tungsten-bast alloy play.It is then desired to propose significantly more efficient incorporation way, guaranteeing WC points
Cloth uniformity and with tungsten good combination performance under the premise of, improve the elevated temperature strength of tungsten-bast alloy.The present invention uses gas carburization
Method reaction in-situ in tungsten powder generates WC ceramic phase, prepares W/WC composite powder, for the excellent tungsten base of preparation high-temperature behavior
Alloy provides a kind of new composite powder.
Summary of the invention
The object of the present invention is to provide a kind of methods that gas carburization method reaction in-situ prepares W/WC composite powder, for preparation
The excellent tungsten-bast alloy of high-temperature behavior provides a kind of new composite powder.
The technical scheme adopted by the invention is that a kind of gas carburization method reaction in-situ prepares the side of W/WC composite powder
Method is specifically implemented according to the following steps:
Step 1, tungsten powder and phenolic resin are weighed, and is laid in Noah's ark respectively；
Step 2, tungsten powder will be covered with and phenolic resin Noah's ark is placed in atmosphere furnace, under Ar atmosphere protection, heat up, heat,
Heat preservation is cooled to room temperature to get W/WC composite powder is arrived.
Feature of the present invention also resides in,
The mass ratio of tungsten powder described in step 1 and phenolic resin is 1:0.5~2.
Tungsten powder and phenolic resin are located at the two sides of Noah's ark in step 1.
In step 1 there are two Noah's ark settings, tungsten powder is located on the left of the boat of left, and phenolic resin is divided into two parts, a part
On the right side of the boat of left, another part is located on the left of the boat of right.
Noah's ark is additionally provided in step 1, upper Noah's ark is located above the Noah's ark of left and right, the phenol in upper Noah's ark covering left and right Noah's ark
Urea formaldehyde.
Ar gas throughput is 0.5~1.5L/min in step 2.
In step 2 heating rate be 10~20 DEG C/min, heating temperature be 800~1000 DEG C, soaking time be 30~
120min。
Ar gas air-flow is passed through from the Noah's ark side for placing phenolic resin in step 2.
The invention has the advantages that a kind of gas carburization method reaction in-situ of the present invention prepares the side of W/WC composite powder
Method weighs tungsten powder and phenolic resin first, in accordance with certain mass ratio, then by the Noah's ark equipped with tungsten powder and phenolic resin in gas
Gas carburization is carried out in atmosphere furnace to get W/WC composite powder.W/WC composite powder obtained, Dispersed precipitate is in W particle surface
On the one hand the high-temperature behavior of tungsten-bast alloy can be improved in WC nano particle, on the other hand play pinning effect to alloy strength.Cause
This, W/WC composite powder prepares tungsten-bast alloy as starting powder, the high-temperature behavior of alloy can be improved, while avoiding directly
The problem of easily reuniting when adding WC nano particle.
Detailed description of the invention
Fig. 1 is each raw material placement schematic diagram in the present invention；
Fig. 2 is the SEM figure for the W/WC composite powder that 3 gas carburization method reaction in-situ of the embodiment of the present invention is prepared.
In figure, 1. left boats, 2. right boats, Noah's ark on 3., 4. tungsten powders, 5. phenolic resin.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of method that gas carburization method reaction in-situ prepares W/WC composite powder of the present invention, it is specifically real according to the following steps
It applies:
Step 1, tungsten powder and phenolic resin are weighed according to mass ratio 1:0.5~2, prepares three Noah's arks, two of them Noah's ark
It is placed adjacent, as shown in Figure 1, tungsten powder 4 to be laid in the left side of left boat 1, phenolic resin 5 is divided into two parts, a part
It is laid in the right side of left boat 1, another part is laid in the left side of right boat 2, and then upper Noah's ark 3 is placed on two Noah's arks
Side, upper Noah's ark cover the phenolic resin in two Noah's arks of left and right；
Step 2, the Noah's ark equipped with powder step 1 set is placed in the middle position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is the Ar atmosphere protection of 0.5~1.5L/min, with 10~20 DEG C/min's
Heating rate is heated to 800~1000 DEG C, the furnace cooling after target temperature keeps the temperature 30~120min, until furnace body temperature drops
After room temperature, protective gas is closed to get W/WC composite powder is arrived.
The mass ratio of tungsten powder and phenolic resin directly determines the carry out degree of carburizing reagent in the present invention, because used in experiment
The Residual carbon of phenolic resin is about 50%, and the process air-flow of gas carburization can also take away a large amount of carbon containing gas in atmosphere furnace in addition
Body if carbon amounts deficiency will be unable to obtain WC, or can only obtain brittle W2C, if carbon amounts is superfluous, remaining carbon source in powder
Also it will affect the use of its later period.
