CN106544538B - The control method of powder oxygen content in a kind of Investigation for Super-fine Cermets preparation process - Google Patents
The control method of powder oxygen content in a kind of Investigation for Super-fine Cermets preparation process Download PDFInfo
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- CN106544538B CN106544538B CN201611204575.0A CN201611204575A CN106544538B CN 106544538 B CN106544538 B CN 106544538B CN 201611204575 A CN201611204575 A CN 201611204575A CN 106544538 B CN106544538 B CN 106544538B
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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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- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/04—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbonitrides
-
- 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
Raw material components are made into mixed powder, raw material components include 40 ~ 61% Ti by the control method of powder oxygen content according to respective weight percent in a kind of Investigation for Super-fine Cermets preparation process（C,N）Powder, 22 ~ 32% Ni powder, 12 ~ 20% Mo powder and 5 ~ 8% WC powder；Then wet grinding media is added, carries out ball milling 36 ~ 50 hours, powder mixes forming agent compression moulding again by dry after ball milling, and the addition of forming agent is the 1 ~ 5% of the mixed powder weight, is finally sintered and Investigation for Super-fine Cermets finished product is made, it is characterised in that：Before ball milling or in mechanical milling process, it is additionally added the benzotriazole and 2 of compounding, 2' di-2-ethylhexylphosphine oxides (4 methyl, 6 tert-butyl phenol), the benzotriazole of compounding and 2, the addition of 2' di-2-ethylhexylphosphine oxides (4 methyl, 6 tert-butyl phenol) are the 0.1 ~ 2% of mixed powder weight.Technical solution of the present invention can effectively control superfine powder oxygen content in 0.5 ~ 0.7Wt%, avoid occurring lacking carbon phase in alloy, the performance of Investigation for Super-fine Cermets obtained significantly improves.
Description
Technical field
The present invention relates to powder in the manufacturing of Investigation for Super-fine Cermets more particularly to a kind of Investigation for Super-fine Cermets preparation process
Expect the control method of oxygen content.
Background technology
Cermet usually has the characteristics that elevated temperature strength is high, density is small, easy processing, corrosion-resistant, thermal conductivity is good, therefore often
Structural member, engine piston, chemical machinery part etc. for manufacturing aircraft and guided missile.In addition cermet not only has higher
Hardness, wearability, red hardness, but also have excellent chemical stability, it is also very low with intermetallic friction coefficient.Such as use
Cutter is prepared, compared with common hard alloy, it has apparent advantage in the following aspects：It allows for higher
Cutting speed and the larger depth of cut, work piece have preferable surface property, the wear-resisting property higher of cutter.Manufacture ultra-fine gold
Belong to the granularity very little of ultra-fine raw material used by ceramics, the wherein grain size of ultrafine ceramic powder is 0.1 ~ 0.2 μm, ultra-fine bonding gold
The grain size for belonging to powder is 0.4 ~ 1.0 μm.In processing these powder process, through 24 ~ 72 hours Intensive ball mills, in powder there is
The activity of prodigious surface energy and distortion of lattice energy, powder is stronger, it is easy to which oxygen uptake aoxidizes, in the inevitable quilt of particle surface
Oxidation forms metal oxide film.If oxidation is serious, the not exclusively remaining TiO phases of η phases and deoxidation are will appear in tissue,
These brittlement phases are the fracture origins in tissue.Moreover, because deoxidation is not thorough, the wetability of Binder Phase and hard phase is poor, brilliant
Grain is coarse, these can all be such that the bending strength of material reduces, by the performance of severe exacerbation Investigation for Super-fine Cermets.Therefore, surpass
The unstable of fine powder material oxygen content brings very big difficulty to production high quality Investigation for Super-fine Cermets.
Invention content
The control of powder oxygen content during being prepared the object of the present invention is to provide a kind of superfine Ti (C, N) based ceramic metal
Method, it is intended to effectively solve superfine powder and cause superfine powder oxygen content super because oxygen uptake aoxidizes in cermet production process
The problem of marking, cermet quality fluctuation, performance caused to decline.
In order to achieve the above objectives, the control of powder oxygen content in a kind of Investigation for Super-fine Cermets preparation process that the present invention uses
The technical solution of method is：Each raw material component is made into mixed powder, the raw material components packet according to respective weight percent
Include 40 ~ 61% titanium carbonitride powder, 22 ~ 32% Ni powder, 12 ~ 20% Mo powder and 5 ~ 8% WC powder；Then wet-milling is added to be situated between
Matter, carries out ball milling 36 ~ 50 hours, and powder mixes forming agent compression moulding again by drying after ball milling, and the addition of forming agent is
The 1 ~ 5% of the mixed powder weight is finally sintered and Investigation for Super-fine Cermets finished product is made；Before ball milling or in mechanical milling process, also
The benzotriazole and 2 of compounding, 2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert-butylphenols), parallel three nitrogen of benzene of the compounding are added
Azoles and 2, the addition of 2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert-butylphenols) are the 0.1 ~ 2% of mixed powder weight, the benzene
The weight ratio of parallel triazole and 2,2' methylene bis-(4- methyl-6-tert-butylphenols) is 3 ~ 7:7~3.
