CN109371308B - The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end - Google Patents
The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The present invention provides a kind of method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end, including, a, the preparation of precursor powder: the dosage of alumina source and source metal is so that it is 3~20% that the total amount of metallic iron, cobalt and nickel, which accounts for the mass percentage of composite powder, in final composite powder, and the molar ratio of iron, cobalt and nickel is 1:0.5~2:0.5~2 in source metal, urea is reactive fuel, glucose is complexing agent and dispersing agent, obtains precursor powder；B, the preparation of composite powder product: carrying out the heat treatment of high temperature two-step for obtained precursor powder, specifically includes precursor powder first in air and then in a reducing atmosphere each isothermal holding 0.5~3 hour at 600-1000 DEG C, obtains the product.The present invention has many advantages, such as that nano metal disperse phase-nanocrystalline structure alumina-based ceramic metal powder provides new thinking for preparation, has with short production cycle, at low cost, easy to operate.
Description
Technical field
The invention belongs to ceramic matric composite research field, specifically provides and a kind of prepare the oxidation of multi-principal elements alloy toughening
The method of aluminium based metal ceramic composite powder.
Background technique
Alumina-based ceramic metal material is a kind of new material by domestic and international extensive concern and research in recent years.This
Kind material is generally distributed in aluminium oxide ceramics matrix using superfine nano metal phase even dispersion, it is made to possess oxidation aluminium
The high intensity of material, high rigidity, it is wear-resistant, high temperature resistant and chemical stability are high the advantages that simultaneously, and because metal disperse phase is added
Preferable toughness can be obtained, is a kind of very important tool materials and structural material.
In aluminium oxide ceramics based nano composite material, the size of metal disperse phase and distribution are the passes for determining its mechanical property
Key factor.Firstly, the introducing of nano metal disperse phase can not only inhibit matrix grain abnormal growth, make the microcosmic knot of basis material
Structure homogenization, promotes toughness of material；Secondly, part metals disperse phase may be wrapped in the inside of oxide matrix, form
Metal/oxide interface abundant makes crackle incline by what the crystal boundary of oxide matrix extended to weaken the effect of crystal boundary
Tropism reduces, and so that grain boundary fracture is converted into transgranular fracture, the toughness of material gets a promotion.Finally, metal disperse phase is uniformly divided
Cloth can inhibit crystal boundary migration and refine crystal grain, and the microstructure of fining can improve the intensity and toughness of material simultaneously.Therefore it is right
In alumina-based ceramic metal material, the distribution of metal disperse phase is more uniform, and size is more tiny, and metal dispersion-strengtherning alumina base is received
The mechanical property of nano composite material is higher.
The method that alumina-based ceramic metal nanocomposite mainly uses powder metallurgy manufactures, and successfully prepares high-performance
The key of alumina-based ceramic metal nanocomposite is the high quality aluminum oxide Base Metal pottery that disperse phase is made and is evenly distributed
Porcelain nano composite powder.The existing method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end is mainly machinery
Alloying, reaction ball milling method and sol-gal process etc..
Mechanical alloying method is mainly by the Al as raw material2O3Powder (matrix) and elemental metalpowder (source metal) are mixed
It attaches together tank and carries out high-energy ball milling under conditions of certain ratio of grinding media to material and atmosphere protection.During ball milling, raw material powder is born
The effect of many kinds of force such as impact, shearing, friction, compression, the processes such as experience flattening, coldwelding, alloying component homogenization, is realized
Metal powder granulates alloying is simultaneously distributed in oxide matrix even dispersion.Ma process can successfully prepare aluminium oxide
Based nano composite material, but have the shortcomings that its is significant: firstly, since in ma process as the ball of ball-milling medium and
Powder raw material sharp impacts, abrading-ball and tank body as medium easily wear during mechanical alloying and are mixed into powder original
In material, impurity is introduced in final powder raw material；Secondly, the high velocity impact in ma process is easy that metal disperse is made to meet
Conjunction is grown up, and finally obtained block materials performance is influenced；Finally, mechanical alloying is a highly energy-consuming, the lower process of efficiency,
It is unfavorable for the large-scale production of powder.
Reaction ball milling method is the modification method of mechanical alloying method, Tohru Sekino et al. (Journal of the
1997,80 (5): American Ceramic Society 1139-1148) uses Al2O3Powder and nitrate (source metal) are molten
Liquid is that raw material carries out wet mixing ball milling, so that alumina powder and nitrate are uniformly mixed.It is mixed by what is obtained after ball milling certain time
Close object makes nitrate decompose to obtain metal oxide and Al in 450 DEG C or so heating2O3Mixed-powder, finally will mixing reduction
Obtain metal dispersion-strengtherning alumina-based nano composite powder.Although reaction ball milling method technique is more complex, it is existing research at
Fruit shows, compared with mechanical alloying method, is used as the metal of disperse phase to give birth in situ on blapharoplast during reaction ball milling method
At the size of metal disperse phase being reduced to 100nm from 300nm hereinafter, to promotion aluminium oxide fund by a relatively large margin
Belong to the mechanical property of ceramic nanocomposites.Very important, reaction ball milling method has similar lack with mechanical alloying method
Point: powder is easily doped pollution and mass production cost is excessively high.Specifically, all because of the ball and ball grinder of the rotation of ball milling high speed
It can wear, aluminium oxide ceramics based nano composite material product generally increases weight 20g or more when ball milling 1000g, this just undoubtedly can be to producing
Product bring 2% impurity.And Ball-milling Time is long, energy consumption is high, thus mass production cost is excessively high.
The basic principle of sol-gel method is to be readily able to the metallic compound (inorganic salts or metal alkoxide) of hydrolysis at certain
It reacts in solvent with water or other substances, through hydrolysis and polycondensation process gradually gelation, using calcining and restore
To required material.As E.D.Rodeghiero et al. (Materials Science and Engineering A, 1995,
195:151-161) by aluminium isopropoxide (Al (C3H7O)3) it is dissolved in ethyl alcohol, two water nickel formate (Ni are added after being heated to boiling
(CHO2)2·2H2Mixed solution is then ultrasonically treated 30 minutes at 60 DEG C or more and obtains colloidal sol, colloidal sol is fallen by aqueous solution O)
Enter open container and obtain gel for a period of time at room temperature, gel is sieved to obtain precursor in 100 DEG C or less drying and grindings
End, finally by precursor powder, 1000 DEG C of heat preservations obtain metal target ceramic powders in hydrogen atmosphere.E.BREVAL et al.
(Journal of Materials Science, 1992,27:1464-1468) aluminium secondary butylate is dissolved in isopropanol formed it is molten
HNO is added after stirring solution 15 minutes in liquid3PH value is adjusted to 2.Nickel nitrate (Ni is added after stirring 1 hour at 80 DEG C
(NO3)2·6H2O colloidal sol) is formed, colloidal sol forms gel after the dry some time.Again by obtained gel in air gas
500 DEG C of calcinings obtain precursor powder in atmosphere, and finally by precursor powder, 1000 DEG C of heat preservations obtain mesh in 4 hours in hydrogen atmosphere
Mark metal ceramic powder.By previously mentioned it is found that sol-gel method preparation process is complicated, and it is prepared in target powder
Disperse phase metal partial size is larger.Therefore, it is necessary to develop the system of new metal dispersion-strengtherning alumina ceramic-base nano composite powder
Standby technique.
In addition, the Metal toughened of usually alumina-based ceramic metal is mutually pure metal (Fe, Ni, Co, W etc.), or by two
The alloy of kind metal composition.2018, Liu Jinchuan of City University of Hong Kong et al. (Science, 2018,362:933-937) was ground
Study carefully discovery, compared to single metal pivot material, tri- kinds of element 1:1:1 of Fe, Co, Ni are mixed can be significantly as alloy pivot
Increase material intensity and toughness.It is inspired by this research, we intend developing a kind of aluminium oxide using multi-principal elements alloy toughening
Based ceramic metal.
Summary of the invention
The purpose of the present invention is to provide a kind of multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder ends of preparing
A kind of method, it is intended to develop efficient, energy-efficient alumina-based ceramic metal nanometer of the method preparation with superfine metal disperse phase
Composite powder.The designability of superfine metal disperse phase enhanced oxidation aluminium ceramic base nano composite powder is strong, metal disperse phase is special
Not tiny (5-20nm).
The present invention uses solution combustion synthetic method to prepare nano composite oxide precursor powder first, then by oxide
Precursor powder air roasting and in hydrogen carry out selective reduction obtain alumina-based ceramic metal nano composite powder.
Therefore, the present invention provides a kind of method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end,
Described method includes following steps, the preparation of a, precursor powder: alumina source is Al (NO in raw material3)3·9H2O, source metal
For Fe (NO3)3·9H2O、Ni(NO3)2·6H2O and Co (NO3)2·6H2O, and the molar ratio of iron, cobalt and nickel is 1 in source metal:
The dosage of 0.5~2:0.5~2, the alumina source and source metal is the metal so that in the composite powder being finally prepared
The mass percentage that the total amount of iron, cobalt and nickel accounts for composite powder is 3~20%, and urea is reactive fuel, and glucose is complexing
Agent and dispersing agent, alumina source, source metal, urea and glucose, which are dissolved in deionized water, obtains mixed solution, described in heating
The precursor powder is prepared in mixed solution reaction；B, the preparation of composite powder product: by obtained precursor powder into
The heat treatment of row high temperature two-step specifically includes precursor powder first in air isothermal holding 0.5~3 hour at 600-1000 DEG C,
Then it obtains in a reducing atmosphere isothermal holding 0.5~3 hour at 600-1000 DEG C with γ-Al2O3For the mostly main of ceramic matrix
First alloy toughened aluminum oxide base metal-ceramic composite powder end.
In a kind of specific embodiment, the partial size of the metal of nanoscale is 5~20nm in product.
In a kind of specific embodiment, the molar ratio of urea and raw material aluminum nitrate is 0.9~1.2:1, Portugal in step a
The molar ratio of grape sugar and raw material aluminum nitrate is 0.2~0.5:1.
In a kind of specific embodiment, the reaction temperature that in step a prepared by precursor powder is 120~350 DEG C, excellent
It is selected as 200~300 DEG C.
In a kind of specific embodiment, the reducing atmosphere in step b is hydrogen atmosphere.
In a kind of specific embodiment, in step a, stop heating when 5~10min of heating is to solution vigorous reaction,
After waiting 1~2 minute, reaction terminates to obtain precursor powder.
In a kind of specific embodiment, in step b, precursor powder is first in air at 700-900 DEG C at heat preservation
Reason 1~2 hour, then in a reducing atmosphere isothermal holding 1~2 hour at 700~900 DEG C.
In a kind of specific embodiment, in step a, the molar ratio of iron, cobalt and nickel is 1:0.8~1.2 in source metal:
0.8~1.2, the preferably molar ratio of iron, cobalt and nickel is 1:1:1.
The present invention correspondingly provides a kind of multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end, more pivots
As above any one the method is prepared at alloy toughened aluminum oxide base metal-ceramic composite powder end.
The advantages of the present invention:
1, it in the present invention, either prepares in the heating process or high temperature two-step heat treatment process of precursor powder all
It does not need to stir, is more not required to be related to the ball milling method of high energy consumption.Consersion unit using can be vented in time after heating crucible, burn
The common devices such as cup, electrothermal furnace and Muffle furnace.Equipment is simple, easy to operate.
2, the present invention in nano composite powder using aluminium oxide as matrix, and be specifically with crystal form be γ type gamma oxidation
Aluminium is ceramic matrix, is heat-treated to obtain by the high temperature two-step after precursor preparation, so that amorphous alumina in treatment process
All it is converted into gama-alumina.
3, multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end provided by the invention product can be used for replacing " carbon
Wear-resistant material of change tungsten and the cobalt hard alloy " as high rigidity.The product combines the high rigidity and metal material of ceramic material
Toughness, which for example forms a kind of hard wear-resistant material haveing excellent performance after tabletting.
Generally speaking, the present invention passes through control raw material proportioning in-situ preparation target in the solution that liquid-liquid atom level mixes
Nano composite powder for preparation there is nano metal disperse phase-nanocrystalline structure alumina-based ceramic metal powder to provide
New thinking, it has many advantages, such as with short production cycle, at low cost, easy to operate.Ultra-fine metallic particles can not only refine aluminium oxide
Crystal grain, improve sintering activity, and can effectively inhibit the crystal grain in its sintering process to grow up, to obtain high-compactness, nanogold
Belong to the Ultra-fine Grained alumina-based ceramic metal that disperse phase is evenly distributed to lay a good foundation.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
The reaction temperature that in step a of the present invention prepared by precursor powder is 120~350 DEG C, preferably 200~300 DEG C.Step
The precursor powder being prepared in rapid a is the mixture of iron oxide, cobalt oxide and nickel oxide these three oxides and aluminium oxide,
200~300 DEG C are heated to after mixing raw material during precursor preparation, nitrogen, dioxy may be released in reaction process
Change the gases such as carbon and water vapour.
Reducing atmosphere in step b of the present invention is, for example, hydrogen atmosphere.In the present invention, at the high temperature two-step heat of presoma
Reason includes air heat treatment and hydrogen is heat-treated two steps, may roast iron oxide, cobalt oxide and nickel oxide in air heat treatment
It burns to form compound with aluminium oxide, then is heat-treated under hydrogen, the oxide of iron-cobalt-nickel all will be reduced to simple substance, and aoxidize
Aluminium will not be reduced, but amorphous alumina can be transformed into the gama-alumina of crystal form.If by precursor powder directly in hydrogen gas
It is heat-treated in atmosphere, then can not form the metal-ceramic nano composite powder of gamma oxidation aluminium base.
Embodiment 1:3wt.% (FeCoNi)-Al2O3The preparation of nano composite powder
Weigh 0.00182mol Fe (NO3)3·9H2O、0.00182mol Co(NO3)2·6H2O、0.00182mol Ni
(NO3)2·6H2O、0.2mol Al(NO3)3·9H2O, 0.18mol urea and 0.05mol glucose are dissolved in deionized water,
It is stirred evenly in container, obtains mixed solution.Mixed solution agitating and heating in controllable temperature furnace, evaporates aqueous solution.With anti-
The progress answered, the heat of releasing make raw material that pyrolysis and violent redox reaction occur, and object element is then converted into granularity pole
Thin composite precursor particle.Carry out two-step heat treatment to precursor powder: first step heat treatment keeps the temperature for 700 DEG C in air
Time is 1 hour, and second step heat treatment is 700 DEG C heat preservation 1 hour in hydrogen.Finally obtain 3wt.% (FeCoNi)-Al2O3
Nano composite powder.
Embodiment 2:10wt.% (FeCoNi)-Al2O3The preparation of nano composite powder
Weigh 0.00651mol Fe (NO3)3·9H2O、0.00651mol Co(NO3)2·6H2O、0.00651mol Ni
(NO3)2·6H2O、0.2molAl(NO3)3·9H2O, 0.2mol urea and 0.08mol glucose are dissolved in deionized water, are being held
It is stirred evenly in device, obtains mixed solution.Mixed solution agitating and heating in controllable temperature furnace, evaporates aqueous solution.With reaction
Progress, the heat of releasing makes raw material that pyrolysis and violent redox reaction occur, and it is superfine that object element is then converted into granularity
Composite precursor particle.Two-step heat treatment is carried out to precursor powder: when first step heat treatment is 800 DEG C of heat preservations in air
Between be 1 hour, second step heat treatment in hydrogen 700 DEG C keep the temperature 1 hour.Finally obtain 10wt.% (FeCoNi)-Al2O3It receives
Rice composite powder.
Embodiment 3:15wt.% (FeCoNi)-Al2O3The preparation of nano composite powder
Weigh 0.0104mol Fe (NO3)3·9H2O、0.0104mol Co(NO3)2·6H2O、0.0104mol Ni
(NO3)2·6H2O、0.2mol Al(NO3)3·9H2O, 0.22mol urea and 0.09mol glucose are dissolved in deionized water,
It is stirred evenly in container, obtains mixed solution.Mixed solution agitating and heating in controllable temperature furnace, evaporates aqueous solution.With anti-
The progress answered, the heat of releasing make raw material that pyrolysis and violent redox reaction occur, and object element is then converted into granularity pole
Thin composite precursor particle.Carry out two-step heat treatment to precursor powder: first step heat treatment keeps the temperature for 800 DEG C in air
Time is 1 hour, and second step heat treatment is 800 DEG C heat preservation 1 hour in hydrogen.Finally obtain 15wt.% (FeCoNi)-Al2O3
Nano composite powder.
Embodiment 4:20wt.% (FeCoNi)-Al2O3The preparation of nano composite powder
Weigh 0.0147mol Fe (NO3)3·9H2O、0.0147mol Co(NO3)2·6H2O、0.0147mol Ni
(NO3)2·6H2O、0.2mol Al(NO3)3·9H2O, 0.24mol urea and 0.1mol glucose are dissolved in deionized water, are being held
It is stirred evenly in device, obtains mixed solution.Mixed solution agitating and heating in controllable temperature furnace, evaporates aqueous solution.With reaction
Progress, the heat of releasing makes raw material that pyrolysis and violent redox reaction occur, and it is superfine that object element is then converted into granularity
Composite precursor particle.Two-step heat treatment is carried out to precursor powder: when first step heat treatment is 900 DEG C of heat preservations in air
Between be 2 hours, second step heat treatment in hydrogen 900 DEG C keep the temperature 1 hour.Finally obtain 20wt.% (FeCoNi)-Al2O3It receives
Rice composite powder.
In step a of the present invention, the molar ratio of aluminum nitrate generates in reaction process between 0.9~1.2 in urea and raw material
Bulk gas can prevent the reunion of precursor powder；The effect of glucose is metal ion in complex reaction system, absorbs
Part reaction generate heat prevent from reuniting, and increase it is gas generated, generate dispersion powders effect, further refine powder,
Reaction temperature is reduced, the molar ratio of aluminum nitrate is between 0.2~0.5 in glucose and raw material.
The present invention is after the heat treatment of step b high temperature two-step, and the oxide of Fe, Co, Ni are converted to gold in precursor powder
Belong to or crystallization occurs after heat treatment for solid solution alloy, aluminium oxide, by unformed Al2O3It is converted into γ-Al2O3, final
To alumina-based ceramic metal nano composite powder.
The above content is combine specific preferred embodiment to the further description of the invention made, and it cannot be said that originally
The specific implementation of invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, not
Under the premise of being detached from present inventive concept, several simple deductions and replacement can also be made, all shall be regarded as belonging to guarantor of the invention
Protect range.
Claims (9)
1. a kind of method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end, which is characterized in that the side
Method includes the following steps,
A, the preparation of precursor powder: alumina source is Al (NO in raw material3)3·9H2O, source metal are Fe (NO3)3·9H2O、Ni
(NO3)2·6H2O and Co (NO3)2·6H2O, and the molar ratio of iron, cobalt and nickel is 1:0.5~2:0.5~2 in source metal, it is described
The dosage of alumina source and source metal is so that the total amount of metallic iron, cobalt and nickel in the composite powder being finally prepared accounts for again
The mass percentage for closing powder is 3~20%, and urea is reactive fuel, and glucose is complexing agent and dispersing agent, alumina source,
Source metal, urea and glucose, which are dissolved in deionized water, obtains mixed solution, heats the mixed solution reaction and is prepared
The precursor powder；
B, the preparation of composite powder product: obtained precursor powder is subjected to the heat treatment of high temperature two-step, specifically includes presoma
Powder is first in air isothermal holding 0.5~3 hour at 600-1000 DEG C, then keeps the temperature at 600-1000 DEG C in a reducing atmosphere
Processing 0.5~3 hour, obtains with γ-Al2O3For the multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder of ceramic matrix
End.
2. the method according to claim 1, wherein the partial size of the metal of nanoscale is 5~20nm in product.
3. the method according to claim 1, wherein the molar ratio of urea and raw material aluminum nitrate is 0.9 in step a
The molar ratio of~1.2:1, glucose and raw material aluminum nitrate is 0.2~0.5:1.
4. the method according to claim 1, wherein the reaction temperature that in step a prepared by precursor powder is 120
~350 DEG C.
5. the method according to claim 1, wherein the reducing atmosphere in step b is hydrogen atmosphere.
6. the method according to claim 1, wherein in step a, when 5~10min of heating is to solution vigorous reaction
Stop heating, after waiting 1~2 minute, reaction terminates to obtain precursor powder.
7. method described according to claim 1~any one of 6, which is characterized in that in step b, precursor powder first exists
Isothermal holding 1~2 hour at 700~900 DEG C in air, then isothermal holding 1~2 is small at 700~900 DEG C in a reducing atmosphere
When.
8. method described according to claim 1~any one of 6, which is characterized in that in step a, iron in source metal, cobalt and
The molar ratio of nickel is 1:0.8~1.2:0.8~1.2.
9. a kind of multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end, which is characterized in that the multi-principal elements alloy increases
Any one of tough alumina-based ceramic metal composite powder such as claim 1~8 the method is prepared.
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