CN107793149A - A kind of preparation method of ZTA nano composite powders - Google Patents
A kind of preparation method of ZTA nano composite powders Download PDFInfo
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- CN107793149A CN107793149A CN201711055867.7A CN201711055867A CN107793149A CN 107793149 A CN107793149 A CN 107793149A CN 201711055867 A CN201711055867 A CN 201711055867A CN 107793149 A CN107793149 A CN 107793149A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
- C04B35/62615—High energy or reactive ball milling
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/40—Metallic constituents or additives not added as binding phase
- C04B2235/402—Aluminium
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Abstract
The invention discloses a kind of preparation method of ZTA nano composite powders, comprise the following steps：(1) by the spherical Al of raw material2O3、ZrO2, MgO, additive powder weighed by proportioning configuration, and premixed；(2) ball milling ball is agate ball, is 45 according to ratio of grinding media to material：1 is put into premix powders and agate ball in nylon ball grinder, makees ball-milling medium using absolute ethyl alcohol, absolute ethyl alcohol addition is not cross the 2cm of ball milling ball horizontal plane 1 in nylon tank, adition process controlling agent；(3) ball milling uses horizontal ball mill, controls ball milling speed and Ball-milling Time to carry out ball milling；(4) ball material separation is carried out with absolute ethyl alcohol after the completion of ball milling, separation mixed liquor is dried, powder crosses 80 mesh sieve after the completion of drying, and ZTA nano composite powders are made.Present invention process flow is short, and technological operation is easy, and equipment requirement is low, and cost is low, and three waste discharge is few, smaller to environment and human body harm, is easy to promote and industrial-scale continuous production.
Description
Technical field
It is nano combined more particularly, to a kind of extensive quick ZTA the invention belongs to nonmetal nano material technical field
Raw powder's production technology.
Background technology
《Ceramic journal》The text of magazine the 15th phase in 2016 " nano-powder prepares the performance study of ZTA complex phase ceramics " one is introduced
A kind of to use Preparation of ZTA nanoceramic composites by liquid-phase precipitation method material, its method is NH4Al(SO4)2、ZrOCl2、Y(NO3)3
And NH4HCO3For presoma, mixed by a certain percentage with sequencing, obtain being deposited in 1000 DEG C and be sintered into powder.Deficiency
Place is that liquid-phase precipitation method preparation ZTA composite nano-powder technological processes are complicated, and control variable is more, and process cycle is longer, unfavorable
Large-scale industrial production is carried out in promoting.
At present, a kind of preparation method of the easy ZTA nano composite powders of technological operation is lacked.
The content of the invention
A kind of regarding the issue above, the present invention provides preparation of the ZTA nano composite powders of technological operation simplicity
Method.
To reach above-mentioned purpose, present invention employs following technical proposal：A kind of system of ZTA nano composite powders of the present invention
Preparation Method, comprise the following steps：
(1) by the spherical Al of raw material2O3、ZrO2, MgO, additive powder weighed by proportioning configuration, and premixed；
(2) ball milling ball is agate ball, is 4-5 according to ratio of grinding media to material：Premix powders and agate ball are put into nylon ball grinder by 1
It is interior, ball-milling medium is made using absolute ethyl alcohol, absolute ethyl alcohol addition adds not cross ball milling ball horizontal plane 1-2cm in nylon tank
Process control agent；
(3) ball milling uses horizontal ball mill, controls ball milling speed and Ball-milling Time to carry out ball milling；
(4) ball material separation is carried out with absolute ethyl alcohol after the completion of ball milling, separation mixed liquor is dried, powder, which is dried, to be completed
80 mesh sieve are crossed afterwards, and ZTA nano composite powders are made.
Further, in step (1), described material powder includes forming according to the following component of mass percent：
15%≤ZrO2≤ 30%,
MgO 0.25,
0.5%≤Al≤5%,
Surplus is additive powder.
Further, in step (1), described additive powder is Al powder, its purity >=99.5%, Al powder size
≤Al2O3Powder size.
Further, in step (2), described spherical Al2O3、ZrO2, MgO powder, Al2O3Powder size≤10um,
ZrO2 powder size≤100nm, MgO powder size≤100nm.
