CN109354501B - A kind of preparation method of MgAlON crystalline ceramics - Google Patents
A kind of preparation method of MgAlON crystalline ceramics Download PDFInfo
- Publication number
- CN109354501B CN109354501B CN201811439795.0A CN201811439795A CN109354501B CN 109354501 B CN109354501 B CN 109354501B CN 201811439795 A CN201811439795 A CN 201811439795A CN 109354501 B CN109354501 B CN 109354501B
- Authority
- CN
- China
- Prior art keywords
- mgalon
- purity
- powder
- crystalline ceramics
- slurry
- 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.)
- Active
Links
- 239000011222 crystalline ceramic Substances 0.000 title claims abstract description 43
- 229910002106 crystalline ceramic Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000000498 ball milling Methods 0.000 claims abstract description 35
- 239000002002 slurry Substances 0.000 claims abstract description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 235000015895 biscuits Nutrition 0.000 claims abstract description 23
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 17
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 17
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 8
- 238000005498 polishing Methods 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000003825 pressing Methods 0.000 claims description 13
- 230000003068 static effect Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 9
- 238000002156 mixing Methods 0.000 abstract description 7
- 238000001272 pressureless sintering Methods 0.000 abstract description 7
- 230000001681 protective effect Effects 0.000 abstract description 7
- 239000012071 phase Substances 0.000 description 17
- 239000000919 ceramic Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 5
- 238000001513 hot isostatic pressing Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052596 spinel Inorganic materials 0.000 description 3
- 229910017109 AlON Inorganic materials 0.000 description 2
- 229910026161 MgAl2O4 Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- 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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
-
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- 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
- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
-
- 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
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
-
- 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
- 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
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
-
- 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
- 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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
- C04B2235/445—Fluoride containing anions, e.g. fluosilicate
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Ceramic Products (AREA)
Abstract
The present invention relates to a kind of preparation methods of MgAlON crystalline ceramics, particularly relate to: one kind is by complex phase sintering aid, the method for preparing MgAlON crystalline ceramics by pressureless sintering.It is characterized in that, it is the following steps are included: (1) weighs MgAlON powder；(2) according to certain formula, LiF, Y are weighed2O3、SiO2Mixing, as complex phase sintering aid；(3) powder obtained by step (1) and (2) is taken, mixing is scattered in dehydrated alcohol, ball milling obtains slurry；(4) gained slurry is taken, is pressed into biscuit after dry；(5) biscuit obtained by step (4) is taken, is fitted into BN crucible, is placed in high temperature sintering furnace; using high pure nitrogen as protective gas, it is warming up to 1750 DEG C~1850 DEG C heat preservation 10h~30h, natural cooling; through sanding and polishing after taking-up, MgAlON crystalline ceramics is obtained.The process employs complex phase sintering aids, can suitably reduce sintering temperature, and MgAlON crystalline ceramics obtained has compared with high transmittance, and operating process is simple, and require appointed condition low, suitable popularization and application.
Description
Technical field
The present invention relates to a kind of preparation method of MgAlON crystalline ceramics, one kind is particularly related to by complex phase sintering aid simultaneously
The method for preparing MgAlON crystalline ceramics by pressureless sintering, belongs to field of inorganic nonmetallic material.
Background technique
MgAlON crystalline ceramics and AlON, MgAl2O4Equally, it is a kind of cubic spinel structure material, there is isotropism
Optical property, thus powder granule can be carried out by densification arrangement accumulation by the method for ceramic post sintering, prepared transparent
Polycrystalline structure.Transparent MgAlON ceramics, have excellent optical property, such as: its transparency range is very wide, spans nearly purple
The middle infrared band of outside-visible light-(0.2 μm~6.5 μm) can be used to make the detectable optical response window of a variety of wave bands；It
Excellent in mechanical performance, there are the performances such as high intensity, high rigidity, thus may be used as high temperature and pressure observation window, antenna house, transparent
The fields such as plate armour.
The preparation method of MgAlON crystalline ceramics mainly has: reaction sintering, reaction-sintered/hot isostatic pressing method, without pressure
Sintering process, etc..Mathers et al. (US Patent No.5231062 (1993)) uses AlN, Al2O3, MgO be raw material, mix
It by reaction-sintered after conjunction, settles at one go and obtains MgAlON crystalline ceramics, thus may also be referred to as one-step method.This method advantage is
Operating procedure is simply controllable, the disadvantage is that sintering progress usually synchronous with reaction, process is complex, is easy to produce the second phase；And
And there are also volume expansions to lead to the problem of secondary blowhole for the reaction process of this kind of material, these can all make optical property
At seriously affecting.The MgAlON crystalline ceramics sample transmitance of this method report is not often high.For this purpose, Zhang et al.
