CN115283670A - Ti (C, N) -Mo-Fe composite powder and preparation method and application thereof - Google Patents
Ti (C, N) -Mo-Fe composite powder and preparation method and application thereof Download PDFInfo
- Publication number
- CN115283670A CN115283670A CN202210951119.1A CN202210951119A CN115283670A CN 115283670 A CN115283670 A CN 115283670A CN 202210951119 A CN202210951119 A CN 202210951119A CN 115283670 A CN115283670 A CN 115283670A
- Authority
- CN
- China
- Prior art keywords
- composite powder
- solution
- powder
- cermet
- core
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- B22F1/18—Non-metallic particles coated with metal
-
- 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
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
Abstract
The present invention provides a Ti (C, N) -Mo-Fe composite powder comprising: a core comprising Ti (C, N); a shell covering the core; the shell is selected from Mo and/or Fe. The invention provides iron-based cermet powder with good performance, which takes Ti (C, N) as a hard phase and Fe and Mo composite powder as a binder phase, and also provides a preparation method of the Ti (C, N) -Mo-Fe composite powder with simple process, simple equipment and low cost, and application of the Ti (C, N) -Mo-Fe composite powder in preparation of cermet. The Ti (C, N) -Mo-Fe composite powder provided by the invention has good dispersibility and excellent sintering performance, can effectively improve the non-uniformity of the distribution of hard phase and binder phase in the metal ceramic, and can obviously improve the performance of the metal ceramic.
Description
Technical Field
The invention belongs to the technical field of metal ceramics, and particularly relates to Ti (C, N) -Mo-Fe composite powder as well as a preparation method and application thereof.
Background
Ti (C, N) -based cermets, which are composite materials consisting of Ti (C, N) solid solution as a hard phase and Co or Ni as a binder phase, have been successfully applied to high-performance wear-resistant parts and semi-finishing or finishing tools due to their high hardness, thermal stability, thermal conductivity, excellent creep resistance and wear resistance, and are one of the best alternatives to WC-based cemented carbides, however, the binder metals Co and Ni are rare metals, are expensive in the market, and are relatively unstable in price. It is therefore of great interest to find a satisfactory substitute binder phase to replace them completely or partially, thereby reducing the future dependence on these strategic materials.
Disclosure of Invention
In view of this, an object of the embodiments of the present invention is to provide a Ti (C, N) -Mo-Fe composite powder, and a preparation method and an application thereof.
The present invention provides a Ti (C, N) -Mo-Fe composite powder comprising:
a core comprising Ti (C, N);
a shell covering the core; the shell is selected from Mo and/or Fe.
Preferably, the mass content of the outer shell in the Ti (C, N) -Mo-Fe composite powder is 3-40%;
the mass content of Mo in the shell in the Ti (C, N) -Mo-Fe composite powder is 2-20%.
Preferably, the Ti (C, N) is Ti (C) X ,N 1-X ) X is 0 to 1;
the average particle diameter of Ti (C, N) is preferably 0.1 to 5.0. Mu.m.
The invention provides a preparation method of Ti (C, N) -Mo-Fe composite powder, which comprises the following steps:
carrying out first mixing on Ti (C, N) powder, a dispersing agent and an ammonium molybdate solution to obtain a suspension;
and carrying out second mixing on the suspension, the alkaline solution and the iron salt solution, drying, calcining and reducing the obtained mixture to obtain the Ti (C, N) -Mo-Fe composite powder.
Preferably, the ferric salt solution is selected from a ferrous salt solution and/or a ferric salt solution; the iron salt is selected from at least one of sulfate, chloride, nitrate and oxalate;
the alkaline solution is selected from ammonia solution and/or sodium hydroxide solution.
Preferably, the dispersant is selected from one or more of organic amine, organic amine salt, surfactant and titanate coupling agent;
the dosage of the dispersant is 0.2 to 8 percent of the mass of the ammonium molybdate solution.
Preferably, the calcining temperature is 500-800 ℃; the calcination time is preferably 1 to 4 hours.