Further, in step (2), described agate ball is 3mm≤sphere diameter≤5mm.
Further, in step (2), described process control agent is stearic acid, 1%≤stearic addition≤
2% (ω %).
Further, in step (2), described ball milling speed is 40-50rpm, and the Ball-milling Time is that 48-60 is small
When.
Further, in step (4), the drying temperature of described separation mixed liquor is≤80 DEG C.
Beneficial effect：Present invention process flow is short, and technological operation is easy, and equipment requirement is low, and cost is low, and three waste discharge is few,
It is smaller to environment and human body harm, be advantageous to the protection to environment, be easy to promote and industrial-scale continuous production.
Brief description of the drawings
Fig. 1 is morphology microstructure variation diagram before and after additive of the present invention addition；
Fig. 2 is powder sintering sample ingredient variation diagram before and after additive of the present invention addition；
Fig. 3 is sintered sample mechanical property variation diagram before and after additive of the present invention addition；
Fig. 4 is crystal formation ZrO2 changes of contents figures in powder sintering sample before and after additive of the present invention addition.
Embodiment
Following examples only exist in illustrative purpose, without being intended to limit the scope of the present invention.
Embodiment 1
As shown in Figure 1 to Figure 3, Fig. 1 is morphology microstructure variation diagram before and after additive of the present invention addition；Comparative example powder reuniting
Seriously, ZrO2 skewness, embodiment powder granule is tiny, reunites lighter, and ZrO2 is distributed in spheric granules surface, disperses equal
It is even；
Fig. 2 is powder sintering sample ingredient variation diagram before and after additive of the present invention addition；T-ZrO2 substantially increases, and is advantageous to carry
The high strength of materials and toughness；
Fig. 3 is sintered sample mechanical property variation diagram before and after additive of the present invention addition.Addition Al causes ZrO2 in powder
Dispersiveness improves, and ZrO2 crystal grain is tiny after sintering, forms the increase of t-ZrO2 contents, and strength of materials hardness improves.
Fig. 4 is crystal formation ZrO2 changes of contents figures in powder sintering sample before and after additive of the present invention addition.
A kind of preparation method of ZTA nano composite powders of the present invention, comprises the following steps：
(1) by the spherical Al of raw material2O3、ZrO2, MgO, additive powder by proportioning configuration premixed；Described raw material powder
End includes forming according to the following component of mass percent：
15%≤ZrO2≤ 30%,
MgO 0.25,
0.5%≤Al≤5%,
Surplus is additive powder.
Described additive powder is Al powder, its purity >=99.5%, Al powder size≤Al2O3Powder size.
(2) ball milling ball is agate ball, is 5 according to ratio of grinding media to material：1 is put into premix powders and agate ball in nylon ball grinder,
Ball-milling medium is made using absolute ethyl alcohol, absolute ethyl alcohol addition is not cross ball milling ball horizontal plane 1cm in nylon tank, adition process control
Preparation；Described spherical Al2O3、ZrO2, MgO powder, Al2O3Powder size≤10um, ZrO2Powder size≤100nm, MgO
Powder size≤100nm.Described agate ball is 3mm≤sphere diameter≤5mm.Described process control agent is stearic acid, 1%≤
Stearic addition≤2% (ω %).
Described ball milling speed is 40rpm, and the Ball-milling Time is 60 hours.The drying temperature of described separation mixed liquor
For≤80 DEG C.
(3) ball milling uses horizontal ball mill, controls ball milling speed and Ball-milling Time to carry out ball milling；
(4) ball material separation is carried out with absolute ethyl alcohol after the completion of ball milling, separation mixed liquor is dried, powder, which is dried, to be completed
80 mesh sieve are crossed afterwards, and ZTA nano composite powders are made.
Embodiment 2
The difference of embodiment 2 and embodiment 1 is：
A kind of preparation method of ZTA nano composite powders of the present invention, comprises the following steps：
In step (1), by the spherical Al of raw material2O3、ZrO2, MgO, additive powder by proportioning configuration premixed；It is described
Material powder include according to mass percent following component form：
15%≤ZrO2≤ 30%,
MgO 0.25,
0.5%≤Al≤5%,
Surplus is additive powder.