(Ceram.Inter., 44 (2018) 17383-17390) by reaction-sintered/hot isostatic pressing method, i.e., by hot isostatic pressing after
Processing, effectively increases transmitance, has benefited from the abundant exclusion of Residual Pores.But hot isostatic apparatus is expensive, reaction is burnt
Knot/hot isostatic pressing method is difficult to large-scale promotion application.Wang et al. (J.Am.Ceram.Soc, 97 (2014), 63-66) report
Pressureless sintering method prepares the MgAlON crystalline ceramics haveing excellent performance, and transmitance reaches 80% or more.This method advantage is behaviour
It is simple to make process, it is harsher to the requirement of MgAlON powder characteristic due to there is no sintering aid, for example granularity will carefully, to protect
Demonstrate,prove sufficiently high sintering activity.Ma et al. uses LiF for sintering aid, and optimizes to non-pressure sintering technology, also obtains
The MgAlON crystalline ceramics of high transmittance.This shows to pass through addition sintering aid and is precisely controlled sintering process, and realizes
The effective way and method of MgAlON crystalline ceramics pressureless sintering preparation.
Sintering aid play the role of in crystalline ceramics sintering process it is very important, such as: AlON crystalline ceramics be sintered
In, Y is added2O3The optimization of ceramic transmitance may be implemented；In MgAl2O4Middle addition LiF can purify crystal boundary, and then improve it
Optical transmittance；SiO is added in YAG preparation process2Liquid phase can be formed, reduce sintering temperature, etc..These previous works are given
Our very big inspirations.MgAlON crystalline ceramics is a kind of very promising new material, but the report about its preparation at present
Road is simultaneously few, and in order to optimize preparation process, the optimum choice of sintering aid is an effectively approach, but at present about this
The research report of material sintering aid is seldom.
Based on above-mentioned consideration, the present invention proposes to prepare using complex sintering aids scheme for MgAlON crystalline ceramics, this
Before have not been reported, new approaches and new breakthrough mouth can be provided for the preparation of MgAlON crystalline ceramics.
Summary of the invention
To solve the above problems, the invention discloses a kind of preparation methods of MgAlON crystalline ceramics.Present invention employs
Complex phase sintering aid can suitably reduce sintering temperature, and MgAlON crystalline ceramics obtained has compared with high transmittance, operation stream
Journey is simple, and requires appointed condition low, suitable popularization and application, has been obtained by pressureless sintering a kind of with high transmittance feature
MgAlON crystalline ceramics.
For this purpose, the technical solution that the present invention takes:
A kind of preparation method of MgAlON crystalline ceramics, it the following steps are included:
Step 1: taking MgAlON powder, spare；
Step 2: Y is weighed2O3Powder, LiF powder, SiO2Powder, and be 15%~40%, Y according to LiF content2O3Content is 20%
~55%, SiO2The mass ratio that content is 25%~60% is mixed, and complex phase sintering aid is obtained, spare；
Step 3: taking MgAlON powder and complex phase sintering aid, and the mass percent of complex phase sintering aid is 0.2%~
1.0%, the mass percent of MgAlON powder is 99%~99.8%, is scattered in dehydrated alcohol, dehydrated alcohol purity is not less than
In 99.5%, slurry is obtained after ball milling；
Step 4: after slurry drying, it is pressed into biscuit；
Step 5: biscuit being fitted into high-purity BN crucible, then is placed in high temperature sintering furnace together, using high pure nitrogen as
Protective gas is warming up to 1750 DEG C~1850 DEG C heat preservation 10h~30h, takes out after natural cooling, sanding and polishing is saturating up to MgAlON
Bright ceramics.
Further to improve, MgAlON powder described in step 1, average particle size particle size is not more than 1.5 μm, and purity is not
Lower than 98%.
It is further to improve, Y described in step 22O3、LiF、SiO2Powder, average particle size particle size no more than 1 μm, it is pure
Degree is not less than 98%.