Preferably, the reduction is carried out in the presence of a reducing agent; the reducing agent is selected from H 2 Ammonia and/or CO; the reduction temperature is 700-1000 ℃; the reduction time is 60-120 min.
The invention provides a metal ceramic which is prepared from the raw materials of the Ti (C, N) -Mo-Fe composite powder in the technical scheme.
Preferably, the microstructure of the cermet has a coreless/ring structure or a weak core/ring structure.
Because Fe belongs to the same group with Co and Ni in the periodic table of elements and is considered as an ideal substitute binder, fe can be strengthened by heat treatment, and the Fe is low in price and rich in resources. Despite extensive research on iron binder-containing cermets, difficulties were found in preparing Ti (C, N) -Fe cermets, such as difficulty in achieving uniform Fe dispersion and poor wettability between Fe and Ti (C, N), and thus, ti (C, N) -based cermets containing an Fe binder phase have not been industrially produced.
The physical mixing method of ball milling is generally adopted in the production process of the metal ceramic to prepare the mixture, but the metal phase and the ceramic phase are difficult to be uniformly mixed, so that the microstructure is not uniform. The invention adopts the coated composite powder to improve the uniformity of the alloy microstructure, and the coated composite powder is prepared in the solution, so that the molecular level mixing can be realized, the diffusion in the solid phase sintering process can be easier, and the core/ring structure of the metal ceramic can be further regulated and controlled.
The invention provides iron-based cermet powder with good performance, which takes Ti (C, N) as a hard phase, takes Fe and Mo composite powder as a bonding phase, takes Ti (C, N) powder as an inner core, and is coated with a shell consisting of metal powder outside the inner core, wherein the metal powder is powder consisting of Mo and Fe. Meanwhile, the invention also provides a preparation method of the Ti (C, N) -Mo-Fe composite powder, which has the advantages of simple process, simple equipment and low cost, and application of the Ti (C, N) -Mo-Fe composite powder in preparation of metal ceramics. The Ti (C, N) -Mo-Fe composite powder provided by the invention has good dispersibility and excellent sintering performance, can effectively improve the nonuniformity of hard phase and bonding phase distribution in the metal ceramic, and can obviously improve the performance of the metal ceramic.
Drawings
FIG. 1 is an SEM photograph of a virgin Ti (C, N) powder in example 1 of the present invention;
FIG. 2 is an SEM photograph of a Ti (C, N) -Mo-Fe composite powder prepared in example 1 of the present invention;
FIG. 3 is a surface EDS diagram of a Ti (C, N) -Mo-Fe composite powder prepared in example 1 of the present invention;
FIG. 4 is an SEM photograph of a cermet prepared from a Ti (C, N) -Mo-Fe composite powder according to example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The present invention provides a Ti (C, N) -Mo-Fe composite powder comprising:
a core comprising Ti (C, N);
a shell covering the core; the shell is selected from Mo and/or Fe.
In the present invention, the Ti (C, N) may be represented as Ti (C) X ,N 1-X ) X is between 0 and 1Any value of (1), including 0 and 1, refers to TiC X And/or TiN 1-X 。
In the present invention, the Ti (C, N) is preferably Ti (C, N) powder; the average particle diameter of the Ti (C, N) powder is preferably 0.1 to 5.0. Mu.m, more preferably 0.5 to 4 μm, more preferably 1 to 3 μm, and most preferably 2 μm.
In the present invention, the Mo is preferably Mo powder; the Fe is preferably Fe powder.
In the invention, the Ti (C, N) -Mo-Fe composite powder takes Ti (C, N) powder as an inner core, the outer core is coated with an outer shell consisting of metal powder, and the metal powder is powder consisting of Mo and Fe.
In the present invention, the mass content of the outer shell in the Ti (C, N) -Mo-Fe composite powder is preferably 3 to 40%, more preferably 10 to 30%, more preferably 15 to 25%, most preferably 20%; the content of Mo in the Ti (C, N) -Mo-Fe composite powder in the outer shell is preferably 2 to 20% by mass, more preferably 5 to 15% by mass, more preferably 8 to 12% by mass, and most preferably 10% by mass.
In the invention, the mass fraction of metal Mo and Fe in the Ti (C, N) -Mo-Fe composite powder is 3-40%; the mass fraction of the metal Mo in the composite powder is 2-20%.
The invention provides a preparation method of Ti (C, N) -Mo-Fe composite powder, which comprises the following steps:
carrying out first mixing on Ti (C, N) powder, a dispersing agent and an ammonium molybdate solution to obtain a suspension;
and secondly, mixing the suspension, the alkaline solution and the ferric salt solution, drying, calcining and reducing the obtained mixture to obtain the Ti (C, N) -Mo-Fe composite powder.
In the present invention, the Ti (C, N) powder is the same as the Ti (C, N) powder described in the above technical solution, and is not described herein again.
In the invention, the dispersant is preferably selected from one or more of organic amine, organic amine salt, surfactant and titanate coupling agent; the surfactant is preferably polyethylene glycol.
In the present invention, the ammonium molybdate may be ammonium molybdate solid or ammonium molybdate solution.
In the present invention, the Ti (C, N) powder is preferably added in an amount of 5 to 200g, more preferably 10 to 150g, more preferably 50 to 100g, and most preferably 60 to 80g per liter of the ammonium molybdate solution.
In the present invention, the dispersant is preferably used in an amount of 0.2 to 8%, more preferably 1 to 7%, more preferably 2 to 6%, more preferably 3 to 5%, and most preferably 4% by mass of the ammonium molybdate solution.
In the present invention, the first mixing is preferably performed by adding Ti (C, N) powder into an ammonium molybdate solution, performing ultrasonic oscillation and stirring, and then adding a dispersant under the conditions of ultrasonic oscillation and stirring to obtain a suspension.
In the present invention, the iron salt solution is preferably selected from a ferrous salt solution and/or a ferric salt solution; the iron salt is preferably selected from at least one of sulfate, chloride, nitrate and oxalate; the iron salt can be iron salt solid or iron salt solution.
In the present invention, the alkaline solution is preferably selected from an aqueous ammonia solution and/or a sodium hydroxide solution, more preferably an aqueous ammonia solution; the concentration of the aqueous ammonia solution is preferably 1 to 3mol/L, more preferably 1.5 to 2.5mol/L, and most preferably 2mol/L. In the present invention, the amount of the alkaline solution (aqueous ammonia solution) added is preferably controlled so that the pH of the system is 8 to 12, more preferably 9 to 11, and most preferably 10.
In the invention, the ammonia water solution is added into the suspension liquid in the second mixing preferably under the conditions of ultrasonic oscillation and stirring, and the pH value of the solution system is controlled to be 8-12; dropwise adding an iron salt solution, aging for 2-8 h after dropwise adding, and performing full reaction and precipitation to obtain a mixture; the aging time is preferably 3 to 6 hours, more preferably 4 to 5 hours.
In the present invention, the obtained mixture is preferably separated and washed before the drying; the separation is preferably carried out by filtration or a high-speed centrifuge; the washing is preferably carried out by washing with water and then with ethanol; the water is preferably deionized water, and the ethanol is preferably absolute ethanol; the number of times of the water washing is preferably 2 to 4 times, more preferably 3 times; the drying temperature is preferably 70-90 ℃, more preferably 75-85 ℃, and most preferably 80 ℃; and drying to obtain precursor powder.
In the present invention, the temperature of the calcination is preferably 500 to 800 ℃, more preferably 600 to 700 ℃, and most preferably 650 ℃; the calcination time is preferably 1 to 4 hours, more preferably 2 to 3 hours, and most preferably 2.5 hours; the calcination sufficiently decomposes the precursor powder to obtain a metal oxide composite powder.
In the present invention, the reduction is preferably carried out in an industrial tubular reduction furnace. In the present invention, the reduction is preferably carried out in the presence of a reducing agent, preferably selected from H 2 Ammonia and/or CO; the ammonia is preferably decomposed ammonia; the cross-sectional flow rate of the reducing agent is preferably 10 to 30ml/cm 2 Min, more preferably 15 to 25ml/cm 2 Min, most preferably 20ml/cm 2 Min. In the present invention, the temperature of the reduction is preferably 700 to 1000 ℃, more preferably 800 to 900 ℃, and most preferably 850 ℃; the time for the reduction (time for high-temperature retention) is preferably 60 to 120min, more preferably 70 to 110min, more preferably 80 to 100min, and most preferably 90min.