Related content in above-mentioned technical proposal is explained as follows：
1, in said program, before ball milling or in mechanical milling process, the benzotriazole of compounding can be both directly added into
It, can also be in advance by the benzotriazole of compounding and 2,2'- methylenes with 2,2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert-butylphenols)
Base pair-(4- methyl-6-tert-butylphenols) dissolves in the organic solvents such as acetone, hexane, is then then added to ball milling system,
Organic solvent is acetone, hexane, any one or arbitrary two kinds of mixture in alcohol or three kinds of mixture.
2, in said program, preferable scheme is that the wet grinding media is any one in industrial alcohol, acetone, hexane
Kind or arbitrary two kinds of mixture or three kinds of mixture.
3, in said program, preferable scheme be forming agent used be PEG, paraffin, in buna any one or
Arbitrary two kinds of mixture or three kinds of mixture.
4, in said program, preferable scheme is the Ti（C,N）The particle size size of powder is the thin grade of sub-micro 0.5 ~ 0.8
μm or 0.2 μm of 0.2~0.5 μm of ultra-fine grade or nanoscale ＜；The granularity of the Ni powder is 0.8~1.5 μm, the Mo powder
Granularity be 0.5~0.8 μm；The granularity of the WC powder is 0.2~0.8 μm.
5, in said program, dry temperature is 80 ~ 120 DEG C after ball milling；Sintering is 1300 ~ 1400 in low-pressure sintering furnace
50 ~ 80min is sintered at DEG C.
The present invention design principle be：In order to reduce the oxygen content in Investigation for Super-fine Cermets powder product, the present invention is existing
Some improvement have been carried out on the basis of some Investigation for Super-fine Cermets technologies of preparing.In general, superfine Ti（C,N）Powder, Ni powder, Mo
These superfines such as powder, WC powder are different for the adsorption effect of different organic matters, must to obtain good adsorption effect
Palpus selects the adsorption activity position to mixed powder, and targetedly organic matter, present invention spy have found benzene of the mixed powder for compounding
The adsorption effect of parallel triazole and 2,2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert-butylphenols) both organic matters is fine, especially
It is the benzotriazole and 2,2' methylene bis-(4- methyl-6-tert-butylphenols) that compounding is added in ball milling process.It is added
Later, benzotriazole and 2,2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert-butylphenols) azoles are adsorbed on superfine powder surface not
On the one hand same active sites change the state of charge and interfacial property on superfine powder surface, ultra-fine grain surface energy state are made to become
In stabilization, slow down oxidation rate；On the other hand the organic molecule adsorbed forms layer protecting film, obstruction and oxygen on powder surface
Change the transfer for reacting related charge or substance, is also obviously reduced the oxidation rate of powder.It is adsorbed on superfines surface
Organic protective film, other than playing the role of preventing Powder Oxidation in mechanical milling process, in the storage stage of powder（It is unstamped
Before forming）It can continue to play a role, to delay powder to aoxidize.Comparative test result shows benzene a pair of horses going side by side three that compounding is not added
The oxygen content of the mixed powder of nitrogen azoles and 2,2' methylene bis-(4- methyl-6-tert-butylphenols) is 1.0~1.2%（Weight hundred
Divide ratio）, and the benzotriazole and 2 of compounding is added, 2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert-butylphenols) mixed powder
Oxygen content is reduced to 0.5~0.7%（Weight percent）.
The substantive distinguishing features outstanding and significant progress of technical solution of the present invention are mainly reflected in：
（1）Before ball milling or in mechanical milling process, the benzotriazole and 2 of compounding, 2'- methylenes are added into mixed powder
Base pair-(4- methyl-6-tert-butylphenols), can effectively control the oxygen content of superfine powder, to more accurately control superfine metal
The carbon content of ceramics avoids occurring lacking carbon phase, the quality of stable alloy, the usability of obtained Investigation for Super-fine Cermets in alloy
It can significantly improve；
（2）The program is easy to operate, easy implementation, is suitable for the various precision instruments such as accurate lathe tool and the milling cutter of metal cutting
Processing and manufacturing, have a wide range of application, economic benefit is very notable.