Further to improve, mechanical milling process described in step 3 is the high pure zirconia for being not less than 99.5% using purity
Aluminium ball is that 10:1~5:1 carries out ball milling, ball milling as ball-milling medium, and according to high purity aluminium oxide ball and mixture gross mass ratio
Time be 10h~30h, rotational speed of ball-mill be 100r/m~250r/m.
Further to improve, slurry drying means described in step 4 is as follows: slurry being poured into receiving flask, by true
Empty heating evaporation, so that the dehydrated alcohol in slurry is sufficiently volatilized.Wherein, vacuum degree is not higher than 1000Pa, heating temperature
It is 50 DEG C~90 DEG C, the time is not less than 5h.
Further to improve, biscuit drawing method described in step 4 is as follows: first using axial dry-pressing formed machine, pressurization is dry
Slurry after dry, pressure 10MPa~30MPa；150MPa~250MPa is forced by isostatic cool pressing again.
Further to improve, in step 5: the BN crucible purity is not less than 97%；Nitrogen gas purity is not less than
99.99%；In temperature-rise period, rate is 5 DEG C/min~15 DEG C/min.
Beneficial effects of the present invention:
(1) with the help of complex sintering aids, the MgAlON crystalline ceramics of pressureless sintering preparation has excellent optics
Through performance, and without carrying out stage control to sintered heat insulating temperature, so that the dependence to sintering process system is reduced,
Strong operability.
(2) using the MgAlON crystalline ceramics of complex sintering aids preparation, with no sintering aid or single adjuvant system phase
Than the present invention can reduce the temperature or soaking time of non-pressure sintering technology to a certain extent；It is quiet with pressureless sintering/heat etc.
Pressure, reaction-sintered/hot isostatic pressing method are compared, it does not need expensive hot isostatic apparatus, be also beneficial to reduce energy consumption and at
This, has good promotion and application value.
(3) the complex sintering aids system that this method proposes, does not have been reported that in MgAlON crystalline ceramics direction before this, and makes
Standby MgAlON crystalline ceramics has excellent optical transmittance.This provides new method and technique for the preparation of such material, tool
There is preferable academic reference significance.
Attached drawing table explanation
Fig. 1 is the transmittance curve of MgAlON crystalline ceramics prepared by case study on implementation 1 of the present invention；
Fig. 2 is the transmittance curve of MgAlON crystalline ceramics prepared by case study on implementation 3 of the present invention；
Fig. 3 is the transmittance curve of MgAlON crystalline ceramics prepared by case study on implementation 5 of the present invention.
Specific embodiment
For a better understanding of the present invention, with reference to the accompanying drawing, the case study on implementation content that the present invention is further explained, but this
The content of invention is not limited solely to following case study on implementation.
Embodiment 1:
A kind of preparation method of MgAlON transparent ceramic powder, it the following steps are included:
(1) MgAlON powder is weighed, it is spare.MgAlON powder average particle size (D50) is 0.5 μm, purity 98.5%；
(2) by certain formula, LiF, Y are weighed2O3、SiO2Mixing, it is spare as complex phase sintering aid.Wherein:
The mass ratio of LiF is 15%, purity 98.5%, average particle size (D50) are 0.97 μm；
Y2O3Mass ratio be 55%, purity 98%, average particle size (D50) be 0.85 μm；
SiO2Mass ratio be 30%, purity 98.5%, average particle size (D50) be 0.70 μm.
(3) powder obtained by step (1) and (2) is taken, mixes, is scattered in dehydrated alcohol, ball milling according to certain mass ratio
16h obtains slurry.Wherein:
Dehydrated alcohol purity is 99.5%；
The ratio of complex phase sintering aid is that the ratio of 0.7%%, MgAlON powder is 99.3%；
Ball-milling technology is such that using high purity aluminium oxide ball (purity 99.5%) as ball-milling medium, according to ball and powder
Body gross mass ratio is that 5:1 carries out ball milling, and the time of ball milling is 10h, rotational speed of ball-mill 250r/m.
(4) slurry obtained by step (3) is taken, is pressed into biscuit after dry, it is spare.Wherein:
Dry method is such that pour into slurry in receiving flask, is evaporated by heating in vacuum, so that the nothing in slurry
Water-ethanol is sufficiently volatilized.Vacuum degree is lower than 1000Pa, and heating temperature is 90 DEG C, time 5h；
Biscuit pressing process is such that be forced into 10MPa using traditional dry-pressing formed machine of axial direction；Again by cold etc.
Static pressure is forced into 250MPa.