In an embodiment of the present invention, the method for preparing the Ti (C, N) -Mo-Fe composite powder preferably includes the steps of:
(1) Preparing ammonium molybdate solution, ferrous or ferric salt solution and ammonia solution according to the Mo and Fe contents required by the composite powder;
(2) Adding Ti (C, N) powder into an ammonium molybdate solution, wherein the addition amount is 5-200 g per liter of solution, and obtaining a uniformly dispersed suspension under the conditions of ultrasound and stirring;
(3) Adding a dispersing agent into the suspension prepared in the step (2) under the conditions of ultrasonic oscillation and stirring;
(4) Under the conditions of ultrasonic oscillation and stirring, adding an ammonia water solution into the solution in the step (3), controlling the pH value of the solution to be 8-12, then dropwise adding an iron salt solution, aging for 2-8 h after complete dropwise addition, fully reacting and precipitating, and filtering or separating, washing and drying the reaction solution by a high-speed centrifuge to obtain precursor powder;
(5) Placing the precursor powder at the temperature of 500-800 ℃ for full calcination to decompose the precursor powder to obtain metal oxide composite powder;
(6) And carrying out reduction reaction on the metal oxide composite powder at the reduction temperature of 700-1000 ℃, and obtaining the Ti (C, N) -Mo-Fe composite powder after the reduction reaction is finished.
The invention provides a metal ceramic which is prepared from the raw materials of the Ti (C, N) -Mo-Fe composite powder in the technical scheme.
In the present invention, the cermet is a Ti (C, N) -based cermet; the microstructure of the cermet alloy is preferably a coreless/ring structure or a weak core/ring structure.
In the present invention, the method for preparing the cermet preferably includes:
and mixing the Ti (C, N) -Mo-Fe composite powder with rubber, drying, sieving, pressing and sintering to obtain the metal ceramic.
In the present invention, the rubber is preferably a butadiene rubber.
In the present invention, the amount of the Ti (C, N) -Mo-Fe composite powder and the rubber is preferably 150 to 250ml, more preferably 180 to 220ml, and most preferably 200ml, per kg of the rubber.
In the present invention, the drying time is preferably 20 to 40min, more preferably 25 to 35min, and most preferably 30min; the screening mesh number is preferably 60-80 meshes, more preferably 65-75 meshes, and most preferably 70 meshes; the dimensions of the pressing are preferably 8mm × 6.7mm × 25mm; the sintering is preferably vacuum sintering, and the sintering temperature is preferably 1450-1490 ℃, more preferably 1460-1480 ℃ and most preferably 1470 ℃.
The invention provides an application of the Ti (C, N) -Mo-Fe composite powder in preparing Ti (C, N) -based metal ceramic; in the application of preparing the metal ceramic, except for the difference of production raw materials, the rest process steps and process parameters are basically the same as the prior metal ceramic preparation process.
The preparation method provided by the invention has the advantages of simple process, simple equipment, low cost and the like, the surface of the fully dispersed Ti (C, N) ceramic particles is uniformly coated with the pre-alloyed powder, the grain size of the pre-alloyed powder is nano-scale, the coating thickness is uniform and controllable, and the Ti (C, N) -Mo-Fe composite powder prepared by the method has good dispersibility and excellent sintering performance. The cermet prepared by the Ti (C, N) -Mo-Fe composite powder provided by the invention can effectively solve the problem of uneven distribution of metal phases and ceramics in the cermet, has better obdurability, and has a microstructure in a coreless/ring structure or a weak core/ring structure.
Ti (C) used in the following example 1 of the present invention x ,N 1-x ) Is a product provided by Nisshinokung hard material Co., ltd, and X is 0.5; ti (C) used in example 2 x ,N 1-x ) Is a product provided by Fuzhongkun rigid material Co., ltd, and X is 0.4.
Example 1
The Ti (C, N) -Mo-Fe composite powder prepared in this example was a core-shell structure, with the Ti (C, N) powder (as shown in fig. 1) as the core, the core being surrounded by a shell composed of metal powder, the metal powder being pre-alloyed powder composed of Mo and Fe; the mass fraction of the metal Fe in the composite powder is 15%, and the mass fraction of the metal Mo in the composite powder is 10%; the preparation method comprises the following steps:
24.54g ammonium molybdate ((NH) was weighed out 4 ) 6 Mo 7 O 24 ·4H 2 O) into a 1000mL flask, 300mL of deionized water was added, and 96.80g of ferric chloride (FeCl) was weighed 3 ·6H 2 O) adding 150mL of deionized water into a 250mL flask, and ultrasonically dissolving in an ultrasonic cleaning instrument until a transparent solution is formed; preparing an ammonia solution according to the concentration of 2mol/L.
Ti (C) with FSSS (Fisher grain size-air permeation method) of 0.8 μm is selected 0.5 ,N 0.5 ) Weighing 100g of the raw materials, adding the weighed raw materials into the prepared ammonium molybdate solution, obtaining uniformly dispersed suspension under the conditions of ultrasonic oscillation and stirring, weighing 3.2g of surfactant polyethylene glycol (PEG 6000) and adding the surfactant polyethylene glycol into the solution, continuing the ultrasonic oscillation and stirring, and adding an ammonia water solution into the solutionControlling the pH value of the solution to be 11.5, then dropwise adding the prepared ferric chloride solution, aging for 4h after complete dropwise adding, filtering and precipitating, washing with deionized water for three times, washing with absolute ethyl alcohol once, and then placing the precipitate in an oven to be dried at 80 ℃ to obtain precursor powder.
Putting the prepared precursor powder into a muffle furnace, calcining for 2h at the temperature of 700 ℃ to decompose the precursor powder, and obtaining Ti (C, N) metal oxide composite powder; placing the calcined powder in an industrial tubular reduction furnace, and reducing by using hydrogen at 850 ℃ and with the cross-sectional flow of the hydrogen of 20ml/cm 2 Min, the high temperature retention time was 90min, and finally the Ti (C, N) -Mo-Fe composite powder shown in fig. 2 was obtained, and the surface of the Ti (C, N) -Mo-Fe composite powder shown in fig. 2 was subjected to the energy spectrum EDS analysis, as shown in fig. 3, and it was found that the surface of the Ti (C, N) powder was indeed coated with Mo and Fe.
The Ti (C, N) -Mo-Fe composite powder prepared in example 1 is applied to the preparation of Ti (C, N) -based cermet, and the Ti (C, N) -Mo-Fe composite powder is doped with butadiene rubber (200 ml of butadiene rubber per kilogram), dried for 30min, sieved by a 70-mesh sieve, pressed into a green compact of 8mm × 6.7mm × 25mm, and sintered at 1470 ℃ in vacuum to obtain the cermet alloy shown in FIG. 4; as can be seen from FIG. 4, the cermet prepared by using the Ti (C, N) -Mo-Fe composite powder prepared by the invention can effectively solve the problem of uneven distribution of metal phases and ceramic phases, and the microstructure structure is a coreless/ring structure or a weak core/ring structure.
Example 2
The Ti (C, N) -Mo-Fe composite powder prepared in this example is a core-shell structure, the Ti (C, N) powder is used as an inner core, a shell composed of metal powder is coated outside the inner core, and the metal powder is pre-alloyed powder composed of Mo and Fe; the mass fraction of the metal Fe in the composite powder is 20%, and the mass fraction of the metal Mo in the composite powder is 15%; the preparation method comprises the following steps:
36.52g ammonium molybdate ((NH) was weighed out 4 ) 6 Mo 7 O 24 ·4H 2 O) into a 1000mL flask, 400mL of deionized water was added, and 81.45g of iron nitrate (Fe) was weighed 3 (NO 3 ) 3 ·9H 2 O) adding 150mL of deionized water into a 250mL flask, and ultrasonically dissolving in an ultrasonic cleaning instrument until a transparent solution is formed; preparing an ammonia solution according to the concentration of 2mol/L.