The placement order of powder and the modes of emplacement of Noah's ark are the carbonaceous gas in order to guarantee phenolic resin thermal decomposition generation
Carbon can be made more to be deposited on the table of tungsten powder at high temperature as far as possible along the airflow channel flowing that three Noah's arks are formed
Face.
Furthermore the present invention makes the pyrolysis carbonaceous gas of phenolic resin be carbonized with tungsten powder by argon gas stream, compared to
Solid-state carbon source is easier to react with W, generates WC ceramic phase at low temperature, reduces reaction temperature, and improve preparation process can
Control property；By the regulation of thermodynamic condition, size and quantity to the WC particle of generation carry out controllable preparation.
A kind of method that gas carburization method reaction in-situ prepares W/WC composite powder of the present invention, first, in accordance with certain quality
Than weighing tungsten powder and phenolic resin, then the Noah's ark equipped with tungsten powder and phenolic resin is carried out in atmosphere furnace according to group reload request
Gas carburization is to get W/WC composite powder.In W/WC composite powder obtained, Dispersed precipitate is in the WC nanometer of W particle surface
Grain, on the one hand can be improved the high-temperature behavior of tungsten-bast alloy, on the other hand plays pinning effect to alloy strength.Therefore, W/WC
Composite powder prepares tungsten-bast alloy as starting powder, and the high-temperature behavior of alloy can be improved, while avoiding directly addition WC
The problem of easily reuniting when nano particle.
Embodiment 1
Step 1, tungsten powder and phenolic resin are weighed according to mass ratio 2:1, prepares three Noah's arks, two of them Noah's ark is adjacent to be put
It sets, as shown in Figure 1, tungsten powder 4 to be laid in the left side of left boat 1, phenolic resin 5 is divided into two parts, a part is laid in
The right side of left boat 1, another part are laid in the left side of right boat 2, then upper Noah's ark 3 are placed in above two Noah's arks, top
Phenolic resin in two Noah's arks of boat covering left and right；
Step 2, the Noah's ark equipped with powder step 1 set is placed in the middle position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is the Ar atmosphere protection of 0.5L/min, with the heating rate of 20 DEG C/min
800 DEG C are heated to, the furnace cooling after target temperature keeps the temperature 30min closes protection gas after furnace body temperature is reduced to room temperature
Body to get arrive W/WC composite powder.
Embodiment 2
Step 1, tungsten powder and phenolic resin are weighed according to mass ratio 1:1, prepares three Noah's arks, two of them Noah's ark is adjacent to be put
It sets, as shown in Figure 1, tungsten powder 4 to be laid in the left side of left boat 1, phenolic resin 5 is divided into two parts, a part is laid in
The right side of left boat 1, another part are laid in the left side of right boat 2, then upper Noah's ark 3 are placed in above two Noah's arks, top
Phenolic resin in two Noah's arks of boat covering left and right；
Step 2, the Noah's ark equipped with powder step 1 set is placed in the middle position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is the Ar atmosphere protection of 1.5L/min, with the heating rate of 15 DEG C/min
900 DEG C are heated to, the furnace cooling after target temperature keeps the temperature 75min closes protection gas after furnace body temperature is reduced to room temperature
Body to get arrive W/WC composite powder.
Embodiment 3
Step 1, tungsten powder and phenolic resin are weighed according to mass ratio 3:2, prepares three Noah's arks, two of them Noah's ark is adjacent to be put
It sets, as shown in Figure 1, tungsten powder 4 to be laid in the left side of left boat 1, phenolic resin 5 is divided into two parts, a part is laid in
The right side of left boat 1, another part are laid in the left side of right boat 2, then upper Noah's ark 3 are placed in above two Noah's arks, top
Phenolic resin in two Noah's arks of boat covering left and right；
Step 2, the Noah's ark equipped with powder step 1 set is placed in the middle position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is the Ar atmosphere protection of 1.0L/min, with the heating rate of 10 DEG C/min
1000 DEG C are heated to, furnace cooling closes protection after furnace body temperature is reduced to room temperature after target temperature keeps the temperature 120min
Gas to get arrive W/WC composite powder.
Embodiment 4
Step 1, tungsten powder and phenolic resin are weighed according to mass ratio 2:3, prepares three Noah's arks, two of them Noah's ark is adjacent to be put
It sets, as shown in Figure 1, tungsten powder 4 to be laid in the left side of left boat 1, phenolic resin 5 is divided into two parts, a part is laid in
The right side of left boat 1, another part are laid in the left side of right boat 2, then upper Noah's ark 3 are placed in above two Noah's arks, top
Phenolic resin in two Noah's arks of boat covering left and right；
Step 2, the Noah's ark equipped with powder step 1 set is placed in the middle position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is the Ar atmosphere protection of 1.3L/min, with the heating rate of 13 DEG C/min
850 DEG C are heated to, furnace cooling closes protection after furnace body temperature is reduced to room temperature after target temperature keeps the temperature 100min
Gas to get arrive W/WC composite powder.
Embodiment 5
Step 1, tungsten powder and phenolic resin are weighed according to mass ratio 1:2, prepares three Noah's arks, two of them Noah's ark is adjacent to be put
It sets, as shown in Figure 1, tungsten powder 4 to be laid in the left side of left boat 1, phenolic resin 5 is divided into two parts, a part is laid in
The right side of left boat 1, another part are laid in the left side of right boat 2, then upper Noah's ark 3 are placed in above two Noah's arks, top
Phenolic resin in two Noah's arks of boat covering left and right；
Step 2, the Noah's ark equipped with powder step 1 set is placed in the middle position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is the Ar atmosphere protection of 0.8L/min, with the heating rate of 18 DEG C/min
950 DEG C are heated to, the furnace cooling after target temperature keeps the temperature 50min closes protection gas after furnace body temperature is reduced to room temperature
Body to get arrive W/WC composite powder.
Attached drawing 2 is the SEM figure for the W/WC composite powder that the embodiment of the present invention 3 is prepared.It can see by attached drawing 2, in W
Particle surface growth in situ goes out the WC nano particle of Dispersed precipitate, and the distribution of particle is more uniform, passes through concrete technology scheme
Regulation, can size to particle and quantity control.The high-temperature behavior of tungsten-bast alloy can be improved in its one side, another
Aspect plays pinning effect to alloy strength.Therefore, tungsten-bast alloy is prepared as starting powder, the high temperatures of alloy can be improved
Energy.
Claims (5)
1. a kind of method that gas carburization method reaction in-situ prepares W/WC composite powder, which is characterized in that specifically according to following step
It is rapid to implement:
Step 1, tungsten powder and phenolic resin are weighed, there are two Noah's ark settings, and tungsten powder is located on the left of the boat of left, and phenolic resin is divided into
Two parts, a part are located on the right side of the boat of left, and another part is located on the left of the boat of right, and tungsten powder and phenolic resin are laid in respectively
In Noah's ark；It is additionally provided with Noah's ark simultaneously, upper Noah's ark is located above the Noah's ark of left and right, the phenolic aldehyde tree in upper Noah's ark covering left and right Noah's ark
Rouge；
Step 2, tungsten powder will be covered with and phenolic resin Noah's ark is placed in atmosphere furnace, under Ar atmosphere protection, heating, heating, heat preservation,
It is cooled to room temperature to get W/WC composite powder is arrived.
2. the method that a kind of gas carburization method reaction in-situ according to claim 1 prepares W/WC composite powder, feature
It is, the mass ratio of tungsten powder described in the step 1 and phenolic resin is 1:0.5~2.
3. the method that a kind of gas carburization method reaction in-situ according to claim 1 prepares W/WC composite powder, feature
It is, Ar gas throughput is 0.5~1.5L/min in the step 2.
4. the method that a kind of gas carburization method reaction in-situ according to claim 1 prepares W/WC composite powder, feature
Be, in the step 2 heating rate be 10~20 DEG C/min, heating temperature be 800~1000 DEG C, soaking time be 30~
120min。
5. the side that a kind of gas carburization method reaction in-situ according to claim 1-4 prepares W/WC composite powder
Method, which is characterized in that Ar gas air-flow is passed through from the Noah's ark side for placing phenolic resin in the step 2.
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| JPS61141662A (en) * | 1984-12-12 | 1986-06-28 | 三井化学株式会社 | Composition for manufacturing ceramic |
| KR100721780B1 (en) * | 2005-05-30 | 2007-05-25 | 주식회사 다이너머트리얼스 | Method for manufacturing high strength ultra-fine/nano-structured Al/AlN or Al alloy/AlN composite materials |
| CN100999018A (en) * | 2007-01-11 | 2007-07-18 | 上海交通大学 | Aluminium-in situ titanium boride composite powder |
| CN103302301A (en) * | 2012-03-12 | 2013-09-18 | 吴伟 | Novel method for preparing C/Ag composite nanomaterial with controllable Ag coating layer thickness |
| CN105478753B (en) * | 2015-12-15 | 2018-02-06 | 北京矿冶研究总院 | Tungsten carbide and tungsten composite powder and preparation method thereof |
| CN105618788B (en) * | 2016-03-04 | 2018-02-16 | 西安理工大学 | A kind of method that reaction in-situ prepares WC/W composite powders |
| CN107116227B (en) * | 2017-04-25 | 2018-11-30 | 北京工业大学 | A kind of preparation method of ultrafine WC-Ni composite powder |
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