Specific implementation mode
Below and embodiment the invention will be further described：
Embodiment one：The control method of powder oxygen content in a kind of Investigation for Super-fine Cermets preparation process
Raw material components are made into mixed powder according to respective weight percent, the raw material components include 54% granularity
For 0.2 μm of Ti（C,N）Powder, 25% granularity be 0.8 μm Ni powder, 15% granularity be 0.5 μm Mo powder and 6% granularity
For 0.5 μm of WC powder；The mixed powder being made into is put into ball grinder, and the weight ratio of alloying pellet and mixed powder is 5:1, per public
The alcohol of 350ml is added in jin mixed powder, then the benzotriazole and 2,2'- that compounding is added by the 1.5% of mixed powder weight
Di-2-ethylhexylphosphine oxide-(4- methyl-6-tert-butylphenols), the benzotriazole and 2,2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert butyl
Phenol) weight ratio be 6:4, ball milling 48 hours, the powder after ball milling is dry at a temperature of 100 DEG C, and PEG is mixed again after dry
As forming agent compression moulding, the addition of forming agent is the 2.5% of mixed powder weight, in low-pressure sintering furnace at 1330 DEG C
It is sintered 60min, obtains finished product.
Comparative example：
In addition to being added without benzotriazole and 2, except 2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert-butylphenols), other
Part is identical with embodiment one, and finished product is to compare.
After testing, embodiment one and the comparative example gained respective performance indicator of Investigation for Super-fine Cermets are as shown in table 1.
Table 1
Data listed by table 1 can be seen that using after technical solution of the present invention, and oxygen content significantly reduces, porosity
Also it decreases, alloy bending strength significantly improves.
Embodiment 2：The control method of powder oxygen content in a kind of Investigation for Super-fine Cermets preparation process
Raw material components are made into mixed powder according to respective weight percent, the raw material components include 60% granularity
For 0.5 μm of Ti（C,N）Powder, 22% granularity be 1.0 μm Ni powder, 12% granularity be 0.8 μm Mo powder and 6% granularity
For 0.8 μm of WC powder；The mixed powder being made into is put into ball grinder, and the weight ratio of alloying pellet and mixed powder is 5:1, per public
The hexane of the acetone and 150ml of 200ml is added in jin mixed powder, then benzene a pair of horses going side by side that compounding is added by the 1.5% of mixed powder weight
Triazole and 2,2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert-butylphenols), the benzotriazole and 2,2'- di-2-ethylhexylphosphine oxides-(4-
Methyl-6-tert-butylphenol) weight ratio be 3:7, ball milling 48 hours, the powder after ball milling is dry at a temperature of 100 DEG C, does
The mixture of PEG, paraffin, buna three are mixed after dry again as forming agent compression moulding, the addition of forming agent is mixed
The 3.5% of powder weight is closed, 60min is sintered at 1330 DEG C in low-pressure sintering furnace, obtains finished product.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (4)
1. the control method of powder oxygen content in a kind of Investigation for Super-fine Cermets preparation process, by raw material components according to respective weight
Percentage is made into mixed powder, and the raw material components include 40 ~ 61% Ti（C,N）Powder, 22 ~ 32% Ni powder, 12 ~ 20% Mo
Powder and 5 ~ 8% WC powder；Then wet grinding media is added, carries out ball milling 36 ~ 50 hours, powder mixes again by drying after ball milling
Forming agent compression moulding, the addition of forming agent are the 1 ~ 5% of the mixed powder weight, are finally sintered and superfine metal pottery is made
Porcelain finished product, forming agent used is PEG, paraffin, any one or arbitrary two kinds of mixture in buna or three kinds
Mixture, it is characterised in that：Before ball milling or in mechanical milling process, it is additionally added the benzotriazole and 2 of compounding, 2'- methylene
Double-(4- methyl-6-tert-butylphenols), the benzotriazole of the compounding and 2,2'- di-2-ethylhexylphosphine oxides-(4- methyl-6-tert butyl
Phenol) addition be mixed powder weight 0.1 ~ 2%, the benzotriazole and 2,2'- di-2-ethylhexylphosphine oxides-(4- methyl -6-
Tert-butyl phenol) weight ratio be 3 ~ 7:7~3.
2. the control method of powder oxygen content, feature exist in Investigation for Super-fine Cermets preparation process according to claim 1
In：The benzotriazole and 2,2' methylene bis-(4- methyl-6-tert-butylphenols) of the compounding are first molten in organic solvent
Solution, organic solvent are acetone, hexane, any one or arbitrary two kinds of mixture in alcohol or three kinds of mixture, then
It is then added in the mixed powder by ball milling.
3. the control method of powder oxygen content, feature exist in Investigation for Super-fine Cermets preparation process according to claim 1
In：The wet grinding media be industrial alcohol, acetone, any one or arbitrary two kinds of mixture in hexane or three kinds it is mixed
Close object.
4. the control method of powder oxygen content, feature exist in Investigation for Super-fine Cermets preparation process according to claim 1
In：The Ti（C,N）The particle size size of powder is 0.2~0.5 μm of 0.5 ~ 0.8 μm of the thin grade of sub-micro or ultra-fine grade or nanoscale
0.2 μm of ＜；The granularity of the Ni powder is 0.8~1.5 μm, and the granularity of the Mo powder is 0.5~0.8 μm；The WC powder
Granularity is 0.2~0.8 μm.
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