Ti (C) with FSSS (Fisher grain size-air permeation method) of 1.1 μm is selected 0.4 ,N 0.6 ) Weighing 86g of raw materials, adding the weighed raw materials into the prepared ammonium molybdate solution, obtaining uniformly dispersed suspension under the conditions of ultrasonic oscillation and stirring, then weighing 4.4g of surfactant polyethylene glycol (PEG 6000) and adding the mixture into the solution, continuing the ultrasonic oscillation and stirring, adding an ammonia water solution into the solution, controlling the pH value of the solution to be 11.0, then dropwise adding the prepared ferric nitrate solution, after complete dropwise addition, aging for 6 hours, filtering and precipitating, washing with deionized water for three times, washing with absolute ethyl alcohol once, and then placing the precipitate in an oven to be dried at 80 ℃ to obtain precursor powder.
Putting the prepared precursor powder into a muffle furnace, calcining for 2h at the temperature of 700 ℃ to decompose the precursor powder, and obtaining Ti (C, N) metal oxide composite powder; placing the calcined powder in an industrial tubular reduction furnace, and reducing with hydrogen at 850 deg.C and a cross-sectional flow of 20ml/cm 2 Min, and the high-temperature retention time is 90min, so as to finally obtain the Ti (C, N) -Mo-Fe composite powder.
The Ti (C, N) -Mo-Fe composite powder prepared in example 2 was applied to prepare a Ti (C, N) -based cermet according to the method of example 1, to obtain a cermet alloy.
Performance detection
The cermet alloys prepared in the embodiments 1 and 2 of the present invention were subjected to physical and mechanical property tests and metallographic tests, and the test results are shown in table 1, which can meet the use requirements of engineering materials.
TABLE 1 results of performance tests of cermet alloys prepared in examples
The preparation method provided by the invention has the advantages of simple process, simple equipment, low cost and the like, the surface of the fully dispersed Ti (C, N) ceramic particles is uniformly coated with the prealloy powder, the grain size of the prealloy powder is nano-scale, the coating thickness is uniform and controllable, and the Ti (C, N) -Mo-Fe composite powder prepared by the method has good dispersibility and excellent sintering performance. The cermet prepared by the Ti (C, N) -Mo-Fe composite powder provided by the invention can effectively solve the problem of uneven distribution of metal phases and ceramics in the cermet, has better obdurability, and has a microstructure in a coreless/ring structure or a weak core/ring structure.
While the invention has been described and illustrated with reference to specific embodiments thereof, such description and illustration are not intended to limit the invention. It will be clearly understood by those skilled in the art that various changes in form and details may be made therein without departing from the true spirit and scope of the invention as defined by the appended claims, to adapt a particular situation, material, composition of matter, substance, method or process to the objective, spirit and scope of this application. All such modifications are intended to be within the scope of the claims appended hereto. Although the methods disclosed herein have been described with reference to particular operations being performed in a particular order, it should be understood that these operations may be combined, sub-divided, or reordered to form equivalent methods without departing from the teachings of the present disclosure. Accordingly, unless specifically indicated herein, the order and grouping of the operations is not a limitation of the present application.
Claims (10)
1. A Ti (C, N) -Mo-Fe composite powder comprising:
a core comprising Ti (C, N);
a shell covering the core; the shell is selected from Mo and/or Fe.
2. The Ti (C, N) -Mo-Fe composite powder according to claim 1, wherein the mass content of the outer shell in the Ti (C, N) -Mo-Fe composite powder is 3 to 40%;
the mass content of Mo in the Ti (C, N) -Mo-Fe composite powder in the shell is 2-20%.
3. The Ti (C, N) -Mo-Fe composite powder of claim 1 wherein the Ti (C, N) is Ti (C) X ,N 1-X ) X is 0 to 1;
the average particle diameter of Ti (C, N) is preferably 0.1 to 5.0. Mu.m.
4. A method of preparing the Ti (C, N) -Mo-Fe composite powder of claim 1, comprising:
carrying out first mixing on Ti (C, N) powder, a dispersing agent and an ammonium molybdate solution to obtain a suspension;
and carrying out second mixing on the suspension, the alkaline solution and the iron salt solution, drying, calcining and reducing the obtained mixture to obtain the Ti (C, N) -Mo-Fe composite powder.
5. The method according to claim 4, wherein the ferric salt solution is selected from a ferrous salt solution and/or a ferric salt solution; the iron salt is selected from at least one of sulfate, chloride, nitrate and oxalate;
the alkaline solution is selected from ammonia solution and/or sodium hydroxide solution.
6. The method according to claim 4, wherein the dispersant is selected from one or more of organic amine, organic amine salt, surfactant and titanate coupling agent;
the dosage of the dispersant is 0.2 to 8 percent of the mass of the ammonium molybdate solution.
7. The method of claim 4, wherein the temperature of the calcination is 500 to 800 ℃; the calcination time is preferably 1 to 4 hours.
8. The method of claim 4, wherein the reduction is carried out in the presence of a reducing agent; the reducing agent is selected from H 2 Ammonia and/or CO; the reduction temperature is 700-1000 ℃; the reduction time is 60-120 min.
9. A cermet prepared from a feedstock comprising the Ti (C, N) -Mo-Fe composite powder of claim 1.
10. The cermet according to claim 9, characterised in that the microstructure of the cermet is a coreless/ring structure or a weak core/ring structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210951119.1A CN115283670A (en) | 2022-08-09 | 2022-08-09 | Ti (C, N) -Mo-Fe composite powder and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210951119.1A CN115283670A (en) | 2022-08-09 | 2022-08-09 | Ti (C, N) -Mo-Fe composite powder and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115283670A true CN115283670A (en) | 2022-11-04 |
Family
ID=83828015
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210951119.1A Pending CN115283670A (en) | 2022-08-09 | 2022-08-09 | Ti (C, N) -Mo-Fe composite powder and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115283670A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115846624A (en) * | 2023-02-28 | 2023-03-28 | 昆明理工大学 | Preparation method of ceramic/iron-based honeycomb-configuration composite material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854104A (en) * | 2005-04-19 | 2006-11-01 | 财团法人Seoul大学校产学协力财团 | Solid-solution powder, method to prepare the solid-solution powder, ceramic using the solid-solution powder, method to prepare the ceramic, cermet powder including the solid-solution powder, method to |
| CN102294473A (en) * | 2011-08-31 | 2011-12-28 | 株洲钻石切削刀具股份有限公司 | TiC/Ti(C,N)-Mo-Ni/Co composite powder and preparation method and application thereof |
| CN102534335A (en) * | 2012-01-17 | 2012-07-04 | 四川大学 | Rare earth alloy powder-modified Ti(C,N)-based metal ceramic and preparation method thereof |
| CN109175396A (en) * | 2018-11-15 | 2019-01-11 | 中南大学 | A kind of preparation method of nanometer of covered composite yarn powder |
| CN112247142A (en) * | 2020-10-21 | 2021-01-22 | 九江学院 | Double-hard-phase double-bonding-phase metal carbide ceramic powder with core-shell structure and preparation method thereof |
-
2022
- 2022-08-09 CN CN202210951119.1A patent/CN115283670A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854104A (en) * | 2005-04-19 | 2006-11-01 | 财团法人Seoul大学校产学协力财团 | Solid-solution powder, method to prepare the solid-solution powder, ceramic using the solid-solution powder, method to prepare the ceramic, cermet powder including the solid-solution powder, method to |
| CN102294473A (en) * | 2011-08-31 | 2011-12-28 | 株洲钻石切削刀具股份有限公司 | TiC/Ti(C,N)-Mo-Ni/Co composite powder and preparation method and application thereof |
| CN102534335A (en) * | 2012-01-17 | 2012-07-04 | 四川大学 | Rare earth alloy powder-modified Ti(C,N)-based metal ceramic and preparation method thereof |
| CN109175396A (en) * | 2018-11-15 | 2019-01-11 | 中南大学 | A kind of preparation method of nanometer of covered composite yarn powder |
| CN112247142A (en) * | 2020-10-21 | 2021-01-22 | 九江学院 | Double-hard-phase double-bonding-phase metal carbide ceramic powder with core-shell structure and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 朱刚;谢明;刘颖;陈家林;李再久;杨有才;: "Fe添加量对Ti(C, N)基金属陶瓷显微组织及力学性能的影响", 稀有金属与硬质合金, vol. 44, no. 02, pages 30 - 34 * |
| 朱刚;谢明;刘颖;陈家林;陈永泰;王松;: "Ti(C, N)/Fe-Co-Ni金属陶瓷烧结过程中的结构和相变", 稀有金属, vol. 40, no. 12, pages 1220 - 1225 * |
| 罗成: "超细Ti（C，N）粉体表面包覆及其金属陶瓷的制备", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 06, pages 020 - 254 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115846624A (en) * | 2023-02-28 | 2023-03-28 | 昆明理工大学 | Preparation method of ceramic/iron-based honeycomb-configuration composite material |
| CN115846624B (en) * | 2023-02-28 | 2023-04-28 | 昆明理工大学 | Preparation method of ceramic/iron-based honeycomb structural composite material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP3273448A1 (en) | Graphene/silver composite material and preparation method thereof | |
| CN101651050B (en) | Submicron particle reinforced Ag-based electrical contact material and preparation method thereof | |
| CN102294473B (en) | TiC/Ti(C,N)-Mo-Ni/Co composite powder and preparation method and application thereof | |
| KR20020064950A (en) | Powder mixture or composite powder, a method for production thereof and the use thereof in composite materials | |
| CN101186990A (en) | Ultra-fine hard alloy coated powder and method for preparing same | |
| CN103920875B (en) | The preparation method of WC-rare earth-Co successively coated composite hard alloy powder | |
| CN107186218B (en) | A kind of preparation method of modified superfine noble metal powder | |
| CN109576545A (en) | A kind of Ti (C, N) based ceramic metal and preparation method thereof with duplex grain structure | |
| CN115283670A (en) | Ti (C, N) -Mo-Fe composite powder and preparation method and application thereof | |
| CN103056376B (en) | Method for preparing spherical nanostructure tungsten/cobalt carbide compound powder | |
| CN107245628A (en) | Make Hardmetal materials of Binder Phase and preparation method thereof using Ni Cu continuous solid solutions | |
| CN108866418A (en) | A kind of preparation method of oxide dispersion intensifying iron-cobalt-nickel medium entropy alloy | |
| CN110983142B (en) | Preparation method of tungsten carbide-nickel hard alloy | |
| CN108165791B (en) | Preparation method of binderless superfine tungsten carbide hard alloy | |
| CN107217171B (en) | A kind of rare earth doped oxide Cu-base composites of liquid liquid and preparation method thereof | |
| CN116497293B (en) | High-temperature-resistant oxidation-resistant tungsten-lanthanum alloy wire and preparation method thereof | |
| CN112209446A (en) | Method for recycling Cr-containing tungsten carbide waste and application thereof | |
| CN108531764B (en) | Silver tungsten carbide graphene electrical contact material and preparation method thereof | |
| CN106653410B (en) | A kind of high-performance environment protection type siller tin oxide electric contact material and preparation method thereof | |
| CN111020337B (en) | Inhibitor applied to preparation of superfine tungsten carbide and preparation method thereof | |
| CN107868948A (en) | A kind of method of the chemical plating cobalt coated tungsten carbide based on cobalt salt activation | |
| CN113774264A (en) | Preparation method of coarse-grain WC-Co-X hard alloy based on addition of ultrafine powder | |
| CN113857474A (en) | Preparation method of WC surface-coated Co powder added with Ce element | |
| CN112898025A (en) | Method for preparing vanadium boride ultrafine powder by carbon-thermal boron-thermal method | |
| CN107162038B (en) | A kind of cuprous oxide powder and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |