CN107716917A - A kind of method that gas carburization method reaction in-situ prepares W/WC composite powders - Google Patents
A kind of method that gas carburization method reaction in-situ prepares W/WC composite powders Download PDFInfo
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- CN107716917A CN107716917A CN201710853077.7A CN201710853077A CN107716917A CN 107716917 A CN107716917 A CN 107716917A CN 201710853077 A CN201710853077 A CN 201710853077A CN 107716917 A CN107716917 A CN 107716917A
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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
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Abstract
The invention discloses a kind of method that gas carburization method reaction in-situ prepares W/WC composite powders, is specially：Tungsten powder and phenolic resin are weighed, and is laid in respectively in Noah's ark；Noah's ark is placed in atmosphere furnace, under Ar atmosphere protections, heating, heating, insulation, room temperature is cooled to, that is, obtains W/WC composite powders.Using W/WC composite powders made from the inventive method, on the one hand Dispersed precipitate can improve the high-temperature behavior of tungsten-bast alloy in the WC nano particles of W particle surfaces, on the other hand play pinning effect to alloy strength.Therefore, W/WC composite powders prepare tungsten-bast alloy as starting powder, can improve the high-temperature behavior of alloy, while avoid the problem of easily reuniting when directly adding WC nano particles.
Description
Technical field
The invention belongs to composite powder preparing technical field, and in particular to a kind of gas carburization method reaction in-situ prepares W/WC
The method of composite powder.
Background technology
Tungsten-bast alloy is widely used in height and pressed off because it has the performances such as tungsten high-melting-point, high rigidity, low thermal coefficient of expansion
Close 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 has well 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 strengthens phase as one kind, suitable when its mechanical property in high temperature is with room temperature, thus introduces ceramic particle and increase
It is mutually the optimal selection for improving tungsten-bast alloy high-temperature behavior by force.In order to be uniformly distributed, with matrix there is good interface to be combined
Ceramic particle enhancing tungsten-bast alloy, need to also be improved from source powder.As a kind of ceramic phase, it not only has WC at room temperature
There is higher hardness, and it is suitable when hardness is with room temperature at high temperature, it can add as one kind of hard material and high temperature material
Add agent.Existing researcher 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 as the refinement of WC particle, its performance are more excellent.But WC is sent out as a kind of additional particle unavoidably in preparation process
Raw agglomeration, the performance for influenceing tungsten-bast alloy play.It is then desired to propose significantly more efficient incorporation way, ensureing WC points
Cloth uniformity and with tungsten good combination performance on the premise of, improve the elevated temperature strength of tungsten-bast alloy.The present invention uses gas carburization
Method reacts generation WC ceramic phases in tungsten powder situ, prepares W/WC composite powders, to prepare the excellent tungsten base of high-temperature behavior
Alloy provides a kind of new composite powder.
The content of the invention
It is an object of the invention to provide a kind of method that gas carburization method reaction in-situ prepares W/WC composite powders, to prepare
The excellent tungsten-bast alloy of high-temperature behavior provides a kind of new composite powder.
The technical solution adopted in the present invention is that a kind of gas carburization method reaction in-situ prepares the side of W/WC composite powders
Method, specifically implement according to following steps：
Step 1, tungsten powder and phenolic resin are weighed, and is laid in respectively in Noah's ark；
Step 2, tungsten powder will be covered with and phenolic resin Noah's ark is placed in atmosphere furnace, under Ar atmosphere protections, heat up, heat,
Insulation, is cooled to room temperature, that is, obtains W/WC composite powders.
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 both sides of Noah's ark respectively in step 1.
Noah's ark is provided with two in step 1, and 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 with 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.
Heating rate is 10~20 DEG C/min in step 2, and heating-up temperature is 800~1000 DEG C, soaking time is 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 powders
Method, it is first according to certain mass ratio and weighs tungsten powder and phenolic resin, then by the Noah's ark equipped with tungsten powder and phenolic resin in gas
Gas carburization is carried out in atmosphere stove, produces W/WC composite powders.Obtained W/WC composite powders, Dispersed precipitate is in W particle surfaces
On the one hand WC nano particles can improve the high-temperature behavior of tungsten-bast alloy, on the other hand play pinning effect to alloy strength.Cause
This, W/WC composite powders prepare tungsten-bast alloy as starting powder, can improve the high-temperature behavior of alloy, while avoid directly
The problem of easily reuniting when adding WC nano particles.
Brief description of the drawings
Fig. 1 is each raw material placement schematic diagram in the present invention；
Fig. 2 is the SEM figures for the W/WC composite powders that the gas carburization method reaction in-situ of the embodiment of the present invention 3 is prepared.
In figure, 1. left boats, 2. right boats, Noah's ark on 3., 4. tungsten powders, 5. phenolic resin.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The method that a kind of gas carburization method reaction in-situ of the present invention prepares W/WC composite powders, it is specifically real according to following steps
Apply：
Step 1, according to mass ratio 1:0.5~2 weighs tungsten powder and phenolic resin, prepares three Noah's arks, two of which 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
The right side of left boat 1 is laid in, 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
Phenolic resin in two Noah's arks of side, upper Noah's ark covering or so；
Step 2, the Noah's ark equipped with powder step 1 set is placed in the centre position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is 0.5~1.5L/min Ar atmosphere protections, with 10~20 DEG C/min's
Programming rate is heated to 800~1000 DEG C, the furnace cooling after target temperature is incubated 30~120min, until furnace body temperature drops
After room temperature, protective gas is closed, that is, obtains W/WC composite powders.
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 substantial amounts of carbon containing gas in atmosphere furnace in addition
Body, if carbon amounts deficiency will be unable to obtain WC, or it can only obtain brittle W2C, if carbon amounts is superfluous, the carbon source remained in powder
Also the use of its later stage can be influenceed.
The placement order of powder and the modes of emplacement of Noah's ark are to ensure carbonaceous gas caused by phenolic resin thermal decomposition
Along the gas channel flowing that three Noah's arks are formed carbon can be made more to be deposited on the table of tungsten powder as far as possible at high temperature
Face.
In addition the present invention is carbonized by the pyrolysis carbonaceous gas of argon gas stream phenolic resin with tungsten powder, compared to
Solid-state carbon source, it is more easy to react with W, generates WC ceramic phases at low temperature, reduce reaction temperature, and improve preparation process can
Control property；By the regulation and control of thermodynamic condition, size and quantity to the WC particle of generation carry out controllable preparation.
The method that a kind of gas carburization method reaction in-situ of the present invention prepares W/WC composite powders, is first according to certain quality
Than weighing tungsten powder and phenolic resin, then require to carry out the Noah's ark equipped with tungsten powder and phenolic resin in atmosphere furnace according to assembling
Gas carburization, produce W/WC composite powders.In obtained W/WC composite powders, Dispersed precipitate is in the WC nanometers of W particle surfaces
Grain, on the one hand can improve the high-temperature behavior of tungsten-bast alloy, on the other hand play pinning effect to alloy strength.Therefore, W/WC
Composite powder prepares tungsten-bast alloy as starting powder, can improve the high-temperature behavior of alloy, while avoids directly addition WC
The problem of easily reuniting during nano particle.
Embodiment 1
Step 1, according to mass ratio 2:1 weighs tungsten powder and phenolic resin, prepares three Noah's arks, two of which Noah's ark is adjacent to be put
Put, 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 centre position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is 0.5L/min Ar atmosphere protections, with 20 DEG C/min programming rate
800 DEG C are heated to, the furnace cooling after target temperature is incubated 30min, after furnace body temperature is reduced to room temperature, closes protection gas
Body, that is, obtain W/WC composite powders.
Embodiment 2
Step 1, according to mass ratio 1:1 weighs tungsten powder and phenolic resin, prepares three Noah's arks, two of which Noah's ark is adjacent to be put
Put, 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 centre position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is 1.5L/min Ar atmosphere protections, with 15 DEG C/min programming rate
900 DEG C are heated to, the furnace cooling after target temperature is incubated 75min, after furnace body temperature is reduced to room temperature, closes protection gas
Body, that is, obtain W/WC composite powders.
Embodiment 3
Step 1, according to mass ratio 3:2 weigh tungsten powder and phenolic resin, prepare three Noah's arks, two of which Noah's ark is adjacent to be put
Put, 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 centre position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is 1.0L/min Ar atmosphere protections, with 10 DEG C/min programming rate
1000 DEG C are heated to, the furnace cooling after target temperature is incubated 120min, after furnace body temperature is reduced to room temperature, closes protection
Gas, that is, obtain W/WC composite powders.
Embodiment 4
Step 1, according to mass ratio 2:3 weigh tungsten powder and phenolic resin, prepare three Noah's arks, two of which Noah's ark is adjacent to be put
Put, 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 centre position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is 1.3L/min Ar atmosphere protections, with 13 DEG C/min programming rate
850 DEG C are heated to, the furnace cooling after target temperature is incubated 100min, after furnace body temperature is reduced to room temperature, closes protection
Gas, that is, obtain W/WC composite powders.
Embodiment 5
Step 1, according to mass ratio 1:2 weigh tungsten powder and phenolic resin, prepare three Noah's arks, two of which Noah's ark is adjacent to be put
Put, 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 centre position of atmosphere furnace calandria, air-flow from
Right boat side enters atmosphere furnace, in the case where gas flow is 0.8L/min Ar atmosphere protections, with 18 DEG C/min programming rate
950 DEG C are heated to, the furnace cooling after target temperature is incubated 50min, after furnace body temperature is reduced to room temperature, closes protection gas
Body, that is, obtain W/WC composite powders.
Accompanying drawing 2 is the SEM figures for the W/WC composite powders that the embodiment of the present invention 3 is prepared.It can see by accompanying drawing 2, in W
Particle surface growth in situ goes out the WC nano particles of Dispersed precipitate, and the distribution of particle is more uniform, passes through concrete technology scheme
Regulation and control, the size and quantity of particle can be controlled.Its one side can improve the high-temperature behavior of tungsten-bast alloy, 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 (8)
1. a kind of method that gas carburization method reaction in-situ prepares W/WC composite powders, it is characterised in that specifically according to following step
It is rapid to implement：
Step 1, tungsten powder and phenolic resin are weighed, and is laid in respectively in Noah's ark；
Step 2, tungsten powder will be covered with and phenolic resin Noah's ark is placed in atmosphere furnace, under Ar atmosphere protections, heating, heating, insulation,
Room temperature is cooled to, that is, obtains W/WC composite powders.
2. the method that a kind of gas carburization method reaction in-situ according to claim 1 prepares W/WC composite powders, its feature
It is, the mass ratio of tungsten powder and phenolic resin described in the step 1 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 powders, its feature
It is, tungsten powder and phenolic resin are located at the both sides of Noah's ark respectively in the step 1.
4. the method that a kind of gas carburization method reaction in-situ according to claim 1 prepares W/WC composite powders, its feature
It is, Noah's ark is provided with two in the step 1, and 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.
5. the method that a kind of gas carburization method reaction in-situ according to claim 4 prepares W/WC composite powders, its feature
It is, Noah's ark is additionally provided with the step 1, and upper Noah's ark is located above the Noah's ark of left and right, in upper Noah's ark covering left and right Noah's ark
Phenolic resin.
6. the method that a kind of gas carburization method reaction in-situ according to claim 1 prepares W/WC composite powders, its feature
It is, Ar gas throughput is 0.5~1.5L/min in the step 2.
7. the method that a kind of gas carburization method reaction in-situ according to claim 1 prepares W/WC composite powders, its feature
It is, heating rate is 10~20 DEG C/min in the step 2, and heating-up temperature is 800~1000 DEG C, soaking time is 30~
120min。
8. a kind of gas carburization method reaction in-situ according to claim any one of 1-7 prepares the side of W/WC composite powders
Method, it is characterised 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 |
| WO2006129965A1 (en) * | 2005-05-30 | 2006-12-07 | Dynamaterials Co., Inc | 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 |
| CN105478753A (en) * | 2015-12-15 | 2016-04-13 | 北京矿冶研究总院 | Tungsten carbide and tungsten composite powder and preparation method thereof |
| CN105618788A (en) * | 2016-03-04 | 2016-06-01 | 西安理工大学 | Method for preparing WC/W composite powder through in-situ reaction |
| CN107116227A (en) * | 2017-04-25 | 2017-09-01 | 北京工业大学 | A kind of preparation method of ultrafine WC Ni composite powders |
-
2017
- 2017-09-20 CN CN201710853077.7A patent/CN107716917B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61141662A (en) * | 1984-12-12 | 1986-06-28 | 三井化学株式会社 | Composition for manufacturing ceramic |
| WO2006129965A1 (en) * | 2005-05-30 | 2006-12-07 | Dynamaterials Co., Inc | 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 |
| CN105478753A (en) * | 2015-12-15 | 2016-04-13 | 北京矿冶研究总院 | Tungsten carbide and tungsten composite powder and preparation method thereof |
| CN105618788A (en) * | 2016-03-04 | 2016-06-01 | 西安理工大学 | Method for preparing WC/W composite powder through in-situ reaction |
| CN107116227A (en) * | 2017-04-25 | 2017-09-01 | 北京工业大学 | A kind of preparation method of ultrafine WC Ni composite powders |
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