In step (2), ball milling ball is agate ball, is 4 according to ratio of grinding media to material：Premix powders and agate ball are put into nylon by 1
In ball grinder, ball-milling medium is made using absolute ethyl alcohol, absolute ethyl alcohol addition is not cross ball milling ball horizontal plane in nylon tank
1.2cm, adition process controlling agent；
In step (3), described ball milling speed is 45rpm, and the Ball-milling Time is 48 hours.
Embodiment 3
The difference of embodiment 3 and embodiment 1 is：A kind of preparation method of ZTA nano composite powders of the present invention, including such as
Lower step：
In step (1), by the spherical Al of raw material2O3、ZrO2, MgO, additive powder by proportioning configuration premixed；Institute
The material powder stated includes forming according to the following component of mass percent：
15%≤ZrO2≤ 30%,
MgO 0.25,
0.5%≤Al≤5%,
Surplus is additive powder；
Described additive powder is Al powder, its purity >=99.5%, Al powder size≤Al2O3Powder size.
In step (2), ball milling ball is agate ball, is 4.5 according to ratio of grinding media to material：Premix powders and agate ball are put into Buddhist nun by 1
In imperial ball grinder, ball-milling medium is made using absolute ethyl alcohol, absolute ethyl alcohol addition is not cross ball milling ball horizontal plane in nylon tank
2cm, adition process controlling agent；
In step (3), described ball milling speed is 50rpm, and the Ball-milling Time is 54 hours.
Comparative example
By spherical Al2O3、ZrO2, MgO powder press surplus:25:0.25 proportional arrangement is premixed, and uses ball milling ball as agate
Nao balls, according to 4:1 ratio of grinding media to material, premix powders and agate ball are put into nylon ball grinder, make ball-milling medium using absolute ethyl alcohol,
Absolute ethyl alcohol addition adds 1.2% (ω %) stearic acid and makees process control not cross ball milling ball horizontal plane 2cm in nylon tank
Agent.
Ball milling is carried out on horizontal ball mill, ball milling speed 50rpm, ball milling 48 hours.Nothing is used after the completion of ball milling as early as possible
Water-ethanol carries out ball material separation, and separation mixed liquor is dried at 70 DEG C, and powder crosses 80 mesh sieve after the completion of drying, and is received
Rice composite powder.
Then 1 is added in nano composite powder:70mL artificial rubbers make adhesive, are well mixed, and are carried out below 60 DEG C
Dry, ZTA powders 6x8x25mm moulds, pressing pressure 450MPa compactings is made after 80 mesh sieve in powder after the completion of drying
Shaping, it is degreasing sintered using the progress of high temperature muffle furnace, degreasing sintered, skimming temp is carried out to green compact with 2 DEG C/min heating rates
For 250 DEG C and 370 DEG C, degreasing time is respectively 1 hour and 2 hours.Further heated up after the completion of green compact degreasing, be increased to sintering
1650 DEG C of temperature, 2 hours are incubated, furnace cooling after the completion of sintering.
Its powder ZrO2 particles have a more reunion, and " transgranular type " ZrO2 accounts for the 33.05% of total ZrO2 after powder sintering, bending resistance
Intensity is 254MPa, Vickers hardness 1278HV1.
Product in embodiments of the invention overcomes simple mechanical ball-milling method and prepares nano-ceramic powder batch mixing inequality, powder
Reunite the problems such as serious, it is small to prepare diameter of particle, and ZrO2 particles dispersing uniformity in powder improves.ZTA ceramics are " interior after sintering
Crystal formation " ZrO2 contents improve 171.43%.Interior crystal formation ZrO2 contents improve ceramics, suppress t-ZrO2 phase transformations, and ZTA ceramics room temperature is protected
The interior crystal formation t-ZrO2 contents increase stayed.Improve crystal formation t-ZrO2 contents, transformation toughening and phase change induction micro-crack in ZTA ceramics
Toughening effect strengthens, and improves ZTA Mechanical Property of Ceramics.
Specific embodiment described herein is only to spirit explanation for example of the invention.Technology belonging to the present invention is led
The technical staff in domain can be made various modifications or supplement to described specific embodiment or be replaced using similar mode
Generation, but without departing from the spiritual of the present invention or surmount scope defined in appended claims.
Claims (8)
1. a kind of preparation method of ZTA nano composite powders, it is characterised in that comprise the following steps：
(1) by the spherical Al of raw material2O3、ZrO2, MgO, additive powder weighed by proportioning configuration, and premixed；
(2) ball milling ball is agate ball, is 4-5 according to ratio of grinding media to material：1 is put into premix powders and agate ball in nylon ball grinder, adopts
Make ball-milling medium with absolute ethyl alcohol, absolute ethyl alcohol addition is not cross ball milling ball horizontal plane 1-2cm in nylon tank, adition process control
Preparation；
(3) ball milling uses horizontal ball mill, controls ball milling speed and Ball-milling Time to carry out ball milling；
(4) ball material separation is carried out with absolute ethyl alcohol after the completion of ball milling, separation mixed liquor is dried, mistake after the completion of powder is dried
80 mesh sieve, ZTA nano composite powders are made.
2. the preparation method of ZTA nano composite powders according to claim 1, it is characterised in that：It is described in step (1)
Material powder include according to mass percent following component form：
15%≤ZrO2≤ 30%,
MgO 0.25,
0.5%≤Al≤5%,
Surplus is additive powder.
3. the preparation method of ZTA nano composite powders according to claim 1, it is characterised in that：It is described in step (1)
Additive powder be Al powder, its purity >=99.5%, Al powder size≤Al2O3Powder size.
4. the preparation method of ZTA nano composite powders according to claim 1, it is characterised in that：It is described in step (2)
Spherical Al2O3、ZrO2, MgO powder, Al2O3Powder size≤10um, ZrO2 powder size≤100nm, MgO powder grain
Degree≤100nm.
5. the preparation method of ZTA nano composite powders according to claim 1, it is characterised in that：It is described in step (2)
Agate ball be 3mm≤sphere diameter≤5mm.
6. the preparation method of ZTA nano composite powders according to claim 4, it is characterised in that：It is described in step (2)
Process control agent be stearic acid, 1%≤stearic addition≤2% (ω %).
7. the preparation method of ZTA nano composite powders according to claim 1, it is characterised in that：It is described in step (2)
Ball milling speed be 40-50rpm, the Ball-milling Time is 48-60 hours.
8. the preparation method of the ZTA nano composite powders according to any one of claim 1 to 7, it is characterised in that：In step
(4) in, the drying temperature of described separation mixed liquor is≤80 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109675686A (en) * | 2018-11-29 | 2019-04-26 | 刘永 | A kind of material filling method improving ball mill grinding efficiency |
| CN110732794A (en) * | 2018-07-18 | 2020-01-31 | 西南大学 | ultrasonic and electromagnetic pulse composite welding device and composite welding method |
| CN112871002A (en) * | 2021-01-12 | 2021-06-01 | 长飞光纤光缆股份有限公司 | Uniform mixing method of multi-component powder raw materials |
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| CN103922706A (en) * | 2014-02-28 | 2014-07-16 | 江西泛美亚材料有限公司 | Low temperature sintered low-density high-strength zirconia-alumina composite material and preparation method |
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2017
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| CN103922706A (en) * | 2014-02-28 | 2014-07-16 | 江西泛美亚材料有限公司 | Low temperature sintered low-density high-strength zirconia-alumina composite material and preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110732794A (en) * | 2018-07-18 | 2020-01-31 | 西南大学 | ultrasonic and electromagnetic pulse composite welding device and composite welding method |
| CN109675686A (en) * | 2018-11-29 | 2019-04-26 | 刘永 | A kind of material filling method improving ball mill grinding efficiency |
| CN112871002A (en) * | 2021-01-12 | 2021-06-01 | 长飞光纤光缆股份有限公司 | Uniform mixing method of multi-component powder raw materials |
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Application publication date: 20180313 |