CN106478108A - A kind of method preparing large scale AlON crystalline ceramics - Google Patents
A kind of method preparing large scale AlON crystalline ceramics Download PDFInfo
- Publication number
- CN106478108A CN106478108A CN201510549216.8A CN201510549216A CN106478108A CN 106478108 A CN106478108 A CN 106478108A CN 201510549216 A CN201510549216 A CN 201510549216A CN 106478108 A CN106478108 A CN 106478108A
- Authority
- CN
- China
- Prior art keywords
- alon
- purity
- powder
- sintering
- sand milling
- 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
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a kind of method that can be used for preparing large scale AlON crystalline ceramics, levigate process is carried out to AlON powder body using sand mill, has and can disposably process a large amount of AlON powder body, the sand milling time is short, efficiency high, the little feature of gained diameter of particle.And the AlON powder body after sand milling has preferable molding and sintering character, any binding agent need not be added when compressing, add the AlON powder body after the sand milling of sintering aid to can be used for preparing large scale AlON crystalline ceramics with reference to pressureless sintering.The method preparation efficiency is high, simple to operate, low cost, it is easy to accomplish industrialization.
Description
Technical field
The invention belongs to crystalline ceramics preparing technical field, can be used for preparing the preparation method of large scale AlON crystalline ceramics particularly to a kind of.
Background technology
AlON is Al2O3With the solid solution of AlN, be cubic spinel structure, there is preferable mechanical performance, and its hardness and fusing point all very high.Its optically isotropic property is so that it becomes a kind of excellent selection preparing crystalline ceramics.The transparency range of AlON is wider very high transmitance near ultraviolet to mid infrared region, and its transmission region is 0.2～6 μm, the highest transmitance between 0.3～3 μm up to more than 80%.A lot of performances of AlON all can be comparable with monocrystalline sapphire, and the production technology of monocrystalline sapphire is expensive, and difficult preparation large scale or complex-shaped crystal, by comparison, AlON pottery just occupies obvious advantage in this respect, the preparation cost of polymorph A lON crystalline ceramics is cheap, and can use traditional ceramic preparation to achieve that large scale or the preparation of complicated shape pottery.Therefore, AlON crystalline ceramics becomes replacement sapphire and is used as one of transparent armor, strong candidate material of material of infrared window.
The conventional preparation method of AlON crystalline ceramics mainly has two kinds, and one kind is single step reaction method, mainly by Al2O3Uniformly mix by a certain percentage with AlN powder, then pass through sintering and realize Al simultaneously2O3With solid state reaction kinetics AlON and the sintering densification of AlN, thus preparing ALON crystalline ceramics；Another kind is first to prepare high-purity AlON powder body, then is sintered into the AlON crystalline ceramics of high densification.First method needs, using high-purity, ultra-fine AlN powder body, to increased cost, and whole process is difficult to control to, and easily local sintering and leads to grain morphology uneven and hinder densified sintering product phenomenon.The high-purity AlON powder of sintering carbothermic method synthesis is effective, inexpensive, is easy to the typical two-step preparation of industrialized production AlON crystalline ceramics.In the present invention, homemade high-purity AlON powder is prepared with carbothermic method.
Preparing AlON crystalline ceramics needs powder to have very high sintering activity, the sintering kineticss of AlON and 1/r2Proportional, r is powder granule radius, and the sintering of transparent AlON pottery needs the powder body little using particle diameter in other words, and the most of AlON being obtained at present has more or less reunion mostly, needs to open reunion, refinement powder body by grinding.The lapping mode of the AlON powder body commonly used at present is all using planetary type ball-milling.As the Y that patent CN102875152B is raw material and 0.5wt% with AlON powder body2O3Sintering aid again on planetary ball mill with the rotating speed ball milling 24h of 170r/min, it is little to obtain granularity, has bimodal, narrow ditribution grain size characteristic, obtains, by dry-pressing formed and 1860 DEG C of sintering, the AlON ceramics sample that infrared transmittivity is more than 80%.For another example, patent CN104387081A first prepares the precursor of Al/C using chemical coprecipitation method, then through carbon thermal reduction synthesize AlON powder body, then with 0.08wt%Y2O3
、0.02wt%La2O3
, 0.2wt%MgO sintering aid mixing and ball milling 30min, the powder body after ball milling is pressed into the biscuit of Φ 20mm, eventually passes the AlON crystalline ceramics that 1900 DEG C of insulation 12h pressureless sinterings have obtained transmitance 63.3%.And planetary type ball-milling generally disposably to process powder few, or for reach required ultra-fine grain diameter required time very long, it usually needs more than 20h, therefore, the method is not easy to for preparing large scale AlON crystalline ceramics, or preparation efficiency very low it is difficult to meet industrial requirement.
Content of the invention
Present invention mainly solves the problems referred to above, there is provided a kind of can mass rapid refinement powder body method, add suitable sintering aid, can be used to prepare large scale transparent AlON pottery in conjunction with non-pressure sintering technology.
To achieve these goals, the present invention employs the following technical solutions：A kind of method preparing large scale AlON crystalline ceramics, comprises the following steps that：
（1）To make high-purity AlON powder by oneself as raw material, add the Y of mass ratio 0.15%～0.4%2O3Sintering aid adds absolute ethyl alcohol and stirring to be configured to the slurry of solid content 30% ~ 60%, gained slurry is put into and carries out sand milling in sand mill, and the sand milling time is 5～10h, take out the good slurry of sand milling, dry, cross 200 mesh sieves, powder after sieving removes carbon, temperature retention time 4～16h at 600 DEG C；
（2）Gained powder is carried out under 10～60MPa dry-pressing formed, the sample after dry-pressing is placed in further densification molding under 150～300MPa in cold isostatic press, obtain the base substrate of more high density and even density；
（3）The base substrate of gained is put in high purity graphite crucible, is sintered in pyrographite stove, sintering temperature is 1900～1950 DEG C, temperature retention time 4～12h；
（4）The AlON obtaining pottery is carried out double sided optical polishing, obtains transparent AlON pottery；
The purity of described high-purity AlON powder>99.9%, mean diameter is 22 μm, and purity of alcohol is to analyze more than pure；
The diameter of abrading-ball in described sand mill<2mm, purity>99.5%；
Diameter of particle after described sand milling<1μm；
Described base substrate is put in graphite crucible and is filled with AlON powder, and atmosphere during sintering is the high pure nitrogen atmosphere of pressure-fired.
The beneficial effects of the present invention is：The raw material being used is high-purity AlON powder, the micronization processes mode of powder body adopts sand milling, compared to commonly used planetary type ball-milling mode, it has, and the micronization processes time is short, and effect is good, and can disposably process a large amount of powder body, improve powder refining efficiency, solve the Ball-milling Time that planetary type ball-milling brought long, process the shortcomings of powder amount is little, and preparation large scale AlON crystalline ceramics sample cycle is long.In conjunction with suitable sintering aid, it is equipped with corresponding sintering schedule, can efficiently prepare large scale AlON crystalline ceramics.
Brief description
Fig. 1～3 are respectively the SEM shape appearance figure of powder body after sand milling in embodiment 1～3.
Fig. 4～6 are respectively the straight line transmittance of potsherd after sintering polishing in embodiment 1～3.
Specific embodiment
With reference to specific embodiments and the drawings, the present invention is further illustrated.
Embodiment 1
With high-purity self-control AlON powder body as raw material, add the Y of 0.25wt%2O3For sintering aid, two kinds of mixed powders add the slurry agitation that dehydrated alcohol is made into solid content 50% uniform, gained slurry is put into and is carried out sand milling 5h in sand mill, dry, powder body after drying crosses 200 mesh sieves, removes carbon at 600 DEG C, and temperature retention time is 4h, as shown in figure 1, gained powder body mean diameter after sand milling<1μm；
By gained except toner body carries out being pressed into the disk of Φ 5cm*5mm with the pressure of 10MPa on hydraulic press, subsequently gained biscuit is improved blank density further with the pressure of 200MPa on cold isostatic press；
Gained base substrate is placed in high purity graphite crucible, with high-purity AlON powder landfill, under high pure nitrogen atmosphere, 1930 DEG C are sintered 6h in pyrographite stove, obtains high densification AlON ceramic sintered bodies；
The ceramic sintered bodies obtaining are carried out double sided optical polishing, has obtained the AlON crystalline ceramics that transparency is 72%, such as Fig. 4.
Embodiment 2
With high-purity self-control AlON powder body as raw material, add the Y of 0.25wt%2O3For sintering aid, slurry agitation mixed powder being made into solid content 40% with dehydrated alcohol uniformly, put into and carry out sand milling 8h in sand mill by gained slurry, dry, the powder body after drying crosses 200 mesh sieves, remove carbon at 600 DEG C, temperature retention time is 6h, as shown in Fig. 2 gained powder body mean diameter after sand milling<1μm；
Gained is removed the disk that toner body carries out being pressed into Φ 10cm thickness 1cm with the pressure of 10MPa, then isostatic cool pressing is carried out further with the pressure of 200MPa；
Gained base substrate is placed in high purity graphite crucible, buries burning with high-purity AlON powder, sintering temperature is 1930 DEG C, temperature retention time is 8h, obtain high densification AlON ceramic sintered bodies；
The ceramic sintered bodies obtaining are carried out double sided optical polishing, has obtained the AlON crystalline ceramics that transparency is 71%, such as Fig. 5.
Embodiment 3
With high-purity self-control AlON powder body as raw material, add the Y of 0.35wt%2O3For sintering aid, the slurry agitation being made into solid content 45% with dehydrated alcohol uniformly, is then placed in sand milling 10h in sand mill, dry, the powder body after drying crosses 200 mesh sieves, remove carbon at 600 DEG C, temperature retention time is 10h, as shown in figure 3, gained powder body mean diameter is below 1 μm；
Gained is removed toner body carry out being pressed into the disk of Φ 20cm thickness 2cm with the pressure of 30MPa on hydraulic press, subsequently gained biscuit is improved blank density further with the pressure of 250MPa on cold isostatic press；
Gained base substrate is placed in high purity graphite crucible, buries burning with high-purity AlON powder, 1940 DEG C are sintered 10h under high pure nitrogen atmosphere, obtain high densification AlON ceramic sintered bodies；
The ceramic sintered bodies obtaining are carried out double sided optical polishing, has obtained the AlON crystalline ceramics that transparency is 67%, such as Fig. 6.
Although the present invention is open as above with preferred embodiment; but embodiment and accompanying drawing are not for limiting the present invention, any it is familiar with this those skilled in the art, without departing from the spirit and scope of the invention; can make various changes from working as or retouch, but equally within protection scope of the present invention.Therefore protection scope of the present invention should be by being defined that claims hereof protection domain is defined.
Claims (5)
1. a kind of method preparing large scale AlON crystalline ceramics is it is characterised in that comprise the following steps that：
（1）To make high-purity AlON powder by oneself as raw material, add the Y of mass ratio 0.15%～0.4%2O3Sintering aid adds absolute ethyl alcohol and stirring to be configured to slurry, gained slurry is put into and carries out sand milling in sand mill, and the sand milling time is 5～10h, takes out the good slurry of sand milling, dries, crosses 200 mesh sieves, and the powder after sieving removes carbon, temperature retention time 4～16h at 600 DEG C；
（2）Gained powder is carried out under 10～60MPa dry-pressing formed, the sample after dry-pressing is placed in further densification molding under 150～300MPa in cold isostatic press, obtain the base substrate of more high density and even density；
（3）The base substrate of gained is put in high purity graphite crucible, is sintered in pyrographite stove, sintering temperature is 1900～1950 DEG C, temperature retention time 4～12h；
（4）The AlON obtaining pottery is carried out double sided optical polishing, obtains transparent AlON pottery.
2. method according to claim 1 it is characterised in that：The purity of described high-purity AlON powder>99.9%, mean diameter is 22 μm, and purity of alcohol is to analyze more than pure.
3. method according to claim 1 it is characterised in that：The diameter of abrading-ball in described sand mill<2mm, purity>99.5%.
4. method according to claim 3 it is characterised in that：Diameter of particle after described sand milling<1μm.
5. method according to claim 1 it is characterised in that：Described base substrate is put in graphite crucible and is filled with AlON powder, and atmosphere during sintering is the high pure nitrogen atmosphere of pressure-fired.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510549216.8A CN106478108A (en) | 2015-09-01 | 2015-09-01 | A kind of method preparing large scale AlON crystalline ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510549216.8A CN106478108A (en) | 2015-09-01 | 2015-09-01 | A kind of method preparing large scale AlON crystalline ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106478108A true CN106478108A (en) | 2017-03-08 |
Family
ID=58236439
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510549216.8A Pending CN106478108A (en) | 2015-09-01 | 2015-09-01 | A kind of method preparing large scale AlON crystalline ceramics |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106478108A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721379A (en) * | 2019-03-14 | 2019-05-07 | 大连海事大学 | A method of use AlON powder as raw material connection AlON ceramics |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093057A (en) * | 2010-12-01 | 2011-06-15 | 山东理工大学 | Preparation technology of gamma-ALON transparent ceramic with high light transmittance |
| 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 |
| CN103664189A (en) * | 2013-11-28 | 2014-03-26 | 山东理工大学 | Method for preparing Y-AlON ceramic oven bricks |
| CN104387081A (en) * | 2014-11-18 | 2015-03-04 | 上海大学 | Low-temperature preparation method of transparent aluminum oxynitride (AlON) ceramic |
| CN104844217A (en) * | 2015-04-01 | 2015-08-19 | 苏州工业园区晶冠瓷材料科技有限公司 | Preparation method of AlON transparent ceramic phosphor for warm-color warm-white LED packaging light source |
-
2015
- 2015-09-01 CN CN201510549216.8A patent/CN106478108A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102093057A (en) * | 2010-12-01 | 2011-06-15 | 山东理工大学 | Preparation technology of gamma-ALON transparent ceramic with high light transmittance |
| CN103664189A (en) * | 2013-11-28 | 2014-03-26 | 山东理工大学 | Method for preparing Y-AlON ceramic oven bricks |
| CN104387081A (en) * | 2014-11-18 | 2015-03-04 | 上海大学 | Low-temperature preparation method of transparent aluminum oxynitride (AlON) ceramic |
| CN104844217A (en) * | 2015-04-01 | 2015-08-19 | 苏州工业园区晶冠瓷材料科技有限公司 | Preparation method of AlON transparent ceramic phosphor for warm-color warm-white LED packaging light source |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721379A (en) * | 2019-03-14 | 2019-05-07 | 大连海事大学 | A method of use AlON powder as raw material connection AlON ceramics |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102311266B (en) | Preparation method of (K05Na05) NbO3 (KNN) lead-free piezoelectric ceramic material | |
| CN102145993B (en) | Low-temperature quick sintered high-strength aluminum oxide ceramic and preparation method thereof | |
| CN101817683B (en) | Method for preparing MgAlON transparent ceramic in pressureless sintering way | |
| CN107399989A (en) | A kind of preparation method for strengthening Oxidation of SiC aluminium composite foamed ceramic | |
| CN103011827A (en) | Preparation method of zirconium diboride ceramic with in-situ-introduced boron as additive | |
| CN109941981B (en) | Method for preparing high-purity lithium metaphosphate | |
| CN114455952B (en) | AlON powder, direct nitridation method high-pressure synthesis method and application thereof | |
| CN111004030B (en) | MgTiO (magnesium-titanium-oxide) powder3Microwave-based dielectric ceramic and preparation method thereof | |
| CN101648814A (en) | Method for preparing high-performance ceramics by single-step solid phase reaction method | |
| CN101172845A (en) | Method for producing aluminum oxide titanium white series multiple phase fine ceramics material | |
| CN112299861A (en) | AlON transparent ceramic pseudo-sintering agent and application thereof, and preparation method of transparent ceramic | |
| CN105924175B (en) | A kind of fine grain boron carbide ceramics and preparation method thereof | |
| CN104387081A (en) | Low-temperature preparation method of transparent aluminum oxynitride (AlON) ceramic | |
| CN103086704A (en) | Preparation method of high-porosity mineral-based ceramic membrane support | |
| CN102126858B (en) | Preparation method of erbium ion-doped calcium fluoride laser transparent ceramic material | |
| CN105060878A (en) | Microwave dielectric ceramic with low dielectric constant and high quality factor and preparation method thereof | |
| CN106478108A (en) | A kind of method preparing large scale AlON crystalline ceramics | |
| CN105218100B (en) | A kind of low temperature preparation Ti2The method of AlC ceramic materials | |
| CN101774810B (en) | Industrial production method for surface modification of alpha-SiC micropowder particles | |
| CN103864420A (en) | Preparation method of microwave dielectric ceramic material | |
| CN114685170B (en) | Method for synthesizing silicon carbide by microwave flash firing | |
| CN102910908B (en) | Preparing process of double-perovskite Y2MNCoO6 dielectric ceramic | |
| CN107324388A (en) | With ABO3The high pressure synthesis method of sodium molybdenum/tungsten bronze of structure | |
| CN101643357B (en) | Tetragonal phase converting process for superfine cubic phase barium titanate powder | |
| CN100422111C (en) | Gd2O2Preparation method of S: Pr, Ce, F ceramic scintillator |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170308 |