(5) biscuit obtained by step (4) is taken, is fitted into high-purity BN crucible, then be placed in high temperature sintering furnace together, with high-purity
Nitrogen is warming up to 1750 DEG C of heat preservation 30h as protective gas, and natural cooling is obtained through sanding and polishing to 2mm thickness after taking-up
MgAlON crystalline ceramics.Wherein:
BN crucible purity 97%；
High pure nitrogen purity 99.99%；
Heating rate is 5 DEG C/min.
Embodiment 2:
A kind of preparation method of MgAlON transparent ceramic powder, it the following steps are included:
(1) MgAlON powder is weighed, it is spare.MgAlON powder average particle size (D50) is 0.5 μm, purity 99.5%；
(2) by certain formula, LiF, Y are weighed2O3、SiO2Mixing, it is spare as complex phase sintering aid.Wherein:
The mass ratio of LiF is 40%, purity 98.5%, average particle size (D50) are 0.97 μm；
Y2O3Mass ratio be 20%, purity 98%, average particle size (D50) be 0.85 μm；
SiO2Mass ratio be 40%, purity 98.5%, average particle size (D50) be 0.70 μm.
(3) powder obtained by step (1) and (2) is taken, mixes, is scattered in dehydrated alcohol, ball milling according to certain mass ratio
16h obtains slurry.Wherein:
Dehydrated alcohol purity is 99.5%；
The ratio of complex phase sintering aid is that the ratio of 0.2%%, MgAlON powder is 99.8%；
Ball-milling technology is such that using high purity aluminium oxide ball (purity 99.9%) as ball-milling medium, according to ball and powder
Body gross mass ratio is that 10:1 carries out ball milling, and the time of ball milling is 15h, rotational speed of ball-mill 200r/m.
(4) slurry obtained by step (3) is taken, is pressed into biscuit after dry, it is spare.Wherein:
Dry method is such that pour into slurry in receiving flask, is evaporated by heating in vacuum, so that the nothing in slurry
Water-ethanol is sufficiently volatilized.Vacuum degree is lower than 1000Pa, and heating temperature is 70 DEG C, time 6h；
Biscuit pressing process is such that be forced into 10MPa using traditional dry-pressing formed machine of axial direction；Again by cold etc.
Static pressure is forced into 150MPa.
(5) biscuit obtained by step (4) is taken, is fitted into high-purity BN crucible, then be placed in high temperature sintering furnace together, with high-purity
Nitrogen is warming up to 1750 DEG C of heat preservation 25h as protective gas, and natural cooling is obtained through sanding and polishing to 2mm thickness after taking-up
MgAlON crystalline ceramics.Wherein:
BN crucible purity 97%；
High pure nitrogen purity 99.99%；
Heating rate is 10 DEG C/min.
Embodiment 3:
A kind of preparation method of MgAlON transparent ceramic powder, it the following steps are included:
(1) MgAlON powder is weighed, it is spare.MgAlON powder average particle size (D50) is 1.0 μm, purity 98%；
(2) by certain formula, LiF, Y are weighed2O3、SiO2Mixing, it is spare as complex phase sintering aid.Wherein:
The mass ratio of LiF is 25%, purity 99%, average particle size (D50) are 0.57 μm；
Y2O3Mass ratio be 35%, purity 99%, average particle size (D50) be 0.65 μm；
SiO2Mass ratio be 40%, purity 99.5%, average particle size (D50) be 0.35 μm.
(3) powder obtained by step (1) and (2) is taken, mixes, is scattered in dehydrated alcohol, ball milling according to certain mass ratio
18h obtains slurry, in which:
Dehydrated alcohol purity is 99.7%；
The ratio of complex phase sintering aid is that the ratio of 1.0%, MgAlON powder is 99%%；
Ball-milling technology is such that using high purity aluminium oxide ball (purity 99.5%) as ball-milling medium, according to ball and powder
Body gross mass ratio is that 8:1 carries out ball milling, and the time of ball milling is 20h, rotational speed of ball-mill 150r/m.
(4) slurry obtained by step (3) is taken, is pressed into biscuit after dry, it is spare.Wherein:
Dry method is such that pour into slurry in receiving flask, is evaporated by heating in vacuum, so that the nothing in slurry
Water-ethanol is sufficiently volatilized.Vacuum degree is lower than 700Pa, and heating temperature is 70 DEG C, time 7h；
Biscuit pressing process is such that be forced into 30MPa using traditional dry-pressing formed machine of axial direction；Again by cold etc.
Static pressure is forced into 250MPa.
(5) biscuit obtained by step (4) is taken, is fitted into high-purity BN crucible, then be placed in high temperature sintering furnace together, with high-purity
Nitrogen is warming up to 1800 DEG C of heat preservation 20h as protective gas, and natural cooling is obtained through sanding and polishing to 2mm thickness after taking-up
MgAlON crystalline ceramics.Wherein:
BN crucible purity 99%；
High pure nitrogen purity 99.995%；
Heating rate is 5 DEG C/min.
Embodiment 4:
A kind of preparation method of MgAlON transparent ceramic powder, it the following steps are included:
(1) MgAlON powder is weighed, it is spare.MgAlON powder average particle size (D50) is 1.0 μm, purity 99%；
(2) by certain formula, LiF, Y are weighed2O3、SiO2Mixing, it is spare as complex phase sintering aid.Wherein:
The mass ratio of LiF is 25%, purity 99%, average particle size (D50) are 0.57 μm；
Y2O3Mass ratio be 20%, purity 99%, average particle size (D50) be 0.65 μm；
SiO2Mass ratio be 55%, purity 99.5%, average particle size (D50) be 0.35 μm.
(3) powder obtained by step (1) and (2) is taken, mixes, is scattered in dehydrated alcohol, ball milling according to certain mass ratio
20h obtains slurry, in which:
Dehydrated alcohol purity is 99.7%；
The ratio of complex phase sintering aid is that the ratio of 0.5%, MgAlON powder is 99.5%；
Ball-milling technology is such that using high purity aluminium oxide ball (purity 99.9%) as ball-milling medium, according to ball and powder
Body gross mass ratio is that 8:1 carries out ball milling, and the time of ball milling is 25h, rotational speed of ball-mill 250r/m.
(4) slurry obtained by step (3) is taken, is pressed into biscuit after dry, it is spare.Wherein:
Dry method is such that pour into slurry in receiving flask, is evaporated by heating in vacuum, so that the nothing in slurry
Water-ethanol is sufficiently volatilized.Vacuum degree is lower than 700Pa, and heating temperature is 60 DEG C, time 8h；
Biscuit pressing process is such that be forced into 30MPa using traditional dry-pressing formed machine of axial direction；Again by cold etc.
Static pressure is forced into 150MPa.
(5) biscuit obtained by step (4) is taken, is fitted into high-purity BN crucible, then be placed in high temperature sintering furnace together, with high-purity
Nitrogen is warming up to 1800 DEG C of heat preservation 10h as protective gas, and natural cooling is obtained through sanding and polishing to 2mm thickness after taking-up
MgAlON crystalline ceramics.Wherein:
BN crucible purity 99%；
High pure nitrogen purity 99.995%；
Heating rate is 10 DEG C/min.
Embodiment 5:
A kind of preparation method of MgAlON transparent ceramic powder, it the following steps are included:
(1) MgAlON powder is weighed, it is spare.MgAlON powder average particle size (D50) is 1.5 μm, purity 99.5%；
(2) by certain formula, LiF, Y are weighed2O3、SiO2Mixing, it is spare as complex phase sintering aid.Wherein:
The mass ratio of LiF is 20%, purity 99.5%, average particle size (D50) are 0.2 μm；
Y2O3Mass ratio be 55%, purity 99.9%, average particle size (D50) be 0.2 μm；
SiO2Mass ratio be 25%, purity 99.9%, average particle size (D50) be 0.10 μm.
(3) powder obtained by step (1) and (2) is taken, mixes, is scattered in dehydrated alcohol, ball milling according to certain mass ratio
For 24 hours, slurry is obtained, in which:
Dehydrated alcohol purity is 99.7%；
The ratio of complex phase sintering aid is that the ratio of 0.5%, MgAlON powder is 99.5%；
Ball-milling technology is such that using high purity aluminium oxide ball (purity be not less than 99.5%) as ball-milling medium, according to
Ball and powder gross mass ratio are that 7:1 carries out ball milling, and the time of ball milling is 30h, rotational speed of ball-mill 100r/m.
(4) slurry obtained by step (3) is taken, is pressed into biscuit after dry, it is spare.Wherein:
Dry method is such that pour into slurry in receiving flask, is evaporated by heating in vacuum, so that the nothing in slurry
Water-ethanol is sufficiently volatilized.Vacuum degree is lower than 500Pa, and heating temperature is 50 DEG C, time 10h；
Biscuit pressing process is such that be forced into 20MPa using traditional dry-pressing formed machine of axial direction；Again by cold etc.
Static pressure is forced into 200MPa.
(5) biscuit obtained by step (4) is taken, is fitted into high-purity BN crucible, then be placed in high temperature sintering furnace together, with high-purity
Nitrogen is warming up to 1850 DEG C of heat preservation 10h as protective gas, and natural cooling is obtained through sanding and polishing to 2mm thickness after taking-up
MgAlON crystalline ceramics, in which:
BN crucible purity 99.5%；
High pure nitrogen purity 99.995%；
Heating rate is 8 DEG C/min.
Claims (7)
1. a kind of preparation method of MgAlON crystalline ceramics, which is characterized in that it the following steps are included:
Step 1: taking MgAlON powder, spare；
Step 2: Y is weighed2O3Powder, LiF powder, SiO2Powder, and be 15%~40%, Y according to LiF content2O3Content be 20%~
55%, SiO2The mass ratio that content is 25%~60% is mixed, and complex phase sintering aid is obtained, spare；
Step 3: taking MgAlON powder and complex phase sintering aid, the mass percent of complex phase sintering aid is 0.2%~1.0%,
The mass percent of MgAlON powder is 99%~99.8%, is scattered in dehydrated alcohol, and dehydrated alcohol purity is not less than in 99.5%,
Slurry is obtained after ball milling；
Step 4: after slurry drying, it is pressed into biscuit；
Step 5: biscuit being fitted into high-purity BN crucible, then is placed in high temperature sintering furnace together, using high pure nitrogen as protection
Gas is warming up to 1750 DEG C~1850 DEG C heat preservation 10h~30h, takes out after natural cooling, sanding and polishing is up to the transparent pottery of MgAlON
Porcelain.
2. the preparation method of MgAlON crystalline ceramics as described in claim 1, which is characterized in that MgAlON described in step 1
Powder, average particle size particle size are not more than 1.5 μm, and purity is not less than 98%.
3. the preparation method of MgAlON crystalline ceramics as described in claim 1, which is characterized in that Y described in step 22O3、
LiF、SiO2Powder, average particle size particle size are not less than 98% no more than 1 μm, purity.
4. the preparation method of MgAlON crystalline ceramics as described in claim 1, which is characterized in that ball milling described in step 3
Process is the high purity aluminium oxide ball using purity not less than 99.5% as ball-milling medium, and according to high purity aluminium oxide ball and is mixed
Closing object gross mass ratio is that 10:1~5:1 carries out ball milling, and time of ball milling is 10h~30h, rotational speed of ball-mill be 100r/min~
250r/min。
5. the preparation method of MgAlON crystalline ceramics as described in claim 1, which is characterized in that slurry described in step 4
Drying means is as follows: slurry being poured into receiving flask, is evaporated by heating in vacuum, so that the dehydrated alcohol in slurry is able to sufficiently
Volatilization；Wherein, vacuum degree is not higher than 1000Pa, and heating temperature is 50 DEG C~90 DEG C, and the time is not less than 5h.
6. the preparation method of MgAlON crystalline ceramics as described in claim 1, which is characterized in that biscuit pressure described in step 4
Method processed is as follows: first using axial dry-pressing formed machine, the slurry after high-pressure drying, pressure 10MPa~30MPa；Again by cold etc.
Static pressure is forced into 150MPa~250MPa.
7. the preparation method of MgAlON crystalline ceramics as described in claim 1, which is characterized in that in step 5: the BN
Crucible purity is not less than 97%；Nitrogen gas purity is not less than 99.99%；In temperature-rise period, rate is 5 DEG C/min~15 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811439795.0A CN109354501B (en) | 2018-11-29 | 2018-11-29 | A kind of preparation method of MgAlON crystalline ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811439795.0A CN109354501B (en) | 2018-11-29 | 2018-11-29 | A kind of preparation method of MgAlON crystalline ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109354501A CN109354501A (en) | 2019-02-19 |
| CN109354501B true CN109354501B (en) | 2019-08-23 |
Family
ID=65343515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811439795.0A Active CN109354501B (en) | 2018-11-29 | 2018-11-29 | A kind of preparation method of MgAlON crystalline ceramics |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109354501B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113416409A (en) * | 2021-06-07 | 2021-09-21 | 苏州海晨塑胶有限公司 | Preparation method of elastic and plastic polyester material |
| CN115196969B (en) * | 2022-07-13 | 2023-01-17 | 大连海事大学 | Solid-phase reaction rapid pressureless sintering method of MgAlON transparent ceramic with high infrared transmittance |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817683A (en) * | 2010-03-30 | 2010-09-01 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic in pressureless sintering way |
| CN106342083B (en) * | 2010-06-28 | 2013-04-17 | 中国科学院上海硅酸盐研究所 | A kind of low temperature is prepared the method for aluminum nitride oxygen transparent ceramic |
| CN104446497A (en) * | 2014-12-01 | 2015-03-25 | 中国航天科工集团第三研究院第八三五八研究所 | Preparation method of nitric oxide transparent ceramic with wide frequency and light transmission performance |
-
2018
- 2018-11-29 CN CN201811439795.0A patent/CN109354501B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817683A (en) * | 2010-03-30 | 2010-09-01 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic in pressureless sintering way |
| CN106342083B (en) * | 2010-06-28 | 2013-04-17 | 中国科学院上海硅酸盐研究所 | A kind of low temperature is prepared the method for aluminum nitride oxygen transparent ceramic |
| CN104446497A (en) * | 2014-12-01 | 2015-03-25 | 中国航天科工集团第三研究院第八三五八研究所 | Preparation method of nitric oxide transparent ceramic with wide frequency and light transmission performance |
Non-Patent Citations (1)
| Title |
|---|
| Pressureless sintering and fabrication of highly transparent MgAlON ceramic from the carbothermal powder;Benyuan Ma 等;《Journal of Alloys and Compounds》;20180221;第745卷;第2.2节，第3.1节 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109354501A (en) | 2019-02-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104557013B (en) | Preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics | |
| Jin et al. | ZrO2-doped Y2O3 transparent ceramics via slip casting and vacuum sintering | |
| CN101935208B (en) | Rare earth aluminate single-phase or complex-phase nanocrystalline transparent ceramic material and preparation method thereof | |
| CN110550946B (en) | Method for producing transparent ceramic material for Faraday rotator | |
| CN109354501B (en) | A kind of preparation method of MgAlON crystalline ceramics | |
| CN100387548C (en) | Prepn process of transparent toughened magnesia alumina spinel ceramic | |
| CN101985398A (en) | Method for preparing transparent polycrystalline Re:YAG ceramic | |
| CN102020470A (en) | Preparation method of transparent yttria ceramics with high optical quality | |
| Huang et al. | Sintering of transparent Nd: YAG ceramics in oxygen atmosphere | |
| CN103011827A (en) | Preparation method of zirconium diboride ceramic with in-situ-introduced boron as additive | |
| CN106673625B (en) | The preparation method of grain orientation transparent polycrystalline alumina ceramics | |
| CN102815941B (en) | Rare-earth-ion-doped lanthanum gadolinium zirconate transparent ceramic material and preparation method thereof | |
| Duan et al. | Fabrication of transparent Tb3Al5O12 ceramics by hot isostatic pressing sintering | |
| Huang et al. | Fabrication and characterization of Tb3Al5O12 magneto-optical ceramics by solid-state reactive sintering | |
| Fang et al. | Effect of heat treatment of green bodies on the sintering and optical properties of large-size and thick transparent YAG ceramics | |
| WO2020155243A1 (en) | Method for preparing high-density magnesia from magnesite by means of spark plasma sintering | |
| CN103232237A (en) | Preparation method of normal-pressure-sintered transparent zirconium oxide ceramic material | |
| CN101486574A (en) | Method for preparing YAG transparent ceramic powder by solid-phase reaction | |
| An et al. | Fabrication of transparent La2Zr2O7 by reactive spark plasma sintering | |
| CN102815945B (en) | Lanthanum gadolinium zirconate transparent ceramic material and preparation method thereof | |
| CN107324805A (en) | A kind of multicomponent garnet-base laser transparent ceramic material and preparation method thereof | |
| CN103482970A (en) | Laser transparent ceramics and preparation method thereof | |
| CN110590353B (en) | Method for improving solid solubility of doped ions of YAG-based transparent ceramic | |
| CN101851098B (en) | Method for fast preparing translucent Li-alpha-SiAlON ceramic material | |
| Li et al. | Densification and microstructure evolution of Cr4+, Nd3+: YAG transparent ceramics for self-Q-switched laser |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |